Deprecated: The each() function is deprecated. This message will be suppressed on further calls in /home/zhenxiangba/zhenxiangba.com/public_html/phproxy-improved-master/index.php on line 456
WO2013084948A1 - Container, vapor phase cracking method, vapor phase cracking device, analysis method, and analysis device - Google Patents
[go: Go Back, main page]

WO2013084948A1 - Container, vapor phase cracking method, vapor phase cracking device, analysis method, and analysis device - Google Patents

Container, vapor phase cracking method, vapor phase cracking device, analysis method, and analysis device Download PDF

Info

Publication number
WO2013084948A1
WO2013084948A1 PCT/JP2012/081533 JP2012081533W WO2013084948A1 WO 2013084948 A1 WO2013084948 A1 WO 2013084948A1 JP 2012081533 W JP2012081533 W JP 2012081533W WO 2013084948 A1 WO2013084948 A1 WO 2013084948A1
Authority
WO
WIPO (PCT)
Prior art keywords
compound sample
silicon carbide
decomposition
container
sample
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2012/081533
Other languages
French (fr)
Japanese (ja)
Inventor
亮 町田
星野　英樹
高史 末包
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sumika Chemical Analysis Service Ltd
Original Assignee
Sumika Chemical Analysis Service Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sumika Chemical Analysis Service Ltd filed Critical Sumika Chemical Analysis Service Ltd
Priority to KR1020147018491A priority Critical patent/KR20140105810A/en
Publication of WO2013084948A1 publication Critical patent/WO2013084948A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Images

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition

Definitions

  • the present invention relates to a container for decomposing a compound sample or silicon carbide compound sample comprising carbon atoms, a gas phase decomposition method and a gas phase decomposition apparatus using the vessel, and a compound sample or silicon carbide comprising decomposed carbon atoms.
  • the present invention relates to an analysis method and an analysis apparatus for compound samples.
  • Non-Patent Document 1 As a method for analyzing impurities contained in a silicon carbide compound, a chemical analysis method for silicon carbide fine powder described in Non-Patent Document 1 is known. According to the method described in Non-Patent Document 1, silicon carbide is immersed in a mixed acid solution in which a plurality of acids are mixed, heated and pressurized, and silicon carbide is dissolved in the mixed acid solution to obtain a measurement sample solution. And the metal impurity contained in this measurement sample is detected.
  • Non-Patent Document 1 since the silicon carbide compound sample and the mixed acid solution are in direct contact, the metal contained in the mixed acid solution is contained in the measurement sample solution, and contamination to the measurement sample solution is not caused. appear. Further, the metal adhering to the inner wall of the container containing the mixed acid solution or contained as an impurity dissolves into the mixed acid solution by coming into contact with the mixed acid solution and is contained in the measurement sample solution.
  • the present invention has been made in view of the above-mentioned problems, and its purpose is to prevent contamination of metal impurities derived from the decomposition solution, and more accurately in a compound sample or a silicon carbide compound sample composed of carbon atoms.
  • a container for decomposing a compound sample comprising silicon atoms or a silicon carbide compound sample capable of analyzing a metal impurity, a gas phase decomposition method and a gas phase decomposition apparatus using the container, and a decomposed carbon atom An analysis method and an analysis apparatus for a compound sample or a silicon carbide compound sample are provided.
  • a container according to the present invention is a container for decomposing a compound sample or silicon carbide compound sample comprising carbon atoms, and the compound sample or silicon carbide compound comprising carbon atoms therein.
  • An outer container portion having a sealed space for containing a decomposition solution for decomposing the sample, and having pressure resistance against pressure for decomposing the compound sample or silicon carbide compound sample composed of the carbon atom, and the outer container portion
  • An inner container that is formed of a material that is resistant to the decomposition solution and contains the compound sample or the silicon carbide compound sample composed of the carbon atom from the opened upper part. Is characterized in that when the decomposition solution is accommodated in the outer container part, the decomposition solution is not in contact with the inner wall.
  • a decomposition solution for decomposing a compound sample or a silicon carbide compound sample made of carbon atoms is accommodated in the outer container portion of any of the above-described containers, and carbon atoms are placed on the mounting table.
  • a preparatory step for placing the compound sample or silicon carbide compound sample comprising, and pressurizing by heating the inside of the outer container portion containing the compound sample or silicon carbide compound sample comprising the carbon atom and the decomposition solution A decomposition step of decomposing the compound sample composed of the carbon atom or the silicon carbide compound sample with a decomposition solution gas obtained by vaporizing the decomposition solution.
  • the method for analyzing a compound sample consisting of carbon atoms or a silicon carbide compound sample according to the present invention is a measurement obtained by decomposing a compound sample consisting of carbon atoms or a silicon carbide compound sample by any of the vapor phase decomposition methods described above. It includes a step of detecting metal impurities in the sample.
  • the vapor phase decomposition apparatus for a compound sample comprising silicon atoms or a silicon carbide compound sample according to the present invention is characterized by comprising any of the above-described containers and a heating means for heating the container.
  • the analyzer for analyzing a compound sample consisting of carbon atoms or a silicon carbide compound sample according to the present invention is obtained by vapor-phase decomposition of any of the above-described containers and a compound sample or silicon carbide compound sample consisting of carbon atoms in the container. And detecting means for detecting metal impurities in the measured sample.
  • a container for decomposing a compound sample comprising silicon atoms or a silicon carbide compound sample according to the present invention has a sealed space containing a decomposition solution for decomposing the compound sample comprising silicon atoms or the silicon carbide compound sample, An outer container portion that is pressure resistant to a pressure for decomposing a compound sample or silicon carbide compound sample composed of carbon atoms, and a material that is provided in the outer container portion and is resistant to the decomposition solution. And an inner container in which the compound sample composed of the carbon atoms or the silicon carbide compound sample is accommodated from the opened upper part, and the inner container is disposed when the decomposition solution is accommodated in the outer container part.
  • the decomposition solution does not come into contact with the inner wall, it is derived from the decomposition solution in the compound sample consisting of decomposed carbon atoms or the silicon carbide compound sample. Genus impurities prevents the contamination, it is more accurately can analyze metallic impurities of the compound samples or silicon carbide compound sample composed of carbon atoms.
  • FIG. 1 is a cross-sectional view showing a container for decomposing a compound sample or silicon carbide compound sample comprising carbon atoms according to an embodiment of the present invention.
  • the compound sample consisting of carbon atoms is a compound sample containing only carbon atoms.
  • Examples of compound samples comprising carbon atoms are intended to be diamond, graphite, graphene, amorphous carbon, diamond-like carbon, tetrahedral amorphous carbon, carbon nanotubes, carbon nanocoils, carbon fibers, carbon, etc.
  • the silicon carbide compound sample is intended to be a silicon carbide based sample containing SiC, SiOC, SiCN and the like. In the present embodiment, a mode using a silicon carbide compound sample will be described as an example.
  • the container 10 includes an outer container portion 1 and an inner container 6.
  • the container 10 is used for decomposing the silicon carbide compound sample 7.
  • the container 10 may further include a support portion 4 including a table (mounting table) 5 on which the inner container 6 is placed.
  • Outer container part 1 The outer container part 1 has a sealed space in which a silicon carbide compound sample 7 and a decomposition solution 8 for decomposing the silicon carbide compound sample 7 are accommodated. Outer container portion 1 is pressure resistant to the pressure applied to decompose silicon carbide compound sample 7 accommodated therein. Moreover, it is preferable that the outer container part 1 is heat resistant with respect to the heat
  • the pressure resistance against the pressure applied to decompose the silicon carbide compound sample 7 is difficult to expand or soften when pressure is applied to decompose the silicon carbide compound sample 7, It is intended to keep the shape constant and not deform.
  • heat resistance to heat applied to decompose the silicon carbide compound sample 7 means that when heated to decompose the silicon carbide compound sample 7, elution or softening is difficult and the shape is kept constant. It is intended not to deform.
  • the outer container part 1 has a double wall structure of an inner cylinder part 3 and an outer cylinder part 2 outside thereof.
  • the inner cylinder portion 3 faces the sealed space and is formed of a material that is resistant to the decomposition solution 8.
  • the inner cylinder portion 3 is formed of a material that is resistant to the decomposition solution 8 because the decomposition solution 8 is in direct contact with the decomposition solution 8 when the decomposition solution 8 is accommodated in the sealed space.
  • the material that is resistant to the decomposition solution 8 is intended to be a material that does not elute metal components from the decomposition solution 8, and is more preferably a material that does not elute metal components from the decomposition solution 8. preferable.
  • Examples of the material that is resistant to the decomposition solution 8 include a fluororesin, platinum, or a ceramic material.
  • PTFE polytetrafluoroethylene (tetrafluoride)
  • PFA tetrafluoroethylene / perfluoroalkyl vinyl ether copolymer
  • PVDF polyvinylidene fluoride (difluoride)
  • PCTFE polychlorotrifluoro Ethylene (trifluoride) etc.
  • the ceramic material include alumina, zirconia, calcia, magnesia, yttria and the like.
  • the shape of the inner cylinder part 3 is not particularly limited as long as the sealed space exists inside, the support part 4 is installed in the sealed space, and the silicon carbide compound sample 7 and the decomposition solution 8 can be accommodated.
  • the inner cylinder portion 3 is divided into two members, a lower portion and a lid portion. A support portion 4 is installed in the lower portion, the decomposition solution 8 is accommodated, and the lid portion is placed and sealed so as to close it from above. May be.
  • the thickness of the lower wall, the side wall, and the upper wall of the inner cylinder part 3 is not particularly limited as long as it is a thickness capable of preventing the stored decomposition solution 8 from flowing out and sealing the inner space.
  • the outer cylinder part 2 is located outside the inner cylinder part 3 and is provided so as to wrap around the inner cylinder part 3. And the outer cylinder part 2 is pressure-resistant with respect to the pressure for melt
  • FIG. Therefore, in order to decompose the silicon carbide compound sample 7 accommodated in the inside, even if pressure is applied by heating and the inner cylinder part 3 is deformed, the outer cylinder part 2 has pressure resistance. Deformation of the entire container unit 1 can be prevented. Moreover, it is preferable that the outer cylinder part 2 is heat resistant with respect to the heat applied in order to dissolve the silicon carbide compound sample 7. FIG. Thereby, the deformation
  • the outer cylinder portion 2 only needs to have pressure resistance and heat resistance against the pressure and heat for dissolving the silicon carbide compound sample 7, and is formed of, for example, stainless steel.
  • the outer cylinder part 2 should just be provided so that the inner cylinder part 3 may be wrapped at least at the time of pressurization and heating. That is, the outer cylinder part 2 is divided into two members, a lower part and a lid part. The inner cylinder part 3 is accommodated in the lower part, and the lid part is placed and sealed so as to close it from above. And may be subjected to heating.
  • the thickness of the lower wall, the side wall, and the upper wall of the outer cylinder part 2 is not particularly limited as long as desired pressure resistance and heat resistance can be obtained.
  • the inner cylinder part 3 faces the sealed space in which the decomposition liquid 8 is accommodated, and the outer cylinder part 2 and the decomposition liquid 8 are not in contact with each other. It is possible to prevent the derived metal impurities from being dissolved into the decomposition solution 8 and causing contamination, and to suppress the elution of the metal into the decomposition solution 8.
  • the inner cylinder part 3 may be further made into a two-layer structure to prevent the metal impurities derived from the outer cylinder part 2 from dissolving into the decomposition solution 8 more reliably.
  • the inner container 6 is formed of a material that is resistant to the decomposition solution 8 and is a columnar container having an open top.
  • the silicon carbide compound sample 7 is accommodated in the inner container 6 from the upper open part.
  • the inner container 6 is provided in the outer container part 1 so that the decomposition solution 8 does not contact the inner wall. Since the inner container 6 is exposed to the decomposition liquid gas in which the decomposition liquid 8 is vaporized, the inner container 6 is formed of a material that does not elute the metal component with respect to the decomposition liquid 8. Need to be.
  • Examples of the material that is resistant to the decomposition solution 8 constituting the inner container 6 include a fluororesin, platinum, or a ceramic material.
  • PTFE polytetrafluoroethylene (tetrafluoride)
  • PFA tetrafluoroethylene / perfluoroalkyl vinyl ether copolymer
  • PVDF polyvinylidene fluoride (difluoride)
  • PCTFE polychlorotrifluoro Ethylene (trifluoride) etc.
  • the ceramic material include alumina, zirconia, calcia, magnesia, yttria and the like.
  • the inner container 6 may be placed on the table 5, and the decomposition solution 8 may be stored below the table 5 positioned above the liquid surface of the decomposition solution 8.
  • the container 6 and a decomposition liquid container (not shown) containing the decomposition liquid may be placed adjacent to the table 5, and the inner container 6 is placed under the table 5.
  • a decomposition solution container (not shown) containing the decomposition solution may be placed on the upper side of the table. That is, the inner container 6 may be configured such that the decomposition liquid 8 does not contact the inner wall of the inner container 6 and the silicon carbide compound sample 7 in the inner container 6 is exposed to the decomposition liquid gas vaporized from the decomposition liquid 8.
  • a decomposition liquid container it is formed of a material that is resistant to the decomposition liquid, and a container in which the decomposition liquid is accommodated from an opened upper portion can be used.
  • a plurality of inner containers 6 may be placed on the table 5, whereby a plurality of silicon carbide compound samples 7 can be decomposed simultaneously.
  • the size of the inner container 6 is not particularly limited as long as the contained silicon carbide compound sample 7 is sufficiently exposed to the decomposition liquid gas from which the decomposition liquid 8 is vaporized.
  • the support part 4 is provided in the outer container part 1.
  • the support portion 4 includes a stand provided so as to protrude from the bottom surface inside the outer container portion 1 and a table 5 provided on the top of the stand.
  • the table 5 is provided so as to be supported from below by support pins (not shown) provided so as to protrude from at least two positions of the side wall of the outer container part 1 (side wall of the inner cylinder part 3). Also good.
  • the support part 4 is comprised by the table 5 and the support pin.
  • the table 5 may be formed integrally with a stand or a support pin, or may be formed separately and assembled before use.
  • the support unit 4 may be configured to be able to change the height of the stand.
  • the support portion 4 is preferably made of a material resistant to the decomposition solution 8.
  • the diameter of the table 5 is the same as the inner diameter of the inner cylinder part 3, and is provided so as to contact the side wall of the inner cylinder part 3.
  • the table 5 is a porous body provided with holes for allowing the cracked liquid gas to pass therethrough. Therefore, the hole provided in the table 5 becomes a flow path of the decomposition liquid gas in which the decomposition liquid 8 accommodated below is vaporized, and the decomposition liquid gas reaches the silicon carbide compound sample 7.
  • the inner diameter of the table 5 may be smaller than the inner diameter of the inner cylinder portion 3 so that a gap is formed between the table 5 and the inner wall of the inner cylinder portion 3. In this case, since the decomposition gas flows from the gap and reaches the silicon carbide compound sample 7, the table 5 does not have to be provided with holes.
  • the silicon carbide compound sample 7 is accommodated in the inner container 6 provided in the pressure-resistant outer container part 1 that accommodates the decomposition solution 8, and the inside of the outer container part 1 is heated.
  • the silicon carbide compound sample 7 is vapor-phase decomposed by the decomposition liquid gas obtained by vaporizing the decomposition liquid 8. Therefore, the metal impurities contained in the decomposition solution 8 and the metal impurities adhering to the inner wall of the outer container part 1 (inner wall of the inner cylinder part 3) and the inner wall of the inner container 6 are obtained by decomposing the silicon carbide compound sample 7. It can prevent mixing in the measured sample.
  • the silicon carbide compound sample 7 is decomposed using the container 10, it can be subjected to an analysis that more accurately detects a trace amount of metal contained in the silicon carbide compound sample 7.
  • a compound sample composed of carbon atoms can be decomposed even under atmospheric pressure using a decomposition solution such as a mixed acid of sulfuric acid, nitric acid and perchloric acid (for example, Reference 1 (“Wet oxidative decomposition: curcumin absorption Quantitative determination of boron in graphite by photometric method ", Kazuo Watanabe et al., Analytical Chemistry, 44 (11), 939-942, 1995)).
  • a decomposition solution such as a mixed acid of sulfuric acid, nitric acid and perchloric acid
  • the silicon carbide compound sample 7 which is harder to decompose than the compound sample made of carbon atoms can be decomposed. Therefore, it is clear that the compound sample made of carbon atoms can be decomposed using the container 10. is there.
  • the gas phase decomposition method is a method for decomposing a compound sample or silicon carbide compound sample comprising carbon atoms, wherein a decomposition solution for decomposing the sample or carbon carbide compound sample comprising carbon atoms is provided. It includes a decomposition step of decomposing by the vaporized decomposition gas. According to the present invention, since a compound sample comprising silicon atoms or a silicon carbide compound sample is vapor-phase decomposed, metal impurities contained in the decomposition solution are mixed into a measurement sample obtained by decomposing the sample. Can be prevented.
  • a decomposition solution for decomposing a compound sample composed of carbon atoms or a silicon carbide compound sample is accommodated in the outer container portion 1 of the container 10 described above before the decomposition step.
  • the container 10 described above is an embodiment of a container used in the vapor phase decomposition method according to the present invention. Therefore, the description of the container used in the vapor phase decomposition method according to the present invention conforms to the description of the container 10 described above. In the present embodiment, a case where a silicon carbide compound sample is used will be described as an example.
  • a decomposition solution for decomposing the silicon carbide compound sample is stored in the outer container portion 1 of the container 10, and the silicon carbide compound sample is stored in the inner container 6.
  • the decomposition liquid is accommodated so as not to touch the inner wall of the inner container 6.
  • the silicon carbide compound sample is efficiently decomposed if the decomposition solution is accommodated in an amount of 5 to 40% of the volume of the outer container portion 1. This is preferable.
  • the amount of the decomposition solution accommodated in the outer container portion 1 may be an amount capable of sufficiently decomposing the silicon carbide compound sample. Therefore, for example, 2 to 20 ml of decomposition solution may be accommodated per 1 g of the silicon carbide compound sample to be decomposed.
  • An acid solution containing at least one acid selected from the group consisting of hydrofluoric acid, nitric acid, hydrochloric acid, sulfuric acid, phosphoric acid, hydrogen peroxide, and perchloric acid is used as a decomposition solution for decomposing the silicon carbide compound sample.
  • it is a mixed acid solution of hydrofluoric acid and nitric acid.
  • the silicon carbide compound sample may be placed in the inner container 6 and placed on the table 5.
  • the silicon carbide compound sample may be a bulk or a thin film. After accommodating the silicon carbide compound sample and the decomposition solution in the outer container part 1, the outer container part 1 is sealed.
  • the silicon carbide compound sample and the decomposition solution are accommodated and pressurized by heating the inside of the sealed outer container part 1.
  • the pressurization and heating in the outer container part 1 can be suitably performed by a conventionally known method.
  • the heating temperature of the outer container part 1 may be any desired pressurization that will be described later and may be any temperature that vaporizes the decomposition solution, preferably 100 to 240 ° C, more preferably 150 to 240 ° C. Preferably, the temperature is from 180 to 240 ° C.
  • the heating time of the outer container part 1 is preferably 1 to 96 hours, more preferably 1 to 48 hours, and most preferably 5 to 48 hours per 1 g of the silicon carbide compound sample.
  • the pressure applied to the outer container part 1 by heating at the above-described temperature is a pressure at which the silicon carbide compound sample can be decomposed by the vaporized decomposition solution, preferably 1 to 15 MPa, and preferably 5 to 15 MPa. Is more preferable, and 7 to 15 MPa is most preferable.
  • the silicon carbide compound sample is decomposed in the gas phase by the decomposition solution gas from which the decomposition solution is vaporized. Therefore, metal impurities contained in the decomposition solution and metal impurities attached to the inner wall of the outer container part 1 (inner wall of the inner cylinder part 3) and the inner wall of the inner container 6 were obtained by decomposing the silicon carbide compound sample. Mixing in the measurement sample can be prevented. As a result, it can be subjected to an analysis that more accurately detects a trace amount of metal contained in a silicon carbide compound sample.
  • the method for analyzing a compound sample comprising silicon atoms or a silicon carbide compound sample is the method of analyzing a compound sample comprising silicon atoms or a silicon carbide compound sample obtained by decomposing the compound sample comprising silicon atoms or the silicon carbide compound sample.
  • the method includes a step of detecting a metal impurity.
  • the metal impurities contained in the sample are contained in the inner container 6 in which the sample is accommodated. Remains. In the present embodiment, the remaining metal impurities are used as detection targets using the measurement sample.
  • the metal impurities remaining in the inner container 6 may be recovered using a recovery liquid.
  • a conventionally known solution can be used as the recovery solution, and is not particularly limited.
  • nitric acid or a mixed acid of nitric acid and hydrochloric acid can be used.
  • the recovered liquid is dropped into the inner container 6 to dissolve and recover the metal impurities attached to the inner wall of the inner container 6.
  • the metal impurities may be recovered by dropping the recovered liquid into the inner container 6 and further heating.
  • the recovered metal impurities may be further adjusted with a recovery solution and used for measurement.
  • ICP-MS inductively coupled plasma mass spectrometry
  • ICP-AES inductively coupled plasma emission spectroscopy
  • AAS atomic absorption spectrometry
  • the metal impurities contained in the compound sample or silicon carbide compound sample consisting of carbon atoms are reduced. More accurate detection is possible.
  • a vapor phase decomposition apparatus for a compound sample comprising silicon atoms or a silicon carbide compound sample according to the present invention is characterized by comprising the container described above and a heating means for heating the container.
  • the container 10 used in the above-described gas phase decomposition method is an embodiment of the container used in the gas phase decomposition apparatus according to the present invention. Therefore, the description of the vapor phase decomposition apparatus according to the present invention is based on the above description of the vapor phase decomposition method. In addition, a conventionally well-known heating apparatus can be used as a heating means.
  • the analyzer for analyzing a compound sample or silicon carbide compound sample comprising carbon atoms comprises the above-described container and a measurement obtained by vapor phase decomposition of the compound sample or silicon carbide compound sample comprising carbon atoms in the container. And a detecting means for detecting metal impurities in the sample.
  • the container 10 used in the analysis method described above is an embodiment of a container used in the analyzer according to the present invention. Therefore, the description of the analysis apparatus according to the present invention conforms to the description of the analysis method described above.
  • the detection means a conventionally known detection device can be used, and an example is ICP-MS manufactured by PerkinElmer.
  • the quality control method for a compound sample or silicon carbide compound sample comprising carbon atoms according to the present invention was obtained by decomposing a compound sample or silicon carbide compound sample comprising carbon atoms by any one of the vapor phase decomposition methods described above.
  • the metal element remaining by decomposing the compound sample or silicon carbide compound sample composed of carbon atoms by the gas phase decomposition method according to the present invention is recovered as a metal impurity, and a conventionally known measurement method is used as a measurement sample.
  • Elemental analysis by Examples of the method for elemental analysis of the measurement sample include inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma emission spectroscopy (ICP-AES), and atomic absorption spectrometry (AAS).
  • a compound sample or a silicon carbide compound sample consisting of carbon atoms in which the amount of metal impurities detected in the analysis step is equal to or less than a predetermined reference amount is extracted. That is, a compound sample or a silicon carbide compound sample consisting of carbon atoms is selected based on the amount of metal impurities detected in the analysis step. In the extraction step, a compound sample or a silicon carbide compound sample made of carbon atoms may be selected based on the type of metal impurity detected in the analysis step.
  • the metal impurity contained in the compound sample or silicon carbide compound sample made of carbon atoms can be accurately detected.
  • the quality of the compound sample or silicon carbide compound sample comprising carbon atoms can be kept constant. Therefore, the quality control method according to the present invention is also suitable for quality control of a compound sample composed of carbon atoms or a silicon carbide compound sample used for semiconductor manufacturing, which requires more accurate quality control.
  • the container which concerns on this invention is a container for decomposing
  • the outer container portion faces the sealed space, and is located outside the inner tube portion and an inner tube portion formed of a material resistant to the decomposition solution. And it is preferable that it is a double wall structure with the outer cylinder part which is pressure-resistant with respect to the pressure for dissolving the compound sample or silicon carbide compound sample which consists of the said carbon atom.
  • the inner container may be provided on a mounting table located above the liquid level of the decomposition liquid when the decomposition liquid is accommodated in the outer container portion. preferable.
  • a container according to the present invention is a decomposition liquid container that is provided in the outer container part, is formed of a material that is resistant to the decomposition liquid, and contains the decomposition liquid from the opened upper part. Furthermore, it is preferable to provide.
  • a decomposition solution for decomposing a compound sample or a silicon carbide compound sample made of carbon atoms is accommodated in the outer container portion of any of the above-described containers, and carbon atoms are placed on the mounting table.
  • a preparatory step for placing the compound sample or silicon carbide compound sample comprising, and pressurizing by heating the inside of the outer container portion containing the compound sample or silicon carbide compound sample comprising the carbon atom and the decomposition solution A decomposition step of decomposing the compound sample composed of the carbon atom or the silicon carbide compound sample with a decomposition solution gas obtained by vaporizing the decomposition solution.
  • the decomposition step it is preferable to pressurize at 1 to 15 MPa by heating the inside of the outer container portion at 100 to 240 ° C.
  • the decomposition solution is at least one selected from the group consisting of hydrofluoric acid, nitric acid, hydrochloric acid, sulfuric acid, phosphoric acid, hydrogen peroxide solution, and perchloric acid.
  • An acid solution containing an acid is preferable.
  • the method for analyzing a compound sample consisting of carbon atoms or a silicon carbide compound sample according to the present invention is a measurement obtained by decomposing a compound sample consisting of carbon atoms or a silicon carbide compound sample by any of the vapor phase decomposition methods described above. It includes a step of detecting metal impurities in the sample.
  • the vapor phase decomposition apparatus for a compound sample comprising silicon atoms or a silicon carbide compound sample according to the present invention is characterized by comprising any of the above-described containers and a heating means for heating the container.
  • the analyzer for analyzing a compound sample consisting of carbon atoms or a silicon carbide compound sample according to the present invention is obtained by vapor-phase decomposition of any of the above-described containers and a compound sample or silicon carbide compound sample consisting of carbon atoms in the container. And detecting means for detecting metal impurities in the measured sample.
  • the quality control method for a compound sample or silicon carbide compound sample comprising carbon atoms according to the present invention was obtained by decomposing a compound sample or silicon carbide compound sample comprising carbon atoms by any one of the vapor phase decomposition methods described above.
  • a blank test of vapor phase decomposition using the container 10 was performed.
  • the metal impurities contained in the decomposition solution and the outer container part 1 The amount of metal impurities adhering to the inner wall mixed into the measurement sample was examined.
  • a decomposition solution As a decomposition solution, a mixed acid solution of 40% hydrofluoric acid and 68% nitric acid (1: 1) was used.
  • the inner container 6 was evacuated and exposed to the vaporized decomposition gas, and the inside of the outer container 1 was heated at 200 ° C. for 5 hours to obtain high-temperature pressurization conditions.
  • a SUS container was used as the outer cylinder part 2
  • a PTFE container was used as the inner cylinder part 3.
  • Two PTFE inner containers 6 (VPD-1 and VPD-2) were placed on the table 5. The inner container 6 was taken out and nitric acid was dropped to collect metal impurities in each inner container 6 to obtain a measurement sample.
  • the measurement sample was measured by ICP-MS (manufactured by PerkinElmer). As a result, the amount of metal impurities contained in the measurement sample was as shown in Table 1. The values shown in Table 1 were calculated by multiplying the concentration (ng / g) measured by ICP-MS and the liquid amount (g) adjusted with the liquid.
  • the silicon carbide compound sample (SiC sample) was vapor-phase decomposed using the container 10.
  • a mixed acid solution of 40% hydrofluoric acid and 68% nitric acid (1: 1) was used as the decomposition solution.
  • the silicon carbide compound sample is placed in the inner container 6 and exposed to the decomposed liquid gas in which the decomposed liquid is vaporized, and the inside of the outer container 1 is heated at 200 ° C. for 5 hours. did.
  • the silicon carbide compound sample in the inner container 6 was decomposed and sublimated.
  • a silicon carbide certified reference material (CRM NMIJ 8001A) was vapor-phase decomposed.
  • As the decomposition solution a mixed acid solution of 40% hydrogen fluoride and 68% nitric acid (1: 1) was used. High temperature pressurization conditions were obtained by heating at 230 ° C. for 96 hours. After the decomposition treatment, the inner container 6 was taken out and nitric acid was added dropwise to collect metal impurities in the inner container 6 to obtain a measurement sample.
  • the above measurement sample was measured by ICP-MS (manufactured by PerkinElmer). As a result, the measured values and certified values of the samples were as shown in Table 2. The values listed in Table 2 were calculated by multiplying the concentration (ng / g) measured by ICP-MS by the liquid amount (g) prepared by liquid adjustment and dividing by the decomposed sample amount (g). .
  • the present invention can be used for metal impurity analysis of compound samples composed of carbon atoms or silicon carbide compound samples used in various fields.

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

A container (10) comprises: an outer container part (1) having an airtight space which houses therewithin either a compound sample formed from carbon atoms or a silicon carbide compound sample and a cracking fluid which cracks the sample, said outer container part being resilient against pressure to crack the sample; and an inner container (6) which is disposed within the outer container part (1) such that the cracking fluid does not make contact with the inner wall thereof, and which houses the sample. Metallic impurities arising from the cracking fluid are thus prevented from mixing with a cracked sample.

Description

容器、気相分解方法、気相分解装置、分析方法、及び分析装置Container, gas phase decomposition method, gas phase decomposition apparatus, analysis method, and analysis apparatus

　本発明は、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解するための容器、当該容器を用いた気相分解方法及び気相分解装置、並びに分解された炭素原子からなる化合物試料又は炭化ケイ素化合物試料の分析方法及び分析装置に関する。 The present invention relates to a container for decomposing a compound sample or silicon carbide compound sample comprising carbon atoms, a gas phase decomposition method and a gas phase decomposition apparatus using the vessel, and a compound sample or silicon carbide comprising decomposed carbon atoms. The present invention relates to an analysis method and an analysis apparatus for compound samples.

　炭化ケイ素化合物中に含まれる不純物を分析する方法として、非特許文献１に記載の炭化ケイ素微粉末の化学分析方法が知られている。非特許文献１に記載の方法によれば、複数の酸を混合した混酸溶液中に炭化ケイ素を浸漬して加熱及び加圧し、混酸溶液中に炭化ケイ素を溶解させて測定試料液を得る。そして、この測定試料中に含まれる金属不純物を検出する。 As a method for analyzing impurities contained in a silicon carbide compound, a chemical analysis method for silicon carbide fine powder described in Non-Patent Document 1 is known. According to the method described in Non-Patent Document 1, silicon carbide is immersed in a mixed acid solution in which a plurality of acids are mixed, heated and pressurized, and silicon carbide is dissolved in the mixed acid solution to obtain a measurement sample solution. And the metal impurity contained in this measurement sample is detected.

ＪＩＳ　Ｒ　１６１６－２００７「加圧酸分解－ＩＣＰ発光分光法」JIS R 1616-2007 “Pressure Acid Decomposition-ICP Emission Spectroscopy”

　しかしながら、非特許文献１に記載の方法によれば、炭化ケイ素化合物試料と混酸溶液とが直接接触するため、混酸溶液に含まれる金属が測定試料液に含まれ、測定試料液へのコンタミネーションが発生する。また、混酸溶液を収容する容器の内壁に付着または、不純物として含まれる金属が、混酸溶液に接触することによって混酸溶液中に溶け出し、測定試料液に含まれてしまう。 However, according to the method described in Non-Patent Document 1, since the silicon carbide compound sample and the mixed acid solution are in direct contact, the metal contained in the mixed acid solution is contained in the measurement sample solution, and contamination to the measurement sample solution is not caused. appear. Further, the metal adhering to the inner wall of the container containing the mixed acid solution or contained as an impurity dissolves into the mixed acid solution by coming into contact with the mixed acid solution and is contained in the measurement sample solution.

　近年、炭素原子からなる化合物又は炭化ケイ素化合物の半導体材料としての応用が視野に入れられており、より高純度の炭素原子からなる化合物又は炭化ケイ素化合物が求められている。したがって、炭素原子からなる化合物又は炭化ケイ素化合物中に含まれる金属不純物を、より正確に分析する必要があり、従来は問題にならなかった、分析時の微量金属の混入が問題になる。 In recent years, the application of a compound comprising a carbon atom or a silicon carbide compound as a semiconductor material has been taken into consideration, and a compound or silicon carbide compound comprising a higher purity carbon atom has been demanded. Therefore, it is necessary to analyze the metal impurities contained in the compound composed of carbon atoms or the silicon carbide compound more accurately, and contamination of trace metals during analysis, which has not been a problem in the past, becomes a problem.

　本発明は、上記の問題点に鑑みて成されたものであり、その目的は、分解液に由来する金属不純物の混入を防ぎ、より正確に炭素原子からなる化合物試料又は炭化ケイ素化合物試料中の金属不純物を分析することが可能な、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解するための容器、当該容器を用いた気相分解方法及び気相分解装置、並びに分解された炭素原子からなる化合物試料又は炭化ケイ素化合物試料の分析方法及び分析装置を提供することにある。 The present invention has been made in view of the above-mentioned problems, and its purpose is to prevent contamination of metal impurities derived from the decomposition solution, and more accurately in a compound sample or a silicon carbide compound sample composed of carbon atoms. A container for decomposing a compound sample comprising silicon atoms or a silicon carbide compound sample capable of analyzing a metal impurity, a gas phase decomposition method and a gas phase decomposition apparatus using the container, and a decomposed carbon atom An analysis method and an analysis apparatus for a compound sample or a silicon carbide compound sample are provided.

　上記の課題を解決するために、本発明に係る容器は、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解するための容器であって、内部に上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解する分解液を収容する密閉空間を有し、上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解するための圧力に対して耐圧性である外容器部と、上記外容器部内に設けられ、上記分解液に対して耐溶性である材料により形成されており、開放された上部から上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料が収容される内容器とを備え、上記内容器は、上記分解液が上記外容器部に収容されたときに、その内壁に上記分解液が接触しないように設けられていることを特徴としている。 In order to solve the above problems, a container according to the present invention is a container for decomposing a compound sample or silicon carbide compound sample comprising carbon atoms, and the compound sample or silicon carbide compound comprising carbon atoms therein. An outer container portion having a sealed space for containing a decomposition solution for decomposing the sample, and having pressure resistance against pressure for decomposing the compound sample or silicon carbide compound sample composed of the carbon atom, and the outer container portion An inner container that is formed of a material that is resistant to the decomposition solution and contains the compound sample or the silicon carbide compound sample composed of the carbon atom from the opened upper part. Is characterized in that when the decomposition solution is accommodated in the outer container part, the decomposition solution is not in contact with the inner wall.

　本発明に係る気相分解方法は、上述したいずれかの容器の上記外容器部内に、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解する分解液を収容し、上記載置台上に炭素原子からなる化合物試料又は炭化ケイ素化合物試料を載置する準備工程と、上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料と上記分解液とが収容された上記外容器部内を加熱することによって加圧し、上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料を、上記分解液が気化した分解液ガスにより分解する分解工程とを包含することを特徴としている。 In the gas phase decomposition method according to the present invention, a decomposition solution for decomposing a compound sample or a silicon carbide compound sample made of carbon atoms is accommodated in the outer container portion of any of the above-described containers, and carbon atoms are placed on the mounting table. A preparatory step for placing the compound sample or silicon carbide compound sample comprising, and pressurizing by heating the inside of the outer container portion containing the compound sample or silicon carbide compound sample comprising the carbon atom and the decomposition solution, A decomposition step of decomposing the compound sample composed of the carbon atom or the silicon carbide compound sample with a decomposition solution gas obtained by vaporizing the decomposition solution.

　本発明に係る炭素原子からなる化合物試料又は炭化ケイ素化合物試料の分析方法は、上述したいずれかの気相分解方法により、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解して得られた測定試料中の金属不純物を検出する工程を包含することを特徴としている。 The method for analyzing a compound sample consisting of carbon atoms or a silicon carbide compound sample according to the present invention is a measurement obtained by decomposing a compound sample consisting of carbon atoms or a silicon carbide compound sample by any of the vapor phase decomposition methods described above. It includes a step of detecting metal impurities in the sample.

　本発明に係る炭素原子からなる化合物試料又は炭化ケイ素化合物試料の気相分解装置は、上述したいずれかの容器と、上記容器を加熱する加熱手段とを備えたことを特徴としている。 The vapor phase decomposition apparatus for a compound sample comprising silicon atoms or a silicon carbide compound sample according to the present invention is characterized by comprising any of the above-described containers and a heating means for heating the container.

　本発明に係る炭素原子からなる化合物試料又は炭化ケイ素化合物試料の分析装置は、上述したいずれかの容器と、上記容器内において炭素原子からなる化合物試料又は炭化ケイ素化合物試料を気相分解して得られた測定試料中の金属不純物を検出する検出手段とを備えたことを特徴としている。 The analyzer for analyzing a compound sample consisting of carbon atoms or a silicon carbide compound sample according to the present invention is obtained by vapor-phase decomposition of any of the above-described containers and a compound sample or silicon carbide compound sample consisting of carbon atoms in the container. And detecting means for detecting metal impurities in the measured sample.

　本発明に係る炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解するための容器は、上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解する分解液を収容する密閉空間を有し、上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解するための圧力に対して耐圧性である外容器部と、上記外容器部内に設けられ、上記分解液に対して耐溶性である材料により形成されており、開放された上部から上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料が収容される内容器とを備え、上記内容器は、上記分解液が上記外容器部に収容されたときに、その内壁に上記分解液が接触しないように設けられているので、分解した炭素原子からなる化合物試料又は炭化ケイ素化合物試料中に分解液に由来する金属不純物が混入するのを防ぎ、より正確に炭素原子からなる化合物試料又は炭化ケイ素化合物試料中の金属不純物を分析することが可能である。 A container for decomposing a compound sample comprising silicon atoms or a silicon carbide compound sample according to the present invention has a sealed space containing a decomposition solution for decomposing the compound sample comprising silicon atoms or the silicon carbide compound sample, An outer container portion that is pressure resistant to a pressure for decomposing a compound sample or silicon carbide compound sample composed of carbon atoms, and a material that is provided in the outer container portion and is resistant to the decomposition solution. And an inner container in which the compound sample composed of the carbon atoms or the silicon carbide compound sample is accommodated from the opened upper part, and the inner container is disposed when the decomposition solution is accommodated in the outer container part. Since the decomposition solution does not come into contact with the inner wall, it is derived from the decomposition solution in the compound sample consisting of decomposed carbon atoms or the silicon carbide compound sample. Genus impurities prevents the contamination, it is more accurately can analyze metallic impurities of the compound samples or silicon carbide compound sample composed of carbon atoms.

本発明の一実施形態に係る、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解するための容器を示す断面図である。It is sectional drawing which shows the container for decomposing | disassembling the compound sample which consists of carbon atoms, or a silicon carbide compound sample based on one Embodiment of this invention.

　〔容器１０〕
　以下、本発明に係る容器の一実施形態について、図１を参照して詳細に説明する。図１は、本発明の一実施形態に係る、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解するための容器を示す断面図である。 [Container 10]
Hereinafter, an embodiment of a container according to the present invention will be described in detail with reference to FIG. FIG. 1 is a cross-sectional view showing a container for decomposing a compound sample or silicon carbide compound sample comprising carbon atoms according to an embodiment of the present invention.

　ここで、炭素原子からなる化合物試料は、炭素原子のみを含む化合物試料である。炭素原子からなる化合物試料の例として、ダイヤモンド、グラファイト、グラフェン、アモルファスカーボン、ダイヤモンドライクカーボン、テトラヘドラルアモルファスカーボン、カーボンナノチューブ、カーボンナノコイル、炭素繊維、及び、カーボン等であることが意図される。炭化ケイ素化合物試料は、ＳｉＣ、ＳｉＯＣ、ＳｉＣＮ等を含む炭化ケイ素系の試料であることが意図される。本実施形態においては、炭化ケイ素化合物試料を用いる形態を例として説明する。 Here, the compound sample consisting of carbon atoms is a compound sample containing only carbon atoms. Examples of compound samples comprising carbon atoms are intended to be diamond, graphite, graphene, amorphous carbon, diamond-like carbon, tetrahedral amorphous carbon, carbon nanotubes, carbon nanocoils, carbon fibers, carbon, etc. . The silicon carbide compound sample is intended to be a silicon carbide based sample containing SiC, SiOC, SiCN and the like. In the present embodiment, a mode using a silicon carbide compound sample will be described as an example.

　図１に示すように、容器１０は、外容器部１と内容器６とを備えている。容器１０は、炭化ケイ素化合物試料７を分解するために用いられる。本実施形態において、容器１０は、内容器６を載置するテーブル（載置台）５を備えた支持部４をさらに備えていてもよい。 As shown in FIG. 1, the container 10 includes an outer container portion 1 and an inner container 6. The container 10 is used for decomposing the silicon carbide compound sample 7. In the present embodiment, the container 10 may further include a support portion 4 including a table (mounting table) 5 on which the inner container 6 is placed.

　（外容器部１）
　外容器部１は、内部に炭化ケイ素化合物試料７と炭化ケイ素化合物試料７を分解する分解液８とを収容する密閉空間を有している。外容器部１は、内部に収容した炭化ケイ素化合物試料７を分解するために加えられる圧力に対して耐圧性である。また、外容器部１は、内部に収容した炭化ケイ素化合物試料７を分解するために加えられる熱に対して耐熱性であることが好ましい。 (Outer container part 1)
The outer container part 1 has a sealed space in which a silicon carbide compound sample 7 and a decomposition solution 8 for decomposing the silicon carbide compound sample 7 are accommodated. Outer container portion 1 is pressure resistant to the pressure applied to decompose silicon carbide compound sample 7 accommodated therein. Moreover, it is preferable that the outer container part 1 is heat resistant with respect to the heat | fever applied in order to decompose | disassemble the silicon carbide compound sample 7 accommodated in the inside.

　ここで、炭化ケイ素化合物試料７を分解するために加えられる圧力に対して耐圧性であるとは、炭化ケイ素化合物試料７を分解するために圧力が加えられたときに、膨張又は軟化しにくく、形状を一定に保ち変形しないことを意図している。また、炭化ケイ素化合物試料７を分解するために加えられる熱に対して耐熱性であるとは、炭化ケイ素化合物試料７を分解するために加熱したとき、溶出又は軟化しにくく、形状を一定に保ち変形しないことを意図している。 Here, the pressure resistance against the pressure applied to decompose the silicon carbide compound sample 7 is difficult to expand or soften when pressure is applied to decompose the silicon carbide compound sample 7, It is intended to keep the shape constant and not deform. Further, heat resistance to heat applied to decompose the silicon carbide compound sample 7 means that when heated to decompose the silicon carbide compound sample 7, elution or softening is difficult and the shape is kept constant. It is intended not to deform.

　＜内筒部３＞
　外容器部１は、内筒部３と、その外側の外筒部２との２重壁構造である。内筒部３は、密閉空間に面し、分解液８に対して耐溶性である材料により形成されている。内筒部３は、密閉空間に分解液８が収容されたとき、分解液８に直接接触するため、分解液８に対して耐溶性である材料により形成される。分解液８に対して耐溶性である材料とは、分解液８に対して金属成分の溶出が少ない材料を意図しており、分解液８に対して金属成分が溶出しない材料であることがより好ましい。 <Inner cylinder part 3>
The outer container part 1 has a double wall structure of an inner cylinder part 3 and an outer cylinder part 2 outside thereof. The inner cylinder portion 3 faces the sealed space and is formed of a material that is resistant to the decomposition solution 8. The inner cylinder portion 3 is formed of a material that is resistant to the decomposition solution 8 because the decomposition solution 8 is in direct contact with the decomposition solution 8 when the decomposition solution 8 is accommodated in the sealed space. The material that is resistant to the decomposition solution 8 is intended to be a material that does not elute metal components from the decomposition solution 8, and is more preferably a material that does not elute metal components from the decomposition solution 8. preferable.

　分解液８に対して耐溶性である材料として、例えば、フッ素樹脂、白金、又はセラミックス材料が挙げられる。フッ素樹脂として、例えば、ＰＴＦＥ＝ポリテトラフルオロエチレン（４フッ化）、ＰＦＡ＝テトラフルオロエチレン・パーフルオロアルキルビニルエーテル共重合体、ＰＶＤＦ＝ポリビニリデンフルオライド（２フッ化）、ＰＣＴＦＥ＝ポリクロロトリフルオロエチレン（３フッ化）等が挙げられる。セラミックス材料として、例えば、アルミナ、ジルコニア、カルシア、マグネシア、イットリア等が挙げられる。 Examples of the material that is resistant to the decomposition solution 8 include a fluororesin, platinum, or a ceramic material. For example, PTFE = polytetrafluoroethylene (tetrafluoride), PFA = tetrafluoroethylene / perfluoroalkyl vinyl ether copolymer, PVDF = polyvinylidene fluoride (difluoride), PCTFE = polychlorotrifluoro Ethylene (trifluoride) etc. are mentioned. Examples of the ceramic material include alumina, zirconia, calcia, magnesia, yttria and the like.

　内筒部３の形状は特に限定されず、内側に密閉空間が存在し、当該密閉空間内に支持部４が設置され、炭化ケイ素化合物試料７及び分解液８が収容可能であればよい。内筒部３は、下部と蓋部との２つの部材に分割されており、下部に支持部４を設置し、分解液８を収容し、これを上から塞ぐように蓋部を載せて密閉してもよい。内筒部３の下壁、側壁、及び上壁の厚みは、収容される分解液８の流出を防ぎ、内側の空間を密閉することが可能な厚みであれば特に限定されない。 The shape of the inner cylinder part 3 is not particularly limited as long as the sealed space exists inside, the support part 4 is installed in the sealed space, and the silicon carbide compound sample 7 and the decomposition solution 8 can be accommodated. The inner cylinder portion 3 is divided into two members, a lower portion and a lid portion. A support portion 4 is installed in the lower portion, the decomposition solution 8 is accommodated, and the lid portion is placed and sealed so as to close it from above. May be. The thickness of the lower wall, the side wall, and the upper wall of the inner cylinder part 3 is not particularly limited as long as it is a thickness capable of preventing the stored decomposition solution 8 from flowing out and sealing the inner space.

　＜外筒部２＞
　外筒部２は、内筒部３の外側に位置し、内筒部３を包みこむように設けられている。そして、外筒部２は、炭化ケイ素化合物試料７を溶解させるための圧力に対して耐圧性である。したがって、内部に収容した炭化ケイ素化合物試料７を分解するために、加熱して圧力が加えられ、内筒部３が変形したとしても、外筒部２が耐圧性を有しているため、外容器部１全体の変形を防ぐことができる。また、外筒部２は、炭化ケイ素化合物試料７を溶解させるために加えられる熱に対して耐熱性であることが好ましい。これにより、外容器部１の熱による変形を防ぐことができる。 <Outer cylinder part 2>
The outer cylinder part 2 is located outside the inner cylinder part 3 and is provided so as to wrap around the inner cylinder part 3. And the outer cylinder part 2 is pressure-resistant with respect to the pressure for melt | dissolving the silicon carbide compound sample 7. FIG. Therefore, in order to decompose the silicon carbide compound sample 7 accommodated in the inside, even if pressure is applied by heating and the inner cylinder part 3 is deformed, the outer cylinder part 2 has pressure resistance. Deformation of the entire container unit 1 can be prevented. Moreover, it is preferable that the outer cylinder part 2 is heat resistant with respect to the heat applied in order to dissolve the silicon carbide compound sample 7. FIG. Thereby, the deformation | transformation by the heat | fever of the outer container part 1 can be prevented.

　外筒部２は、炭化ケイ素化合物試料７を溶解させるための圧力及び熱に対して耐圧性及び耐熱性であればよく、例えば、ステンレススチールにより形成される。外筒部２は、少なくとも加圧及び加熱時に内筒部３を包み込むように設けられていればよい。すなわち、外筒部２は、下部と蓋部との２つの部材に分割されており、下部に内筒部３を収容し、これを上から塞ぐように蓋部を載せて密閉し、加圧及び加熱に供してもよい。外筒部２の下壁、側壁、及び上壁の厚みは、所望の耐圧性及び耐熱性が得られる厚みであれば特に限定されない。 The outer cylinder portion 2 only needs to have pressure resistance and heat resistance against the pressure and heat for dissolving the silicon carbide compound sample 7, and is formed of, for example, stainless steel. The outer cylinder part 2 should just be provided so that the inner cylinder part 3 may be wrapped at least at the time of pressurization and heating. That is, the outer cylinder part 2 is divided into two members, a lower part and a lid part. The inner cylinder part 3 is accommodated in the lower part, and the lid part is placed and sealed so as to close it from above. And may be subjected to heating. The thickness of the lower wall, the side wall, and the upper wall of the outer cylinder part 2 is not particularly limited as long as desired pressure resistance and heat resistance can be obtained.

　外容器部１においては、内筒部３が、分解液８が収容される密閉空間に面し、外筒部２と分解液８とが接触しないようになっているので、外筒部２に由来する金属不純物が分解液８に溶け出し、コンタミネーションが発生するのを防ぎ、分解液８への金属の溶出を抑えることができる。なお、内筒部３をさらに２層構造にし、より確実に外筒部２に由来する金属不純物が分解液８に溶け出すのを防いでもよい。 In the outer container part 1, the inner cylinder part 3 faces the sealed space in which the decomposition liquid 8 is accommodated, and the outer cylinder part 2 and the decomposition liquid 8 are not in contact with each other. It is possible to prevent the derived metal impurities from being dissolved into the decomposition solution 8 and causing contamination, and to suppress the elution of the metal into the decomposition solution 8. In addition, the inner cylinder part 3 may be further made into a two-layer structure to prevent the metal impurities derived from the outer cylinder part 2 from dissolving into the decomposition solution 8 more reliably.

　（内容器６）
　内容器６は、分解液８に対して耐溶性である材料により形成されており、上部が開放された柱状の容器である。炭化ケイ素化合物試料７は上部の開放部分から内容器６内に収容される。内容器６は、その内壁に分解液８が接触しないように、外容器部１内に設けられている。内容器６は、分解液８が気化した分解液ガス中に曝されるので、分解液８に対して金属成分の溶出が少ない、又は分解液８に対して金属成分が溶出しない材料により形成されている必要がある。 (Inner container 6)
The inner container 6 is formed of a material that is resistant to the decomposition solution 8 and is a columnar container having an open top. The silicon carbide compound sample 7 is accommodated in the inner container 6 from the upper open part. The inner container 6 is provided in the outer container part 1 so that the decomposition solution 8 does not contact the inner wall. Since the inner container 6 is exposed to the decomposition liquid gas in which the decomposition liquid 8 is vaporized, the inner container 6 is formed of a material that does not elute the metal component with respect to the decomposition liquid 8. Need to be.

　内容器６を構成する、分解液８に対して耐溶性である材料として、例えば、フッ素樹脂、白金、又はセラミックス材料が挙げられる。フッ素樹脂として、例えば、ＰＴＦＥ＝ポリテトラフルオロエチレン（４フッ化）、ＰＦＡ＝テトラフルオロエチレン・パーフルオロアルキルビニルエーテル共重合体、ＰＶＤＦ＝ポリビニリデンフルオライド（２フッ化）、ＰＣＴＦＥ＝ポリクロロトリフルオロエチレン（３フッ化）等が挙げられる。セラミックス材料として、例えば、アルミナ、ジルコニア、カルシア、マグネシア、イットリア等が挙げられる。 Examples of the material that is resistant to the decomposition solution 8 constituting the inner container 6 include a fluororesin, platinum, or a ceramic material. For example, PTFE = polytetrafluoroethylene (tetrafluoride), PFA = tetrafluoroethylene / perfluoroalkyl vinyl ether copolymer, PVDF = polyvinylidene fluoride (difluoride), PCTFE = polychlorotrifluoro Ethylene (trifluoride) etc. are mentioned. Examples of the ceramic material include alumina, zirconia, calcia, magnesia, yttria and the like.

　内容器６は、例えば、内容器６をテーブル５上に載置して、分解液８の液面よりも上側に位置するテーブル５の下側に分解液８が収容されてもよいし、内容器６と、分解液が収容された分解液容器（図示せず）とを、テーブル５上に隣接して載置してもよく、さらに、内容器６をテーブル５の下側に載置し、分解液が収容された分解液容器（図示せず）をテーブルの上側に載置してもよい。つまり、内容器６は、その内壁に分解液８が接触せず、分解液８が気化した分解液ガスに内容器６内の炭化ケイ素化合物試料７が曝されるようになっていればよい。なお、分解液容器（図示せず）としては、分解液に対して耐溶性である材料により形成されており、開放された上部から分解液が収容されるものを用いることができる。 For example, the inner container 6 may be placed on the table 5, and the decomposition solution 8 may be stored below the table 5 positioned above the liquid surface of the decomposition solution 8. The container 6 and a decomposition liquid container (not shown) containing the decomposition liquid may be placed adjacent to the table 5, and the inner container 6 is placed under the table 5. A decomposition solution container (not shown) containing the decomposition solution may be placed on the upper side of the table. That is, the inner container 6 may be configured such that the decomposition liquid 8 does not contact the inner wall of the inner container 6 and the silicon carbide compound sample 7 in the inner container 6 is exposed to the decomposition liquid gas vaporized from the decomposition liquid 8. In addition, as a decomposition liquid container (not shown), it is formed of a material that is resistant to the decomposition liquid, and a container in which the decomposition liquid is accommodated from an opened upper portion can be used.

　内容器６は、テーブル５上に複数載置されてもよく、これにより、複数の炭化ケイ素化合物試料７を同時に分解することが可能である。内容器６の大きさは、収容された炭化ケイ素化合物試料７が、分解液８が気化した分解液ガスに十分に曝されるような大きさであれば特に限定されない。 A plurality of inner containers 6 may be placed on the table 5, whereby a plurality of silicon carbide compound samples 7 can be decomposed simultaneously. The size of the inner container 6 is not particularly limited as long as the contained silicon carbide compound sample 7 is sufficiently exposed to the decomposition liquid gas from which the decomposition liquid 8 is vaporized.

　（支持部４）
　支持部４は、外容器部１内に設けられている。支持部４は、外容器部１内部の底面から突出するように設けられたスタンドと、スタンドの上部に設けられたテーブル５とを備えている。また、テーブル５は、外容器部１の側壁（内筒部３の側壁）の少なくとも２箇所から突出するように設けられた支持ピン（図示せず）により下から支えられるように設けられていてもよい。この場合、テーブル５と支持ピンとにより支持部４が構成される。 (Supporting part 4)
The support part 4 is provided in the outer container part 1. The support portion 4 includes a stand provided so as to protrude from the bottom surface inside the outer container portion 1 and a table 5 provided on the top of the stand. The table 5 is provided so as to be supported from below by support pins (not shown) provided so as to protrude from at least two positions of the side wall of the outer container part 1 (side wall of the inner cylinder part 3). Also good. In this case, the support part 4 is comprised by the table 5 and the support pin.

　テーブル５は、スタンド又は支持ピンと一体形成されていてもよいし、別々に形成され、使用前に組み立てられてもよい。支持部４は、スタンドの高さを変更可能に構成されていてもよい。支持部４は、分解液８に対して耐溶性の材料により形成されていることが好ましい。 The table 5 may be formed integrally with a stand or a support pin, or may be formed separately and assembled before use. The support unit 4 may be configured to be able to change the height of the stand. The support portion 4 is preferably made of a material resistant to the decomposition solution 8.

　＜テーブル５＞
　テーブル５上には、炭化ケイ素化合物試料７を収容した内容器６が載置される。テーブル５の径は、内筒部３の内径と同一であり、内筒部３の側壁に接触するように設けられている。また、テーブル５は、分解液ガスを通過するための孔が設けられた多孔体である。したがって、テーブル５に設けられた孔が、その下方に収容される分解液８が気化した分解液ガスの流路となり、分解液ガスが炭化ケイ素化合物試料７まで到達するようになっている。なお、テーブル５の内径を内筒部３の内径よりも小さくし、テーブル５と内筒部３の内壁との間に隙間ができるようにしてもよい。この場合、その隙間から分解液ガスが流れ込み、炭化ケイ素化合物試料７まで到達するので、テーブル５に孔が設けられていなくてもよい。 <Table 5>
On the table 5, the inner container 6 containing the silicon carbide compound sample 7 is placed. The diameter of the table 5 is the same as the inner diameter of the inner cylinder part 3, and is provided so as to contact the side wall of the inner cylinder part 3. The table 5 is a porous body provided with holes for allowing the cracked liquid gas to pass therethrough. Therefore, the hole provided in the table 5 becomes a flow path of the decomposition liquid gas in which the decomposition liquid 8 accommodated below is vaporized, and the decomposition liquid gas reaches the silicon carbide compound sample 7. The inner diameter of the table 5 may be smaller than the inner diameter of the inner cylinder portion 3 so that a gap is formed between the table 5 and the inner wall of the inner cylinder portion 3. In this case, since the decomposition gas flows from the gap and reaches the silicon carbide compound sample 7, the table 5 does not have to be provided with holes.

　以上のように、容器１０を用いれば、分解液８を収容する耐圧性の外容器部１内に設けられた内容器６内に炭化ケイ素化合物試料７を収容し、外容器部１内を加熱して加圧することによって、分解液８が気化した分解液ガスにより炭化ケイ素化合物試料７が気相分解される。したがって、分解液８中に含まれる金属不純物や、外容器部１の内壁（内筒部３の内壁）及び内容器６の内壁に付着した金属不純物が、炭化ケイ素化合物試料７を分解して得られた測定試料中に混入するのを防ぐことができる。その結果、容器１０を用いて炭化ケイ素化合物試料７を分解すれば、炭化ケイ素化合物試料７中に含まれる微量な金属をより正確に検出するような分析に供することができる。 As described above, when the container 10 is used, the silicon carbide compound sample 7 is accommodated in the inner container 6 provided in the pressure-resistant outer container part 1 that accommodates the decomposition solution 8, and the inside of the outer container part 1 is heated. By applying pressure, the silicon carbide compound sample 7 is vapor-phase decomposed by the decomposition liquid gas obtained by vaporizing the decomposition liquid 8. Therefore, the metal impurities contained in the decomposition solution 8 and the metal impurities adhering to the inner wall of the outer container part 1 (inner wall of the inner cylinder part 3) and the inner wall of the inner container 6 are obtained by decomposing the silicon carbide compound sample 7. It can prevent mixing in the measured sample. As a result, if the silicon carbide compound sample 7 is decomposed using the container 10, it can be subjected to an analysis that more accurately detects a trace amount of metal contained in the silicon carbide compound sample 7.

　炭素原子からなる化合物試料は、硫酸、硝酸及び過塩素酸の混酸等の分解液を用いて大気圧下においても分解できることが知られている（例えば、参考文献１（「湿式酸化分解：クルクミン吸光光度法による黒鉛中ホウ素の定量」、渡部和男等、分析化学、44(11)、939-942、1995）を参照のこと）。一方、炭化ケイ素化合物試料７は、同様の分解液を用いても大気圧下では分解しない。すなわち、容器１０を用いれば、炭素原子からなる化合物試料よりも難分解性の炭化ケイ素化合物試料７を分解することができるため、容器１０を用いて炭素原子からなる化合物試料を分解できることは明らかである。 It is known that a compound sample composed of carbon atoms can be decomposed even under atmospheric pressure using a decomposition solution such as a mixed acid of sulfuric acid, nitric acid and perchloric acid (for example, Reference 1 (“Wet oxidative decomposition: curcumin absorption Quantitative determination of boron in graphite by photometric method ", Kazuo Watanabe et al., Analytical Chemistry, 44 (11), 939-942, 1995)). On the other hand, the silicon carbide compound sample 7 is not decomposed under atmospheric pressure even when a similar decomposition solution is used. That is, if the container 10 is used, the silicon carbide compound sample 7 which is harder to decompose than the compound sample made of carbon atoms can be decomposed. Therefore, it is clear that the compound sample made of carbon atoms can be decomposed using the container 10. is there.

　なお、炭化ケイ素化合物試料７を分解する分解液８の種類、量等、炭化ケイ素化合物試料７を分解するために外容器部１に加えられる圧力及び熱、加圧及び加熱時間等の詳細については、後述する。 For details such as the type and amount of the decomposition liquid 8 for decomposing the silicon carbide compound sample 7, the pressure and heat applied to the outer container part 1 for decomposing the silicon carbide compound sample 7, the pressurization and heating time, etc. This will be described later.

　〔炭素原子からなる化合物試料又は炭化ケイ素化合物試料の気相分解方法〕
　本発明に係る気相分解方法は、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解する方法であって、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を、当該試料を分解する分解液が気化した分解液ガスにより分解する分解工程を包含することを特徴としている。本発明によれば、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を気相分解するので、分解液中に含まれる金属不純物が、当該試料を分解して得られた測定試料中に混入するのを防ぐことができる。 [Method of vapor phase decomposition of a compound sample comprising carbon atoms or a silicon carbide compound sample]
The gas phase decomposition method according to the present invention is a method for decomposing a compound sample or silicon carbide compound sample comprising carbon atoms, wherein a decomposition solution for decomposing the sample or carbon carbide compound sample comprising carbon atoms is provided. It includes a decomposition step of decomposing by the vaporized decomposition gas. According to the present invention, since a compound sample comprising silicon atoms or a silicon carbide compound sample is vapor-phase decomposed, metal impurities contained in the decomposition solution are mixed into a measurement sample obtained by decomposing the sample. Can be prevented.

　また、本発明に係る気相分解方法は、上記分解工程の前に、上述した容器１０の上記外容器部１内に、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解する分解液を収容し、テーブル５上に炭素原子からなる化合物試料又は炭化ケイ素化合物試料を載置する準備工程を包含し、上記分解工程において、上記試料と上記分解液とが収容された上記外容器部１内を加圧及び加熱することが好ましい。 Further, in the vapor phase decomposition method according to the present invention, a decomposition solution for decomposing a compound sample composed of carbon atoms or a silicon carbide compound sample is accommodated in the outer container portion 1 of the container 10 described above before the decomposition step. And a preparatory step of placing a carbon atom compound sample or a silicon carbide compound sample on the table 5, and in the decomposition step, the inside of the outer container part 1 in which the sample and the decomposition solution are accommodated. It is preferable to pressurize and heat.

　すなわち、上述した容器１０は、本発明に係る気相分解方法において用いられる容器の一実施形態である。したがって、本発明に係る気相分解方法において用いられる容器の説明は、上述した容器１０の説明に準じる。なお、本実施形態においては、炭化ケイ素化合物試料を用いる場合を例として説明する。 That is, the container 10 described above is an embodiment of a container used in the vapor phase decomposition method according to the present invention. Therefore, the description of the container used in the vapor phase decomposition method according to the present invention conforms to the description of the container 10 described above. In the present embodiment, a case where a silicon carbide compound sample is used will be described as an example.

　（準備工程）
　準備工程において、まず、容器１０の外容器部１内に、炭化ケイ素化合物試料を分解する分解液を収容し、内容器６内に炭化ケイ素化合物試料を収容する。分解液は、内容器６の内壁に触れないように収容される。このとき、外容器部１の容積を１００％としたとき、分解液を、外容器部１の容積の５～４０％の量になるように収容すれば、効率よく炭化ケイ素化合物試料を分解することができるので、好ましい。 (Preparation process)
In the preparation step, first, a decomposition solution for decomposing the silicon carbide compound sample is stored in the outer container portion 1 of the container 10, and the silicon carbide compound sample is stored in the inner container 6. The decomposition liquid is accommodated so as not to touch the inner wall of the inner container 6. At this time, when the volume of the outer container portion 1 is 100%, the silicon carbide compound sample is efficiently decomposed if the decomposition solution is accommodated in an amount of 5 to 40% of the volume of the outer container portion 1. This is preferable.

　また、外容器部１内に収容される分解液の量は、炭化ケイ素化合物試料を十分に分解することが可能な量であり得る。したがって、例えば、分解する炭化ケイ素化合物試料１ｇ当たり２～２０mlの分解液を収容してもよい。 Further, the amount of the decomposition solution accommodated in the outer container portion 1 may be an amount capable of sufficiently decomposing the silicon carbide compound sample. Therefore, for example, 2 to 20 ml of decomposition solution may be accommodated per 1 g of the silicon carbide compound sample to be decomposed.

　炭化ケイ素化合物試料を分解する分解液としては、フッ化水素酸、硝酸、塩酸、硫酸、リン酸、過酸化水素水、及び過塩素酸からなる群より選択される少なくとも１つの酸を含む酸溶液を用いることができ、好ましくは、フッ化水素酸と硝酸との混酸溶液である。 An acid solution containing at least one acid selected from the group consisting of hydrofluoric acid, nitric acid, hydrochloric acid, sulfuric acid, phosphoric acid, hydrogen peroxide, and perchloric acid is used as a decomposition solution for decomposing the silicon carbide compound sample. Preferably, it is a mixed acid solution of hydrofluoric acid and nitric acid.

　炭化ケイ素化合物試料は、内容器６に入れてテーブル５上に載置すればよい。炭化ケイ素化合物試料はバルクであっても、薄膜であってもよい。炭化ケイ素化合物試料と分解液とを外容器部１内に収容した後、外容器部１を密閉する。 The silicon carbide compound sample may be placed in the inner container 6 and placed on the table 5. The silicon carbide compound sample may be a bulk or a thin film. After accommodating the silicon carbide compound sample and the decomposition solution in the outer container part 1, the outer container part 1 is sealed.

　（分解工程）
　分解工程において、炭化ケイ素化合物試料と分解液とが収容され、密閉された外容器部１内を加熱することによって加圧する。外容器部１内の加圧及び加熱は、従来公知の方法により好適に行うことができる。 (Disassembly process)
In the decomposition step, the silicon carbide compound sample and the decomposition solution are accommodated and pressurized by heating the inside of the sealed outer container part 1. The pressurization and heating in the outer container part 1 can be suitably performed by a conventionally known method.

　外容器部１の加熱温度は、後述する所望の加圧が可能であり、分解液を気化させる温度であればよく、１００～２４０℃であることが好ましく、１５０～２４０℃であることがより好ましく、１８０～２４０℃であることが最も好ましい。また、外容器部１の加熱時間は、炭化ケイ素化合物試料１ｇ当たり１～９６時間であることが好ましく、１～４８時間であることがより好ましく、５～４８時間であることが最も好ましい。 The heating temperature of the outer container part 1 may be any desired pressurization that will be described later and may be any temperature that vaporizes the decomposition solution, preferably 100 to 240 ° C, more preferably 150 to 240 ° C. Preferably, the temperature is from 180 to 240 ° C. The heating time of the outer container part 1 is preferably 1 to 96 hours, more preferably 1 to 48 hours, and most preferably 5 to 48 hours per 1 g of the silicon carbide compound sample.

　上述した温度で加熱することによって外容器部１内に加わる圧力は、気化した分解液により炭化ケイ素化合物試料が分解可能な圧力であり、１～１５ＭＰａであることが好ましく、５～１５ＭＰａであることがより好ましく、７～１５ＭＰａであることが最も好ましい。 The pressure applied to the outer container part 1 by heating at the above-described temperature is a pressure at which the silicon carbide compound sample can be decomposed by the vaporized decomposition solution, preferably 1 to 15 MPa, and preferably 5 to 15 MPa. Is more preferable, and 7 to 15 MPa is most preferable.

　外容器部１の加熱時には、外容器部１全体を加熱することが好ましい。また、特に外容器部１の上部に熱を加えれば、外容器部１内の上壁（内筒部３の上壁）に凝集した液滴が炭化ケイ素化合物試料上に落下して、コンタミネーションが発生するのを防ぐことができる。 When heating the outer container part 1, it is preferable to heat the entire outer container part 1. In particular, if heat is applied to the upper part of the outer container part 1, droplets aggregated on the upper wall in the outer container part 1 (upper wall of the inner cylinder part 3) fall on the silicon carbide compound sample and are contaminated. Can be prevented.

　このように、炭化ケイ素化合物試料及び分解液が収容された外容器部１内を加熱して加圧することによって、分解液が気化した分解液ガスにより炭化ケイ素化合物試料が気相分解される。したがって、分解液中に含まれる金属不純物や、外容器部１の内壁（内筒部３の内壁）及び内容器６の内壁に付着した金属不純物が、炭化ケイ素化合物試料を分解して得られた測定試料中に混入するのを防ぐことができる。その結果、炭化ケイ素化合物試料中に含まれる微量な金属をより正確に検出するような分析に供することができる。 Thus, by heating and pressurizing the inside of the outer container 1 in which the silicon carbide compound sample and the decomposition solution are stored, the silicon carbide compound sample is decomposed in the gas phase by the decomposition solution gas from which the decomposition solution is vaporized. Therefore, metal impurities contained in the decomposition solution and metal impurities attached to the inner wall of the outer container part 1 (inner wall of the inner cylinder part 3) and the inner wall of the inner container 6 were obtained by decomposing the silicon carbide compound sample. Mixing in the measurement sample can be prevented. As a result, it can be subjected to an analysis that more accurately detects a trace amount of metal contained in a silicon carbide compound sample.

　〔炭素原子からなる化合物試料又は炭化ケイ素化合物試料の分析方法〕
　本発明に係る炭素原子からなる化合物試料又は炭化ケイ素化合物試料の分析方法は、上述した気相分解方法により、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解して得られた測定試料中の金属不純物を検出する工程を包含することを特徴としている。 [Analyzing Method of Compound Sample Containing Carbon Atom or Silicon Carbide Compound Sample]
The method for analyzing a compound sample comprising silicon atoms or a silicon carbide compound sample according to the present invention is the method of analyzing a compound sample comprising silicon atoms or a silicon carbide compound sample obtained by decomposing the compound sample comprising silicon atoms or the silicon carbide compound sample. The method includes a step of detecting a metal impurity.

　炭素原子からなる化合物試料又は炭化ケイ素化合物試料は、分解液ガスにより気相分解されて昇華するため、当該試料が収容されていた内容器６内には、試料中に含まれていた金属不純物が残存する。本実施形態においては、残存した金属不純物を測定試料として、検出の対象とする。 Since a compound sample or a silicon carbide compound sample made of carbon atoms is vapor-phase decomposed by a decomposition liquid gas and sublimates, the metal impurities contained in the sample are contained in the inner container 6 in which the sample is accommodated. Remains. In the present embodiment, the remaining metal impurities are used as detection targets using the measurement sample.

　内容器６内に残存した金属不純物は、回収液を用いて回収すればよい。回収液としては、従来公知の溶液を使用可能であり、特に限定されないが、例えば、硝酸、又は硝酸と塩酸との混酸を用いることができる。内容器６内に回収液を滴下し、内容器６の内壁に付着した金属不純物を溶解させて回収する。このとき、内容器６内に回収液を滴下し、さらに加熱することによって、金属不純物を回収してもよい。回収した金属不純物は、回収液によりさらに液調整して測定に供してもよい。 The metal impurities remaining in the inner container 6 may be recovered using a recovery liquid. A conventionally known solution can be used as the recovery solution, and is not particularly limited. For example, nitric acid or a mixed acid of nitric acid and hydrochloric acid can be used. The recovered liquid is dropped into the inner container 6 to dissolve and recover the metal impurities attached to the inner wall of the inner container 6. At this time, the metal impurities may be recovered by dropping the recovered liquid into the inner container 6 and further heating. The recovered metal impurities may be further adjusted with a recovery solution and used for measurement.

　回収した金属不純物を測定試料とし、従来公知の測定方法により元素分析する。測定試料を元素分析する方法として、例えば、誘導結合プラズマ質量分析法（ＩＣＰ－ＭＳ）、誘導結合プラズマ発光分光分析法（ＩＣＰ－ＡＥＳ）、原子吸光分析法（ＡＡＳ）等が挙げられる。 Using the collected metal impurities as a measurement sample, elemental analysis is performed by a conventionally known measurement method. Examples of the method for elemental analysis of the measurement sample include inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma emission spectroscopy (ICP-AES), and atomic absorption spectrometry (AAS).

　このように、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を気相分解して得られた測定試料を分析することによって、炭素原子からなる化合物試料又は炭化ケイ素化合物試料中に含まれる金属不純物をより正確に検出することができる。 Thus, by analyzing the measurement sample obtained by vapor-phase decomposition of the compound sample or silicon carbide compound sample consisting of carbon atoms, the metal impurities contained in the compound sample or silicon carbide compound sample consisting of carbon atoms are reduced. More accurate detection is possible.

　〔炭素原子からなる化合物試料又は炭化ケイ素化合物試料の気相分解装置〕
　本発明に係る炭素原子からなる化合物試料又は炭化ケイ素化合物試料の気相分解装置は、上述した容器と、上記容器を加熱する加熱手段とを備えたことを特徴としている。 [Gas phase decomposition apparatus for compound sample of carbon atom or silicon carbide compound sample]
A vapor phase decomposition apparatus for a compound sample comprising silicon atoms or a silicon carbide compound sample according to the present invention is characterized by comprising the container described above and a heating means for heating the container.

　すなわち、上述した気相分解方法において用いられる容器１０は、本発明に係る気相分解装置において用いられる容器の一実施形態である。したがって、本発明に係る気相分解装置の説明は、上述した気相分解方法の説明に準じる。なお、加熱手段としては、従来公知の加熱装置を用いることができる。 That is, the container 10 used in the above-described gas phase decomposition method is an embodiment of the container used in the gas phase decomposition apparatus according to the present invention. Therefore, the description of the vapor phase decomposition apparatus according to the present invention is based on the above description of the vapor phase decomposition method. In addition, a conventionally well-known heating apparatus can be used as a heating means.

　〔炭素原子からなる化合物試料又は炭化ケイ素化合物試料の分析装置〕
　本発明に係る炭素原子からなる化合物試料又は炭化ケイ素化合物試料の分析装置は、上述した容器と、上記容器内において炭素原子からなる化合物試料又は炭化ケイ素化合物試料を気相分解して得られた測定試料中の金属不純物を検出する検出手段とを備えたことを特徴としている。 [Analyzer for compound sample or silicon carbide compound sample comprising carbon atoms]
The analyzer for analyzing a compound sample or silicon carbide compound sample comprising carbon atoms according to the present invention comprises the above-described container and a measurement obtained by vapor phase decomposition of the compound sample or silicon carbide compound sample comprising carbon atoms in the container. And a detecting means for detecting metal impurities in the sample.

　すなわち、上述した分析方法において用いられる容器１０は、本発明に係る分析装置において用いられる容器の一実施形態である。したがって、本発明に係る分析装置の説明は、上述した分析方法の説明に準じる。なお、検出手段としては、従来公知の検出装置を用いることができ、例として、パーキンエルマー社製のＩＣＰ－ＭＳが挙げられる。 That is, the container 10 used in the analysis method described above is an embodiment of a container used in the analyzer according to the present invention. Therefore, the description of the analysis apparatus according to the present invention conforms to the description of the analysis method described above. As the detection means, a conventionally known detection device can be used, and an example is ICP-MS manufactured by PerkinElmer.

　〔炭素原子からなる化合物試料又は炭化ケイ素化合物試料の品質管理方法〕
　本発明に係る炭素原子からなる化合物試料又は炭化ケイ素化合物試料の品質管理方法は、上述したいずれかの気相分解方法により、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解して得られた測定試料中の金属不純物を検出する分析工程と、上記分析工程において検出された金属不純物の量が、予め定められた基準量以下である炭素原子からなる化合物試料又は炭化ケイ素化合物試料を抽出する抽出工程とを包含する。 [Quality Control Method for Compound Sample Containing Carbon Atom or Silicon Carbide Compound Sample]
The quality control method for a compound sample or silicon carbide compound sample comprising carbon atoms according to the present invention was obtained by decomposing a compound sample or silicon carbide compound sample comprising carbon atoms by any one of the vapor phase decomposition methods described above. An analysis step for detecting metal impurities in a measurement sample, and an extraction for extracting a compound sample or silicon carbide compound sample consisting of carbon atoms in which the amount of metal impurities detected in the analysis step is equal to or less than a predetermined reference amount Process.

　分析工程においては、本発明に係る気相分解方法により、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解して残存した金属元素を金属不純物として回収し、測定試料として、従来公知の測定方法により元素分析する。測定試料を元素分析する方法として、例えば、誘導結合プラズマ質量分析法（ＩＣＰ－ＭＳ）、誘導結合プラズマ発光分光分析法（ＩＣＰ－ＡＥＳ）、原子吸光分析法（ＡＡＳ）等が挙げられる。 In the analysis step, the metal element remaining by decomposing the compound sample or silicon carbide compound sample composed of carbon atoms by the gas phase decomposition method according to the present invention is recovered as a metal impurity, and a conventionally known measurement method is used as a measurement sample. Elemental analysis by Examples of the method for elemental analysis of the measurement sample include inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma emission spectroscopy (ICP-AES), and atomic absorption spectrometry (AAS).

　そして、抽出工程において、分析工程において検出された金属不純物の量が、予め定められた基準量以下である炭素原子からなる化合物試料又は炭化ケイ素化合物試料を抽出する。すなわち、分析工程において検出された金属不純物の量に基づいて炭素原子からなる化合物試料又は炭化ケイ素化合物試料を選別する。なお、抽出工程においては、分析工程において検出された金属不純物の種類に基づいて炭素原子からなる化合物試料又は炭化ケイ素化合物試料を選別してもよい。 In the extraction step, a compound sample or a silicon carbide compound sample consisting of carbon atoms in which the amount of metal impurities detected in the analysis step is equal to or less than a predetermined reference amount is extracted. That is, a compound sample or a silicon carbide compound sample consisting of carbon atoms is selected based on the amount of metal impurities detected in the analysis step. In the extraction step, a compound sample or a silicon carbide compound sample made of carbon atoms may be selected based on the type of metal impurity detected in the analysis step.

　このように、本発明に係る品質管理方法によれば、炭素原子からなる化合物試料又は炭化ケイ素化合物試料中に含まれる金属不純物を正確に検出することができるため、検出結果に基づいて炭素原子からなる化合物試料又は炭化ケイ素化合物試料を選別することにより、炭素原子からなる化合物試料又は炭化ケイ素化合物試料の品質を一定に保つことができる。したがって、本発明に係る品質管理方法は、より正確な品質管理が求められる、半導体の製造に用いられる炭素原子からなる化合物試料又は炭化ケイ素化合物試料の品質管理にも適している。 As described above, according to the quality control method of the present invention, the metal impurity contained in the compound sample or silicon carbide compound sample made of carbon atoms can be accurately detected. By selecting the compound sample or silicon carbide compound sample to be formed, the quality of the compound sample or silicon carbide compound sample comprising carbon atoms can be kept constant. Therefore, the quality control method according to the present invention is also suitable for quality control of a compound sample composed of carbon atoms or a silicon carbide compound sample used for semiconductor manufacturing, which requires more accurate quality control.

　本発明に係る容器は、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解するための容器であって、内部に上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解する分解液を収容する密閉空間を有し、上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解するための圧力に対して耐圧性である外容器部と、上記外容器部内に設けられ、上記分解液に対して耐溶性である材料により形成されており、開放された上部から上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料が収容される内容器とを備え、上記内容器は、上記分解液が上記外容器部に収容されたときに、その内壁に上記分解液が接触しないように設けられていることを特徴としている。 The container which concerns on this invention is a container for decomposing | disassembling the compound sample or silicon carbide compound sample which consists of carbon atoms, Comprising: The decomposition solution which decomposes | disassembles the compound sample or silicon carbide compound sample which consists of the said carbon atom is accommodated in an inside An outer container portion having a sealed space and being pressure resistant to a pressure for decomposing the compound sample or silicon carbide compound sample comprising the carbon atom, and provided in the outer container portion, An inner container that is formed of a material that is resistant to dissolution and contains a compound sample or a silicon carbide compound sample composed of the carbon atoms from the opened upper part, and the inner container is configured such that the decomposition liquid is the outer container. It is characterized in that it is provided so that the decomposition solution does not come into contact with the inner wall when housed in the part.

　また、本発明に係る容器において、上記外容器部は、上記密閉空間に面し、上記分解液に対して耐溶性である材料により形成された内筒部と、上記内筒部の外側に位置し、上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料を溶解させるための圧力に対して耐圧性である外筒部との二重壁構造であることが好ましい。 Further, in the container according to the present invention, the outer container portion faces the sealed space, and is located outside the inner tube portion and an inner tube portion formed of a material resistant to the decomposition solution. And it is preferable that it is a double wall structure with the outer cylinder part which is pressure-resistant with respect to the pressure for dissolving the compound sample or silicon carbide compound sample which consists of the said carbon atom.

　さらに、本発明に係る容器において、上記内容器は、上記外容器部内に上記分解液が収容されたとき、上記分解液の液面よりも上側に位置する載置台上に設けられていることが好ましい。 Furthermore, in the container according to the present invention, the inner container may be provided on a mounting table located above the liquid level of the decomposition liquid when the decomposition liquid is accommodated in the outer container portion. preferable.

　また、本発明に係る容器は、上記外容器部内に設けられ、上記分解液に対して耐溶性である材料により形成されており、開放された上部から上記分解液が収容される分解液容器をさらに備えていることが好ましい。 In addition, a container according to the present invention is a decomposition liquid container that is provided in the outer container part, is formed of a material that is resistant to the decomposition liquid, and contains the decomposition liquid from the opened upper part. Furthermore, it is preferable to provide.

　本発明に係る気相分解方法は、上述したいずれかの容器の上記外容器部内に、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解する分解液を収容し、上記載置台上に炭素原子からなる化合物試料又は炭化ケイ素化合物試料を載置する準備工程と、上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料と上記分解液とが収容された上記外容器部内を加熱することによって加圧し、上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料を、上記分解液が気化した分解液ガスにより分解する分解工程とを包含することを特徴としている。 In the gas phase decomposition method according to the present invention, a decomposition solution for decomposing a compound sample or a silicon carbide compound sample made of carbon atoms is accommodated in the outer container portion of any of the above-described containers, and carbon atoms are placed on the mounting table. A preparatory step for placing the compound sample or silicon carbide compound sample comprising, and pressurizing by heating the inside of the outer container portion containing the compound sample or silicon carbide compound sample comprising the carbon atom and the decomposition solution, A decomposition step of decomposing the compound sample composed of the carbon atom or the silicon carbide compound sample with a decomposition solution gas obtained by vaporizing the decomposition solution.

　さらに、本発明に係る気相分解方法は、上記分解工程において、上記外容器部内を１００～２４０℃で加熱することによって、１～１５ＭＰａで加圧することが好ましい。 Furthermore, in the vapor phase decomposition method according to the present invention, in the decomposition step, it is preferable to pressurize at 1 to 15 MPa by heating the inside of the outer container portion at 100 to 240 ° C.

　また、本発明に係る気相分解方法において、上記分解液は、フッ化水素酸、硝酸、塩酸、硫酸、リン酸、過酸化水素水、及び過塩素酸からなる群より選択される少なくとも１つの酸を含む酸溶液であることが好ましい。 In the vapor phase decomposition method according to the present invention, the decomposition solution is at least one selected from the group consisting of hydrofluoric acid, nitric acid, hydrochloric acid, sulfuric acid, phosphoric acid, hydrogen peroxide solution, and perchloric acid. An acid solution containing an acid is preferable.

　本発明に係る炭素原子からなる化合物試料又は炭化ケイ素化合物試料の分析方法は、上述したいずれかの気相分解方法により、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解して得られた測定試料中の金属不純物を検出する工程を包含することを特徴としている。 The method for analyzing a compound sample consisting of carbon atoms or a silicon carbide compound sample according to the present invention is a measurement obtained by decomposing a compound sample consisting of carbon atoms or a silicon carbide compound sample by any of the vapor phase decomposition methods described above. It includes a step of detecting metal impurities in the sample.

　本発明に係る炭素原子からなる化合物試料又は炭化ケイ素化合物試料の気相分解装置は、上述したいずれかの容器と、上記容器を加熱する加熱手段とを備えたことを特徴としている。 The vapor phase decomposition apparatus for a compound sample comprising silicon atoms or a silicon carbide compound sample according to the present invention is characterized by comprising any of the above-described containers and a heating means for heating the container.

　本発明に係る炭素原子からなる化合物試料又は炭化ケイ素化合物試料の分析装置は、上述したいずれかの容器と、上記容器内において炭素原子からなる化合物試料又は炭化ケイ素化合物試料を気相分解して得られた測定試料中の金属不純物を検出する検出手段とを備えたことを特徴としている。 The analyzer for analyzing a compound sample consisting of carbon atoms or a silicon carbide compound sample according to the present invention is obtained by vapor-phase decomposition of any of the above-described containers and a compound sample or silicon carbide compound sample consisting of carbon atoms in the container. And detecting means for detecting metal impurities in the measured sample.

　本発明に係る炭素原子からなる化合物試料又は炭化ケイ素化合物試料の品質管理方法は、上述したいずれかの気相分解方法により、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解して得られた測定試料中の金属不純物を検出する分析工程と、上記分析工程において検出された金属不純物の量が、予め定められた基準量以下である炭素原子からなる化合物試料又は炭化ケイ素化合物試料を抽出する抽出工程とを包含することを特徴としている。 The quality control method for a compound sample or silicon carbide compound sample comprising carbon atoms according to the present invention was obtained by decomposing a compound sample or silicon carbide compound sample comprising carbon atoms by any one of the vapor phase decomposition methods described above. An analysis step for detecting metal impurities in a measurement sample, and an extraction for extracting a compound sample or silicon carbide compound sample consisting of carbon atoms in which the amount of metal impurities detected in the analysis step is not more than a predetermined reference amount And a process.

　容器１０を用いた気相分解のブランク試験を行った。ブランク試験では、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を用いずに、容器１０を用いて気相分解と同様の処理を行うことによって、分解液に含まれる金属不純物及び外容器部１の内壁に付着した金属不純物が、測定試料にどれくらい混入するかを調べた。 A blank test of vapor phase decomposition using the container 10 was performed. In the blank test, by performing the same process as the vapor phase decomposition using the container 10 without using the compound sample consisting of carbon atoms or the silicon carbide compound sample, the metal impurities contained in the decomposition solution and the outer container part 1 The amount of metal impurities adhering to the inner wall mixed into the measurement sample was examined.

　分解液として４０％フッ化水素酸と６８％硝酸（１：１）との混酸溶液を用いた。内容器６内を空の状態にし、分解液が気化した分解液ガスに曝される状態にして、外容器部１内を、２００℃で５時間加熱することで、高温加圧条件とした。外筒部２としてＳＵＳ容器を用い、内筒部３としてＰＴＦＥ容器を用いた。ＰＴＦＥ製の内容器６を２つ（ＶＰＤ－１及びＶＰＤ－２）、テーブル５上に載置した。内容器６を取り出し、硝酸を滴下してそれぞれの内容器６内の金属不純物を回収し、測定試料とした。 As a decomposition solution, a mixed acid solution of 40% hydrofluoric acid and 68% nitric acid (1: 1) was used. The inner container 6 was evacuated and exposed to the vaporized decomposition gas, and the inside of the outer container 1 was heated at 200 ° C. for 5 hours to obtain high-temperature pressurization conditions. A SUS container was used as the outer cylinder part 2, and a PTFE container was used as the inner cylinder part 3. Two PTFE inner containers 6 (VPD-1 and VPD-2) were placed on the table 5. The inner container 6 was taken out and nitric acid was dropped to collect metal impurities in each inner container 6 to obtain a measurement sample.

　上記測定試料をＩＣＰ－ＭＳ(パーキンエルマー社製)により測定した。その結果、測定試料中に含まれる金属不純物量は、表１に示すとおりであった。なお、表１に記載した値は、ＩＣＰ－ＭＳにより測定した濃度（ｎｇ／ｇ）に、液調整した液量（ｇ）を乗じて算出した。 The measurement sample was measured by ICP-MS (manufactured by PerkinElmer). As a result, the amount of metal impurities contained in the measurement sample was as shown in Table 1. The values shown in Table 1 were calculated by multiplying the concentration (ng / g) measured by ICP-MS and the liquid amount (g) adjusted with the liquid.

Figure JPOXMLDOC01-appb-T000001
Ｎ．Ｄ．：未検出
Figure JPOXMLDOC01-appb-T000001
 N. D. : Not detected

　容器１０を用いて炭化ケイ素化合物試料（ＳｉＣ試料）を気相分解した。分解液として４０％フッ化水素酸と６８％硝酸（１：１）の混酸溶液を用いた。内容器６内に炭化ケイ素化合物試料を入れ、分解液が気化した分解液ガスに曝される状態にして、外容器部１内を、２００℃で５時間加熱することで、高温加圧条件とした。内容器６中の炭化ケイ素化合物試料は分解昇華されていた。 The silicon carbide compound sample (SiC sample) was vapor-phase decomposed using the container 10. A mixed acid solution of 40% hydrofluoric acid and 68% nitric acid (1: 1) was used as the decomposition solution. The silicon carbide compound sample is placed in the inner container 6 and exposed to the decomposed liquid gas in which the decomposed liquid is vaporized, and the inside of the outer container 1 is heated at 200 ° C. for 5 hours. did. The silicon carbide compound sample in the inner container 6 was decomposed and sublimated.

　容器１０を用いて炭化ケイ素の認証標準物質（ＣＲＭ　ＮＭＩＪ　８００１Ａ）を、気相分解した。分解液としては、４０％フッ化水素と６８％硝酸（１：１）との混酸溶液を用いた。２３０℃で９６時間加熱することで高温加圧条件とした。分解処理後内容器６を取り出し、硝酸を滴下して内容器６内の金属不純物を回収し、測定試料とした。 Using the container 10, a silicon carbide certified reference material (CRM NMIJ 8001A) was vapor-phase decomposed. As the decomposition solution, a mixed acid solution of 40% hydrogen fluoride and 68% nitric acid (1: 1) was used. High temperature pressurization conditions were obtained by heating at 230 ° C. for 96 hours. After the decomposition treatment, the inner container 6 was taken out and nitric acid was added dropwise to collect metal impurities in the inner container 6 to obtain a measurement sample.

　上記測定試料をＩＣＰ－ＭＳ（パーキンエルマー社製）により測定した。その結果、試料の測定値と認証値は、表２に示すとおりであった。なお、表２に記載した値は、ＩＣＰ－ＭＳにより測定した濃度（ｎｇ／ｇ）に、液調整した液量（ｇ）を乗じて、分解した試料量（ｇ）で除することで算出した。 The above measurement sample was measured by ICP-MS (manufactured by PerkinElmer). As a result, the measured values and certified values of the samples were as shown in Table 2. The values listed in Table 2 were calculated by multiplying the concentration (ng / g) measured by ICP-MS by the liquid amount (g) prepared by liquid adjustment and dividing by the decomposed sample amount (g). .

Figure JPOXMLDOC01-appb-T000002
　本発明は上述した各実施形態に限定されるものではなく、請求項に示した範囲で種々の変更が可能であり、異なる実施形態にそれぞれ開示された技術的手段を適宜組み合わせて得られる実施形態についても本発明の技術的範囲に含まれる。
Figure JPOXMLDOC01-appb-T000002
 The present invention is not limited to the above-described embodiments, and various modifications are possible within the scope shown in the claims, and embodiments obtained by appropriately combining technical means disclosed in different embodiments. Is also included in the technical scope of the present invention.

　本発明は、種々の分野に用いられる炭素原子からなる化合物試料又は炭化ケイ素化合物試料の金属不純物分析に利用することができる。 The present invention can be used for metal impurity analysis of compound samples composed of carbon atoms or silicon carbide compound samples used in various fields.

　１　外容器部
　２　外筒部
　３　内筒部
　４　支持部
　５　テーブル（載置台）
　６　内容器 DESCRIPTION OF SYMBOLS 1 Outer container part 2 Outer cylinder part 3 Inner cylinder part 4 Support part 5 Table (mounting table)
6 Inner container

Claims (11)

　炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解するための容器であって、
　内部に上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解する分解液を収容する密閉空間を有し、上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解するための圧力に対して耐圧性である外容器部と、
　上記外容器部内に設けられ、上記分解液に対して耐溶性である材料により形成されており、開放された上部から上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料が収容される内容器とを備え、
　上記内容器は、上記分解液が上記外容器部に収容されたときに、その内壁に上記分解液が接触しないように設けられていることを特徴とする容器。 A container for decomposing a compound sample comprising carbon atoms or a silicon carbide compound sample,
It has a sealed space for containing a decomposition solution for decomposing the compound sample or silicon carbide compound sample composed of the carbon atom, and is resistant to pressure for decomposing the compound sample or silicon carbide compound sample composed of the carbon atom. An outer container part that is sex,
An inner container that is provided in the outer container portion and is formed of a material that is resistant to the decomposition solution, and in which the compound sample composed of the carbon atoms or the silicon carbide compound sample is accommodated from the opened upper portion. Prepared,
The said inner container is provided so that the said decomposition liquid may not contact the inner wall, when the said decomposition liquid is accommodated in the said outer container part. 　上記外容器部は、
　　上記密閉空間に面し、上記分解液に対して耐溶性である材料により形成された内筒部と、
　　上記内筒部の外側に位置し、上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料を溶解させるための圧力に対して耐圧性である外筒部と
の二重壁構造であることを特徴とする請求項１に記載の容器。 The outer container part is
An inner cylinder portion that is formed of a material that faces the sealed space and is resistant to the decomposition solution;
It is located outside the inner cylinder part, and has a double wall structure with an outer cylinder part that is pressure resistant to the pressure for dissolving the compound sample or silicon carbide compound sample comprising the carbon atom. The container according to claim 1. 　上記内容器は、上記外容器部内に上記分解液が収容されたとき、上記分解液の液面よりも上側に位置する載置台上に設けられていることを特徴とする請求項１又は２に記載の容器。 The said inner container is provided on the mounting base located above the liquid level of the said decomposition liquid, when the said decomposition liquid is accommodated in the said outer container part, The Claim 1 or 2 characterized by the above-mentioned. Container as described. 　上記外容器部内に設けられ、上記分解液に対して耐溶性である材料により形成されており、開放された上部から上記分解液が収容される分解液容器をさらに備えていることを特徴とする請求項１～３のいずれか１項に記載の容器。 It is provided in the outer container part, is formed of a material that is resistant to the decomposition liquid, and further includes a decomposition liquid container that accommodates the decomposition liquid from an opened upper part. The container according to any one of claims 1 to 3. 　請求項１～４のいずれか１項に記載の容器の上記外容器部内に、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解する分解液を収容し、上記内容器内に炭素原子からなる化合物試料又は炭化ケイ素化合物試料を収容する準備工程と、
　上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料と上記分解液とが収容された上記外容器部内を加熱することによって加圧し、上記炭素原子からなる化合物試料又は炭化ケイ素化合物試料を、上記分解液が気化した分解液ガスにより分解する分解工程と
を包含することを特徴とする気相分解方法。 A decomposition solution for decomposing a compound sample comprising silicon atoms or a silicon carbide compound sample is accommodated in the outer container part of the container according to any one of claims 1 to 4, and comprising the carbon atoms in the inner container. A preparatory step for accommodating a compound sample or a silicon carbide compound sample;
Pressurization is performed by heating the inside of the outer container in which the compound sample or silicon carbide compound sample composed of the carbon atom and the decomposition solution are contained, and the compound sample or silicon carbide compound sample composed of the carbon atom is converted into the decomposition solution. A gas phase decomposition method comprising: a decomposition step of decomposing by vaporized decomposition gas. 　上記分解工程において、上記外容器部内を１００～２４０℃で加熱することによって、１～１５ＭＰａで加圧することを特徴とする請求項５に記載の気相分解方法。 6. The vapor phase decomposition method according to claim 5, wherein in the decomposition step, the inside of the outer container portion is heated at 100 to 240 ° C. so as to be pressurized at 1 to 15 MPa. 　上記分解液は、フッ化水素酸、硝酸、塩酸、硫酸、リン酸、過酸化水素水、及び過塩素酸からなる群より選択される少なくとも１つの酸を含む酸溶液であることを特徴とする請求項５又は６に記載の気相分解方法。 The decomposition solution is an acid solution containing at least one acid selected from the group consisting of hydrofluoric acid, nitric acid, hydrochloric acid, sulfuric acid, phosphoric acid, hydrogen peroxide solution, and perchloric acid. The vapor phase decomposition method according to claim 5 or 6. 　請求項５～７のいずれか１項に記載の気相分解方法により、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解して得られた測定試料中の金属不純物を検出する工程
を包含することを特徴とする炭素原子からなる化合物試料又は炭化ケイ素化合物試料の分析方法。 A method of detecting metal impurities in a measurement sample obtained by decomposing a compound sample comprising carbon atoms or a silicon carbide compound sample by the vapor phase decomposition method according to any one of claims 5 to 7. A method for analyzing a compound sample comprising silicon atoms or a silicon carbide compound sample. 　請求項１～４のいずれか１項に記載の容器と、
　上記容器を加熱する加熱手段とを備えたことを特徴とする炭素原子からなる化合物試料又は炭化ケイ素化合物試料の気相分解装置 A container according to any one of claims 1 to 4;
A vapor phase decomposition apparatus for a compound sample comprising carbon atoms or a silicon carbide compound sample, characterized by comprising heating means for heating the container 　請求項１～４のいずれか１項に記載の容器と、
　上記容器内において炭素原子からなる化合物試料又は炭化ケイ素化合物試料を気相分解して得られた測定試料中の金属不純物を検出する検出手段とを備えたことを特徴とする炭素原子からなる化合物試料又は炭化ケイ素化合物試料の分析装置。 A container according to any one of claims 1 to 4;
A compound sample comprising carbon atoms, comprising a detection means for detecting metal impurities in a measurement sample obtained by vapor phase decomposition of a compound sample comprising carbon atoms or a silicon carbide compound sample in the container. Alternatively, a silicon carbide compound sample analyzer. 　請求項５～７のいずれか１項に記載の気相分解方法により、炭素原子からなる化合物試料又は炭化ケイ素化合物試料を分解して得られた測定試料中の金属不純物を検出する分析工程と、
　上記分析工程において検出された金属不純物の量が、予め定められた基準量以下である炭素原子からなる化合物試料又は炭化ケイ素化合物試料を抽出する抽出工程と
を包含することを特徴とする炭素原子からなる化合物試料又は炭化ケイ素化合物試料の品質管理方法。 An analysis step for detecting metal impurities in a measurement sample obtained by decomposing a compound sample comprising carbon atoms or a silicon carbide compound sample by the vapor phase decomposition method according to any one of claims 5 to 7;
An extraction step of extracting a compound sample or a silicon carbide compound sample consisting of carbon atoms in which the amount of metal impurities detected in the analysis step is less than or equal to a predetermined reference amount. A method for quality control of a compound sample or a silicon carbide compound sample.
PCT/JP2012/081533 2011-12-06 2012-12-05 Container, vapor phase cracking method, vapor phase cracking device, analysis method, and analysis device Ceased WO2013084948A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1020147018491A KR20140105810A (en) 2011-12-06 2012-12-05 Container, vapor phase cracking method, vapor phase cracking device, analysis method, and analysis device

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2011267382 2011-12-06
JP2011-267382 2011-12-06

Publications (1)

Publication Number Publication Date
WO2013084948A1 true WO2013084948A1 (en) 2013-06-13

Family

ID=48574306

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2012/081533 Ceased WO2013084948A1 (en) 2011-12-06 2012-12-05 Container, vapor phase cracking method, vapor phase cracking device, analysis method, and analysis device

Country Status (4)

Country Link
JP (1) JPWO2013084948A1 (en)
KR (1) KR20140105810A (en)
TW (1) TW201335593A (en)
WO (1) WO2013084948A1 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104297044A (en) * 2014-11-07 2015-01-21 中山出入境检验检疫局 Acid gas treatment device of graphite digestion system
JP2017146123A (en) * 2016-02-15 2017-08-24 日鉄住金テクノロジー株式会社 Silicon quantitative analysis method

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61206845U (en) * 1985-06-18 1986-12-27
JPH0772056A (en) * 1993-06-25 1995-03-17 Shinetsu Quartz Prod Co Ltd Analytical method and disassembling / drying device for analysis
JPH07333121A (en) * 1994-06-10 1995-12-22 Toshiba Ceramics Co Ltd Processing method and apparatus for highly accurate analysis of impurities in siliconaceous analysis sample
JP2000292326A (en) * 1999-04-01 2000-10-20 Toshiba Ceramics Co Ltd Method for preparing sample for analyzing metal impurities contained in synthetic resin and method for measuring metal impurities using the same
JP2002040009A (en) * 2000-07-28 2002-02-06 Mitsubishi Materials Silicon Corp Micro impurity analytical method in silicon substrate
JP2002090271A (en) * 2000-09-13 2002-03-27 Horiba Ltd Analysis device for measuring constituent in sample

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61206845U (en) * 1985-06-18 1986-12-27
JPH0772056A (en) * 1993-06-25 1995-03-17 Shinetsu Quartz Prod Co Ltd Analytical method and disassembling / drying device for analysis
JPH07333121A (en) * 1994-06-10 1995-12-22 Toshiba Ceramics Co Ltd Processing method and apparatus for highly accurate analysis of impurities in siliconaceous analysis sample
JP2000292326A (en) * 1999-04-01 2000-10-20 Toshiba Ceramics Co Ltd Method for preparing sample for analyzing metal impurities contained in synthetic resin and method for measuring metal impurities using the same
JP2002040009A (en) * 2000-07-28 2002-02-06 Mitsubishi Materials Silicon Corp Micro impurity analytical method in silicon substrate
JP2002090271A (en) * 2000-09-13 2002-03-27 Horiba Ltd Analysis device for measuring constituent in sample

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"Fine Ceramics-yo Tanka Keiso Bifunmatsu no Kagaku Bunseki Hoho, Japanese Industrial Standard (JIS)", JIS R1616:2007, 2007 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104297044A (en) * 2014-11-07 2015-01-21 中山出入境检验检疫局 Acid gas treatment device of graphite digestion system
JP2017146123A (en) * 2016-02-15 2017-08-24 日鉄住金テクノロジー株式会社 Silicon quantitative analysis method

Also Published As

Publication number Publication date
JPWO2013084948A1 (en) 2015-04-27
TW201335593A (en) 2013-09-01
KR20140105810A (en) 2014-09-02

Similar Documents

Publication Publication Date Title
CN110186994A (en) The processing analysis method and processing unit of heavy metal in a kind of silicon wafer
JP3051023B2 (en) Processing method and apparatus for high-precision analysis of impurities in siliconaceous analysis sample
Bagot et al. 3D atom probe study of gas adsorption and reaction on alloy catalyst surfaces I: Instrumentation
US20190391126A1 (en) Method of Analyzing Resins Adhering to Crushed Polysilicon
WO2013084948A1 (en) Container, vapor phase cracking method, vapor phase cracking device, analysis method, and analysis device
JP5459053B2 (en) Impurity evaluation method of silicon single crystal
TW201527731A (en) Method for determining the concentration of metallic impurities in contaminated tantalum products
KR20170112992A (en) Method of determining a concentration of a material not dissolved by silicon etchants contaminating a product
JP6354563B2 (en) Method for manufacturing recovery instrument, method for recovering metal impurity, and method for analyzing metal impurity
JP6687518B2 (en) Analytical sample collection method and its use
JP6346098B2 (en) Vapor phase decomposition method, analysis method, quality control method, manufacturing method, and container
CN111485113B (en) Alkali metal impurity pretreatment device
Birch et al. Wettability techniques to monitor the cleanliness of surfaces
JP2002296269A (en) Apparatus and method for evaluating water quality of sample water
EP1571447A1 (en) Process for measuring mercury concentration within hydrocarbons
JPH0772056A (en) Analytical method and disassembling / drying device for analysis
JP4877897B2 (en) Method for removing impurities from silicon wafer and analysis method
JP2005326219A (en) Analysis sample preparing apparatus, analysis sample preparing method and semiconductor sample analysis method
Thurston Steam film sampling of water for mass spectrometric analysis of the deuterium content
JP2005109292A (en) Method and apparatus for recovering object to be measured around wafer
CN1867818A (en) Quartz product detection method and detection auxiliary device for semiconductor processing device
KR101730354B1 (en) Purification apparatus of hydrofluoric acid
TW201215872A (en) Permeability evaluation device and evaluation method
JP4760458B2 (en) Method for analyzing metal contamination of semiconductor wafer storage container
JP2010145150A (en) Tool for analyzing surface of plate-like body, and metal analysis method using the same

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 12855845

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2013548276

Country of ref document: JP

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

ENP Entry into the national phase

Ref document number: 20147018491

Country of ref document: KR

Kind code of ref document: A

122 Ep: pct application non-entry in european phase

Ref document number: 12855845

Country of ref document: EP

Kind code of ref document: A1