JPH0530209B2 - - Google Patents
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- Publication number
- JPH0530209B2 JPH0530209B2 JP15904284A JP15904284A JPH0530209B2 JP H0530209 B2 JPH0530209 B2 JP H0530209B2 JP 15904284 A JP15904284 A JP 15904284A JP 15904284 A JP15904284 A JP 15904284A JP H0530209 B2 JPH0530209 B2 JP H0530209B2
- Authority
- JP
- Japan
- Prior art keywords
- sample
- container
- acid
- acid solution
- solution
- 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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- 239000002253 acid Substances 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 12
- 238000000354 decomposition reaction Methods 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 239000004065 semiconductor Substances 0.000 claims description 7
- 238000009423 ventilation Methods 0.000 claims description 2
- 239000000523 sample Substances 0.000 description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 239000011734 sodium Substances 0.000 description 11
- 239000012488 sample solution Substances 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 239000012535 impurity Substances 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 235000012431 wafers Nutrition 0.000 description 8
- 229910052804 chromium Inorganic materials 0.000 description 7
- 238000011109 contamination Methods 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 5
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000000889 atomisation Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 239000000538 analytical sample Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000004380 ashing Methods 0.000 description 2
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 229910052805 deuterium Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910000673 Indium arsenide Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- WPYVAWXEWQSOGY-UHFFFAOYSA-N indium antimonide Chemical compound [Sb]#[In] WPYVAWXEWQSOGY-UHFFFAOYSA-N 0.000 description 1
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Description
【発明の詳細な説明】
〔発明の技術分野〕
本発明は、各種試料を酸によつて分解するため
の装置及びその分解方法に関し、更に詳しくは、
シリコン結晶、ガリウムヒ素結晶のような半導体
結晶中の極微量の不純物を分析するための試料溶
液を調製することを目的として用いる試料分解装
置及びその分解方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Technical Field of the Invention] The present invention relates to an apparatus and method for decomposing various samples with acid, and more specifically, to
The present invention relates to a sample decomposition device used for the purpose of preparing a sample solution for analyzing minute amounts of impurities in semiconductor crystals such as silicon crystals and gallium arsenide crystals, and a decomposition method thereof.
シリコン結晶やガリウムヒ素結晶は半導体素子
基板として使用されているが、しかし、この結晶
の中にナトリウム(Na)、カリウム(K)、鉄
(Fe)などの不純物が存在すると、たとえその量
が極微量であつたとしても素子の電気特性に大き
な影響を与える。したがつて、素子の特性を高め
るためには、これら不純物の含有量を可能な限り
低くすることが必要である。
Silicon crystals and gallium arsenide crystals are used as semiconductor device substrates, but if impurities such as sodium (Na), potassium (K), and iron (Fe) are present in these crystals, even if the amount is extremely Even if it is only a small amount, it has a large effect on the electrical characteristics of the device. Therefore, in order to improve the characteristics of the device, it is necessary to reduce the content of these impurities as much as possible.
このための処置をとる前提として、結晶中の不
純物の濃度を正確に分析することが不可欠にな
る。 As a prerequisite for taking such measures, it is essential to accurately analyze the concentration of impurities in the crystal.
従来、その分析方法としてはフレームレス原子
吸光分析法が広く適用されている。この方法にお
いて、分析装置にかける試料溶液は概ね次のよう
にして調製されている。すなわち、例えば、シリ
コン結晶の場合、結晶試料をフツ化水素酸と硝酸
と硫酸との混合酸溶液に溶解せしめて直接分解
し、得られた分解溶液を蒸発乾固して残渣を得、
この残渣を純水で一定容量に稀釈するという方法
である。ガリウムヒ素結晶の場合には、塩酸と硝
酸との混合酸液を用いることが異なるだけであ
る。 Conventionally, flameless atomic absorption spectrometry has been widely applied as an analysis method. In this method, the sample solution to be applied to the analyzer is generally prepared as follows. That is, for example, in the case of a silicon crystal, a crystal sample is directly decomposed by dissolving it in a mixed acid solution of hydrofluoric acid, nitric acid, and sulfuric acid, and the resulting decomposed solution is evaporated to dryness to obtain a residue.
This method involves diluting this residue with pure water to a certain volume. In the case of gallium arsenide crystals, the only difference is that a mixed acid solution of hydrochloric acid and nitric acid is used.
しかしながら、このような試料溶液の調製法に
あつては、用いる各試薬からの汚染が極めて大き
い。 However, in such a method of preparing a sample solution, contamination from each reagent used is extremely large.
例えば、これら試薬は非沸とう蒸留法やイオン
交換法などで精製したものであつても通常Na、
Kなどの不純物を0.1ppb以上含有している。した
がつて、このような試薬を用いた場合、得られた
試料溶液では、5ppb以下の不純物の分析は極め
て困難であつた。 For example, even if these reagents are purified by non-boiling distillation or ion exchange methods, they usually contain Na.
Contains 0.1 ppb or more of impurities such as K. Therefore, when such a reagent is used, it is extremely difficult to analyze impurities of 5 ppb or less in the obtained sample solution.
本発明は、上記した問題点を解消し、試料の分
解用試薬又は環境からの汚染がほとんどない分析
用試料溶液を調製するための装置及びその方法の
提供を目的とする。
SUMMARY OF THE INVENTION An object of the present invention is to solve the above-mentioned problems and provide an apparatus and a method for preparing an analytical sample solution with almost no contamination from a sample decomposition reagent or the environment.
本発明の試料分解装置は、密閉容器;該密閉容
器内に配設された少なくとも1個の酸液貯蔵容
器;該密閉容器内に配設され、内部には試料と純
水が収納されている収納容器;並びに該酸液貯蔵
容器を加熱する加熱手段を具備することを特徴と
し、その分解方法は、密閉容器の中で試料分解用
の酸液を蒸発させ、該酸蒸気を試料が浸漬されて
いる純水に吸収させ、得られた高純度酸液で該試
料を分解することを特徴とする。
The sample decomposition device of the present invention includes: a sealed container; at least one acid solution storage container disposed within the sealed container; a sample and pure water disposed within the sealed container; A storage container; and a heating means for heating the acid solution storage container.The decomposition method involves evaporating an acid solution for sample decomposition in a closed container, and then absorbing the acid vapor into which the sample is immersed. The sample is absorbed into pure water, and the sample is decomposed with the resulting high-purity acid solution.
本発明の装置を図示した例に基づいて説明す
る。図で1は密閉容器であり、この中で試料の分
解が行なわれる。容器1を構成する材質として
は、後述の酸蒸気などに侵蝕されず、またある程
度耐熱性を有する材質であれば何であつてもよ
く、とくに、半導体結晶の分解の場合にはフツ化
水素酸などが用いられるので、例えば、テフロン
などは好適である。 The apparatus of the present invention will be explained based on an illustrated example. In the figure, 1 is a closed container in which the sample is decomposed. The material constituting the container 1 may be any material as long as it is not corroded by acid vapor, which will be described later, and has a certain degree of heat resistance. In particular, in the case of decomposing semiconductor crystals, hydrofluoric acid, etc. may be used. For example, Teflon is suitable.
密閉容器1の中には、2種類の容器が配設され
る。1つは、試料分解用の酸液が収納された酸液
貯蔵容器2であり、他の種類は、分解すべき試料
とそれを浸漬する純水が収納された収納容器3で
ある。これら容器の材質には、容器1の場合と同
様な性状が必要であることは言をまたない。 Two types of containers are arranged in the closed container 1. One type is an acid solution storage container 2 that stores an acid solution for sample decomposition, and the other type is a storage container 3 that stores a sample to be decomposed and pure water for immersing it. Needless to say, the materials of these containers must have properties similar to those of the container 1.
容器2に収納する酸液は試料4の種類によつて
任意に選択される。また、容器2の数は1個であ
つてもよいし、複数個であつてもよく制限を受け
るものではない。例えば、試料4がシリコンウエ
ハーの場合、フツ化水素酸、硝酸を別々の容器2
に収納してもよいし、混酸にして1つの容器に収
納しておいてもよい。 The acid solution stored in the container 2 is arbitrarily selected depending on the type of the sample 4. Moreover, the number of containers 2 may be one or more, and is not limited. For example, if the sample 4 is a silicon wafer, the hydrofluoric acid and nitric acid are stored in separate containers 2.
It may be stored in a container, or it may be mixed acid and stored in one container.
容器3には試料4と純水5が収納されている。
用いる純水としては脱イオン水、蒸留水など、不
純物を除去して得た精製水がよい。試料4の分解
を円滑に行なわせるために、例えば容器3の底に
は図のような凸部6を設けて試料を点支持するこ
とが好ましい。 A sample 4 and pure water 5 are stored in the container 3.
The pure water used is preferably purified water obtained by removing impurities, such as deionized water or distilled water. In order to smoothly decompose the sample 4, it is preferable to provide a convex portion 6 as shown in the figure on the bottom of the container 3, for example, to support the sample at a point.
また、図では容器3が1つであるが、同時に多
数の試料を分解するためには、例えばこの容器3
を複数個積みあげたり、又は1つの容器内を複数
室に間仕切りすればよい。 In addition, although there is only one container 3 in the figure, in order to decompose many samples at the same time, for example, this container 3
You can pile up multiple containers, or partition one container into multiple rooms.
更には、容器3は上面開口することなく、通気
孔を例えば側壁に具備する蓋で覆えば、容器1の
天井等から滴下する酸溶液からの汚染を防止し得
て有効である。 Furthermore, it is effective to cover the ventilation hole with a lid provided on the side wall of the container 3 without opening the top surface, since it is possible to prevent contamination from the acid solution dripping from the ceiling of the container 1 or the like.
7は酸液貯蔵容器の加熱手段であつて、これは
容器2内の酸液を蒸発させて酸蒸気を発生させる
ために配設される。電気抵抗加熱等その加熱手段
の種類は問わない。これら加熱手段は汚染防止の
観点から容器1の外部に配設されることが好まし
い。また、必要に応じては、容器3を加熱するた
めに設けてもよい。 Reference numeral 7 denotes heating means for the acid liquid storage container, which is provided to evaporate the acid liquid in the container 2 and generate acid vapor. The type of heating means, such as electric resistance heating, does not matter. These heating means are preferably disposed outside the container 1 from the viewpoint of preventing contamination. Further, if necessary, it may be provided to heat the container 3.
この装置において、容器2内の酸液は加熱手段
7によつて加熱されて蒸発し、酸蒸気となつて容
器1内を満たす。蒸発に際しては、不純物は蒸気
圧の関係で蒸発しないので得られた酸蒸気の純度
は極めて高い。 In this device, the acid liquid in the container 2 is heated by the heating means 7 and evaporated, turning into acid vapor and filling the container 1. During evaporation, impurities do not evaporate due to vapor pressure, so the purity of the acid vapor obtained is extremely high.
酸蒸気は矢線のように移動して容器3の純水5
に吸収され高純度な酸液に復元する。かくして、
試料はこの高純度酸液によつて分解され、全体と
して外部汚染のない試料溶液が得られる。 The acid vapor moves like the arrow and reaches the pure water 5 in the container 3.
is absorbed and restored to a high-purity acid solution. Thus,
The sample is decomposed by this high-purity acid solution, resulting in a sample solution that is totally free of external contamination.
なお、以上の説明は試料が半導体結晶である場
合を主眼にして行なつたが、この装置及び方法は
これに限定されるものではなく、要するに、各種
の試料(例えばWSix,MoSixのような金属シリ
サイド、InSb,InAsのような化合物半導体)と
それを分解する能力を有する酸液とを組合せたい
かなる場合であつても適用できることは、その原
理からして極めて明瞭である。 Although the above explanation has focused on the case where the sample is a semiconductor crystal, this apparatus and method are not limited to this. It is very clear from its principle that it can be applied to any combination of a compound semiconductor (such as silicide, InSb, or InAs) and an acid solution capable of decomposing it.
〔発明の実施例〕
実施例 1
比抵抗1.5Ωcm、厚み436μmのリンドープシリコ
ンウエハーを用意した。これを脱イオン水50mlと
ともに容器3に収納した。酸液としてそれぞれ50
%フツ化水素酸400mlと60%硝酸400mlを選びそれ
ぞれを別々に容器2に収納した。容器1の空間体
積は約8500cm3であつた。なお、各容器はいずれも
テフロン製であつた。[Embodiments of the Invention] Example 1 A phosphorus-doped silicon wafer having a specific resistance of 1.5 Ωcm and a thickness of 436 μm was prepared. This was stored in container 3 along with 50 ml of deionized water. 50 each as acid solution
% hydrofluoric acid and 400 ml of 60% nitric acid were selected and stored separately in container 2. The spatial volume of container 1 was approximately 8500 cm 3 . Note that each container was made of Teflon.
加熱手段(ヒータプレート)を作動して、各酸
液を210℃で150分間加熱した。ウエハーの溶解が
確認された。 The heating means (heater plate) was activated to heat each acid solution at 210°C for 150 minutes. Wafer melting was confirmed.
得られた試料溶液をフレームレス原子吸光装置
にかけてNa、K、Fe、Crの分析を行なつた。測
定条件は以下の通りである。 The obtained sample solution was applied to a flameless atomic absorption spectrometer to analyze Na, K, Fe, and Cr. The measurement conditions are as follows.
乾燥:120℃で30秒。灰化:Naは600℃、Kは
700℃、FeとCrは1000℃でそれぞれ30秒間。原子
化:Naは2500℃、Kは2700℃、FeとCrは2800℃
でそれぞれ8秒間。キヤリアガス:アルゴンで
300ml/分、ただし原子化のときは通流しない。
測定波長:Naは589.0nm、Kは766.5nm、Feは
248.3nm、Crは359.4nm。妨害吸収補正用光源:
Na、Kのときはハロゲンタングステンランプ、
Fe、Crのときは重水素ランプを使用。 Drying: 30 seconds at 120℃. Ashing: Na is 600℃, K is
700℃, Fe and Cr at 1000℃ for 30 seconds each. Atomization: 2500℃ for Na, 2700℃ for K, 2800℃ for Fe and Cr
for 8 seconds each. Carrier gas: with argon
300ml/min, but no flow during atomization.
Measurement wavelength: Na: 589.0nm, K: 766.5nm, Fe:
248.3nm, Cr is 359.4nm. Light source for interference absorption correction:
For Na and K, use a halogen tungsten lamp.
For Fe and Cr, use a deuterium lamp.
以上の結果、Na:3ppb,K:1ppb,Fe:
7ppb,Cr:0.8ppbであつた。 As a result, Na: 3ppb, K: 1ppb, Fe:
7ppb, Cr: 0.8ppb.
比較例 1
50%フツ化水素酸10ml、60%硝酸5ml、96%硫
酸0.1ml及び純水5mlから成る混酸に、実施例1
で用いたシリコンウエハーを浸漬し、これを約50
℃で20分間かけて分解した。得られた溶液を約
160℃で120分間加熱して蒸発乾固したのち、純水
で5mlに稀釈した。Comparative Example 1 Example 1 was added to a mixed acid consisting of 10 ml of 50% hydrofluoric acid, 5 ml of 60% nitric acid, 0.1 ml of 96% sulfuric acid, and 5 ml of pure water.
Soak the silicon wafer used in
Digested for 20 minutes at °C. The resulting solution is approx.
After heating at 160°C for 120 minutes and evaporating to dryness, it was diluted to 5 ml with pure water.
実施例1と同一の測定条件で分析したところ、
Feは7ppbと分析できたが、10ppb以下のNaやK、
2ppb以下のCrは分析できなかつた。 When analyzed under the same measurement conditions as Example 1,
Fe was analyzed to be 7ppb, but Na and K below 10ppb,
Cr below 2 ppb could not be analyzed.
実施例 2
シリコンウエハーが比抵抗6.9Ωcm、厚み320μm
のホウ素をドープしたものであつたこと、脱イオ
ン水が40mlであつたこと、酸液の加熱時間が130
分であつたことを除いては、実施例1と同様にし
て試料溶液を調製し、同一の測定条件でフレーム
レス原子吸光分析を行なつた。Example 2 Silicon wafer has a specific resistance of 6.9Ωcm and a thickness of 320μm
The amount of deionized water was 40 ml, and the heating time of the acid solution was 130 ml.
A sample solution was prepared in the same manner as in Example 1, except that the temperature was 30 minutes, and flameless atomic absorption spectrometry was performed under the same measurement conditions.
Na:2ppb、K:1ppb、Fe:3ppb、Cr:
0.5ppbの結果が得られた。比較例1の方法の場合
には、いずれの元素も検出できなかつた。 Na: 2ppb, K: 1ppb, Fe: 3ppb, Cr:
A result of 0.5 ppb was obtained. In the case of the method of Comparative Example 1, none of the elements could be detected.
実施例 3
試料が、LEC法による厚み470μmのガリウムヒ
素ウエハーであつたこと、酸液が35%塩酸400ml、
60%硝酸400mlであつたこと、酸液の加熱時間が
140分であつたことを除いては、実施例1と同様
の方法で分析用試料溶液を調製した。Example 3 The sample was a gallium arsenide wafer with a thickness of 470 μm obtained by the LEC method, the acid solution was 400 ml of 35% hydrochloric acid,
400ml of 60% nitric acid was added, and the heating time of the acid solution was
An analytical sample solution was prepared in the same manner as in Example 1, except that the heating time was 140 minutes.
得られた試料溶液をフレームレス原子吸光装置
にかけてFe、Cr、Mgの分析を行なつた。測定条
件は以下の通りである。 The obtained sample solution was applied to a flameless atomic absorption spectrometer to analyze Fe, Cr, and Mg. The measurement conditions are as follows.
乾燥:120℃で30秒。灰化:Feは1250℃、Crは
1350℃、Mgは1100℃でそれぞれ60秒間。原子
化:いずれも2800℃でそれぞれ8秒間。キヤリア
ガス:アルゴンで300ml/分、ただし原子化のと
きは通流しない。測定波長:Feは248.3nm、Crは
359.4nm、Mgは285.2nm、妨害吸収補正用光源:
重水素ランプを使用。 Drying: 30 seconds at 120℃. Ashing: 1250℃ for Fe, Cr
1350℃ and Mg at 1100℃ for 60 seconds each. Atomization: 8 seconds each at 2800℃. Carrier gas: Argon at 300ml/min, but not during atomization. Measurement wavelength: 248.3nm for Fe, 248.3nm for Cr
359.4nm, Mg is 285.2nm, light source for interference absorption correction:
Uses a deuterium lamp.
Fe:28ppb、Cr:3ppb、Mg:3ppbの結果が得
られた。 The results were obtained: Fe: 28ppb, Cr: 3ppb, Mg: 3ppb.
比較例 2
35%塩酸10ml、60%硝酸5mlの混酸(120℃)
で実施例3のウエハーを分解したのち純水で100
mlに稀釈した。この溶液を実施例3と同様の条件
で分析した。Feは28ppbと分析可能であつたが、
5ppb以下のCr、Mgは検出できなかつた。Comparative example 2 Mixed acid of 10ml of 35% hydrochloric acid and 5ml of 60% nitric acid (120℃)
After disassembling the wafer of Example 3 with
diluted to ml. This solution was analyzed under the same conditions as in Example 3. Fe was analyzable at 28 ppb, but
Cr and Mg below 5ppb could not be detected.
以上の説明及び分析結果からも明らかなよう
に、本発明の装置を用いて調製した試料溶液は、
従来のように、試薬、環境等からの汚染が抑制さ
れるので、得られた分析結果は極めて高感度であ
り、例えばシリコンウエハーの場合には約50倍、
ガリウムヒ素の場合には約5倍であり、その有用
性は極めて大きい。
As is clear from the above explanation and analysis results, the sample solution prepared using the device of the present invention is
Unlike conventional methods, contamination from reagents, the environment, etc. is suppressed, so the analysis results obtained are extremely sensitive; for example, in the case of silicon wafers, it is approximately 50 times more sensitive.
In the case of gallium arsenide, it is about five times as large, making it extremely useful.
図は本発明装置の1例を示す模式図である。
1……密閉容器、2……酸液貯蔵容器、3……
試料及び純水の収納容器、4……試料、5……純
水、6……凸部、7……加熱手段。
The figure is a schematic diagram showing an example of the device of the present invention. 1...Airtight container, 2...Acid liquid storage container, 3...
Sample and pure water storage container, 4...sample, 5...pure water, 6...convex portion, 7...heating means.
Claims (1)
とも1個の酸液貯蔵容器;該密閉容器内に配設さ
れ、内部には試料と純水が収納されている収納容
器;並びに該酸液貯蔵容器を加熱する加熱手段を
具備することを特徴とする試料分解装置。 2 該試料が半導体結晶ウエハーである特許請求
の範囲第1項記載の試料分解装置。 3 該収納容器が通気孔を具備した蓋付き容器で
ある特許請求の範囲第1項記載の試料分解装置。 4 密閉容器の中で、試料分解用の酸液を蒸発さ
せ、該酸蒸気を試料が浸漬されている純水に吸収
させ、得られた高純度酸液で該試料を分解するこ
とを特徴とする試料分解方法。 5 該試料が半導体結晶ウエハーであり、該酸液
が硝酸並びにフツ酸若しくは塩酸である特許請求
の範囲第4項記載の方法。[Claims] 1. A sealed container; at least one acid solution storage container disposed within the sealed container; a storage container disposed within the sealed container and containing a sample and pure water; A sample decomposition device comprising: a container; and heating means for heating the acid solution storage container. 2. The sample decomposition device according to claim 1, wherein the sample is a semiconductor crystal wafer. 3. The sample decomposition device according to claim 1, wherein the storage container is a lidded container equipped with a ventilation hole. 4. In a closed container, an acid solution for sample decomposition is evaporated, the acid vapor is absorbed into pure water in which the sample is immersed, and the sample is decomposed with the obtained high-purity acid solution. sample decomposition method. 5. The method according to claim 4, wherein the sample is a semiconductor crystal wafer and the acid solution is nitric acid, hydrofluoric acid or hydrochloric acid.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP15904284A JPS6138547A (en) | 1984-07-31 | 1984-07-31 | Sample analyzing instrument and sample analyzing method using said instrument |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP15904284A JPS6138547A (en) | 1984-07-31 | 1984-07-31 | Sample analyzing instrument and sample analyzing method using said instrument |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS6138547A JPS6138547A (en) | 1986-02-24 |
JPH0530209B2 true JPH0530209B2 (en) | 1993-05-07 |
Family
ID=15684959
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP15904284A Granted JPS6138547A (en) | 1984-07-31 | 1984-07-31 | Sample analyzing instrument and sample analyzing method using said instrument |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS6138547A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2018105793A (en) * | 2016-12-27 | 2018-07-05 | 株式会社Sumco | Decomposition method of quartz sample, method for analyzing metal contamination of quartz sample and manufacturing method of quartz member |
-
1984
- 1984-07-31 JP JP15904284A patent/JPS6138547A/en active Granted
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2018105793A (en) * | 2016-12-27 | 2018-07-05 | 株式会社Sumco | Decomposition method of quartz sample, method for analyzing metal contamination of quartz sample and manufacturing method of quartz member |
Also Published As
Publication number | Publication date |
---|---|
JPS6138547A (en) | 1986-02-24 |
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