JPH0415412B2 - - Google Patents
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- Publication number
- JPH0415412B2 JPH0415412B2 JP11515790A JP11515790A JPH0415412B2 JP H0415412 B2 JPH0415412 B2 JP H0415412B2 JP 11515790 A JP11515790 A JP 11515790A JP 11515790 A JP11515790 A JP 11515790A JP H0415412 B2 JPH0415412 B2 JP H0415412B2
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- JP
- Japan
- Prior art keywords
- light
- gaseous
- peak
- absorption
- valley
- 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.)
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Links
- 238000010521 absorption reaction Methods 0.000 claims description 11
- 230000003595 spectral effect Effects 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 238000011002 quantification Methods 0.000 description 12
- 238000001514 detection method Methods 0.000 description 10
- 238000002835 absorbance Methods 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 6
- 238000000862 absorption spectrum Methods 0.000 description 5
- 230000001066 destructive effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000031700 light absorption Effects 0.000 description 3
- 238000011896 sensitive detection Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 238000000137 annealing Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 240000006829 Ficus sundaica Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- 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〕
本発明を新規なＳの定量方法及び該方法を利用
したその場での高感度な検知定量が可能なＳモニ
ターに関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a novel method for quantifying S and an S monitor capable of highly sensitive detection and quantification on the spot using the method.
本発明はＳを用いる半導体製造品及び製造装
置、廃棄物処理装置等、例えばZnS、Cds、ZnSx
Se1-x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、
Ｓ圧アニーリング炉、MBE装置、MOCVD装置
等にＳ検出定量高感度モニターとして利用した
り、あるいは、Ｓを含有する合金やセラミツク
ス、ガラス等の溶解炉等に利用することができ
る。 The present invention relates to semiconductor manufacturing products, manufacturing equipment, waste processing equipment, etc. using S, such as ZnS, Cds, ZnS x
Epitaxial growth equipment (CVD) for compound semiconductors such as Se 1-x
furnace, LPE furnace, etc.), high pressure HB furnace, annealing furnace,
It can be used as a highly sensitive S detection quantitative monitor in S pressure annealing furnaces, MBE equipment, MOCVD equipment, etc., or it can be used in melting furnaces for S-containing alloys, ceramics, glass, etc.
従来、Ｓを検出する場合に、非破壊で、系を乱
さず、その場でガス状Ｓを検知定量する方法は殆
んど知られておらず、Ｓの検出は破壊検知が主で
ある。ガス状物質の非破壊検出・定量法として
は、ガスクロマトグラフイーが考えられるが、
測定系内に試料を導くまでに、導入管壁に付着
し、正確な定量ができない、系内からのサンプ
リングを要するため系を乱してしまう、という本
質的な問題点があるため不適であり、実用されて
いない。また、原子吸光分析は、原子状態の試料
について厳密に測定できるが、資料を2000℃以上
の高温状態とする必要があり、原子化温度以下の
検知定量は原理的に不可能であるに加え、用いう
るホロカソードランプがない。
Conventionally, when detecting S, there is almost no known method for detecting and quantifying gaseous S on the spot in a non-destructive manner without disturbing the system, and the main method of detecting S is destructive detection. Gas chromatography can be considered as a non-destructive detection/quantification method for gaseous substances.
It is unsuitable because it has the inherent problem that it adheres to the wall of the introduction tube before the sample is introduced into the measurement system, making accurate quantification impossible, and that it disturbs the system because it requires sampling from within the system. , has not been put into practice. In addition, atomic absorption spectrometry can accurately measure samples in the atomic state, but it requires the material to be heated to a high temperature of 2000℃ or higher, and detection and quantification at temperatures below the atomization temperature is theoretically impossible. There are no hollow cathode lamps available.
本発明は上記した現状に鑑みてなされたもの
で、非破壊で、系をみださず、その場でガス状Ｓ
の高感度検知・定量が可能な方法及び該方法を利
用した高感度モニターの提供を目的とするもので
ある。
The present invention has been made in view of the above-mentioned current situation, and is non-destructive, does not disturb the system, and allows gaseous Sulfur to be produced on the spot.
The purpose of the present invention is to provide a method capable of detecting and quantifying with high sensitivity, and a highly sensitive monitor using the method.
すなわち、本発明はガス状Ｓに、波長264.5n
ｍ、267nｍ、269.5nｍ、272nｍ、275nｍ、278n
ｍ及び281nｍに谷部（以下谷ピークという）を
有するスペクトル線のうちの少なくとも１つを、
入射し、上記ガス状Ｓによる上記入射スペクトル
線の吸収を測定し、各光強度のピーク高さからＳ
の検知・定量を行う方法および炉またはヒータ付
容器の光の進行方向に窓部を設け、一方の窓部に
波長264.5nｍ、267nｍ、269.5nｍ、272nｍ、275n
ｍ、278nｍ及び281nｍに谷ピークを有するスペ
クトル線のうちの少なくとも１つの発光部、他方
の窓にはヒータ付容器内のガス状Ｓ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Ｓを検
知定量する受光、測光部を接続してなる、Ｓモニ
ターである。
That is, the present invention applies a wavelength of 264.5n to gaseous S.
m, 267nm, 269.5nm, 272nm, 275nm, 278n
At least one of the spectral lines having a valley (hereinafter referred to as valley peak) at m and 281 nm,
The absorption of the incident spectrum line by the gaseous S is measured, and S is determined from the peak height of each light intensity.
A method for detecting and quantifying
m, a light emitting part of at least one of the spectral lines having valley peaks at 278 nm and 281 nm; This is an S monitor that is connected to a light receiving and photometric section for detection and quantification.
以下に本発明につき詳細に説明する。 The present invention will be explained in detail below.
本発明者らは、ガス大Ｓ（ガス状ではS2、S4、
S6、S8等になると考えられているが、特定されて
いない。）の吸光スペクトルを詳細に研究の結果、
第１図に示すように、波長264.5nｍ、267nｍ、
269.5nｍ、272nｍ、275nｍ、278nｍ及び281nｍ
に吸光の谷ピークを有することを発見した。そし
てこのような谷のピークは温度300℃程度のＳの
分子の状況のスペクトルで得られるという知見を
も得て、ガス状Ｓの吸収による上記各々の吸光ピ
ークを利用することにより、ガス状Ｓを高感度で
かつその場でさえ検出・定量を可能としたもので
ある。こゝで谷ピークがこの検出・定量に利用で
きる理由は次のとおりである。第６図において、
Imはバツクグラウンドの光の透過を示しており、
吸収等がなければImが測定される。それに対し、
光の吸収があれば吸光分Iaだけ光の光量が吸収さ
れIiの値となつて測定されることになる。光の吸
収等はＳの分子の構造にかかわつているものとみ
られ、光の吸収はＳとＳのボンデイング等を振動
などにエネルギー吸収されているためと推定され
るのでバツククラウンドの光透過量Imに対する
光吸収量IaがＳの濃度変化に対し、あらかじめ検
量線が作成されていれば、Iiを測定することによ
つて、つまり谷のピークをImに対して測定する
ことによつてＳに定量することができる。 The present inventors have discovered that the gas size S (in gaseous form, S 2 , S 4 ,
It is thought that it will be S 6 , S 8, etc., but it has not been identified. ) As a result of detailed research on the absorption spectra of
As shown in Figure 1, the wavelengths are 264.5nm, 267nm,
269.5nm, 272nm, 275nm, 278nm and 281nm
It was discovered that there is a valley peak of absorption. We also obtained the knowledge that such a valley peak can be obtained in the spectrum of the state of S molecules at a temperature of about 300°C, and by using each of the above absorption peaks due to gaseous S absorption, gaseous S This enables highly sensitive detection and quantification even on the spot. The reason why the valley peak can be used for this detection and quantification is as follows. In Figure 6,
Im indicates background light transmission,
Im is measured if there is no absorption etc. For it,
If light is absorbed, the amount of light will be absorbed by the amount of absorption Ia and will be measured as the value Ii. The absorption of light seems to be related to the structure of the S molecule, and it is presumed that the absorption of light is due to energy absorption due to vibrations of the bonding between S and S, so the amount of light transmitted in the background is If a calibration curve has been created in advance, the light absorption amount Ia for Im can be adjusted to S by measuring Ii, that is, by measuring the peak of the valley with respect to Im. Can be quantified.
本発明において、上記波長のスペクトル線のう
ちの２つまたはそれ以上のスペクトル線を用いる
場合は、これらを同時に入射し、発光部における
分光器により別々に測定してその平均をとるので
単一のスペクトル線を用いる場合より他物質との
分離がより確実となり、しかもＳ定量の精度が向
上する。 In the present invention, when using two or more spectral lines of the above-mentioned wavelengths, they are incident at the same time, measured separately by a spectrometer in the light emitting part, and then averaged. Separation from other substances is more reliable than when using spectral lines, and the accuracy of S quantification is improved.
本発明は第２図に示すように、炉、ヒータ付セ
ルあるいは筒部１に窓２を取り付け、発光部３に
おいて上記谷ピークのスペクトル線を発光させ、
この光を窓２から入射し、発光部４において光強
度のピーク高さを測定することにより、炉または
セル中のＳを検知定量するものである。このＳの
検知、定量は、上記谷ピークのピーク吸収がＳ濃
度に比例することから求める。ピーク吸収とＳ濃
度の関係は
Ｄ＝log１／Ｔ（％） ……(1)
Ｄ∝Ｃ ……(2)
上記(1)、(2)式で表される。ここでＴはピークで
の吸光度（％）、ＣはＳの濃度である。 As shown in FIG. 2, the present invention attaches a window 2 to a furnace, a cell with a heater, or a cylindrical part 1, and causes a light emitting part 3 to emit the spectral line of the valley peak,
By entering this light through the window 2 and measuring the peak height of the light intensity at the light emitting section 4, S in the furnace or cell is detected and quantified. The detection and quantification of S is determined from the fact that the peak absorption of the valley peak is proportional to the S concentration. The relationship between peak absorption and S concentration is expressed by the above equations (1) and (2). Here, T is the absorbance at the peak (%), and C is the concentration of S.
上記谷ピークのスペクトル発光源としては、ホ
ロカソードランプを用い、上記ピークを中心とし
たフイルターを各々設けたものが使用できる。ま
た該フイルターは受光部に設けることもできる。 As the spectral emission source for the valley peak, a hollow cathode lamp can be used, each provided with a filter centered on the peak. Further, the filter can also be provided in the light receiving section.
さらに検出結果をコンピユータ処理し、その結
果を表示するようにできる。このようにすれば、
ほぼ実時間でＳを定量検出できるので、その場で
のＳの検知定量とＳの投入量Ｓ圧コントロール等
を制御しうる高感度Ｓモニターを実現できる。 Furthermore, the detection results can be processed by a computer and the results can be displayed. If you do this,
Since it is possible to quantitatively detect S in almost real time, it is possible to realize a highly sensitive S monitor that can detect and quantify S on the spot and control the amount of S input, S pressure, etc.
第３図ａは本発明の実施例で用いた装置の概略
図であつて、１はセル、２は窓、３は発光部、４
は受光部、５は加熱手段をあらわす。なお第３図
ｂはこの装置の温度分布を示すグラフである。
FIG. 3a is a schematic diagram of the device used in the embodiment of the present invention, in which 1 is a cell, 2 is a window, 3 is a light emitting part, and 4
5 represents a light receiving section, and 5 represents a heating means. Note that FIG. 3b is a graph showing the temperature distribution of this device.
セル１内にＳを置き加熱手段５によりセル１内
の温度を298℃に一定にして保持したときのスペ
クトルを第４図に示す。波長264.5nｍ、267nｍ、
269.5nｍ、272nｍ、275nｍ、278nｍ及び281nｍ
を谷のピークとした吸収スペクトルが明瞭に測定
された。 FIG. 4 shows the spectrum obtained when S was placed in the cell 1 and the temperature inside the cell 1 was kept constant at 298° C. by the heating means 5. Wavelength 264.5nm, 267nm,
269.5nm, 272nm, 275nm, 278nm and 281nm
The absorption spectrum with trough peak was clearly measured.
一方、Ｓの投入量と、吸光度の間には、一般的
に第５図に示す関係があることを詳細な実験によ
り確認した。ここでガス状Ｓが存在するとき検知
される光強度をＩ、ガラ状Ｓがないときの光強度
をI0とすると、吸光度Ｔ（％）は次式(3)で与えら
れる。 On the other hand, it was confirmed through detailed experiments that there is generally a relationship shown in FIG. 5 between the amount of S added and the absorbance. Here, if the light intensity detected when gaseous S is present is I, and the light intensity when there is no glassy S is I0 , the absorbance T (%) is given by the following equation (3).
Ｔ＝Ｉ／I0×100 ……(3)
したがつて、前記の(1)および(2)式により吸光度
からＳを定量できる。なおＡ点は、温度ｔにおけ
る飽和点をあらわしており、
蒸気圧（logPt（mmHg）＝−6750／ｔ＋11.32）
により規定される。 T=I/I 0 ×100 (3) Therefore, S can be quantified from the absorbance using equations (1) and (2) above. Note that point A represents the saturation point at temperature t, and is defined by vapor pressure (logPt (mmHg) = -6750/t + 11.32).
第５図の関係は夫々の谷の吸収スペクトルにつ
いて成立するので、いずれのピークの測定によつ
てもＳ量を求めることができる。検出は0.01ppm
オーダーまで可能である。 Since the relationship shown in FIG. 5 holds true for the absorption spectrum of each valley, the amount of S can be determined by measuring any peak. Detection is 0.01ppm
It is possible to order.
さらに上記の谷の各スペクトル線のうちの２つ
またはそれ以上を同時に検知し、各々のピーク高
さから同時に定量を行うことができる。この場合
は前記(1)、(3)式にかえて、下記(a)〜(c)の評価手段
による。なお、は夫々の平均値を、ｎ＝１、
２…７は上記７種類のピークについての、夫々の
測定を表す。 Furthermore, two or more of the spectral lines of the valleys described above can be detected simultaneously and quantified simultaneously from the height of each peak. In this case, the following evaluation means (a) to (c) are used instead of the above equations (1) and (3). In addition, are the respective average values, n=1,
2...7 represents the respective measurements for the seven types of peaks mentioned above.
(a) Ｄ＝log１／Ｔ（％）、
（％）＝１／ｎ〓〓〓Ii／Ioi×100
ｎ＝１、２、…７
(b) ＝１／ｎ〓〓〓log１／Ti（％）、
Ti（％）＝Ii／Ioi×100
ｎ＝１、２、…７
(c) Ｄ＝log１／To（％）、
ｎ＝１、２、…７
このような評価はコンピユータ等演算装置によ
れば容易かつ迅速であり、実時間でＳ量を表示で
きるので、系の制御ができる。(a) D=log1/T(%), (%)=1/n〓〓〓Ii/Io i ×100 n=1, 2,...7 (b) =1/n〓〓〓log1/Ti( %), Ti (%) = Ii / Io i × 100 n = 1, 2, ...7 (c) D = log1 / To (%), n=1, 2, . . . 7 Such evaluation is easy and quick using an arithmetic device such as a computer, and since the amount of S can be displayed in real time, the system can be controlled.
本発明の効果は次のとおりである。 The effects of the present invention are as follows.
(1) ガス状Ｓの吸収による上記ピーク（谷）のス
ペクトルを利用することにより、ガス状Ｓの高
感度の検知・定量がその場で可能となつた。(1) Highly sensitive detection and quantification of gaseous S is now possible on the spot by using the spectrum of the above peaks (troughs) due to the absorption of gaseous S.
(2) 上記谷ピークのスペクトルの２つ以上のピー
ク高さから同時に定量を行なうため、他物質か
ら明確に分離して検知精度が向上し、またＳの
定量精度が大巾に向上する。(2) Since quantification is performed simultaneously from the heights of two or more peaks in the spectrum of the valley peak, the detection accuracy is improved by clearly separating it from other substances, and the quantification accuracy of S is greatly improved.
(3) 本発明の高感度ＳモニターはＳ量のその場で
の検知・定量が可能であり、さらにコンピユー
タ等演算装置と組合すことにより、各スペクト
ルの吸光度から実時間でＳ量を検知定量し、該
演算装置の出力信号によりＳ投入量、Ｓ圧等を
その場で制御することができる。(3) The high-sensitivity S monitor of the present invention is capable of detecting and quantifying the amount of S on the spot, and when combined with a calculation device such as a computer, it is possible to detect and quantify the amount of S in real time from the absorbance of each spectrum. However, the S input amount, S pressure, etc. can be controlled on the spot based on the output signal of the arithmetic unit.
第１図はガス状Ｓの吸光スペクトルである。第
２図は本発明方法及びモニターの概略を示す模式
図である。第３図ａは本発明の実施例で用いた装
置の概略図であり、第３図ｂは第３図ａ装置にお
ける温度分布を示すグラフである。第４図は本発
明の実施例で得られた波長と吸光度の関係を示す
グラフ、第５図はＳ量と吸光度の関係を示すグラ
フである。第６図は谷ピークがＳの検知・定量に
利用できる理由を示す吸光スペクトルの模式図で
ある。
FIG. 1 shows the absorption spectrum of gaseous S. FIG. 2 is a schematic diagram showing the outline of the method and monitor of the present invention. FIG. 3a is a schematic diagram of the apparatus used in the embodiment of the present invention, and FIG. 3b is a graph showing the temperature distribution in the apparatus of FIG. 3a. FIG. 4 is a graph showing the relationship between wavelength and absorbance obtained in an example of the present invention, and FIG. 5 is a graph showing the relationship between S amount and absorbance. FIG. 6 is a schematic diagram of an absorption spectrum showing why the valley peak can be used for detecting and quantifying S.
Claims (1)
ｍ、272nｍ、275nｍ、278nｍ及び281nｍの谷ピ
ークを有するスペクトル線のうちの少なくとも１
つを、入射し、上記ガス状Ｓによる上記入射スペ
クトル線の吸収を測定し、各光強度のピーク高さ
からＳの検知・定量を行う方法。 ２ 炉またはヒータ付容器の光の進行方向に窓部
を設け、一方の窓部に波長264.5nｍ、267nｍ、
269.5nｍ、272nｍ、275nｍ、278nｍ及び281nｍ
の谷ピークを有するスペクトル線のうちの少なく
とも１つの発光部、他方の窓にはヒータ付容器内
のガス状Ｓ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Ｓを検知定量する受光、測光部
を接続してなる、Ｓモニター。 ３ 光強度のピーク高さからＳを検知・定量し、
それによりＳ投入量コントロール・Ｓ圧コントロ
ールを実時間で制御する特許請求の範囲第２項記
載のＳモニター。 ４ 発光部がホロカソードランプからなる特許請
求の範囲第２項記載のＳモニター。 ５ 発光部または受光部が264.5nｍ、267nｍ、
269.5nｍ、272nｍ、275nｍ、278nｍおよび281n
ｍのうちの少なくとも１つを中心とするフイルタ
を有する特許請求の範囲第２項記載のＳモニタ
ー。[Claims] 1 Gaseous S has wavelengths of 264.5 nm, 267 nm, and 269.5 nm.
at least one of the spectral lines having valley peaks at m, 272 nm, 275 nm, 278 nm and 281 nm.
A method in which the absorption of the incident spectral line by the gaseous S is measured, and the S is detected and quantified from the peak height of each light intensity. 2 A window is provided in the direction of light propagation of the furnace or container with a heater, and one window has wavelengths of 264.5 nm, 267 nm,
269.5nm, 272nm, 275nm, 278nm and 281nm
a light emitting part for at least one of the spectral lines having a valley peak; the other window has a light receiving unit for detecting and quantifying S from the peak height of the light intensity of the spectral line that has passed through the gaseous S in the container with a heater; S monitor with a photometer connected. 3 Detect and quantify S from the peak height of light intensity,
The S monitor according to claim 2, which controls S input amount control and S pressure control in real time. 4. The S monitor according to claim 2, wherein the light emitting section comprises a hollow cathode lamp. 5 The light emitting part or the light receiving part is 264.5nm, 267nm,
269.5nm, 272nm, 275nm, 278nm and 281n
3. The S monitor according to claim 2, further comprising a filter centered on at least one of m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11515790A JPH0315739A (en) | 1990-05-02 | 1990-05-02 | S detection/quantification method and S monitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11515790A JPH0315739A (en) | 1990-05-02 | 1990-05-02 | S detection/quantification method and S monitor |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP94585A Division JPS61160045A (en) | 1985-01-09 | 1985-01-09 | S detection/quantification method and S monitor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0315739A JPH0315739A (en) | 1991-01-24 |
| JPH0415412B2 true JPH0415412B2 (en) | 1992-03-17 |
Family
ID=14655743
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11515790A Granted JPH0315739A (en) | 1990-05-02 | 1990-05-02 | S detection/quantification method and S monitor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0315739A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4940654B2 (en) * | 2005-12-22 | 2012-05-30 | アイシン精機株式会社 | Vehicle seat device |
-
1990
- 1990-05-02 JP JP11515790A patent/JPH0315739A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0315739A (en) | 1991-01-24 |
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