JPS61144545A - Device for dissolving thin film or thin sheet - Google Patents
Device for dissolving thin film or thin sheetInfo
- Publication number
- JPS61144545A JPS61144545A JP59267185A JP26718584A JPS61144545A JP S61144545 A JPS61144545 A JP S61144545A JP 59267185 A JP59267185 A JP 59267185A JP 26718584 A JP26718584 A JP 26718584A JP S61144545 A JPS61144545 A JP S61144545A
- Authority
- JP
- Japan
- Prior art keywords
- liquid
- thin film
- vessel
- dissolving
- thin
- 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
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
Abstract
Description
【発明の詳細な説明】 〔発明の技術分野〕 本発明は、薄膜薄板溶解装置に関する。[Detailed description of the invention] [Technical field of invention] The present invention relates to a thin film and plate melting apparatus.
半導体基板上に形成された酸化膜等の薄膜や薄板中の極
微量の不純物の濃度を測定する手段として、原子吸光分
析や誘導結合プラズマ発光分析が行われている。このよ
うな分析を行うには、薄膜或は薄板からなる固体試料を
溶解して液体試料を作る必要がある。この場合分析精度
を高めるためには、液体試料が汚染しないようにするこ
とが重要である。このため薄膜や薄板中の不純物の濃度
を測定する手段として、従来、気相分解法や液中分解法
が行われている。Atomic absorption spectrometry and inductively coupled plasma emission spectrometry are used as means for measuring the concentration of extremely small amounts of impurities in thin films and thin plates such as oxide films formed on semiconductor substrates. To perform such an analysis, it is necessary to dissolve a solid sample consisting of a thin film or plate to create a liquid sample. In this case, in order to improve analysis accuracy, it is important to prevent the liquid sample from becoming contaminated. For this reason, gas phase decomposition methods and liquid decomposition methods have conventionally been used as means for measuring the concentration of impurities in thin films and thin plates.
気相分解法は、７ツ化水素の蒸気で薄膜を溶解し、溶解
液を回収して希釈秤量して分析試料液を作る。この分析
試料液を７レームレス原子吸光にかけて分析し、薄膜中
の不純物の濃度を測定するものである。この手段では薄
膜の分解を常温で行うため、７ツ化水素の蒸発速度が遅
く、薄膜の分解に長い時間がかかる。しかも、得られる
分解液は高濃度であっても１００μＬ程度の微量である
ため、フレームレス原子吸光で分析するには２〜．３倍
に希釈して秤量しなければならない。その結果、極めて
作業性が悪い。In the gas phase decomposition method, a thin film is dissolved with hydrogen heptadide vapor, and the dissolved solution is collected, diluted, and weighed to prepare an analysis sample solution. This analytical sample liquid is subjected to 7 frameless atomic absorption and analyzed to measure the concentration of impurities in the thin film. In this method, since the thin film is decomposed at room temperature, the evaporation rate of hydrogen heptadide is slow and it takes a long time to decompose the thin film. Moreover, even if the resulting decomposed solution is highly concentrated, it is only a small amount of about 100 μL, so it is difficult to analyze it by flameless atomic absorption. It must be diluted 3 times and weighed. As a result, workability is extremely poor.
液中分解法は、溶解液に試料全体を浸漬して薄膜、薄板
を溶解し、得られた溶解液を直接分析装置にかけて不純
物の濃度を測定するものである。この手段では、溶解液
の量が多すぎるために１１．膜、薄板の分解時間を短く
できるが、不純物の濃度が低くなるため、気相分解法に
比べて分析の際の感度が２桁以上低下する問題がある。In the liquid decomposition method, the entire sample is immersed in a solution to dissolve the thin film or thin plate, and the resulting solution is directly applied to an analyzer to measure the concentration of impurities. 11. With this method, the amount of solution is too large. Although the decomposition time of membranes and thin plates can be shortened, the concentration of impurities is lowered, so there is a problem that the sensitivity during analysis is lowered by more than two orders of magnitude compared to the gas phase decomposition method.
本発明は、薄膜薄板の分解液を溶解試薬や環境からの汚
染を防止して、しかも高い作業性の下に容易に得ること
ができる薄膜薄板溶解装置を提供することをその目的と
するものである。SUMMARY OF THE INVENTION An object of the present invention is to provide a thin film/plate dissolving device that can easily obtain a thin film/plate decomposition solution with high workability while preventing contamination from dissolving reagents and the environment. be.
本発ＦｊＡは、薄膜、薄板の分解液をフッ素樹脂或は合
成石英からなる密閉容器中で得るようＫして分解液の汚
染を防止すると共に、溶解液の量を蒸発によって少なく
して分解液を高濃度に濃縮し、かつ、溶解部と加熱部を
分離可能にして分解液の回収、供給を容易にして作業性
の向上を達した薄膜薄板溶解装置である。The developed FjA prevents contamination of the decomposition liquid by obtaining the decomposition liquid for thin films and thin plates in a closed container made of fluororesin or synthetic quartz, and also reduces the amount of the dissolution liquid by evaporation. This is a thin film and plate melting device that concentrates the decomposition liquid to a high concentration, and also makes it possible to separate the melting section and the heating section, making it easy to collect and supply the decomposed liquid, thereby improving workability.
以下、本発明の一実施例について図面を参照して説明す
る。第１図中１は、上部を開口した溶解容器である。関
口部には、蓋体２が着脱自在に設けられている。溶解容
器１及び蓋体２は、７ツ素樹脂或は合成石英で形成され
ている。溶解容器１の内部は、幅が１−以下に設定され
てお）、半導体基板３の表面に酸化膜等の薄膜４や薄板
が形成された試料が立設した状態で収容できるようにな
りている。溶解容器１内の底部には、薄膜４を溶解する
ための７．化水素酸からなる溶解液５が例えば濃度約５
０チのもので１ ｍｔ程度収容されている。溶解容器１
は、加熱用プレートヒータ６を内蔵した加熱容器７内に
、密着した状態で出入れ自在にして収容されている。An embodiment of the present invention will be described below with reference to the drawings. 1 in FIG. 1 is a dissolution container with an open top. A lid body 2 is removably provided at the entrance. The melting container 1 and the lid 2 are made of heptadium resin or synthetic quartz. The inside of the dissolution container 1 is set to have a width of 1- or less), so that a sample in which a thin film 4 or a thin plate such as an oxide film is formed on the surface of a semiconductor substrate 3 can be stored in an upright state. There is. At the bottom of the dissolution container 1, there is a 7. for dissolving the thin film 4. For example, the solution 5 made of hydrohydric acid has a concentration of about 5
The capacity is approximately 1 mt. Melting container 1
is housed in a heating container 7 in which a heating plate heater 6 is built, so that it can be taken in and out in close contact with the heating container 7.
このように構成された薄膜薄板溶解装置１０によれば、
例えば厚さ約５ｏｏｏｌの酸化膜からなる薄膜４を表面
に形成した半導体基板３をその底部が溶解液５に浸漬す
るようにして溶解容器１内に設置する。次いで、開口部
を蓋体２で塞いでから溶解容器１を加熱容器７内に収容
する。次に、加熱用グレートヒータ６で溶解液５を加熱
して蒸発させ、その蒸気で薄膜４を分解１１Ｌ８に分解
する。薄膜４の溶解が終了したところで溶解容器１を第
２図に示す如く、加熱容器１から取出し、放冷する。溶
解容器１ｔ−冷却する方法としては、純水を満した水槽
中に溶解容器１を浸漬するようにしても良い。次いで、
溶解液５が十分に冷却して再蒸発しなくなったところで
溶解容器ｌ内に溜った分解液８を７レ一ムレス原子吸光
分析装置にかけて不純物の濃度測定を行う。According to the thin film/plate melting apparatus 10 configured in this way,
For example, a semiconductor substrate 3 having a thin film 4 formed of an oxide film with a thickness of about 5 mm on its surface is placed in a dissolving container 1 so that its bottom is immersed in a dissolving solution 5 . Next, after the opening is closed with the lid 2, the melting container 1 is placed in the heating container 7. Next, the solution 5 is heated and evaporated using the heating grate heater 6, and the thin film 4 is decomposed into decomposition 11L8 using the vapor. When the melting of the thin film 4 is completed, the melting container 1 is taken out from the heating container 1 as shown in FIG. 2 and allowed to cool. As a method for cooling the dissolving container 1t, the dissolving container 1 may be immersed in a water tank filled with pure water. Then,
When the dissolution liquid 5 has sufficiently cooled and no longer evaporates, the decomposition liquid 8 accumulated in the dissolution container 1 is subjected to a 7-remless atomic absorption spectrometer to measure the concentration of impurities.
このようにこの薄膜薄板溶解装置１０では、フッ素樹脂
或は合成石英で形成された循閉型の溶解容器１中で薄膜
４の分解を行うので、分解液８が汚染されるのを阻止す
ることができる。In this way, in this thin film/plate melting apparatus 10, the thin film 4 is decomposed in the circulating type melting container 1 made of fluororesin or synthetic quartz, so that it is possible to prevent the decomposition liquid 8 from being contaminated. I can do it.
また、分解′１ｆＬｓｔ−得る際には、溶＃１に５が蒸
発するので濃縮作用によって高濃既の分解液８を得るこ
とができる。このため分析精度を高めることができる。Furthermore, when obtaining decomposition '1fLst-, 5 is evaporated into solution #1, so a highly concentrated decomposition solution 8 can be obtained by the concentration effect. Therefore, analysis precision can be improved.
また、得られた分解液８は、溶解容器１を加熱容器７か
ら取出して直接分析装置に供給できるので、作業性を向
上させることができる。更に、分解液８の作成及び回収
、供給は、全て分解液８を密閉された溶解容器１内に収
容した状態で行われるので、分解速涙を高めると共に、
外部からの汚染を完全に阻止して行うことができる。Further, the obtained decomposed liquid 8 can be taken out of the dissolution container 1 from the heating container 7 and directly supplied to the analyzer, so that workability can be improved. Furthermore, since the preparation, recovery, and supply of the decomposition liquid 8 are all performed while the decomposition liquid 8 is contained in the sealed dissolution container 1, the decomposition rate is increased, and the decomposition rate is increased.
This can be done while completely preventing contamination from the outside.
因みに、実施例の薄膜薄板溶解装置１０では、薄膜４が
厚さ約１００００ Ｘ（Ｄ ＬＰＣＶＤ −Ｓｔ、Ｎ４
膜の場合、その分解時間は第３図に特性！１ｉ１１にて
示す如く、約２０分であ夛、薄膜４が同じ厚さの熱酸化
ｓｉｏ□膜の場合は同図に特性線■にて示す如く、約１
０分であることが実験的に確認された。これに対して同
様の実験を従来の気相分解法で行ったところＬＰＧＶＤ
−８１，Ｎ４膜の場合は、同図に特性線■で示す如く
、約１００分の分解時間を必要とし、熱酸化ＳｉＯ□膜
の場合は同図に特性線■にて示す如く、約４５分の分解
時間を要することが判りた。Incidentally, in the thin film thin plate melting apparatus 10 of the example, the thin film 4 has a thickness of about 10000 X (D LPCVD -St, N4
In the case of a membrane, its decomposition time is shown in Figure 3. 1i11, it takes about 20 minutes, and when the thin film 4 is a thermally oxidized sio
It was experimentally confirmed that the time was 0 minutes. On the other hand, when similar experiments were conducted using the conventional gas phase decomposition method, LPGV
-81,N4 film requires about 100 minutes of decomposition time, as shown by the characteristic line ■ in the figure, and in the case of thermally oxidized SiO□ film, it takes about 45 minutes to decompose, as shown by the characteristic line It was found that the disassembly time required was several minutes.
また、実施例の薄膜薄板溶解装置１０で得られた熱酸化
８１０□膜の分解液を７レームレス原子吸光法で分析し
たところ、不純物Ｆ・の濃度は３ Ｘ １０１２ａ ｔ
ｏｍ８／２ｍ３であバネ鈍物Ｎａの濃度はＩ Ｘ １
０ ａｔｏｍｓ／Ｉｎであることが判った。これらの
値から分析の除の検出限界は、従来の液中分解法に比べ
て約１桁向上していることが明らかとなった。In addition, when the decomposition liquid of the thermally oxidized 810□ film obtained in the thin film thin plate melting apparatus 10 of the example was analyzed by 7 frameless atomic absorption spectrometry, the concentration of impurity F was 3 x 1012a t.
om8/2m3 and the concentration of spring blunt Na is I x 1
It was found to be 0 atoms/In. These values revealed that the detection limit of analysis was improved by about one order of magnitude compared to the conventional in-liquid decomposition method.
以上説明した如く、本発明に係る薄膜薄板溶解装置によ
れば、薄膜薄板の分解液を溶解試薬や環境からの汚染を
防止して、しかも高い作業性の下に容易に得ることがで
きるものである。As explained above, according to the thin film and plate dissolving apparatus according to the present invention, it is possible to easily obtain a decomposed solution of a thin film and plate while preventing contamination from the dissolving reagent and the environment, and with high workability. be.
第１図は、本発明の一実施例の薄膜薄板溶解装置で薄膜
を溶解している状態を示す説明図、第２図は、同薄膜薄
板溶解装置から密閉容器部を取外した状態を示す説明図
、第３図は、溶解所要時間と十堺体薄膜の厚さとの関係
を示す特性図である。
１・・・溶解容器、２・・・蓋体、３・・・半導体基板
、４・・・薄膜、５・・・溶解液、６−・・加熱用プレ
ートヒータ、７・・・加熱容器、８・・・分解液、１０
・・・薄膜薄板溶解装置。FIG. 1 is an explanatory diagram showing a state in which a thin film is being melted by a thin film/sheet melting apparatus according to an embodiment of the present invention, and FIG. 2 is an explanatory diagram showing a state in which a closed container part is removed from the thin film/sheet melting apparatus. 3 are characteristic diagrams showing the relationship between the time required for dissolution and the thickness of the ten-dimensional thin film. DESCRIPTION OF SYMBOLS 1... Melting container, 2... Lid body, 3... Semiconductor substrate, 4... Thin film, 5... Solving liquid, 6-... Plate heater for heating, 7... Heating container, 8... Decomposition liquid, 10
...Thin film and plate melting equipment.
Claims (1)
理体の溶解液が収容される密閉型の溶解容器と、該溶解
容器に着脱自在に取付けられた蓋体と、該溶解容器を略
密着した状態で出入自在に収容する加熱容器と、該加熱
容器に内蔵されたヒータとを具備することを特徴とする
薄膜薄板溶解装置。A closed type dissolution container in which a sample on which a thin film or thin plate, which is an object to be processed is formed, and a solution of the object to be processed are accommodated; a lid detachably attached to the dissolution container; 1. A thin film and plate melting apparatus comprising: a heating container which is accommodated in a state of substantially close contact with each other so as to be freely accessible and removable; and a heater built into the heating container.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59267185A JPS61144545A (en) | 1984-12-18 | 1984-12-18 | Device for dissolving thin film or thin sheet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59267185A JPS61144545A (en) | 1984-12-18 | 1984-12-18 | Device for dissolving thin film or thin sheet |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS61144545A true JPS61144545A (en) | 1986-07-02 |
Family
ID=17441289
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59267185A Pending JPS61144545A (en) | 1984-12-18 | 1984-12-18 | Device for dissolving thin film or thin sheet |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61144545A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01301142A (en) * | 1988-03-17 | 1989-12-05 | Toshiba Corp | Semiconductor decomposing device |
| WO1991012631A1 (en) * | 1990-02-19 | 1991-08-22 | Purex Co., Ltd. | Semiconductor wafer sample container and sample preparation method |
| JPH05259146A (en) * | 1992-03-09 | 1993-10-08 | Hitachi Ltd | Semiconductor manufacturing apparatus |
| JP2006032859A (en) * | 2004-07-21 | 2006-02-02 | Siltronic Japan Corp | Removal method and analysis method of impurity in silicon wafer |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5310974A (en) * | 1976-07-17 | 1978-01-31 | Mitsubishi Electric Corp | Etching method of oxide film |
| JPS55125632A (en) * | 1979-03-23 | 1980-09-27 | Fujitsu Ltd | Etching |
-
1984
- 1984-12-18 JP JP59267185A patent/JPS61144545A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5310974A (en) * | 1976-07-17 | 1978-01-31 | Mitsubishi Electric Corp | Etching method of oxide film |
| JPS55125632A (en) * | 1979-03-23 | 1980-09-27 | Fujitsu Ltd | Etching |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01301142A (en) * | 1988-03-17 | 1989-12-05 | Toshiba Corp | Semiconductor decomposing device |
| WO1991012631A1 (en) * | 1990-02-19 | 1991-08-22 | Purex Co., Ltd. | Semiconductor wafer sample container and sample preparation method |
| US5284802A (en) * | 1990-02-19 | 1994-02-08 | Purex Co., Ltd. | Container for semiconductor wafer sample and method of preparing sample |
| JPH05259146A (en) * | 1992-03-09 | 1993-10-08 | Hitachi Ltd | Semiconductor manufacturing apparatus |
| JP2006032859A (en) * | 2004-07-21 | 2006-02-02 | Siltronic Japan Corp | Removal method and analysis method of impurity in silicon wafer |
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