JPH01296557A - Glow discharge mass spectrometry for insulator material - Google Patents
Glow discharge mass spectrometry for insulator materialInfo
- Publication number
- JPH01296557A JPH01296557A JP63127288A JP12728888A JPH01296557A JP H01296557 A JPH01296557 A JP H01296557A JP 63127288 A JP63127288 A JP 63127288A JP 12728888 A JP12728888 A JP 12728888A JP H01296557 A JPH01296557 A JP H01296557A
- Authority
- JP
- Japan
- Prior art keywords
- gallium
- powder
- insulator material
- mass spectrometry
- glow discharge
- 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.)
- Pending
Links
- 238000001036 glow-discharge mass spectrometry Methods 0.000 title claims description 11
- 239000012212 insulator Substances 0.000 title abstract description 8
- 239000000463 material Substances 0.000 title abstract description 6
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000000465 moulding Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000011810 insulating material Substances 0.000 claims description 15
- 239000012535 impurity Substances 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 abstract description 5
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 abstract description 2
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 5
- 238000011109 contamination Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- -1 z05 Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 238000002796 luminescence method Methods 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Electron Tubes For Measurement (AREA)
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
本発明は絶縁物材料のグロー放電質量分析法に関するも
のである。DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention relates to glow discharge mass spectrometry of insulating materials.
〈従来の技術〉
近年、ファインセラミック、また電子材料などの分野で
高純度の絶縁物材料が使用され、またそれに伴いこれら
の絶縁物材料中に含まれる微量の不純物の同定、定量を
迅速に行う分析法の確立が要望されている。<Conventional technology> In recent years, high-purity insulating materials have been used in fields such as fine ceramics and electronic materials, and with this, it has become necessary to quickly identify and quantify minute amounts of impurities contained in these insulating materials. There is a need to establish an analytical method.
絶縁物材料中の不純物の分析法としては、発光法、原子
吸光法などが知られているが、発光法ではｐｐｍ以下の
不純物の分析が困難であり、また原子吸光法では分析試
料の分解等の前処理に時間がかかり、多元素の迅速な分
析法とはいえない。Luminescence method, atomic absorption method, etc. are known as methods for analyzing impurities in insulating materials, but it is difficult to analyze impurities of ppm or less with the luminescence method, and atomic absorption method requires decomposition of the sample to be analyzed. It takes time to pre-process, so it cannot be said to be a rapid analysis method for multiple elements.
これらの方法に代わってより微量でかつ多元素を迅速に
分析する方法として近年グロー放電質量分析法（Ｇｌｏ
ｗ Ｄｉｓｃｈａｒｇｅ Ｍａｓｓ Ｓｐｅｃｔｒｏｍ
ｅｔｒｙ：以下ＧＤＭＳ法と呼称する。）が用いられる
ようになってきた。Glow discharge mass spectrometry (Glo
w Discharge Mass Spectrum
etry: Hereinafter referred to as GDMS method. ) has come into use.
〈発明が解決しようとする課題〉
しかしながら、このＧＤＭＳ法は導電性を有する金属や
半導体材料については非常に有効な分析法であるが、絶
縁物材料については材料自身に電場がかけられず、放電
を継続することが困難で測定は難しいとされてきた。こ
の問題に対しては試料を粉末とし、金、銀などの高純度
金属粉やグラファイト粉と混合して導電性を与えて分析
する方法が知られているが、成型した棒状電極の強度が
不足することや高純度の導電粉を得ることが困難なため
、用いた導電粉に含まれる不純物濃度によって検出下限
が左右され、固体質量分析法本来の分折性能を得ること
が困難であった。<Problems to be Solved by the Invention> However, although this GDMS method is a very effective analysis method for conductive metals and semiconductor materials, it is difficult to apply an electric field to the material itself for insulating materials, causing discharge. It has been considered difficult to continue and difficult to measure. To solve this problem, it is known to analyze the sample by making it into powder and mixing it with high-purity metal powder such as gold or silver or graphite powder to give it conductivity, but the strength of the molded rod-shaped electrode is insufficient. Because it is difficult to obtain high-purity conductive powder, the lower limit of detection depends on the concentration of impurities contained in the conductive powder used, making it difficult to obtain the spectroscopic performance inherent to solid-state mass spectrometry.
本発明の目的は上記問題のない絶縁物材料のグロー放電
質量分析法を提供することにある。An object of the present invention is to provide a glow discharge mass spectrometry method for insulating materials that does not have the above-mentioned problems.
く課題を解決するための手段〉
すなわち、本発明は、高純度ガリウムと絶縁物材料の粉
末を混合し、その混合物を加圧成型し″ζ作成した電極
をグロー放重質量分析にかけ絶縁物材料を分析すること
を特徴とする絶縁物材料のグロー放電質量分析法を提供
するものである。Means for Solving the Problems> That is, the present invention mixes high-purity gallium and powder of an insulating material, press-molds the mixture, subjects the resulting electrode to glow mass spectrometry, and analyzes the insulating material. The present invention provides a glow discharge mass spectrometry method for insulating materials, which is characterized by analyzing.
本発明は」１記の実情に鑑み鋭意研究の結果、近年入手
が容易になった高純度でかつ低融点のガリウム（Ｇａ）
を絶縁材料と混合、ついで成型することにより充分な強
度を存し、導電材料と同様にしてＧＤＭＳ法による分析
ができることを見出したことにある。The present invention is based on the results of intensive research in view of the circumstances described in 1.
It has been discovered that by mixing it with an insulating material and then molding it, it has sufficient strength and can be analyzed using the GDMS method in the same way as conductive materials.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
本発明で使用されるガリウムは高純度のもので５Ｎ以」
−が好ましく、最近６Ｎあるいは７Ｎと極めて高純度の
ものも市販されているのでこれらを使用するのがより好
ましい。ガリウムは融点が３０°Ｃと低いため融解操作
が容易であり、操作中に汚染される恐れが少ないという
長所がある。The gallium used in the present invention is of high purity and is 5N or higher.
- is preferable, and it is more preferable to use 6N or 7N, as extremely high purity ones have recently been commercially available. Since gallium has a low melting point of 30° C., it is easy to melt and has the advantage of being less likely to be contaminated during the operation.
分析の対象となる絶縁物試料としては特に限定されるも
のではないが、八１２０３．Ｚｒ０ｚ、Ｔｌ０ｚ、Ｔａ
ｚ０５、Ｙ２Ｏ３等の金属や稀土類酸化物、ＡＩＮ 、
５ＩＪ４等の窒化物、ＳｉＣ等の炭化物などの無機絶縁
体化合物が好適である。The insulator sample to be analyzed is not particularly limited, but 81203. Zr0z, Tl0z, Ta
Metals and rare earth oxides such as z05, Y2O3, AIN,
Inorganic insulating compounds such as nitrides such as 5IJ4 and carbides such as SiC are suitable.
ＧＤＭＳ分析においては分析する絶縁物材料の粉末と上
記ガリウムを混合、加圧成型し、棒状の電極にして使用
する。In GDMS analysis, the powder of the insulating material to be analyzed and the above-mentioned gallium are mixed, pressure-molded, and used as a rod-shaped electrode.
該電極は以下のようにして作製する。The electrode is produced as follows.
絶縁物試料粉末と融解させた高純度ガリウムを容器にと
り、ついで撹拌棒でゆっくりと撹拌・混合していくと絶
縁物表面にガリウムが付着して液体ガリウムが減少して
いく。混合比率は特に限定されないが、充分混合を行っ
たときに液体ガリウムが見えなくなる程度が好ましく、
通常試料に対し重量比３０〜２００χの範囲で適宜法め
ればよいが、ガリウムが少ない方が感度的には有利であ
る。このようにして得られた試料粉末を成型用鋳型に充
填するが、この際、試料表面に（＝ｊ着していたガリウ
ムが再び液体ガリウムとして出て（る場合があるので、
その場合は液体ガリウムを取り除きながら充填する。こ
れを加圧成型することにより強固な棒状電極を作製する
ことができる。When the insulator sample powder and molten high-purity gallium are placed in a container and then slowly stirred and mixed with a stirring rod, the gallium adheres to the surface of the insulator and the amount of liquid gallium decreases. The mixing ratio is not particularly limited, but it is preferable that liquid gallium is no longer visible when sufficiently mixed.
Normally, the weight ratio of the sample to the sample may be adjusted as appropriate within the range of 30 to 200χ, but the smaller the amount of gallium, the more advantageous it is in terms of sensitivity. The sample powder obtained in this way is filled into a mold for molding, but at this time, the gallium that had been deposited on the sample surface may come out as liquid gallium again.
In that case, fill while removing liquid gallium. By press-molding this, a strong rod-shaped electrode can be produced.
成型時に鋳型からの汚染が避りられないため、従来の銀
、金粉末などを導電粉末として用いた場合は分析前に予
備放電を長時間行って試料表面の汚染を取り除く工程が
必要であったが、本発明で作製された電極は強固である
ため、試料電極の先端を切ったり、表面を若干削るなと
の操作により迅速に表面汚染部を除去することかできる
利点を有している。また、カリウム単独では測定中に融
解して冷却なしでは測定できないが、このようにして作
製した棒状電極は室温でも測定か可能であり、通常の条
件で何ら支障なく測定できる。Contamination from the mold is unavoidable during molding, so when conventional silver, gold powder, etc. are used as conductive powder, it is necessary to conduct a preliminary discharge for a long time to remove contamination from the sample surface before analysis. However, since the electrode produced according to the present invention is strong, it has the advantage that surface contamination can be quickly removed by cutting the tip of the sample electrode or slightly scraping the surface. Further, although potassium alone melts during measurement and cannot be measured without cooling, the rod-shaped electrode prepared in this way can be measured even at room temperature and can be measured under normal conditions without any problems.
〈発明の効果〉
本発明によれば従来の方法に比較して迅速、高感度に絶
縁物材料中の不純物の多元素を同時に分析することがで
きる。<Effects of the Invention> According to the present invention, multiple elements of impurities in an insulating material can be simultaneously analyzed quickly and with high sensitivity compared to conventional methods.
〈実施例〉
以上本発明を実施例によってさらに詳細に説明するが本
発明はこれら実施例によって何ら限定されるものではな
い。<Examples> The present invention will be described in more detail with reference to Examples, but the present invention is not limited to these Examples in any way.
実施例１
１００ｍ ｌのポリテトラフルオロエチレン製（以下Ｐ
ＴＦＥ）容器中に融解した７Ｎガリウム（住人化学工業
■製）Ｉｇと高純度アルミナ粉末１ｇ（粒径０．４〜０
．６ μｍ）を加えた。ＰＴＦＥ製棒でこれをゆっくり
と混合し、アルミナ表面にガリウムを付着させ、均一な
粉末とした。この粉末をポリエチレン製鋳型を用いて約
３００Ｋｇ／ｃｍ２の圧力で加圧成型し、約２ｍｍφＸ
２０ｍｍの棒状電極を作製した。Ｔａ製ナイフで棒状
電極の先端約１ｍｍを切り、さらに電極表面を若干削っ
て表面汚染部を除去した。これをグロー放電質量分析装
置（ＶＧ ｌ５ｏｔｏｐｅｓ社製ＶＧ−９０００型）イ
オン源に挿入して測定を行った。測定結果を第１表に示
す。Example 1 100 ml of polytetrafluoroethylene (hereinafter referred to as P)
TFE) molten 7N gallium (manufactured by Sumitomo Chemical Co., Ltd.) Ig and 1 g of high-purity alumina powder (particle size 0.4-0
．． 6 μm) was added. This was mixed slowly with a PTFE rod to adhere gallium to the alumina surface and form a uniform powder. This powder was pressure molded using a polyethylene mold at a pressure of about 300 kg/cm2, and
A 20 mm rod-shaped electrode was produced. Approximately 1 mm of the tip of the rod-shaped electrode was cut with a Ta knife, and the surface of the electrode was slightly scraped to remove surface contamination. This was inserted into an ion source of a glow discharge mass spectrometer (model VG-9000 manufactured by VG 15otopes) and measured. The measurement results are shown in Table 1.
なお、測定条件はグロー放電電流は２ｍＡ 、電圧ＩＫ
Ｖ、分解能４０００、放電ガス：アルゴン、加速電＝６
−
圧８ＫＶである。The measurement conditions are: glow discharge current is 2 mA, voltage IK
V, resolution 4000, discharge gas: argon, accelerating current = 6
- Pressure is 8KV.
第 １ 表Chapter 1 Table
Claims (1)
物を加圧成型して作成した電極をグロー放電質量分析に
かけ絶縁物材料を分析することを特徴とする絶縁物材料
のグロー放電質量分析法A glow discharge mass spectrometry method for insulating materials characterized by mixing high-purity gallium and insulating material powder and applying an electrode made by pressure molding the mixture to glow discharge mass spectrometry to analyze the insulating material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63127288A JPH01296557A (en) | 1988-05-25 | 1988-05-25 | Glow discharge mass spectrometry for insulator material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63127288A JPH01296557A (en) | 1988-05-25 | 1988-05-25 | Glow discharge mass spectrometry for insulator material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01296557A true JPH01296557A (en) | 1989-11-29 |
Family
ID=14956260
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63127288A Pending JPH01296557A (en) | 1988-05-25 | 1988-05-25 | Glow discharge mass spectrometry for insulator material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01296557A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0247548A (en) * | 1988-08-09 | 1990-02-16 | Power Reactor & Nuclear Fuel Dev Corp | Measuring method of impurity in nuclear fuel substance |
| JP2008179898A (en) * | 2008-02-14 | 2008-08-07 | Dowa Holdings Co Ltd | Gallium raw material for forming compound semiconductor |
| CN113533493A (en) * | 2021-05-11 | 2021-10-22 | 宣城开盛新能源科技有限公司 | Glow discharge mass spectrum high-purity gallium testing method |
-
1988
- 1988-05-25 JP JP63127288A patent/JPH01296557A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0247548A (en) * | 1988-08-09 | 1990-02-16 | Power Reactor & Nuclear Fuel Dev Corp | Measuring method of impurity in nuclear fuel substance |
| JP2008179898A (en) * | 2008-02-14 | 2008-08-07 | Dowa Holdings Co Ltd | Gallium raw material for forming compound semiconductor |
| CN113533493A (en) * | 2021-05-11 | 2021-10-22 | 宣城开盛新能源科技有限公司 | Glow discharge mass spectrum high-purity gallium testing method |
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