JPS598775B2 - Active gas partial pressure measuring device - Google Patents
Active gas partial pressure measuring deviceInfo
- Publication number
- JPS598775B2 JPS598775B2 JP51101421A JP10142176A JPS598775B2 JP S598775 B2 JPS598775 B2 JP S598775B2 JP 51101421 A JP51101421 A JP 51101421A JP 10142176 A JP10142176 A JP 10142176A JP S598775 B2 JPS598775 B2 JP S598775B2
- Authority
- JP
- Japan
- Prior art keywords
- target
- active gas
- section
- primary ion
- partial pressure
- 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
- 239000007789 gas Substances 0.000 claims description 30
- 238000004140 cleaning Methods 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 description 47
- 238000010884 ion-beam technique Methods 0.000 description 12
- 238000005259 measurement Methods 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 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
- 230000001678 irradiating effect Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
Landscapes
- Measuring Fluid Pressure (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Description
【発明の詳細な説明】 本発明は活性ガスの分圧測定装置に関する。[Detailed description of the invention] The present invention relates to an active gas partial pressure measuring device.
従来、各種化学プラントや腐食・金属表面反応の研究開
発等において活性ガス濃度の測定は不可欠であつたが、
広い圧力範囲にわたつて再現性よく測定することは困難
であつた。例えば一般に用いられている電離真空計では
、活性ガスを測定しようとすると、活性ガスが熱フィラ
メントあるいは測定球の管壁に吸着されるため測定値の
変動が大きく、特に10−4〜10−3Torr程度の
圧力範囲では吸着のために応答速度が遅くなり、また再
現性の面でも悪くなり、正確な測定ができなかつた。In the past, measurement of active gas concentration was indispensable in various chemical plants and research and development of corrosion and metal surface reactions.
It has been difficult to measure with good reproducibility over a wide pressure range. For example, when trying to measure active gas with a commonly used ionization vacuum gauge, the active gas is adsorbed to the hot filament or the tube wall of the measurement bulb, resulting in large fluctuations in the measured value, especially at 10-4 to 10-3 Torr. In a pressure range of about 100 mL, the response speed becomes slow due to adsorption, and reproducibility also deteriorates, making accurate measurements impossible.
一方隔膜真空計は、高真空部に対し隔膜を介してガスを
導入することによる絶対圧測定であるが、ガス圧が非常
に小さい場合では測定できないこと、またガスが活性ガ
ス、特にハロゲンガス等の場合には隔膜が腐食され寿命
が短かくなるなどの欠点を持つていた。本発明は従来の
欠点を解決し、活性ガスの圧力を広範囲にかつ再現性よ
く測定できる装置を提供するもので、以下にその一実施
例を図面とともに説明する。On the other hand, a diaphragm vacuum gauge measures absolute pressure by introducing gas into a high vacuum area through a diaphragm, but it cannot measure when the gas pressure is extremely low. In this case, the diaphragm corrodes, resulting in a shortened service life. The present invention solves the conventional drawbacks and provides a device that can measure the pressure of active gas over a wide range and with good reproducibility.One embodiment of the present invention will be described below with reference to the drawings.
1は測定装置本体2の上部に設けられた、ヘリウム(H
e)、アルゴン(Ar)等の不活性ガスeオン化させる
一次イオン発生部である。1 is a helium (H
e) A primary ion generating unit that ionizes an inert gas such as argon (Ar).
3は一次イオン発生部より発生した一次イオンを引出し
、収束させイオンビームとする一次イオン収束部で、ア
インツエルレンズ4と静電四極子レンズ5とから構成さ
れている。Reference numeral 3 denotes a primary ion focusing section which extracts primary ions generated from the primary ion generating section and focuses them into an ion beam, and is composed of an Einzel lens 4 and an electrostatic quadrupole lens 5.
6はイオンビームに照射されるターゲットで、12角形
の断面を有する保持体Tの12の面に取りつけられたシ
リコン(Si)、チタン(Ti)等の金属板である。Reference numeral 6 denotes a target to be irradiated with the ion beam, which is a metal plate made of silicon (Si), titanium (Ti), etc. attached to the 12 surfaces of the holder T having a dodecagonal cross section.
この保持体Tは、回転軸8を介して測定装置本体2の外
部から回転させることができ、各種の金属からなる前記
のターゲット6を任意に選択してイオンビームに対置さ
せることができる。また被測定部9が測定装置本体2の
下部に接続されているので、前記保持体7およびターゲ
ット6は活性ガス雰囲気中にある。10はターゲット6
の近傍に設けた二次イオン測定部で、ここではフアラデ
一箱を用いて二次イオン強度を電流量で測定している。This holder T can be rotated from the outside of the measuring device main body 2 via a rotating shaft 8, and the target 6 made of various metals can be arbitrarily selected and placed opposite to the ion beam. Further, since the part to be measured 9 is connected to the lower part of the measuring device main body 2, the holder 7 and the target 6 are in an active gas atmosphere. 10 is target 6
A secondary ion measuring section is installed near the ion beam, and the secondary ion intensity is measured by the amount of current using a box of Farade.
11は2組の平行平板電極を用いたターゲツト清浄部で
、イオン収束部3とターゲツト6との間に配置されてい
る。Reference numeral 11 denotes a target cleaning section using two sets of parallel plate electrodes, which is disposed between the ion focusing section 3 and the target 6.
このターゲツト清浄部11はターゲツト6にイオンビー
ムを照射するとき、酸化等によりターゲツト6の表面が
汚染されていれば発生する二次イオン強度に大きく影響
するので、あらかじめイオンビームをターゲツト6表面
上に走査させて照射し清浄する。12は排気路で拡散ポ
ンプ(図示せず)等に接続されている。When irradiating the target 6 with an ion beam, this target cleaning section 11 cleans the ion beam onto the surface of the target 6 in advance, since if the surface of the target 6 is contaminated due to oxidation etc., this will greatly affect the intensity of the secondary ions generated. Scan, irradiate, and clean. 12 is an exhaust path connected to a diffusion pump (not shown) or the like.
そして一次イオン発生部1と一次イオン収束部3との間
にスリツト13を、一次イオン収束部3とターゲツト清
浄部11との間にスリツト14を、ターゲツト6と二次
イオン測定部10との間にスリツト15をそれぞれ設け
、一次イオン収束部3と二次イオン測定部10とを差動
排気している。これは一次イオン収束部3または二次イ
オン測定部10に活性ガスが次第に混入してくるとイオ
ンの平均自由行程が短かくなり、二次イオン発生効率が
悪くなつたり、測定誤差を生じたりするので、ポンプで
排気することにより常に活性ガス圧力より低い圧力に保
つて悪影響を防止している。A slit 13 is provided between the primary ion generating section 1 and the primary ion focusing section 3, a slit 14 is provided between the primary ion focusing section 3 and the target cleaning section 11, and a slit 14 is provided between the target 6 and the secondary ion measuring section 10. A slit 15 is provided in each, and the primary ion focusing section 3 and the secondary ion measuring section 10 are differentially pumped. This is because as the active gas gradually enters the primary ion focusing section 3 or the secondary ion measuring section 10, the mean free path of ions becomes shorter, resulting in poor secondary ion generation efficiency and measurement errors. Therefore, by evacuating with a pump, the pressure is always kept lower than the active gas pressure to prevent adverse effects.
一次イオン発生部1で発生させた不活性ガスの一次イオ
ンは、一次イオン収束部3に引出されて収束しイオンビ
ームとなる。イオンビームが活性ガス中のターゲツト6
を照射すると、二次イオンが発生し、その;次イオン強
度を二次イオン測定部10で測定する。二次イオンの強
度は、イオンビームの強度が一定のとき、ターゲツト6
の材質、活性ガスの種類、活性ガスの分圧によつて異な
る値を示す。いま被測定部9中の活性ガスの種類と、タ
ーゲツト6の材質を特定し、上記のように二次イオン強
度を測定すれば、活性ガスの分圧を求めることができる
。第2図は、ターゲツト6の材質ごとの活性ガス分圧と
二次イオン強度との関係を示したもので、活性ガスが酸
素(02)の場合である。The primary ions of the inert gas generated by the primary ion generating section 1 are extracted to the primary ion focusing section 3 and converged to form an ion beam. Ion beam hits target 6 in active gas
When irradiated with , secondary ions are generated, and the secondary ion intensity is measured by the secondary ion measuring section 10 . When the intensity of the ion beam is constant, the intensity of the secondary ions is
The value varies depending on the material, type of active gas, and partial pressure of active gas. If the type of active gas in the part to be measured 9 and the material of the target 6 are specified and the secondary ion intensity is measured as described above, the partial pressure of the active gas can be determined. FIG. 2 shows the relationship between the active gas partial pressure and the secondary ion strength for each material of the target 6, in the case where the active gas is oxygen (02).
ここで一次イオン用の不活性ガスにアルゴン(Ar)を
用いて12KVで加速し、照射されるターゲツト6には
、シリコン(Si)、チタン(Ti)、インジウム(I
n)、マグネシウム(Mg)、コバルト(CO)、モリ
ブデン(MO)、銅(Cu)、ゲルマニウム(Ge)、
銀(Ag)、スズ(Sn)、カドミウム(Cd)を用い
た。第2図においてそれぞれの金属ごとに、酸素分圧の
増加に対して二次イオン強度が直線的に増加している部
分があり、その増加ヰの大きな部分を用いれば測定され
た二次イオン強度から正確な圧力値を容易に求めること
ができる。例えばターゲツト6が、チタン(Ti)では
10−7〜3×10−6T0rr(02)、シリコン(
Si)では10−6〜3×10−5T0rr(02)、
インジウム(In)では10−6〜2×10−4T0r
r(02)、カドミウム(Cd)では10−6〜10−
8T0rr(02)等の圧力範囲に対して適当である。
上記の実施例では、ターゲツト6を多数備えた保持体7
を回転させて、適当な金属を選択することにより、広い
範囲にわたつて活性ガス分圧の測定が容易に可能である
。またあらかじめイオンビームをターゲツト6表面に走
査させて照射するターゲツト清浄部11を備え、また差
動排気して一次イオン収束部3、二次イオン測定部10
の活性ガス分圧を低下させているので、被測定ガス分圧
に対する二次イオン強度を正確に測定できる。ここでは
二次イオン測定部10にフアラデ一箱を用いたが、同様
に電流量で測定する場合はエレクトロンマルチプライヤ
を用いればさらに高感度測定が可能である。また電流量
以外の測定器でも使用可能であるので第2図の二次イオ
ン強度は任意単位で表わしてある。さらにターゲツト情
浄部11は2組の平行平板電極からなり、イオンビーム
をターゲツト6表面に走査させているが、これは電極間
にかけるわずかな電圧でイオンビームの照射方向を大き
く偏向させることができ、ターゲツト6表面を広くも狭
くも、また自由に走査させ清浄することができるからで
ある。以上のように本発明は、不活性ガスを一次イオン
種とする一次イオン発生部と、活性ガス被測定部に接続
された測定装置本体内部にあつて、ターゲツトを前記一
次イオン発生部と対置させて活性ガス中に保持するとと
もにそのターゲツトを複数個備えたターゲツト選択装置
と、前記一次イオン発生部とターゲツトとの間に設けた
一次イオン収束部と、前記ターゲツトの近傍に設けたタ
ーゲツト清浄部および二次イオン測定部と、前記一次イ
オン収束部および二次イオン測定部とに連通する排気系
とを有する構造により、ターゲツトを適宜選択すること
により広い範囲の活性ガス分圧の測定が容易で、ターゲ
ツト清浄機能や排気系を有することから測定精度が非常
に高く寿命も長い等、工業的価値の高い活性ガス分圧測
定装置を提供するものである。Here, argon (Ar) is used as an inert gas for primary ions, and the target 6 is accelerated at 12 KV and irradiated with silicon (Si), titanium (Ti), and indium (I).
n), magnesium (Mg), cobalt (CO), molybdenum (MO), copper (Cu), germanium (Ge),
Silver (Ag), tin (Sn), and cadmium (Cd) were used. In Figure 2, for each metal, there is a part where the secondary ion strength increases linearly as the oxygen partial pressure increases, and if the part where the increase is large is used, the measured secondary ion strength Accurate pressure values can be easily obtained from For example, if the target 6 is titanium (Ti), it is 10-7 to 3×10-6T0rr(02), or silicon (
Si) is 10-6 to 3×10-5T0rr(02),
Indium (In): 10-6 to 2×10-4T0r
r(02), 10-6 to 10- for cadmium (Cd)
Suitable for pressure ranges such as 8T0rr(02).
In the above embodiment, the holder 7 is equipped with a large number of targets 6.
By rotating and selecting an appropriate metal, active gas partial pressure can be easily measured over a wide range. It is also equipped with a target cleaning section 11 that scans and irradiates the surface of the target 6 with an ion beam, and also has a primary ion focusing section 3 and a secondary ion measuring section 10 that are differentially pumped.
Since the active gas partial pressure of the active gas is lowered, the secondary ion intensity relative to the gas partial pressure to be measured can be accurately measured. Here, a box of Farade was used in the secondary ion measurement section 10, but when similarly measuring the amount of current, even higher sensitivity measurement is possible by using an electron multiplier. Further, since it is possible to use a measuring device other than the current amount, the secondary ion intensity in FIG. 2 is expressed in arbitrary units. Furthermore, the target information section 11 consists of two sets of parallel plate electrodes, which scan the ion beam over the surface of the target 6, which allows the irradiation direction of the ion beam to be significantly deflected by a small voltage applied between the electrodes. This is because the surface of the target 6 can be scanned widely or narrowly and can be cleaned. As described above, the present invention includes a primary ion generating section that uses an inert gas as a primary ion species, and a target that is placed in opposition to the primary ion generating section within the main body of the measuring device, which is connected to an active gas measurement target section. a target selection device having a plurality of targets held in an active gas; a primary ion convergence unit provided between the primary ion generation unit and the target; a target cleaning unit provided near the target; The structure includes a secondary ion measuring section and an exhaust system communicating with the primary ion converging section and the secondary ion measuring section, making it easy to measure active gas partial pressures over a wide range by appropriately selecting a target. The present invention provides an active gas partial pressure measuring device with high industrial value, such as extremely high measurement accuracy and long life due to its target cleaning function and exhaust system.
第1図は本発明の活性ガス分圧測定装置の一実施例を示
す要部断面構成図、第2図は各種金属の酸素分圧に対す
る二次イオン強度を示す関係図である。
1・・・・・・一次イオン発生部、2・・・・・・測定
装置本体、3・・・・・・一次イオン収束部、6・・・
・・・ターゲツト、7・・・・・・保持体、9・・・・
・・被測定部、10・・・・・・二次イオン測定部、1
1・・・・・・ターゲツト清浄部、12・・・・・・排
気路。FIG. 1 is a sectional view of the essential parts of an embodiment of the active gas partial pressure measuring device of the present invention, and FIG. 2 is a relationship diagram showing the secondary ion strength with respect to the oxygen partial pressure of various metals. DESCRIPTION OF SYMBOLS 1...Primary ion generation part, 2...Measurement device main body, 3...Primary ion convergence part, 6...
...Target, 7...Holder, 9...
...Measurement part, 10...Secondary ion measurement part, 1
1...Target clean section, 12...Exhaust path.
Claims (1)
と、活性ガス分圧被測定部に接続された測定装置本体内
部にあつて、ターゲットを前記一次イオン発生部と対置
させて活性ガス中に保持するとともにそのターゲットを
複数個備えたターゲット選択装置と、前記一次イオン発
生部と前記ターゲットとの間に設けた一次イオン収束部
と、前記ターゲットの近傍に設けたターゲット清浄部お
よび二次イオン測定部と、前記一次イオン収束部および
二次イオン測定部とに連通する排気系とを有することを
特徴とする活性ガス分圧測定装置。 2 ターゲット清浄部は、一次イオン収束部とターゲッ
トとの間に設けられた平行平板電極であることを特徴と
する特許請求の範囲第1項記載の活性ガス分圧測定装置
。[Scope of Claims] 1. Inside the main body of the measuring device, which is connected to a primary ion generating unit that uses an inert gas as a primary ion species and a part to be measured for active gas partial pressure, a target is placed opposite to the primary ion generating unit. a target selection device including a plurality of targets held in an active gas, a primary ion convergence unit provided between the primary ion generation unit and the target, and a target cleaning unit provided near the target. What is claimed is: 1. An active gas partial pressure measuring device comprising: a primary ion focusing section and a secondary ion measuring section; and an exhaust system communicating with the primary ion focusing section and the secondary ion measuring section. 2. The active gas partial pressure measuring device according to claim 1, wherein the target cleaning section is a parallel plate electrode provided between the primary ion focusing section and the target.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP51101421A JPS598775B2 (en) | 1976-08-24 | 1976-08-24 | Active gas partial pressure measuring device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP51101421A JPS598775B2 (en) | 1976-08-24 | 1976-08-24 | Active gas partial pressure measuring device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5327083A JPS5327083A (en) | 1978-03-13 |
| JPS598775B2 true JPS598775B2 (en) | 1984-02-27 |
Family
ID=14300236
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP51101421A Expired JPS598775B2 (en) | 1976-08-24 | 1976-08-24 | Active gas partial pressure measuring device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS598775B2 (en) |
-
1976
- 1976-08-24 JP JP51101421A patent/JPS598775B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5327083A (en) | 1978-03-13 |
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