JPH0226179B2 - - Google Patents
Info
- Publication number
- JPH0226179B2 JPH0226179B2 JP94285A JP94285A JPH0226179B2 JP H0226179 B2 JPH0226179 B2 JP H0226179B2 JP 94285 A JP94285 A JP 94285A JP 94285 A JP94285 A JP 94285A JP H0226179 B2 JPH0226179 B2 JP H0226179B2
- Authority
- JP
- Japan
- Prior art keywords
- gaseous
- wavelength
- spectral line
- temperature
- light
- 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.)
- Expired
Links
- 238000000034 method Methods 0.000 claims description 17
- 230000003595 spectral effect Effects 0.000 claims description 11
- 238000000889 atomisation Methods 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 claims description 7
- 238000000862 absorption spectrum Methods 0.000 description 10
- 238000001514 detection method Methods 0.000 description 8
- 238000011002 quantification Methods 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 7
- 238000000137 annealing Methods 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000011896 sensitive detection Methods 0.000 description 3
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012806 monitoring device Methods 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 108091008695 photoreceptors Proteins 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/74—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using flameless atomising, e.g. graphite furnaces
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (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)
- Investigating Or Analysing Materials By Optical Means (AREA)
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はSeの検知定量方法及びモニターに関
し、特に従来の原子吸光分光分析法におけるより
低温にてガス状Seを検知・定量可能な方法及び
モニターに関する。本発明の方法及びモニター
は、Seを用いる半導体製品及び半導体製造装置、
廃棄物処理装置、例えば、ZnSe、CdSe等の化合
物半導体のエピ成長装置（CVD炉、LPE炉等）、
高圧HB炉、アニーリング炉、Se圧アニーリング
炉、MBE装置、MOCVD装置等に、或いは、Se
を含有する合金やセラミツクス・ガラス等の溶解
炉等におけるSeの検知・定量方法及び上記各装
置において、Seを定量検知し、Seの投入量コン
トロール、Se圧コントロールを現場で行えるモ
ニターとして利用して、多大の効果を奏する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for detecting and quantifying Se and monitoring, and particularly to a method and method capable of detecting and quantifying gaseous Se at a lower temperature than conventional atomic absorption spectrometry. Regarding monitors. The method and monitor of the present invention include semiconductor products and semiconductor manufacturing equipment using Se,
Waste treatment equipment, such as epitaxial growth equipment for compound semiconductors such as ZnSe and CdSe (CVD furnace, LPE furnace, etc.),
For high pressure HB furnaces, annealing furnaces, Se pressure annealing furnaces, MBE equipment, MOCVD equipment, etc., or Se
A method for detecting and quantifying Se in melting furnaces for alloys, ceramics, glasses, etc. containing , has great effects.
近時、産業上の各分野、例えば半導体、合金、
セラミツクス、ガラス等の製造において各種の
Seを含有する化合物が開発されるに伴い、Seの
高感度検知・定量が要求されるが、これに対して
は、従来、Seを2000℃以上の高温度にて原子化
させ、Se特有の原子吸光スペクトルを検知する
原子吸光分光分析法によつていた。Seの原子吸
光スペクトルは第５図〔出典：浜松ホトニクス(株)
カタログ〕に示されるように、波長19603nｍに
おいて鋭いピークを持つ。このピークを利用した
従来の原子吸光分光分析装置の一般的な構成は第
６図に示されるごとくであつて、光源部１からの
光は、試料原子化部２に入射され、原子化部２を
通過した光は、選光部（例えばモノクロメータ
ー）３を経由して４〜６の測光部に入り検知・定
量される。４は検知器、５は増幅器、６はメータ
ー部である。試料原子化部２においてSeを原子
化するためには2000℃以上の原子化温度とする必
要があり、一般的に簡便な方法として炎を用いて
いる。
Recently, various industrial fields such as semiconductors, alloys,
Various types of products are used in the production of ceramics, glass, etc.
As Se-containing compounds are developed, highly sensitive detection and quantification of Se is required. Conventionally, Se is atomized at a high temperature of 2000°C or higher, and Se-specific It was based on atomic absorption spectrometry, which detects the atomic absorption spectrum. The atomic absorption spectrum of Se is shown in Figure 5 [Source: Hamamatsu Photonics Co., Ltd.]
As shown in the catalog], it has a sharp peak at a wavelength of 19603 nm. The general configuration of a conventional atomic absorption spectrometer that utilizes this peak is as shown in FIG. The light that has passed through passes through a light selection section (for example, a monochromator) 3 and enters photometry sections 4 to 6 where it is detected and quantified. 4 is a detector, 5 is an amplifier, and 6 is a meter section. In order to atomize Se in the sample atomization section 2, it is necessary to set the atomization temperature to 2000° C. or higher, and flame is generally used as a simple method.
しかし、上記の原子吸光スペクトルを利用した
Seの検知法は、高温度（原子化温度）を必要と
するため、原子化温度以下でのSeの検知には不
適当であり、そのため原子化温度以下のガス状の
SeXに対してはその検知・定量法が存在しない
し、さらにその場（現場）での検知・定量法及び
モニターも存在していない。
However, using the above atomic absorption spectrum
Se detection methods require high temperatures (atomization temperature) and are therefore unsuitable for detecting Se at temperatures below the atomization temperature.
There is no detection/quantification method for SeX, and no on-site detection/quantification method or monitoring exists.
本発明の目的は、上記の現状に鑑み、従来不可
能であつた原子化温度以下でのSeの高感度検
知・定量を可能とする新規なSeの検知定量方法
及びモニターを提供することにある。 In view of the above-mentioned current situation, an object of the present invention is to provide a novel method and monitor for detecting and quantifying Se that enables highly sensitive detection and quantification of Se at temperatures below the atomization temperature, which was previously impossible. .
本発明は、此度本発明者らが研究途上発見し
た、ガス状Seの吸光スペクトルを利用して検知
定量するものである。
The present invention detects and quantifies using the absorption spectrum of gaseous Se, which the present inventors discovered during their research.
すなわち本発明はSeの原子化温度より低い温
度にて、ガス状Seに波長335nｍのスペクトル線
を入射し、上記ガス状Seによる上記入射スペク
トル線の吸収を測定し、光強度のピーク高さから
Seの検知・定量を行う方法である。さらに本発
明は炉またはヒーター付容器の光の進行方向に窓
部を設け、一方の窓部に波長335nｍのスペクト
ル線発光部、他方の窓にはヒーター付容器内のガ
ス状Seを通過した前記スペクトル線の光強度の
ピーク高さからSeを検知・定量する受光・測光
部を接続してなるSeモニターである。 That is, in the present invention, a spectral line with a wavelength of 335 nm is incident on gaseous Se at a temperature lower than the atomization temperature of Se, and the absorption of the incident spectral line by the gaseous Se is measured, and the peak height of the light intensity is determined from the peak height of the light intensity.
This is a method for detecting and quantifying Se. Furthermore, the present invention provides a window section in the direction of propagation of light in a furnace or a container with a heater, one window section has a spectral line emitting section with a wavelength of 335 nm, and the other window has a window section where the light emitting section has a spectral line emitting section with a wavelength of 335 nm. This is an Se monitor that is connected to a photoreceptor/photometer unit that detects and quantifies Se based on the peak height of the light intensity of spectral lines.
以下に本発明に到達した経緯と、本発明の方
法・モニターを具体的に説明する。 Below, the circumstances that led to the present invention and the method and monitor of the present invention will be specifically explained.
原子化温度以下、220℃〜695℃の温度範囲で
は、Seはガス状Seとなつており、Se2、Se4、Se6
等として存在していると考えられるが特定されて
はいない（O.Kubaschewski等著、
「Metallurgical Thermochemistry」）。 Below the atomization temperature, in the temperature range of 220°C to 695°C, Se becomes gaseous Se, and Se 2 , Se 4 , Se 6
etc., but it has not been identified (written by O. Kubaschewski et al.,
"Metallurgical Thermochemistry").
本発明者らは此度、このガス状Seについて、
第１図に示すような〜の合計16の吸光スペク
トルを新発見した。第１図の縦軸は吸光度（任意
単位）、横軸は波長（ｎｍ）をあらわす。〜
の番号を付した各ピークの波長は、順次次のとお
りである。 The present inventors have recently learned about this gaseous Se.
We discovered a total of 16 new absorption spectra as shown in Figure 1. The vertical axis in FIG. 1 represents absorbance (arbitrary units), and the horizontal axis represents wavelength (nm). ~
The wavelengths of the peaks numbered are as follows.
324nｍ、326nｍ、328nｍ、330nｍ、
332.5nｍ、335nｍ、337.5nｍ、340nｍ、
342nｍ、344.5nｍ、347nｍ、350nｍ、
352.5nｍ、355nｍ、357.5nｍ、360nｍ。第
１図の吸光スペクトルでは、第６番目の波長
335nｍにおけるピークが一番吸光度が大きい。 324nm, 326nm, 328nm, 330nm,
332.5nm, 335nm, 337.5nm, 340nm,
342nm, 344.5nm, 347nm, 350nm,
352.5nm, 355nm, 357.5nm, 360nm. In the absorption spectrum shown in Figure 1, the 6th wavelength
The peak at 335 nm has the highest absorbance.
本発明は、上述の１〜16のピークを利用し、特
に波長335nｍのピークを測定することにより、
Seを高感度に検知することを特徴としている。 The present invention utilizes the peaks 1 to 16 mentioned above, and in particular, by measuring the peak at a wavelength of 335 nm,
It is characterized by highly sensitive detection of Se.
本発明のSeの検出定量方法は、原理的には第
２図にて示される構成にて行われる。第２図にお
いて、１は発光部でガス状Seの上述の〜の
ピークのうち、当該測定対象ピークの波長335n
ｍに対応する光を発光する。該発光部としては例
えばホロカソードランプを発光源とし、波長
335nｍのスペクトル線を中心としたフイルター
を設けたもの等が利用できる。 The method for detecting and quantifying Se of the present invention is carried out in principle with the configuration shown in FIG. In Fig. 2, 1 is the light emitting part, and among the peaks of gaseous Se mentioned above, the wavelength of the peak to be measured is 335n.
It emits light corresponding to m. The light emitting section uses, for example, a hollow cathode lamp as the light source, and the wavelength
A filter equipped with a filter centered on the spectral line of 335 nm can be used.
２は試料室であつて、内部にSeガスを保有し
うる構造を有し、少なくとも発光部１からの入射
光を入れる窓３と、Seガスによつて吸収された
後の透過光を次の受光部５へ出す窓４を有する
炉、あるいは加温手段を有するセルである。 Reference numeral 2 denotes a sample chamber, which has a structure capable of holding Se gas inside, and has a window 3 that lets in at least the incident light from the light emitting part 1, and a window 3 that allows the transmitted light to be absorbed by the Se gas. It is a furnace having a window 4 extending to a light receiving section 5, or a cell having a heating means.
受光部５は通常のモノクロメーター、検出器、
増幅器等の構成による。 The light receiving unit 5 is a normal monochromator, a detector,
Depends on the configuration of the amplifier etc.
本発明の検知・定量方法の原理は、一般の吸光
分光分析と同様であつて、第３図の〜のピー
ク吸収が、特に波長335nｍのピークがガス状Se
の濃度に比例することにより求められる。 The principle of the detection/quantification method of the present invention is the same as that of general absorption spectrometry, and the peak absorption of - in Figure 3 is particularly the peak at a wavelength of 335 nm that is caused by gaseous Se.
It is determined by proportionality to the concentration of
試料室への入射光度をI0、ガス状Seによる吸光
後の透過光強度をＩ、試料室中のガス状Seの光
吸収度をＴ（％）、吸光度をＤ、ガス状Seの濃度
をＣとするとき、
Ｔ（％）＝Ｉ／I0×100
Ｄ＝log１／Ｔ（％）
Ｄ∝Ｃ
の関係であらわされる。 The incident light intensity into the sample chamber is I 0 , the transmitted light intensity after absorption by gaseous Se is I , the light absorption of gaseous Se in the sample chamber is T (%), the absorbance is D , and the concentration of gaseous Se is When C, it is expressed by the relationship: T(%)=I/I 0 ×100 D=log1/T(%) D∝C.
一方、Se投入量とＤの間には第５図の関係の
あることが判明している。第５図においてＡ点は
温度ｔにおけるSeガスの飽和点を表わすもので、
次式のようにSeの蒸気圧により規定される。 On the other hand, it has been found that there is a relationship between the input amount of Se and D as shown in FIG. In Figure 5, point A represents the saturation point of Se gas at temperature t,
It is defined by the vapor pressure of Se as shown in the following equation.
logPt（mmHg）＝−4990／Ｔ＋8.09
ただしここではＴは絶対温度目盛による温度で
ある。 logPt (mmHg)=-4990/T+8.09 However, here, T is the temperature on the absolute temperature scale.
第４図に示すような試料室２がヒーター６を有
するセルである装置を用い、セル内にSeを含有
する試料を入れ、温度を450℃の定温に保持した
時の、吸収スペクトルは、第１図に示したもので
あつた。
Using an apparatus in which the sample chamber 2 is a cell equipped with a heater 6 as shown in Fig. 4, the absorption spectrum when a sample containing Se is placed in the cell and the temperature is maintained at a constant temperature of 450°C is as follows. It was as shown in Figure 1.
以上詳述した本発明のSe検知・定量方法の奏
する効果は下記のとおりである。
The effects of the Se detection/quantification method of the present invention described in detail above are as follows.
(1) 本発明者らにより新発見されたガス状Seの
吸収による335nｍ近辺の第３図〜のスペ
クトル線、特に最も大きいピークである波長
335nｍでの吸収を利用して測定するので、従
来不可能であつたSeの原子化温度（2000℃）
以下の低温での、Seの検知・定量が可能であ
る。(1) The spectral lines in Figure 3 ~ around 335 nm due to the absorption of gaseous Se newly discovered by the present inventors, especially the wavelength of the largest peak.
Since measurement is performed using absorption at 335 nm, the atomization temperature of Se (2000℃), which was previously impossible
Detection and quantification of Se is possible at the following low temperatures.
(2) 上記のように従来よりはるかに低温で検知・
定量できるので、その場分析が可能である。(2) As mentioned above, detection and
Since it can be quantified, on-site analysis is possible.
したがつて本発明方法は、Seを用いる半導体
製品および半導体製造装置、廃棄物処理装置例え
ば、ZnSe、CdSe、などの化合物半導体のエピ成
長装置（CVD炉、LPE炉など）、高圧HB炉、ア
ニーリング炉、Se圧アニーリング炉、MBE装
置、MOCVD装置などにあるいは、Seを含有す
る合金やセラミツクス、ガラス等の溶解炉などに
おける、Seの検出定量方法として用いて多大の
効果を奏する。 Therefore, the method of the present invention is applicable to semiconductor products and semiconductor manufacturing equipment using Se, waste treatment equipment, epitaxial growth equipment (CVD furnace, LPE furnace, etc.) for compound semiconductors such as ZnSe, CdSe, etc., high-pressure HB furnace, annealing It is highly effective when used as a method for detecting and quantifying Se in furnaces, Se pressure annealing furnaces, MBE equipment, MOCVD equipment, etc., or in melting furnaces for Se-containing alloys, ceramics, glass, etc.
さらに上述の各装置において、Seを定量検知
し、Seの投入量コントロール、Se圧のコントロ
ールをその場で行なうことが可能なモニター装置
として利用できる。 Furthermore, each of the above-mentioned devices can be used as a monitoring device that can quantitatively detect Se and control the amount of Se introduced and the Se pressure on the spot.
第１図は450℃におけるガス状Seの吸光スペク
トルで図中〜はピークを示す、第２図は本発
明のSeの検知定量法の構成を説明する図、第３
図はSe量とlog１／Ｔ％の関係を示す図、第４図は
本発明の一実施例の概略の構成及び温度分布を示
す図、第５図はSeの原子吸光スペクトル、第６
図は原子吸光分光分析法の概略フローを示す図で
ある。
Figure 1 shows the absorption spectrum of gaseous Se at 450°C, and ~ in the figure indicates the peaks. Figure 2 is a diagram explaining the configuration of the Se detection and quantitative method of the present invention. Figure 3
The figure shows the relationship between Se content and log1/T%, Figure 4 shows the schematic configuration and temperature distribution of an embodiment of the present invention, Figure 5 shows the atomic absorption spectrum of Se, and Figure 6 shows the atomic absorption spectrum of Se.
The figure is a diagram showing a schematic flow of atomic absorption spectrometry.
Claims (1)
Seに波長335nｍのスペクトル線を入射し、上記
ガス状Seによる上記入射スペクトル線の吸収を
測定し、光強度のピーク高さからSeの検知・定
量を行う方法。 ２ 炉またはヒーター付容器の光の進行方向に窓
部を設け、一方の窓部に波長335nｍのスペクト
ル線発光部、他方の窓にはヒーター付容器内のガ
ス状Seを通過した前記スペクトル線の光強度の
ピーク高さからSeを検知・定量する受光・測光
部を接続してなるSeモニター。[Claims] 1 At a temperature lower than the atomization temperature of Se, gaseous
A method in which a spectral line with a wavelength of 335 nm is incident on Se, the absorption of the incident spectral line by the gaseous Se is measured, and Se is detected and quantified from the peak height of the light intensity. 2. A window is provided in the direction of light propagation in the furnace or heater-equipped container, one window emits a spectral line with a wavelength of 335 nm, and the other window emits the spectral line that has passed through the gaseous Se in the heater-equipped container. Se monitor consists of a light receiving/photometering unit that detects and quantifies Se based on the peak height of light intensity.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP94285A JPS61160042A (en) | 1985-01-09 | 1985-01-09 | Detection and quantitative analysis of se and se monitor |
| US06/811,760 US4731334A (en) | 1985-01-09 | 1985-12-20 | Method and apparatus for detecting and quantitatively determining selenium |
| DE8686300109T DE3681460D1 (en) | 1985-01-09 | 1986-01-08 | QUANTITATIVE DETERMINATION OF SELENIUM. |
| EP86300109A EP0187717B1 (en) | 1985-01-09 | 1986-01-08 | Quantitative determination of selenium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP94285A JPS61160042A (en) | 1985-01-09 | 1985-01-09 | Detection and quantitative analysis of se and se monitor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61160042A JPS61160042A (en) | 1986-07-19 |
| JPH0226179B2 true JPH0226179B2 (en) | 1990-06-07 |
Family
ID=11487724
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP94285A Granted JPS61160042A (en) | 1985-01-09 | 1985-01-09 | Detection and quantitative analysis of se and se monitor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61160042A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4717420B2 (en) * | 2004-11-24 | 2011-07-06 | 株式会社フジシールインターナショナル | Heat-shrinkable cylindrical label |
-
1985
- 1985-01-09 JP JP94285A patent/JPS61160042A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61160042A (en) | 1986-07-19 |
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