JPH0135780B2 - - Google Patents
Info
- Publication number
- JPH0135780B2 JPH0135780B2 JP58146684A JP14668483A JPH0135780B2 JP H0135780 B2 JPH0135780 B2 JP H0135780B2 JP 58146684 A JP58146684 A JP 58146684A JP 14668483 A JP14668483 A JP 14668483A JP H0135780 B2 JPH0135780 B2 JP H0135780B2
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- crucible
- nitrogen
- glass
- present
- 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
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 37
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 230000003628 erosive effect Effects 0.000 claims description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 14
- 239000010703 silicon Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
- 238000000137 annealing Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910017464 nitrogen compound Inorganic materials 0.000 description 2
- 150000002830 nitrogen compounds Chemical class 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/045—Silicon oxycarbide, oxynitride or oxycarbonitride glasses
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Glass Compositions (AREA)
Description
産業上の利用分野
本発明は、耐溶損性石英ガラスからなる単結晶
引上用ルツボに関するものである。
従来の技術
従来から石英ガラスは、半導体工業や化学工業
等で溶融ルツボとして幅広く使用されている。
その中で、シリコン単結晶引上用ルツボとして
使用される場合には、石英ガラスが溶融シリコン
により溶損されることによりSiO混入による酸素
量の制御が困難であつた。
発明が解決しようとする問題点
以上のことから、溶融シリコンに対する耐溶損
性の優れた石英ガラスルツボが望まれていた。
また、従来の石英ガラス製のルツボは、石英ガ
ラス中に微細なクラツクが発生して割れ易いとい
う欠点も有していた。従来の石英ガラスの強度
は、理論強度の約1/200から1/400程度であり、石
英ガラスに強度をもたせるためにアニール等の物
理的強化法を施したり、原料および製品を高純度
にして、不純物が原因で発生する微細なクラツク
を防止していた。
しかし、アニール等による物理的強化法は時間
や熱量などが多くかかるわりには強度の向上はそ
れ程ではなく、あまり効果的なものではなかつ
た。また、原料および製品を高純度にする強化法
にも限界があり、強度向上のための根本的な対策
ではなかつた。このため、従来の石英ガラス製の
ルツボでは、割れによる故障も大きな障害となつ
ていた。
発明の目的
本発明は、上記の実情に鑑みてなされたもので
あり、耐溶損性に優れて割れにくいシリコン単結
晶引上用石英ガラスルツボを提供することを目的
とするものである。
問題点を解決するための手段
本発明は、石英ガラス中の窒素含有量が0.5か
ら20重量％である耐溶損性石英ガラスからなるシ
リコン単結晶引上用ルツボである。
発明の効果
本発明は上記のように構成されているので、ル
ツボを構成する石英ガラス中に窒素−ケイ素結合
が導入され、この窒素−ケイ素結合によつて高密
度で耐溶損性に優れたルツボが得られるものであ
る。
本発明のシリコン単結晶引上用ルツボは、石英
ガラス中の窒素含有量を変化させることにより、
単結晶引上工程においてシリコン単結晶に溶け込
む酸素の量を制御することができる。
この窒素−ケイ素結合を有する本発明のルツボ
は、耐酸および耐アルカリ特性にも優れており、
強度的にも優れているため、シリコン単結晶引上
用ルツボだけでなく、光学ガラス溶融ルツボやそ
の他の化学工業分野にも広く使用できるものであ
る。
本発明者は石英ガラスの密度向上のため鋭意研
究した結果、石英ガラス中の酸素原子を窒素原子
と置き換えて、−Si−Ｏ−Si−を
INDUSTRIAL APPLICATION FIELD The present invention relates to a single crystal pulling crucible made of erosion-resistant quartz glass. BACKGROUND ART Conventionally, quartz glass has been widely used as a melting crucible in the semiconductor industry, chemical industry, etc. Among these, when used as a crucible for pulling silicon single crystals, it has been difficult to control the amount of oxygen due to mixing of SiO because the quartz glass is eroded and damaged by molten silicon. Problems to be Solved by the Invention In light of the above, a quartz glass crucible with excellent erosion resistance against molten silicon has been desired. Further, conventional crucibles made of quartz glass have the disadvantage that they are easily broken due to the occurrence of minute cracks in the quartz glass. The strength of conventional quartz glass is about 1/200 to 1/400 of the theoretical strength, and in order to give quartz glass strength, physical strengthening methods such as annealing are applied, and raw materials and products are made to have high purity. This prevents minute cracks caused by impurities. However, although physical strengthening methods such as annealing require a large amount of time and heat, the improvement in strength is not that great, and is not very effective. In addition, there are limits to strengthening methods that improve the purity of raw materials and products, and they have not been fundamental measures to improve strength. For this reason, failure due to cracking has been a major problem with conventional silica glass crucibles. Purpose of the Invention The present invention has been made in view of the above-mentioned circumstances, and an object of the present invention is to provide a quartz glass crucible for pulling a silicon single crystal that has excellent erosion resistance and is difficult to break. Means for Solving the Problems The present invention is a crucible for pulling silicon single crystals made of erosion-resistant quartz glass in which the nitrogen content in the quartz glass is 0.5 to 20% by weight. Effects of the Invention Since the present invention is configured as described above, a nitrogen-silicon bond is introduced into the quartz glass constituting the crucible, and this nitrogen-silicon bond provides a crucible with high density and excellent corrosion resistance. is obtained. The crucible for pulling silicon single crystals of the present invention has the following properties:
The amount of oxygen dissolved in the silicon single crystal in the single crystal pulling process can be controlled. The crucible of the present invention having this nitrogen-silicon bond also has excellent acid and alkali resistance properties,
Because of its excellent strength, it can be widely used not only in crucibles for pulling silicon single crystals, but also in optical glass melting crucibles and other chemical industry fields. As a result of intensive research to improve the density of silica glass, the inventor replaced the oxygen atoms in silica glass with nitrogen atoms to create -Si-O-Si-.
【式】
にして、耐溶損性に優れたものにすることができ
ることを見出だしたものである。
石英ガラス中の窒素含有量を0.5から20重量％
に限定した理由は、窒素含有量が0.5重量％より
も低いと、耐溶損性に何ら変化が現れず耐溶損性
の石英ガラスを得ることができず、また窒素含有
量が20重量％よりも大きいと、石英ガラス中に泡
やクラツクが発生し耐溶損性が劣つてしまうため
である。
石英ガラス中に窒素を含有させるには、例えば
Si3N4やBN等の窒素化合物を窒素雰囲気中で石
英と同時に溶融させる。窒素化合物としては、前
記化合物に限定されるものではなく、石英ガラス
中に0.5から20重量％の窒素を含有させるもので
あれば何でもよい。
以下、実施例を挙げて本発明のシリコン単結晶
引上用ルツボをより具体的に説明する。
実施例 １
タングステンヒーターをもつモリブデン製の炉
に水晶粉と窒化珪素を入れ、一酸化炭素、窒素雰
囲気に置換した後に密閉して炉内を５から10気圧
にする。徐々に炉内温度を上昇させ2200℃に保持
する。数時間後、炉内部のガスを抜き２気圧まで
下げた後、炉の下部から溶融した石英ガラスを取
り出し、自然放冷し、本発明のルツボを構成する
耐溶損性石英ガラスを製造した。この石英ガラス
のブロツクをを酸水素炎で加工して種々のルツボ
を作るのであるが、加工する際に放出される窒素
の量は極く少量（0.5％以下）であつた。
このようにして製造した本発明の耐溶損性石英
ガラスからなるシリコン単結晶引上用ルツボにつ
いて、窒素含有量、耐溶損性および硬度を測定し
た。その結果を第１表に示す。耐溶損性の試験
は、φ20mmの石英ガラスルツボにシリコン10ｇを
入れ、1440℃で数時間（１時間、４時間）溶融し
て、石英ガラスの溶損量を測定することによつて
行つた。また、硬度はビツカース硬度計により測
定した。
実施例 ２
実施例１と同様の炉に、ケイ砂と窒化ボロンを
入れ、実施例１と同様の方法により本発明の耐溶
損性石英ガラスからなるシリコン単結晶引上用ル
ツボを製造した。
こうして得られた本発明の耐溶損性石英ガラス
からなるシリコン単結晶引上用ルツボについて
も、窒素含有量、耐溶損性および硬度を測定し
た。その結果を第１表に示す。
比較例
比較のために、窒素を含有していない従来の石
英ガラス（比較例１）と、窒素含有量が30重量％
の石英ガラス（比較例２）についても耐溶損性お
よび硬度を測定した。その結果を第１表に示す。
窒素含有量が30重量％のものは、石英ガラス中
に泡が多くクラツクが発生した。It has been discovered that it is possible to obtain a material with excellent erosion resistance by using the following formula. Nitrogen content in quartz glass from 0.5 to 20% by weight
The reason for this limitation is that if the nitrogen content is lower than 0.5% by weight, there will be no change in erosion resistance and it will not be possible to obtain fused silica glass with nitrogen content lower than 20% by weight. If it is too large, bubbles and cracks will occur in the quartz glass, resulting in poor erosion resistance. In order to contain nitrogen in quartz glass, for example,
Nitrogen compounds such as Si 3 N 4 and BN are melted simultaneously with quartz in a nitrogen atmosphere. The nitrogen compound is not limited to the above-mentioned compounds, and any compound may be used as long as it contains 0.5 to 20% by weight of nitrogen in the quartz glass. EXAMPLES Hereinafter, the crucible for pulling a silicon single crystal of the present invention will be described in more detail with reference to Examples. Example 1 Quartz crystal powder and silicon nitride are placed in a molybdenum furnace equipped with a tungsten heater, and after replacing the atmosphere with carbon monoxide and nitrogen, the furnace is sealed and the inside of the furnace is brought to 5 to 10 atmospheres. Gradually raise the temperature inside the furnace and maintain it at 2200℃. After several hours, the gas inside the furnace was removed and the pressure was lowered to 2 atmospheres, and then the molten quartz glass was taken out from the lower part of the furnace and allowed to cool naturally to produce melt-resistant quartz glass that constitutes the crucible of the present invention. Various crucibles are made by processing this quartz glass block with an oxyhydrogen flame, but the amount of nitrogen released during processing is extremely small (less than 0.5%). The nitrogen content, erosion resistance, and hardness of the silicon single crystal pulling crucible made of the erosion-resistant quartz glass of the present invention thus manufactured were measured. The results are shown in Table 1. The erosion resistance test was carried out by placing 10 g of silicon in a 20 mm diameter quartz glass crucible, melting it at 1440° C. for several hours (1 hour, 4 hours), and measuring the amount of erosion of the quartz glass. Further, the hardness was measured using a Bitkers hardness meter. Example 2 Silica sand and boron nitride were placed in the same furnace as in Example 1, and a silicon single crystal pulling crucible made of the melt-resistant quartz glass of the present invention was manufactured in the same manner as in Example 1. The nitrogen content, erosion resistance, and hardness of the silicon single crystal pulling crucible made of the erosion-resistant quartz glass of the present invention thus obtained were also measured. The results are shown in Table 1. Comparative Example For comparison, a conventional quartz glass containing no nitrogen (Comparative Example 1) and a glass glass with a nitrogen content of 30% by weight are used.
The erosion resistance and hardness of the quartz glass (Comparative Example 2) were also measured. The results are shown in Table 1. When the nitrogen content was 30% by weight, there were many bubbles in the quartz glass and cracks occurred.
Claims (1)
である耐溶損性石英ガラスからなるシリコン単結
晶引上用ルツボ。1 Nitrogen content of quartz glass is 0.5 to 20% by weight
A crucible for pulling silicon single crystals made of erosion-resistant quartz glass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14668483A JPS6042244A (en) | 1983-08-12 | 1983-08-12 | Quartz glass having resistance to melting loss |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14668483A JPS6042244A (en) | 1983-08-12 | 1983-08-12 | Quartz glass having resistance to melting loss |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6042244A JPS6042244A (en) | 1985-03-06 |
| JPH0135780B2 true JPH0135780B2 (en) | 1989-07-27 |
Family
ID=15413244
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14668483A Granted JPS6042244A (en) | 1983-08-12 | 1983-08-12 | Quartz glass having resistance to melting loss |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6042244A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63206329A (en) * | 1987-02-20 | 1988-08-25 | Sunao Tsunetomi | Production of glass causing crystallite |
| JPH01172239A (en) * | 1987-04-24 | 1989-07-07 | Tosoh Corp | High-hardness quartz glass and its production |
| JPH03223136A (en) * | 1990-01-26 | 1991-10-02 | Shimadzu Corp | Production of oxynitride glass and glass fiber therefrom |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5087339A (en) * | 1973-11-27 | 1975-07-14 | ||
| JPS53113817A (en) * | 1977-03-17 | 1978-10-04 | Toshiba Ceramics Co | Quartz glass crucible for pulling up single crysal of silicon |
| JPS54157779A (en) * | 1978-06-02 | 1979-12-12 | Toshiba Corp | Production of silicon single crystal |
| JPS5832037A (en) * | 1981-08-13 | 1983-02-24 | Nippon Telegr & Teleph Corp <Ntt> | Preparation of glass containing additive |
-
1983
- 1983-08-12 JP JP14668483A patent/JPS6042244A/en active Granted
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5087339A (en) * | 1973-11-27 | 1975-07-14 | ||
| JPS53113817A (en) * | 1977-03-17 | 1978-10-04 | Toshiba Ceramics Co | Quartz glass crucible for pulling up single crysal of silicon |
| JPS54157779A (en) * | 1978-06-02 | 1979-12-12 | Toshiba Corp | Production of silicon single crystal |
| JPS5832037A (en) * | 1981-08-13 | 1983-02-24 | Nippon Telegr & Teleph Corp <Ntt> | Preparation of glass containing additive |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6042244A (en) | 1985-03-06 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |