JPH02190744A - Fine particle measuring instrument - Google Patents
Fine particle measuring instrumentInfo
- Publication number
- JPH02190744A JPH02190744A JP1010872A JP1087289A JPH02190744A JP H02190744 A JPH02190744 A JP H02190744A JP 1010872 A JP1010872 A JP 1010872A JP 1087289 A JP1087289 A JP 1087289A JP H02190744 A JPH02190744 A JP H02190744A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- sample gas
- cavity
- capillary tube
- reaction pipe
- 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.)
- Granted
Links
- 239000010419 fine particle Substances 0.000 title claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 15
- 238000001514 detection method Methods 0.000 claims abstract description 9
- 238000004451 qualitative analysis Methods 0.000 claims description 3
- 238000004445 quantitative analysis Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 abstract description 21
- 239000012159 carrier gas Substances 0.000 abstract description 5
- 238000007599 discharging Methods 0.000 abstract 2
- 238000000034 method Methods 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000001505 atmospheric-pressure chemical vapour deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
本発明は半導体プロセスにおいてクリーンルーム内或は
常圧ＣＶＤ装置内のような大気圧又は常圧下の空間内に
おける微粒子をインプロセスで検出できる微粒子測定装
置に関する。Detailed Description of the Invention <Industrial Application Field> The present invention is a particulate measurement method that can detect particulates in-process in a space under atmospheric pressure or normal pressure, such as a clean room or an atmospheric pressure CVD apparatus in a semiconductor process. Regarding equipment.
〈従来の技術〉
従来、微粒子測定装置として、反応槽中にレーザ光を照
射し、散乱光に基づきガス中の微粒子の大きさを求める
。方法が公知である。しかしながら、この方法は次のよ
うな欠点がある。<Prior Art> Conventionally, as a particulate measuring device, a laser beam is irradiated into a reaction tank and the size of particulates in a gas is determined based on the scattered light. Methods are known. However, this method has the following drawbacks.
■ レーザ光の波長の制約から、直径が０．１μｍ以下
の微粒子の測定は原理的に出来ない、加えて実際の測定
では測定装置を反応槽外において測定するため窓の汚れ
等によって０．５μｍ以下の微粒子は測定出来ない、一
方、半導体素子の高集積化は急速に進み、ＩＭビットＤ
ＲＡＭ、４ＭビットＤＲＡＭのプロセスでは管理すべき
微粒子の大きさが０．０５μｍのレベルとなっている。■ Due to the limitations of the wavelength of the laser beam, it is theoretically impossible to measure particles with a diameter of 0.1 μm or less.In addition, in actual measurements, the measuring device is placed outside the reaction tank, so particles with a diameter of 0.5 μm may be measured due to dirt on the window, etc. The following fine particles cannot be measured.On the other hand, as semiconductor devices become more highly integrated, IM bit D
In the process of RAM and 4 Mbit DRAM, the size of particles to be managed is at the level of 0.05 μm.
■ 光学的手法による検出のため微粒子の大きさしか分
らず、微粒子の組成についての情報は得られない。■ Because detection is done by optical methods, only the size of the particles can be determined, and no information about the composition of the particles can be obtained.
〈発明が解決しようとする課題〉
本発明の解決しようとする技術的課題は、大気圧又は常
圧下の空間内に存在する直径が０．０５μｍ程度の微粒
子をインラインで検出でき同時に成分の同定も行える微
粒子測定装置を実現することにある。<Problem to be solved by the invention> The technical problem to be solved by the present invention is to detect in-line fine particles with a diameter of about 0.05 μm existing in a space under atmospheric pressure or normal pressure, and to identify the components at the same time. The goal is to realize a particle measuring device that can measure particles.
く課題を解決するための手段〉
本発明の構成は、
Ａ 常圧下の空間内からサンプルガスを圧力差に基づき
導出するキャピラリチューブ
Ｂ マイクロ波源
Ｃマイクロ波源からのマイクロ波が導入されたキャビテ
ィ
Ｄ キャビティ内を貫通し、一端よりキャピラリチュー
ブからのサンプルガスとキャリアガスとが導入され他端
に検出窓が設けられた反応管Ｅ 反応管の他端からガス
を排気する手段Ｆ 反応管の検出窓に隣接して設けられ
、反応管内に生成されたマイクロ波誘導プラズマによっ
て解離（ガス化・イオン化）されたサンプルガス中の微
粒子を定性・定量分析する分析手段とより構成される。Means for Solving the Problems> The configuration of the present invention is as follows: A. A capillary tube that leads out sample gas from a space under normal pressure based on the pressure difference. B. A microwave source. C. A cavity into which microwaves from the microwave source are introduced. D. A cavity. A reaction tube E that penetrates through the inside of the tube, into which the sample gas and carrier gas from the capillary tube are introduced from one end, and a detection window is provided at the other end. Means F for exhausting gas from the other end of the reaction tube. It consists of an analysis means that is provided adjacently and performs qualitative and quantitative analysis of fine particles in the sample gas that have been dissociated (gasified and ionized) by the microwave-induced plasma generated in the reaction tube.
〈作用〉
マイクロ波誘導プラズマの場合、前記反応管の真空度が
１０Ｔｏｒｒ前後の真空度において４０００゛に以上の
熱プラズマが生成される。この励起温度は前記サンプル
ガスに含まれる微粒子を解離（ガス化・イオン化）する
に充分な温度である。<Operation> In the case of microwave-induced plasma, a thermal plasma of 4000° or more is generated when the vacuum degree of the reaction tube is about 10 Torr. This excitation temperature is sufficient to dissociate (gasify and ionize) the fine particles contained in the sample gas.
前記空間は大気圧又は常圧であり、サンプルガスは圧力
差によって前記キャピラリチューブを通じ前記反応管内
に導かれる。サンプルガス中の微粒子は粒径が小さい程
、解離し易く、イオン化された微粒子は成分固有のスペ
クトルで発光する。これを分光器を用いて測定し、或は
原子イオンを質量分析装置に導いて測定し、微粒子の量
的測定並びに成分の同定を行う。The space is at atmospheric pressure or normal pressure, and the sample gas is guided into the reaction tube through the capillary tube due to the pressure difference. The smaller the particle size of the fine particles in the sample gas, the more easily they dissociate, and the ionized fine particles emit light with a spectrum unique to the component. This is measured using a spectrometer, or the atomic ions are introduced into a mass spectrometer and measured to quantitatively measure the particles and identify their components.
〈実施例〉
以下図面に従い本発明を説明する。第１図は本発明実施
例装置の構成図である０図中、１は半導体プロセスにお
けるクリーンルーム、或は常圧ＣＶＤ装置のよう゛な大
気圧又は常圧下の空間を示す。<Example> The present invention will be described below with reference to the drawings. FIG. 1 is a block diagram of an apparatus according to an embodiment of the present invention. In FIG. 1, reference numeral 1 indicates a space under atmospheric pressure or normal pressure, such as a clean room in a semiconductor process or an atmospheric pressure CVD apparatus.
２はサンプルガスＳＧを採取するため一端が空間１内に
挿入されたキャピラリチューブ、３はマイクロ波源、４
はマイクロ波源３からのマイクロ波が導入されたキャビ
ティである。５は石英製の反応管で、キャビティ４内を
貫通して設置され、その一端にはキャピラリチューブ１
が接続されると共に、アルゴン、ヘリウム等のキャリア
ガスＣＧを導入するキャリアガス導入部５ａが設けられ
ている。この反応管の他端には検出窓５ｂが設けられる
と共に、ガス排出部５ｃが設けられている。2 is a capillary tube whose one end is inserted into space 1 to collect sample gas SG; 3 is a microwave source; 4
is a cavity into which microwaves from the microwave source 3 are introduced. 5 is a reaction tube made of quartz, which is installed to penetrate inside the cavity 4, and a capillary tube 1 is attached to one end of the reaction tube.
A carrier gas introduction section 5a is provided to which a carrier gas CG such as argon or helium is introduced. The other end of this reaction tube is provided with a detection window 5b and a gas discharge section 5c.
６は排気手段でガス排出部５ｃを通じ反応管５内を真空
に引く、７は検出窓５ｂに向けて設けられサンプルガス
ＳＧ中の微粒子を定性・定量分析する分析手段である。Reference numeral 6 denotes an evacuation means that evacuates the inside of the reaction tube 5 through the gas discharge part 5c. Reference numeral 7 denotes an analysis means provided toward the detection window 5b for qualitative and quantitative analysis of particles in the sample gas SG.
この分析手段には、分光分析器、或は四重極質量分析計
のような質量分析装置が用いられる。７ａは検出部とし
ての光電子増倍管である。８は信号検出部で、この中に
は前置増幅器８ａ、Ａ／Ｄ変換器８ｂ、マイクロプロセ
ッサを用いた演算処理回路８０等が含まれる。As this analysis means, a spectrometer or a mass spectrometer such as a quadrupole mass spectrometer is used. 7a is a photomultiplier tube as a detection section. Reference numeral 8 denotes a signal detection section, which includes a preamplifier 8a, an A/D converter 8b, an arithmetic processing circuit 80 using a microprocessor, and the like.
第２図は本発明実施例装置の要部を示す断面図である０
本図において、第１図における部分に対応する部分に同
一符号が付されている。キャビティ４には円板型で、外
周部よりマイクロ波が導入され、中心にマイクロ波が集
中する、例えば、Ｂｅｅｎａｋｋｅｒ型キャビティが用
いられる。FIG. 2 is a sectional view showing the main parts of the device according to the present invention.
In this figure, parts corresponding to those in FIG. 1 are given the same reference numerals. For example, a Beenakker type cavity is used as the cavity 4, which has a disk shape, into which microwaves are introduced from the outer periphery and concentrated at the center.
反応管５はキャビティ４の中心部を通るように設置され
る。The reaction tube 5 is installed so as to pass through the center of the cavity 4.
このような構成で、排気手段６によって反応管５内の真
空度を１０Ｔｏ ｒ ｒ前後に引き、マイクロ波源３か
ら周波数が２．４５ＧＨｚのマイクロ波をキャビティ４
内に導き、キャリアガスＣＧを流すと、反応管５内に４
０００°に以上の熱プラズマＰＬが生成される。With this configuration, the degree of vacuum in the reaction tube 5 is drawn to around 10 Torr by the exhaust means 6, and microwaves with a frequency of 2.45 GHz are applied from the microwave source 3 to the cavity 4.
When the carrier gas CG is introduced into the reaction tube 5, 4
000° or higher thermal plasma PL is generated.
一方、空間１内は大気圧又は常圧に保たれておりサンプ
ルガスＳＧは圧力差によってキャピラリチューブ２を通
じ反応管５内に導かれる。プラズマＰＬに導かれたサン
プルガスＳＧ中の微粒子は解離されイオン化される。プ
ラズマによって解離される微粒子は直径が小さい程解離
しやすく、直径が０．１〜０．０５μｍまでの微粒子を
解離することができる。On the other hand, the inside of the space 1 is maintained at atmospheric pressure or normal pressure, and the sample gas SG is guided into the reaction tube 5 through the capillary tube 2 due to the pressure difference. Fine particles in the sample gas SG guided by the plasma PL are dissociated and ionized. The smaller the diameter of fine particles dissociated by plasma, the more easily they are dissociated, and fine particles having a diameter of 0.1 to 0.05 μm can be dissociated.
イオン化された微粒子は成分固有のスペクトルで発光す
る。この発光を例えば分光器を用いた分析手段７で検出
すれば、スペクトルの強度から微粒子の量的情報が得ら
れ、スペクトルの波長に基づき成分の同定を行う。Ionized fine particles emit light in a spectrum unique to the component. If this emission is detected by an analysis means 7 using a spectrometer, for example, quantitative information on the particles can be obtained from the intensity of the spectrum, and the components can be identified based on the wavelength of the spectrum.
〈発明の効果〉 本発明によれば以下のような効果を有する。<Effect of the invention> According to the present invention, the following effects are achieved.
■ 従来の光学的方法によっては原理的に測定が不可能
であった直径が０．１〜０．０５μｍレベルの微粒子を
インラインで検出することができる。(2) Fine particles with a diameter of 0.1 to 0.05 μm, which cannot be measured in principle using conventional optical methods, can be detected in-line.
■ 微粒子の量的情報が得られる他、成分の同定も同時
に行える。■In addition to obtaining quantitative information on fine particles, the components can also be identified at the same time.
■ キャピラリチューブを使って前記反応管と前記キャ
ビティとの圧力差でサンプリングを行うのでサンプルガ
スを移送する特別の手段が要らない。(2) Since sampling is performed using a capillary tube based on the pressure difference between the reaction tube and the cavity, no special means for transferring the sample gas is required.
■ マイクロ波誘導に基づくプラズマ中では微粒子の径
が小さい程、解離、イオン化し易く原理的に径の小さな
微粒子の測定に向いている。■ In plasma based on microwave induction, the smaller the particle size, the easier it is to dissociate and ionize it, making it suitable in principle for measuring small particles.
第１図は本発明実施例装置の構成図、第２図は本発明実
施例装置の要部を示す断面図である。FIG. 1 is a block diagram of an apparatus according to an embodiment of the present invention, and FIG. 2 is a sectional view showing a main part of the apparatus according to an embodiment of the present invention.
Claims (1)
測定装置。 Ａ 常圧下の空間内からサンプルガスを圧力差に基づき
導出するキャピラリチューブ Ｂ マイクロ波源 Ｃ マイクロ波源からのマイクロ波が導入されたキャビ
ティ Ｄ キャビティ内を貫通し、一端よりキャピラリチュー
ブからのサンプルガスとキャリアガスとが導入され他端
に検出窓が設けられた反応管 Ｅ 反応管の他端からガスを排気する手段 Ｆ 反応管の検出窓に隣接して設けられ、反応管内に生
成されたマイクロ波誘導プラズマによつて解離、イオン
化されたサンプルガス中の微粒子を定性・定量分析する
分析手段[Scope of Claims] A particle measuring device characterized by comprising the following components A to F. A Capillary tube that leads sample gas from a space under normal pressure based on the pressure difference B Microwave source C Cavity into which microwaves from the microwave source are introduced D Sample gas and carrier from the capillary tube penetrate through the cavity and enter from one end A reaction tube E into which a gas is introduced and a detection window provided at the other end. A means F for exhausting gas from the other end of the reaction tube. Analytical means for qualitative and quantitative analysis of fine particles in sample gas dissociated and ionized by plasma
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1010872A JPH0754294B2 (en) | 1989-01-19 | 1989-01-19 | Particle measuring device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1010872A JPH0754294B2 (en) | 1989-01-19 | 1989-01-19 | Particle measuring device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02190744A true JPH02190744A (en) | 1990-07-26 |
| JPH0754294B2 JPH0754294B2 (en) | 1995-06-07 |
Family
ID=11762431
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1010872A Expired - Lifetime JPH0754294B2 (en) | 1989-01-19 | 1989-01-19 | Particle measuring device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0754294B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01269555A (en) * | 1988-04-20 | 1989-10-27 | Fuji Photo Film Co Ltd | Thermal printer device |
| JPH04328450A (en) * | 1991-04-26 | 1992-11-17 | Yokogawa Electric Corp | Plasma generating spectrometer |
| US5432601A (en) * | 1992-12-17 | 1995-07-11 | Mitsubishi Denki Kabushiki Kaisha | Fine particle analyzing device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57108655A (en) * | 1980-12-25 | 1982-07-06 | Tsukasa Sotsuken:Kk | Device for measuring air fuel ratio of internal combustion engine or other burning apparatus |
| JPS57130433U (en) * | 1981-02-06 | 1982-08-14 |
-
1989
- 1989-01-19 JP JP1010872A patent/JPH0754294B2/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57108655A (en) * | 1980-12-25 | 1982-07-06 | Tsukasa Sotsuken:Kk | Device for measuring air fuel ratio of internal combustion engine or other burning apparatus |
| JPS57130433U (en) * | 1981-02-06 | 1982-08-14 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01269555A (en) * | 1988-04-20 | 1989-10-27 | Fuji Photo Film Co Ltd | Thermal printer device |
| JPH04328450A (en) * | 1991-04-26 | 1992-11-17 | Yokogawa Electric Corp | Plasma generating spectrometer |
| US5432601A (en) * | 1992-12-17 | 1995-07-11 | Mitsubishi Denki Kabushiki Kaisha | Fine particle analyzing device |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0754294B2 (en) | 1995-06-07 |
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