CN102528899A - Production process for preparing silica ceramic crucible by use of pressure grouting method - Google Patents
Production process for preparing silica ceramic crucible by use of pressure grouting method Download PDFInfo
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Abstract
The invention relates to a production process for preparing a silica ceramic crucible by use of a pressure grouting method and belongs to the technical field of high-grade refractory materials in a polycrystalline silicon industry. The pressure grouting comprises steps of preparation of pouring slurry, die assembling, molding by pouring slurry and demolding for fetching a green body, i.e., (1) ball-milling fused silica grain composition into slurry; and (2) fixing a resin die and assembling the die, grouting, pressurizing quartz slurry with the initial pressure being 0.1-0.2Mpa, enhancing the pressure to 0.3-1.5Mpa after a die cavity is filled with quartz slurry, keeping the pressure for about 5 minutes to filter water in the silica slurry by virtue of a micro-reticular resin mold to form a square crucible green body, and during demolding of the green body, and applying pressure of 0.2-0.3Mpa to the surface of the green body through the back layer of the micro-reticular resin mold by utilizing compression air. The green body of the silica ceramic crucible, prepared by the process, has high intensity, does not have residual air holes and is easy to demold, the product is good in thermal shock resistance and high in temperature resistance, and can meet the process requirements of polycrystalline silicon production; and the process has the advantages of high biscuit drying speed, small occupied area for production, shortened manufacturing period, low cost, and suitability for scale production.
Description
One, technical field
The present invention relates to the production technology that a kind of pressure grout method prepares quartz ceramic crucible, belong to the polysilicon industry and use the high grade refractory technical field, be specially and be used for the slip casing by pressure production technology of polycrystalline silicon ingot casting with quartz ceramic crucible.
Two, background technology
At present, the gypsum mold that in the production of pottery, is widely used, this is because plaster mold has suction and demolding performace preferably, can give required moulding, its shortcoming be intensity low, wear no resistance and be slightly soluble in water.In addition, the access times of gypsum mold are less, and the average access times of general cleaners and polishes mould are merely 60-70 time.Like this, both consumed a large amount of gypsum, and be prone to cause product defects again, for example, the gypsum bits are sneaked into and are produced fusion hole in the goods, and the die surface wearing and tearing make the burnt product rough surface and reduce product purity etc.
The manufacturing process of quartz ceramic crucible mainly contains two kinds on the market now: common slip casting method is coagulated method with notes.CN200810124615.X discloses the process that a kind of slip casting method prepares ceramic crucible: adopt gypsum mold, the high purity quartz raw material is gone into to grind slurry by the certain granules proportioning, after old homogenizing, inject gypsum mold, drying is burnt till after the demoulding.This preparation method's advantage is that the product light transmission is good, is easy to quality testing; Shortcoming is that molding time is longer, and the product inner core is difficult for the demoulding, and very easily produces internal fissure at four jiaos after the demoulding; And bubble is difficult for discharging; This in addition common slip casting is easy to generate gross blow hole, is exactly in addition to adopt common gypsum mould corrosion-resistant, pollutes the high-purity silica pot product easily; CN200910087303.0 discloses a kind of technology that adopts the gel injection-moulding legal system to make quartz ceramic crucible.These technological characteristics are under adding organic monomer, crosslinking agent, initator condition, to carry out high-temp in-situ to annotate the type that congeals into; Through controlling the grain size distribution of quartzy powder; The acquisition institutional framework is even, controlled porosity, the quartz ceramic crucible with good anti-thermal shock and resistance to elevated temperatures.But there is certain defective in this method.At first,, has the elasticity of rubber like, because the size of biscuit is bigger, so the distortion of the deadweight before its finish-drying is difficult to control through the biscuit of ceramics that the gel injection-moulding method obtains; Secondly, the quartz-ceramics slurry because air is discharged rapidly, is prone to cause pulp gelization to carry out in advance in vacuumizing the process of degasification, so difficult control hardening time; Adopt the gel injection-moulding method to make quartz ceramic crucible in addition, arid cycle is very long, is exactly that blank density is less than slip casting in addition.In sum, two kinds of moulding process all have weak point, common casting, and shaping demoulding difficulty, biscuit intensity is low, and the shaping finished product rate is not high; It is long arid cycle that gel is annotated method, and moisture content is difficult to discharge, and process synthesis costs such as drying are high, therefore seek to make the quartz ceramic crucible new technology, still are the research directions in solar energy polycrystalline silicon ingot casting field.
Three, summary of the invention
The defective that the object of the invention exists to prior art; Provide a kind of pressure grout method to prepare the production technology of quartz ceramic crucible; It adopts micropore high-strength resin mould to replace the common gypsum mould, and the applying high voltage slip casting method prepares polycrystalline silicon ingot casting and uses quartz ceramic crucible.
The objective of the invention is to realize like this; Utilize the micro-porous resin mould to replace conventional cast; The slip casing by pressure process comprises: the base step is got in preparation cast slurry, matched moulds, injection forming and Qi Mo, the demoulding; (1), preparation cast slurry: silica flour is added the thin slurrying of water mill; The quartzy dry powder that adds the certain granules grating then, the mass percent of quartzy dry powder are (40-80): (60-20), mix the back and stir formation cast slurry; (2), resin die is fixed under the high-pressure slip-casting frame; Begin slip casting behind the matched moulds, to quartzy slurry pressurization, initial pressure is 0.1-0.2MPa; After letting mud fully fill up die cavity pressure is brought up to 0.3-1.5MPa; Pressurize 4-6 minute, the moisture content in the mud is filtered away through mould micro-porous resin layer, form square crucible base substrate; During the base substrate demoulding, utilize compressed air to exert pressure to billet surface through demoulding tracheae and air-permeable mould backing layer, pressure is 0.2-0.3MPa, makes base substrate break away from die cavity under pressure, takes out base substrate then, accomplishes bad body and mould separating; Described micro-porous resin material average pore size is the 2-5 micron; Used resin die comprises: core rod and coaming plate are formed: Grouting Pipe, drainpipe, demoulding tracheae all are located in the framed and micro-porous resin layer of metal; The micro-porous resin layer is as the silica crucible forming surface; After accomplishing each moulding circulation, adopt the deionization press water of 0.2Mpa to carry out blowback, to remove remaining quartzy slurry.
Compared with present technology the present invention has the following advantages:
(1), press filling forming method to compare with traditional nothing: owing to used special micro-porous resin mould, can bear higher grouting pressure, thereby accelerate injection forming speed, improve operating efficiency.Common slip casting method was produced the quartz ceramic crucible molding cycle about 24 hours, and adopted method of the present invention only to need can the demoulding get base in about 25 minutes; And mould can reuse, can continuous slip casting 24 hours every days.
(2), adopt the grouting method of traditional use gypsum mold, mould suction back oven dry needs to consume a large amount of heats, and this grouting method need not dried mould, so but also energy savings.And the base substrate chemical composition of cast is even, and blank density is high, and the shaping finished product rate is high, and molding cycle is short, and product has excellent anti-thermal shock, resistance to elevated temperatures and chemical stability, can satisfy the technological requirement that polycrystalline silicon ingot casting is produced with quartz ceramic crucible.
Most preferred embodiment of the present invention.
Embodiment 1:
(a), preparation cast slurry: vitreous silica is added deionized water, electrolyte, the levigate slurrying of surfactant; Make silica crucible magma; The quartzy dry powder that adds fixed mixing ratio then; Magma wherein: the mass fraction ratio of quartzy dry powder is 40: 60, mixes the back and stirs to vacuumize and form the cast slurry.
(b), pressure forming base substrate: the cast slurry that will prepare adopts slush pump to inject in the cavity of micro-porous resin mould; Initial pressure is 0.15MPa; After letting mud fully fill up die cavity pressure is brought up to 1.0MPa; Moisture content in the mud is filtered away through mould micro-porous resin layer, forms square crucible base substrate.During the base substrate demoulding, utilize compressed air to exert pressure to billet surface through demoulding tracheae and air-permeable mould backing layer, pressure is 0.3MPa, makes base substrate break away from die cavity under pressure, takes out base substrate then.Demoulding base substrate is put into drying oven, dried 4 hours down for 180 ℃; Burnt till 20 hours at 1100 ℃ then, make the requirement that to satisfy polycrystalline silicon ingot casting at silica crucible.
Embodiment 2:
(a), preparation cast slurry: vitreous silica is added deionized water, electrolyte, the levigate slurrying of surfactant; Make silica crucible magma; The quartzy dry powder that adds fixed mixing ratio then; Magma wherein: the mass fraction ratio of quartzy dry powder is 50: 50, mixes the back and stirs to vacuumize and form the cast slurry.
(b), pressure forming base substrate: the cast slurry that will prepare adopts membrane pump to inject in the cavity of micro-porous resin mould; Initial pressure is 0.15MPa, pressure is brought up to 0.8Mpa after letting mud fully fill up die cavity, and the dwell time is 420s ± 30s; Sending slurry pressure is 0.80 ± 0.05MPa; Plasma discharge pressure 0.25 ± 0.10Mpa during the base substrate demoulding, utilizes compressed air to exert pressure to the core rod billet surface through demoulding tracheae and air-permeable mould backing layer; Ejection pressure 0.25MPa puts into drying oven with demoulding base substrate and dried 4 hours down for 180 ℃; Burnt till 22 hours at 1120 ℃ then, make the requirement that to satisfy polycrystalline silicon ingot casting at silica crucible.
Claims (2)
1. the production technology of quartz ceramic crucible is produced in a slip casing by pressure; It is characterized in that: utilize the micro-porous resin mould to replace conventional cast; The slip casing by pressure process comprises: the base step is got in preparation cast slurry, matched moulds, injection forming and Qi Mo, the demoulding, (1), preparation cast slurry: silica flour is added the levigate slurrying of deionized water, add the quartzy dry powder of certain granules grating then; The mass percent of quartzy dry powder is (40-80): (60-20), mix the back and stir formation cast slurry; (2), resin die is fixed under the high-pressure slip-casting frame; Begin slip casting behind the matched moulds, to quartzy slurry pressurization, initial pressure is 0.1-0.2MPa; After letting mud fully fill up die cavity pressure is brought up to 0.3-1.5MPa; Pressurize 4-6 minute, the moisture content in the mud is filtered away through mould micro-porous resin layer, form square crucible base substrate; During the base substrate demoulding, utilize compressed air to exert pressure to billet surface through demoulding tracheae and air-permeable mould backing layer, pressure is 0.2-0.3MPa, makes base substrate break away from die cavity under pressure, takes out base substrate then, accomplishes base substrate and mould separating.
2. the production technology of quartz ceramic crucible is produced in a kind of slip casing by pressure according to claim 1; It is characterized in that: described micro-porous resin material average pore size is the 2-5 micron; Used resin die comprises: core rod and coaming plate are formed; Grouting Pipe, drainpipe, demoulding tracheae all are located in the framed and micro-porous resin layer of metal, and the micro-porous resin layer is as the silica crucible forming surface, after accomplishing each moulding circulation; Adopt the deionization press water of 0.2Mpa to carry out blowback, to remove remaining quartzy slurry.
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| CN102815858A (en) * | 2012-07-17 | 2012-12-12 | 连云港桃盛熔融石英有限公司 | Preparation method of high-purity ultrathin quartz ceramic crucible |
| CN103274583A (en) * | 2013-06-07 | 2013-09-04 | 英利能源（中国）有限公司 | Quartz crucible and production method thereof, and P-type silicon casting ingot and production method thereof |
| CN103978540A (en) * | 2014-05-30 | 2014-08-13 | 和成(中国)有限公司 | Method for producing squatting pan by high-pressure molds |
| CN104355610A (en) * | 2014-09-28 | 2015-02-18 | 中国船舶重工集团公司第七二五研究所 | Method for preparing large-scale ITO (Indium Tin Oxide) target material by using automatic slip casting technology |
| CN105330315A (en) * | 2015-12-09 | 2016-02-17 | 中钢集团洛阳耐火材料研究院有限公司 | Method for eliminating air holes in surface of cast refractory material product |
| CN106904974A (en) * | 2017-04-20 | 2017-06-30 | 石婷 | Normal pressure solid-phase sintered silicon carbide ceramics shaped piece and its manufacture method |
| CN106915966A (en) * | 2017-03-22 | 2017-07-04 | 宁波伏尔肯陶瓷科技有限公司 | A kind of preparation method of reaction sintering silicon carbide ceramic product |
| CN107021743A (en) * | 2017-04-28 | 2017-08-08 | 山东工业陶瓷研究设计院有限公司 | The preparation method of vitreous silica matter ceramics revolving body |
| CN107140962A (en) * | 2017-05-31 | 2017-09-08 | 山东工业陶瓷研究设计院有限公司 | The preparation method of quartziferous ceramics revolving body |
| CN108516831A (en) * | 2018-03-22 | 2018-09-11 | 宁波哈泰雷碳化物有限公司 | A kind of preparation method of bulletproof ceramic whole plate |
| CN110845231A (en) * | 2019-10-31 | 2020-02-28 | 中国船舶重工集团公司第七二五研究所 | Method for preparing ceramic cylinder sleeve for petroleum drilling by high-pressure slip casting |
| CN112589956A (en) * | 2020-10-23 | 2021-04-02 | 中材江苏太阳能新材料有限公司 | Novel forming and curing process for quartz device |
| CN113967961A (en) * | 2021-11-18 | 2022-01-25 | 重庆臻宝实业有限公司 | Ceramic slip casting method and mould thereof |
| CN114905618A (en) * | 2022-06-17 | 2022-08-16 | 中国船舶重工集团公司第七二五研究所 | Device and method for preparing seamless ceramic hollow floating ball |
| CN115636663A (en) * | 2022-10-20 | 2023-01-24 | 无锡市尚领石英科技有限公司 | Preparation process of high-strength high-compactness quartz crucible |
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| CN102815858A (en) * | 2012-07-17 | 2012-12-12 | 连云港桃盛熔融石英有限公司 | Preparation method of high-purity ultrathin quartz ceramic crucible |
| CN102815858B (en) * | 2012-07-17 | 2015-01-28 | 连云港桃盛熔融石英有限公司 | Preparation method of high-purity ultrathin quartz ceramic crucible |
| CN103274583A (en) * | 2013-06-07 | 2013-09-04 | 英利能源（中国）有限公司 | Quartz crucible and production method thereof, and P-type silicon casting ingot and production method thereof |
| CN103274583B (en) * | 2013-06-07 | 2016-03-30 | 英利能源（中国）有限公司 | Quartz crucible and preparation method thereof, P-type silicon ingot casting and preparation method thereof |
| CN103978540A (en) * | 2014-05-30 | 2014-08-13 | 和成(中国)有限公司 | Method for producing squatting pan by high-pressure molds |
| CN104355610A (en) * | 2014-09-28 | 2015-02-18 | 中国船舶重工集团公司第七二五研究所 | Method for preparing large-scale ITO (Indium Tin Oxide) target material by using automatic slip casting technology |
| CN104355610B (en) * | 2014-09-28 | 2017-02-15 | 中国船舶重工集团公司第七二五研究所 | Method for preparing large-scale ITO (Indium Tin Oxide) target material by using automatic slip casting technology |
| CN105330315A (en) * | 2015-12-09 | 2016-02-17 | 中钢集团洛阳耐火材料研究院有限公司 | Method for eliminating air holes in surface of cast refractory material product |
| CN106915966A (en) * | 2017-03-22 | 2017-07-04 | 宁波伏尔肯陶瓷科技有限公司 | A kind of preparation method of reaction sintering silicon carbide ceramic product |
| CN106904974A (en) * | 2017-04-20 | 2017-06-30 | 石婷 | Normal pressure solid-phase sintered silicon carbide ceramics shaped piece and its manufacture method |
| CN107021743A (en) * | 2017-04-28 | 2017-08-08 | 山东工业陶瓷研究设计院有限公司 | The preparation method of vitreous silica matter ceramics revolving body |
| CN107021743B (en) * | 2017-04-28 | 2019-09-06 | 山东工业陶瓷研究设计院有限公司 | The preparation method of vitreous silica matter ceramics revolving body |
| CN107140962A (en) * | 2017-05-31 | 2017-09-08 | 山东工业陶瓷研究设计院有限公司 | The preparation method of quartziferous ceramics revolving body |
| CN107140962B (en) * | 2017-05-31 | 2019-09-06 | 山东工业陶瓷研究设计院有限公司 | The preparation method of quartziferous ceramics revolving body |
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| CN108516831B (en) * | 2018-03-22 | 2020-12-29 | 宁波哈泰雷碳化物有限公司 | Preparation method of bulletproof ceramic whole plate |
| CN110845231A (en) * | 2019-10-31 | 2020-02-28 | 中国船舶重工集团公司第七二五研究所 | Method for preparing ceramic cylinder sleeve for petroleum drilling by high-pressure slip casting |
| CN112589956A (en) * | 2020-10-23 | 2021-04-02 | 中材江苏太阳能新材料有限公司 | Novel forming and curing process for quartz device |
| CN113967961A (en) * | 2021-11-18 | 2022-01-25 | 重庆臻宝实业有限公司 | Ceramic slip casting method and mould thereof |
| CN114905618A (en) * | 2022-06-17 | 2022-08-16 | 中国船舶重工集团公司第七二五研究所 | Device and method for preparing seamless ceramic hollow floating ball |
| CN114905618B (en) * | 2022-06-17 | 2024-05-10 | 中国船舶重工集团公司第七二五研究所 | Device and method for preparing seamless ceramic hollow floating ball |
| CN115636663A (en) * | 2022-10-20 | 2023-01-24 | 无锡市尚领石英科技有限公司 | Preparation process of high-strength high-compactness quartz crucible |
| CN115636663B (en) * | 2022-10-20 | 2023-05-16 | 无锡市尚领石英科技有限公司 | Preparation process of high-strength high-compactness quartz crucible |
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Application publication date: 20120704 |