JP4471692B2 - Method for manufacturing container for melting silicon having release layer - Google Patents
Method for manufacturing container for melting silicon having release layer Download PDFInfo
- Publication number
- JP4471692B2 JP4471692B2 JP2004090562A JP2004090562A JP4471692B2 JP 4471692 B2 JP4471692 B2 JP 4471692B2 JP 2004090562 A JP2004090562 A JP 2004090562A JP 2004090562 A JP2004090562 A JP 2004090562A JP 4471692 B2 JP4471692 B2 JP 4471692B2
- Authority
- JP
- Japan
- Prior art keywords
- container
- silicon
- release layer
- slurry
- powder
- 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 - Fee Related
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Description
本発明は、シリコンインゴットを製造する際に使用するシリコンの溶融及び保持のための容器、特に、離型層付きのシリコン溶融用容器の製造方法に関する。 The present invention relates to a container for melting and holding silicon used for manufacturing a silicon ingot, and more particularly to a method for manufacturing a container for melting silicon with a release layer.
シリコン溶融用容器は、太陽電池用多結晶シリコンなどを製造する際のシリコンの溶融用容器、具体的には鋳型容器、もしくは、金属シリコンを溶融、清浄化後に鋳造工場に運搬する際の運搬用容器として、さらには、シリコン浴湯を注湯までの間保持しておくための保持容器として使用されるものである。 The silicon melting container is a container for melting silicon when manufacturing polycrystalline silicon for solar cells, specifically, a mold container, or for transporting metal metal to a foundry after melting and cleaning. The container is further used as a holding container for holding silicon bath water until pouring.
近年、太陽光をエネルギー源として利用することが盛んに行われるようになってきており、太陽電池の材料として多結晶シリコンが実用化されてきている。多結晶シリコンは、溶融シリコンを冷却固化して多結晶シリコンのインゴットとして製造されるが、鋳造の際に溶融シリコンを入れる鋳型容器としてシリコン溶融用容器が使用されている。 In recent years, sunlight has been actively used as an energy source, and polycrystalline silicon has been put into practical use as a material for solar cells. Polycrystalline silicon is manufactured as an ingot of polycrystalline silicon by cooling and solidifying molten silicon, and a silicon melting container is used as a mold container into which molten silicon is placed during casting.
抵抗加熱、または、高周波誘導加熱などにより溶融されたシリコンが、シリコン溶融用容器中で冷却固化されてシリコンインゴットとなるが、シリコンインゴットが容器に付着し、冷却時にインゴットが割れてしまうという問題があった。 Silicon melted by resistance heating or high-frequency induction heating is cooled and solidified in a silicon melting container to become a silicon ingot, but the silicon ingot adheres to the container and the ingot breaks during cooling. there were.
このため、多結晶シリコンインゴットを製造する場合、シリコン溶融用容器にあらかじめ離型剤を塗布し、離型層を容器内面に形成してシリコン融液の凝固の際のシリコンインゴットと容器との付着を防止していた。 For this reason, when manufacturing a polycrystalline silicon ingot, a release agent is applied in advance to a silicon melting vessel, and a release layer is formed on the inner surface of the vessel to adhere the silicon ingot to the vessel during the solidification of the silicon melt. Was preventing.
容器の素材は、グラファイトや窒化ホウ素、溶融シリカなどが使用され、離型剤は炭化珪素や窒化珪素、酸化イットリウムなどにポリビニルアルコールなどのバインダーを含ませたスラリー状のものを容器内表面に塗布して焼成し、容器内面に離型層を形成していた。
しかしながら、前述した離型剤を容器内面にコーティングして離型層を形成したものは、炭化物、酸化物、または、窒化物といった離型剤自体が難焼結性であるため、容器内面への付着強度が弱く、部分的に剥離するという欠点があった。
離型層が剥離した個所においてはシリコンインゴットが容器に付着して凝固の際にクラックが生じたり、割れたりする危険性が高くなる。しかも、剥離した離型層は、そのままシリコン融液中に混入してしまい、溶融シリコン中に不純物として取り込まれ、シリコンインゴットの純度を低下させるといった問題を生じさせていた。
However, in the case where the release agent is coated on the inner surface of the container to form the release layer, the release agent itself such as carbide, oxide, or nitride is difficult to sinter. Adhesion strength was weak, and there was a drawback that it partially peeled off.
Where the release layer is peeled off, the silicon ingot adheres to the container and there is a high risk of cracking or breaking during solidification. In addition, the peeled release layer is directly mixed into the silicon melt, and is taken in as an impurity in the molten silicon, causing a problem that the purity of the silicon ingot is lowered.
また、窒化珪素は金属元素を含まないため、溶融シリコンとの非反応性にも優れており、離型剤として優れた材料といえるが、窒化珪素自体は焼結性に乏しい上に、機械強度を実用レベルのものにするには、ホットプレスやＨＩＰなどによる成形・焼結の処理が不可欠であり、生産性が低いという問題があった。 Also, since silicon nitride does not contain a metal element, it is excellent in non-reactivity with molten silicon and can be said to be an excellent material as a release agent, but silicon nitride itself has poor sinterability and mechanical strength. In order to achieve a practical level, it is indispensable to perform a molding / sintering process by hot pressing, HIP, or the like, resulting in a problem of low productivity.
すなわち、シリコンインゴットに要求される品質が高品位になればなるほど、容器内面に形成する離型層の離型性能を向上させて製造される製品の歩留り向上、また離型層の容器への付着強度を向上させて離型層の剥離を防止してシリコンインゴットの汚染防止を図る必要が生じ、これらの問題の解決が求められていた。 In other words, the higher the quality required for a silicon ingot, the higher the yield of manufactured products by improving the release performance of the release layer formed on the inner surface of the container, and the adhesion of the release layer to the container There has been a need to improve the strength and prevent the release layer from being peeled to prevent the silicon ingot from being contaminated, and there has been a need to solve these problems.
本発明は、離型層のシリコン溶融用容器への付着強度を向上させて離型層の剥離を防止し、シリコン溶融用容器のシリコン融液との接触面に、シリコン融液と反応しにくく、しかも金属汚染が少なく、高品質・高歩留りのシリコンインゴットを得るために高価な設備を導入することなく、生産性にも優れた離型層を有するシリコン溶融用容器の製造方法を提供することを目的とする。 The present invention improves the adhesion strength of the release layer to the silicon melting vessel to prevent the release layer from peeling off, and hardly reacts with the silicon melt on the contact surface of the silicon melting vessel with the silicon melt. To provide a method for producing a silicon melting container having a release layer with excellent productivity without introducing expensive equipment to obtain a high quality and high yield silicon ingot with little metal contamination With the goal.
本発明は、こうした問題点について鋭意検討した結果、既に焼結等によって完成したシリコン溶融容器の内面に離型剤を塗布するのではなく、シリコン溶融容器を製造する工程において、粉末成型体とした時点で離型剤を塗布することで、その後の焼成工程で粉末成型体が容器に焼成されると共に、離型層が同時に焼成されて強固に容器内面に形成されるようにしたものである。 As a result of diligent investigations on these problems, the present invention is not formed by applying a mold release agent to the inner surface of a silicon melting vessel that has already been completed by sintering or the like, but in the process of manufacturing a silicon melting vessel, a powder molding is obtained. By applying the release agent at the time, the powder molded body is fired into the container in the subsequent firing step, and the release layer is simultaneously fired to be firmly formed on the inner surface of the container.
すなわち、本発明は、シリコン溶融用容器の焼成前にＳｉ、Ｓｉ3Ｎ4、ＳｉＯ2又はそれらの複合剤からなる離型剤を塗布し、容器の焼成と共に離型層を容器内面に同時に形成してシリコン溶融用容器とするものである。
離型剤は、粉末を純水またはポリビニルアルコールを溶解させた水に混合してスラリー化し、塗布、乾燥、焼結の工程を経て離型層を形成することが好ましい。容器の原料粉末が離型剤と同じく珪素を含有するものであると、珪素が仲介層となって容器と離型層との付着強度が増大するので好ましく、特に、シリカ粉末は、製造するポリシリコンの純度という観点からも望ましい。
That is, the present invention applies a release agent composed of Si, Si 3 N 4 , SiO 2 or a composite agent thereof before firing the silicon melting container, and simultaneously forms the release layer on the inner surface of the container as the container is fired. Thus, a silicon melting container is obtained.
The release agent is preferably mixed with pure water or water in which polyvinyl alcohol is dissolved to form a slurry, and a release layer is formed through steps of coating, drying, and sintering. It is preferable that the raw material powder of the container contains silicon as well as the release agent, since silicon serves as a mediating layer and the adhesion strength between the container and the release layer is increased. It is also desirable from the viewpoint of silicon purity.
離型剤スラリーは、Ｓｉ、Ｓｉ3Ｎ4、Ｓｉ3Ｎ4＋ＳｉＯ2、Ｓｉ＋Ｓｉ3Ｎ4＋ＳｉＯ2のいずれか又はそれらを組み合せたものを用い、かつそのスラリー濃度を１０〜８０質量％とする。濃度が１０％未満の場合は離型効果が減少し、８０％を超えると均一なスラリー層を固定形成できない。これにより、純度が高く、容器内面に離型層としてのシリコン化合物が強固に付着したシリコン溶融用容器を製造することができる。 As the release agent slurry, one of Si, Si 3 N 4 , Si 3 N 4 + SiO 2 , Si + Si 3 N 4 + SiO 2 or a combination thereof is used, and the slurry concentration is 10 to 80% by mass. . When the concentration is less than 10%, the mold release effect decreases, and when it exceeds 80%, a uniform slurry layer cannot be fixedly formed. As a result, a silicon melting container having high purity and having a silicon compound as a release layer firmly attached to the inner surface of the container can be produced.
Ｓｉ粉末は純度９９．９％のもの、Ｓｉ3Ｎ4は純度９９．８％、ＳｉＯ2は純度９９．９％のものを使用した。
実施例１
シリカ（ＳｉＯ2）粉末、バインダー、及び水をオムニミキサーで混合して流動性スラリーとし、ステンレス製の鋳型に振動をかけながら流し込んだ。鋳型の空洞をスラリーで満たした後、鋳型に蓋をし、スラリーで満たした鋳型を電気炉内に設置し、９０℃で３時間加熱した。
加熱後冷却して３０℃、湿度７０％の恒温恒湿度条件で２４時間保持後、鋳型の中子部分を取り除き、さらに３０℃、湿度７０％の調湿乾燥機で５日間乾燥させてシリカ粉末からなる４００ｍｍ×４００ｍｍ×４００ｍｍ、厚さ１５ｍｍの角型形状の容器を成型した。１Ｌポリ容器にスターラーチップを入れ、Ｓｉ3Ｎ4（９０ｇ）、純水（２１０ｇ）をマグネッチックスターラーで１０分間攪拌混合して濃度３０％のスラリーとした。このスラリーをエアーブラシタンクに充填し、成型した保持容器内面に均一に塗布して乾燥させた後、焼成炉内で１２００℃で焼成し、内面に離型層が形成された溶融シリコン用容器を得た。
Si powder having a purity of 99.9%, Si 3 N 4 having a purity of 99.8%, and SiO 2 having a purity of 99.9% were used.
Example 1
Silica (SiO 2 ) powder, binder, and water were mixed with an omni mixer to form a fluid slurry, and poured into a stainless steel mold while being vibrated. After the mold cavity was filled with the slurry, the mold was capped, and the mold filled with the slurry was placed in an electric furnace and heated at 90 ° C. for 3 hours.
After heating and cooling and holding at constant temperature and humidity conditions of 30 ° C and 70% humidity for 24 hours, the core part of the mold is removed, and further dried for 5 days in a humidity dryer at 30 ° C and 70% humidity to obtain silica powder. A rectangular container having a shape of 400 mm × 400 mm × 400 mm and a thickness of 15 mm was formed. A stirrer chip was placed in a 1 L plastic container, and Si 3 N 4 (90 g) and pure water (210 g) were stirred and mixed with a magnetic stirrer for 10 minutes to obtain a slurry having a concentration of 30%. This slurry is filled in an airbrush tank, uniformly applied to the inner surface of the molded holding container and dried, and then fired at 1200 ° C. in a firing furnace, and a molten silicon container having a release layer formed on the inner surface is obtained. Obtained.
実施例２
実施例１と同様に製作した乾燥シリカ粉末を成型した容器に、実施例１に準じて作製したＳｉ3Ｎ4粉末と水とを混合溶解した濃度５０％のスラリーを、エアーブラシを用いて容器内面に均一に塗布した。この容器を１２００℃で焼成し、４００ｍｍ×４００ｍｍ×４００ｍｍ、厚さ１５ｍｍの角型形状の離型層を有する溶融シリコン用容器を得た。
Example 2
In a container in which dry silica powder produced in the same manner as in Example 1 was molded, a slurry having a concentration of 50% prepared by mixing and dissolving Si 3 N 4 powder prepared in accordance with Example 1 and water was containerized using an air brush. Uniformly applied to the inner surface. This container was baked at 1200 ° C. to obtain a molten silicon container having a square-shaped release layer of 400 mm × 400 mm × 400 mm and a thickness of 15 mm.
実施例３
実施例１と同様に製作した乾燥シリカ粉末を成型した容器に、Ｓｉ3Ｎ4粉末と水を溶解した濃度８０％のスラリーを、エアーブラシを用いて容器内面を均一に塗布した。この容器を１２００℃で焼成し、４００ｍｍ×４００ｍｍ×４００ｍｍ、厚さ１５ｍｍの角型形状の離型層を有する溶融シリコン用容器を得た。
Example 3
A slurry with a concentration of 80%, in which Si 3 N 4 powder and water were dissolved, was uniformly applied on the inner surface of the container using an air brush in a container formed with the dry silica powder produced in the same manner as in Example 1. This container was baked at 1200 ° C. to obtain a molten silicon container having a square-shaped release layer of 400 mm × 400 mm × 400 mm and a thickness of 15 mm.
比較例４
実施例１と同様に製作した乾燥シリカ粉末を成型した容器に、Ｓｉ3Ｎ4粉末と水を溶解した濃度９０％のスラリーを、エアーブラシを用いて容器内面に塗布しようとしたが、均一なスラリー層を形成できなかった。
Comparative Example 4
An attempt was made to apply a slurry having a concentration of 90% obtained by dissolving Si 3 N 4 powder and water to the inner surface of the container using an air brush in a container formed with dry silica powder produced in the same manner as in Example 1. A slurry layer could not be formed.
実施例４
実施例１と同様に製作した乾燥シリカ粉末を成型した容器に、Ｓｉ3Ｎ4粉末と水を混合してスラリーとした。分散剤としてポリビニルアルコール（水１００ｇに対して０．２ｇを溶解したもの）を添加した。このスラリーをエアーブラシで容器内面に均一に塗布した。この容器を１２００℃で焼成し、４００ｍｍ×４００ｍｍ×４００ｍｍ、厚さ１５ｍｍの角型形状の離型層を有する溶融シリコン用容器を得た。
Example 4
Si 3 N 4 powder and water were mixed into a container in which dry silica powder produced in the same manner as in Example 1 was molded to form a slurry. Polyvinyl alcohol (0.2 g dissolved in 100 g of water) was added as a dispersant. This slurry was uniformly applied to the inner surface of the container with an air brush. This container was baked at 1200 ° C. to obtain a molten silicon container having a square-shaped release layer having a size of 400 mm × 400 mm × 400 mm and a thickness of 15 mm.
参考例
実施例１と同様にシリカ粉末で容器を成型し、離型剤としてＳｉ3Ｎ4＋ＳｉＯ2球状粉のスラリーを内面に塗布して１２００℃で焼成し、４００ｍｍ×４００ｍｍ×４００ｍｍ、厚さ１５ｍｍの角型形状の離型層を有する溶融シリコン用容器を得た。
Reference Example A container is molded with silica powder in the same manner as in Example 1, and a slurry of Si 3 N 4 + SiO 2 spherical powder is applied to the inner surface as a release agent and baked at 1200 ° C., 400 mm × 400 mm × 400 mm, thickness A molten silicon container having a 15 mm square release layer was obtained.
比較例１
シリカ粉末、バインダー、水をオムニミキサーで混合しスラリーとして鋳型に流し込み、４００ｍｍ×４００ｍｍ×４００ｍｍ、厚さ１５ｍｍの角型形状の容器を成型し、３０℃、湿度７０％の調湿乾燥機で５日間乾燥させた後、１２００℃で焼成して溶融シリコン用容器を得た。
この焼成した後の容器内面にＳｉ3Ｎ4粉末を水と混合してスラリーとし、分散剤としてポリビニルアルコールを添加した。このスラリーをエアーブラシで塗布して乾燥させ、１２００℃で焼成して容器内面に離型層を形成した。
Comparative Example 1
Silica powder, binder, and water are mixed with an omni mixer and poured into a mold as a slurry. A 400 mm × 400 mm × 400 mm, 15 mm thick rectangular container is molded, and 5% by a humidity control dryer at 30 ° C. and 70% humidity. After drying for a day, it was baked at 1200 ° C. to obtain a container for molten silicon.
Si 3 N 4 powder was mixed with water on the inner surface of the baked container to form a slurry, and polyvinyl alcohol was added as a dispersant. This slurry was applied with an air brush and dried, and fired at 1200 ° C. to form a release layer on the inner surface of the container.
比較例２
比較例１と同様に容器を焼成し、離型剤としてＳｉ3Ｎ4＋Ｓｉ粉末のスラリーを容器内面に塗布して焼成し、離型層を形成した。
比較例３
比較例１と同様に容器を焼成し、離型剤としてＳｉ3Ｎ4＋ＳｉＯ2粉末のスラリーを容器内面に塗布して焼成し、離型層を形成した。
Comparative Example 2
The container was fired in the same manner as in Comparative Example 1, and a slurry of Si 3 N 4 + Si powder as a release agent was applied to the container inner surface and fired to form a release layer.
Comparative Example 3
The container was fired in the same manner as in Comparative Example 1, and a slurry of Si 3 N 4 + SiO 2 powder as a release agent was applied to the inner surface of the container and baked to form a release layer.
以上の実施例と比較例について機械強度と焼結性について検討し、結果を焼結後の膜密着性として表１に示す。 The mechanical strength and sinterability of the above examples and comparative examples were examined, and the results are shown in Table 1 as film adhesion after sintering.
○：均一に密着していることが観察され、膜表面を石英ガラス棒で触っても剥離しないもの
×：既に一部の剥離が観察されるもの、膜表面を石英ガラス棒で触って剥離するもの
表１に示す結果から明らかなように、本発明は、焼結性と機械強度が従来方法によるものより向上しており、また、二段階の焼成工程が一段階となったので、生産性が格段に向上するものである。
高純度が要求される金属シリコン用の容器において、その内面に離型層を効率よく形成することができると共に、その機械強度や焼結性が高いものが得られる。その結果、高純度シリコンインゴットの製品歩留りの向上が達成される。
As is apparent from the results shown in Table 1, the present invention has improved sinterability and mechanical strength as compared with the conventional method, and the two-stage firing process becomes one stage. This is a significant improvement.
In a metal silicon container that requires high purity, a release layer can be efficiently formed on the inner surface of the container, and a high mechanical strength and sinterability can be obtained. As a result, the product yield of the high purity silicon ingot is improved.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2004090562A JP4471692B2 (en) | 2004-03-25 | 2004-03-25 | Method for manufacturing container for melting silicon having release layer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2004090562A JP4471692B2 (en) | 2004-03-25 | 2004-03-25 | Method for manufacturing container for melting silicon having release layer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2005271058A JP2005271058A (en) | 2005-10-06 |
| JP4471692B2 true JP4471692B2 (en) | 2010-06-02 |
Family
ID=35171249
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2004090562A Expired - Fee Related JP4471692B2 (en) | 2004-03-25 | 2004-03-25 | Method for manufacturing container for melting silicon having release layer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP4471692B2 (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007053284A1 (en) * | 2007-11-08 | 2009-05-20 | Esk Ceramics Gmbh & Co. Kg | Firmly adhering silicon nitride-containing separating layer |
| JP5130323B2 (en) * | 2010-05-07 | 2013-01-30 | 信越石英株式会社 | Square silica container for producing polycrystalline silicon ingot and method for producing the same |
| WO2012046673A1 (en) * | 2010-10-08 | 2012-04-12 | Jx日鉱日石金属株式会社 | Silicon ingot manufacturing vessel |
| CN103140443B (en) * | 2010-10-08 | 2015-10-14 | 吉坤日矿日石金属株式会社 | Silicon ingot manufacture container |
| JP5867414B2 (en) * | 2010-12-21 | 2016-02-24 | 日東紡績株式会社 | Glass melting apparatus, glass fiber manufacturing apparatus, and glass fiber manufacturing method |
| JP5867413B2 (en) * | 2010-12-21 | 2016-02-24 | 日東紡績株式会社 | Glass melting apparatus, glass fiber manufacturing apparatus, and glass fiber manufacturing method |
| WO2012093563A1 (en) * | 2011-01-06 | 2012-07-12 | 日東紡績株式会社 | Glass melting apparatus, glass fiber producing apparatus, and method for changing glass composition |
| JP5653857B2 (en) * | 2011-07-25 | 2015-01-14 | 株式会社トクヤマ | Polysilicon container |
| JP2013151386A (en) * | 2012-01-25 | 2013-08-08 | Kyodo Fine Ceramics Co Ltd | Casting mold for casting polysilicon ingot, method for producing casting mold for casting polysilicon ingot, and method for producing polysilicon ingot |
| KR102093398B1 (en) * | 2018-11-09 | 2020-03-25 | 이레정밀씰 주식회사 | Maknig method of floating seal including special spray method for deviation materials |
-
2004
- 2004-03-25 JP JP2004090562A patent/JP4471692B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JP2005271058A (en) | 2005-10-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP1745164B1 (en) | Crucible for the crystallization of silicon | |
| ES2269794T3 (en) | CONTAINER FOR SILICON CONTAINMENT AND PROCEDURE FOR PRODUCTION. | |
| CN101370968A (en) | Crucible for treating molten silicon | |
| JP4471692B2 (en) | Method for manufacturing container for melting silicon having release layer | |
| CN107640963A (en) | A kind of preparation method of graded ceramicses core material | |
| CN108044042A (en) | A kind of titanium or titanium alloy casting graphite-based core and preparation method thereof | |
| CN101429045B (en) | Zirconium acetate agglutinate yttrium oxide shuttering and method for producing the same | |
| JP7112215B2 (en) | Silicon melting crucible, method for manufacturing silicon melting crucible, and method for manufacturing reaction-sintered SiC | |
| JP2005125380A (en) | Mold for casting silicon and its production method | |
| CN106278302B (en) | A kind of preparation process of the high-purity fused silica crucible of gradient | |
| JP2010280529A (en) | Method for manufacturing crucible for polycrystalline silicon production | |
| JP5417448B2 (en) | Adhesives and coatings for heat-resistant materials and ceramics | |
| JP3981538B2 (en) | Silicon holding container and manufacturing method thereof | |
| JPS61101430A (en) | Fused silica and composition containing same | |
| JP4497943B2 (en) | Silicon casting mold and silicon casting apparatus using the same | |
| JP2006334671A (en) | Method for manufacturing silicon casting mold | |
| CN107243591A (en) | MgO‑CaZrO3Composite shell and preparation method thereof | |
| JP2006327912A (en) | Casting mold for forming silicon ingot and method for manufacturing silicon ingot | |
| JP4889306B2 (en) | Silicone coagulation mold with mold release material | |
| KR101764889B1 (en) | Method of fabricating silicon carbide sintered body by reaction sintering | |
| JP4025671B2 (en) | Manufacturing method of mold for silicon casting | |
| CN114538961B (en) | SiC/Y on surface of C-based material 2 O 3 Method for repairing coating crack | |
| TW201002417A (en) | Method of coating protective layer on crucible for crystal growth | |
| TWI239283B (en) | Blank body forming device and forming process thereof | |
| JP4484501B2 (en) | Silicon casting equipment |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20070201 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20080122 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20090811 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20091008 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20091124 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20100121 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20100223 |
|
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20100302 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130312 Year of fee payment: 3 |
|
| R150 | Certificate of patent or registration of utility model |
Ref document number: 4471692 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20140312 Year of fee payment: 4 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| LAPS | Cancellation because of no payment of annual fees |