CN101531368B - Method for preparing cristobalite material by taking quartz crucible as raw material - Google Patents
Method for preparing cristobalite material by taking quartz crucible as raw material Download PDFInfo
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- CN101531368B CN101531368B CN2009100385592A CN200910038559A CN101531368B CN 101531368 B CN101531368 B CN 101531368B CN 2009100385592 A CN2009100385592 A CN 2009100385592A CN 200910038559 A CN200910038559 A CN 200910038559A CN 101531368 B CN101531368 B CN 101531368B
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- cristobalite
- quartz crucible
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Abstract
The invention discloses a method for preparing a cristobalite material by taking a quartz crucible as a raw material, which adopts the quartz crucible subjected to high temperature treatment of 1,400 to 1,600 DEG C is subjected to surface impurity removal, crushing and grinding processes to obtain a high-purity cristobalite material of which the SiO2 content is more than 99 percent by weight. The method has the advantages of simple production process, low production cost, good product quality, energy conservation, environmental protection and the like.
Description
Technical field
The present invention relates to cristobalite material technology field, being specifically related to the quartz crucible is the method for feedstock production cristobalite material.
Background technology
The cristobalite material has characteristics such as extremely low linear expansion and internal stress, high temperature tolerance, low-activity, resistance to chemical attack, and is widely used in fields such as coating, rubber, printing ink, precision casting and high-grade ceramic.
Quartz crystal has multiple variant, and they can be divided into 3 series, i.e. quartz, tridymite and cristobalite series.Crystal formation can take place and transform into cristobalite in quartz crystal under 1400～1600 ℃ of hot conditionss.Existing cristobalite production technology normally with quartz crystal through high-temperature calcination, cooling obtains again after 1400～1600 ℃ of insulations, so be also referred to as high quartz (seeing C N 1318527A, C N 1739882A).Because prior art adopts the high-temperature calcination method, need to consume a large amount of energy; And existing cristobalite production technology normally directly adopts the natural quartz ore deposit as raw material, and associated minerals such as mica, feldspar are contained in the natural quartz ore deposit, must remove these impurity through certain technological process, could obtain the high purity cristobalite.Because above factor causes the complex manufacturing of existing cristobalite product, production cost height.
Summary of the invention
The objective of the invention is to overcome the prior art above shortcomings, providing a kind of is the method for feedstock production cristobalite material with the quartz crucible.Quartz crucible is the container that is used to produce silicon materials, and is that disposable use is just discarded later on.Original quartz crucible is the vitreous state quartz material, but it produces in the silicon materials process through 1400～1600 ℃ of insulations having as container, is the cristobalite attitude thereby make quartz crucible by glass transition.The present invention utilizes this principle exactly, and the exhausted quartz crucible is processed into the cristobalite material, and its specific implementation is as follows:
With the quartz crucible is the method for feedstock production cristobalite material, and described quartz crucible through pyroprocessing, is removed surface impurity with this quartz crucible in producing the silicon materials process, and fragmentation is ground and screening, obtains SiO
2Content is greater than the high purity cristobalite material of 99% (weight).
In the aforesaid method, described quartz crucible is a used quartz ceramic crucible in the silicon fusion process.
In the aforesaid method, described quartz crucible is through 1400～1600 ℃ of pyroprocessing, and quartz crucible changes the cristobalite crystalline form into by primary vitreous state quartz.
In the aforesaid method, described quartz crucible surface removal of impurities is the pollutent that removes the surface, and method has physics or chemical process.Physical method is an impurity of removing the crucible surface secure adhesion by mechanical grinding or sandblast technology.Chemical process is that the technology that adopts chemical solution to soak is removed crucible surface impurity, and this chemical solution contains fluorine cpd in being, as hydrofluoric acid, hydrogen fluoride ammonia etc.
In the aforesaid method, described high purity cristobalite material is powder or piece material, and the size range of cristobalite powder can be 1～1000 micron, and cristobalite piece material size can be 1～200 millimeter, and fragmentation is ground and sieving technology can be dry method or wet method.
With respect to prior art, the present invention has following advantage and effect: cristobalite piece material preparation technology of the present invention obtains finished product through surperficial removal of impurities, fragmentation after can grinding as raw material with the quartz crucible that 1400～1600 ℃ of pyroprocessing are crossed.The present invention utilizes silicon materials factory used quartz crucible material processing cristobalite product (silicon materials factory is at 1400～1600 ℃ of use quartz crucibles), and production technique is simple, and production cost is low, turns waste into wealth.The prepared cristobalite material purity of the present invention height (SiO
2Content is greater than 99%).The present invention provides the new and innovative ways of a kind of energy-conserving and environment-protective, high economic benefit for the production of cristobalite material.
Description of drawings
Fig. 1 is for making the X ray powder crystal diffractogram of cristobalite in the embodiment of the invention 1.
Fig. 2 is for making the X ray powder crystal diffractogram of cristobalite powder in the embodiment of the invention 2.
Fig. 3 makes the cristobalite powder particle size distribution figure in the embodiment of the invention 2.
Embodiment
Below in conjunction with specific embodiment enforcement of the present invention is described further.
Embodiment 1:
Take out used quartz ceramic crucible from silicon materials factory, this quartz ceramic crucible has been used for the molten heavy stone used as an anchor of polysilicon, the temperature of the molten heavy stone used as an anchor of polysilicon is 1500～1550 ℃, crucible disc cooling back grinder buffing, remove surface impurity, with the tap water flushing, be broken into 10～50 millimeters cristobalite piece after the drying again.The composition (mass percent) that this method obtains the cristobalite material sees Table 1, illustrates that this is the very high quartz material of a kind of purity.The X ray powder crystal diffractogram of cristobalite is seen Fig. 1, shows that the crystalline phase composition mainly is the cristobalite phase in the cristobalite material.
Table 1
| SiO 2 | Al 2O 3 | Fe 2O 3 | Li 2O | Na 2O | K 2O | MgO | TiO 2 | CuO | Ca?O |
| ＞99.8 | 0.08 | 0.02 | ＜0.01 | ＜0.01 | ＜0.01 | ＜0.01 | ＜0.01 | ＜0.01 | 0.02 |
Embodiment 2:
Take out used quartz ceramic crucible from silicon materials factory, this quartz ceramic crucible has been used for the molten heavy stone used as an anchor of polysilicon, and the temperature of the molten heavy stone used as an anchor of polysilicon is 1500～1550 ℃.Through cleaning with tap water, be immersed in the hydrofluoric acid solution after the crucible disc cooling, the hydrofluoric acid consumption in 1 ton of water is 200 liters again.After soaking 2 days at normal temperatures, the crucible disc surface becomes white by grey, and crucible is taken out, and cleans with tap water again.With the white crucible disc fragmentation of cleaning,, behind the slurry drying, just obtain the cristobalite powder that certain particle size distributes with ball mill grinding with corundum medium.The composition (mass percent) that this method obtains cristobalite powder sees Table 2, because adopt the corundum medium in the process of lapping, the alumina content in the powder raises to some extent, but owing to use acid treatment, iron oxide content has wherein descended, and total dioxide-containing silica is still greater than 99.5%.The X ray powder crystal diffractogram of cristobalite powder is seen Fig. 2, shows that the crystalline phase composition mainly is the cristobalite phase in the cristobalite material.The size-grade distribution of cristobalite powder is seen Fig. 3, shows that the size range of cristobalite powder is 1～60 micron.
Table 2
| SiO 2 | Al 2O 3 | Fe 2O 3 | Li 2O | Na 2O | K 2O | MgO | TiO 2 | CuO | CaO |
| ＞99.5 | 0.36 | ＜0.01 | ＜0.01 | ＜0.01 | ＜0.01 | ＜0.01 | ＜0.01 | ＜0.01 | 0.02 |
Embodiment 3:
Take out used quartz ceramic crucible from silicon materials factory, this quartz ceramic crucible has been used for the molten heavy stone used as an anchor of polysilicon, and the temperature of the molten heavy stone used as an anchor of polysilicon is 1500～1550 ℃.Through cleaning with tap water, be immersed in the ammonium hydrogen fluoride solution after the crucible disc cooling, the ammonium bifluoride consumption in 1 ton of water is 100 kilograms again.After soaking 2 days at normal temperatures, the grey on crucible disc surface becomes white, and crucible disc is taken out, and cleans with tap water again.Adopt dry process, promptly dried white crucible disc again at the ball mill grinding of corundum liner and medium, just obtains the cristobalite powder that certain particle size distributes through broken after the grading.
Claims (8)
1. be the method for feedstock production cristobalite material with the quartz crucible, it is characterized in that described quartz crucible in the silicon materials production process through the pyroprocessing mistake, this quartz crucible obtains SiO after surperficial removal of impurities, fragmentation, grinding and screening
2Content is greater than the high purity cristobalite material of 99% (weight); Described silicon materials production process comprises the silicon fusion process, and described quartz crucible is a used quartz ceramic crucible in the silicon fusion process; The temperature of described pyroprocessing is 1400～1600 ℃, and quartz crucible changes the cristobalite crystalline form into by primary vitreous state quartz after the pyroprocessing.
2. according to claim 1 described be the method for feedstock production cristobalite material with the quartz crucible, the temperature that it is characterized in that described pyroprocessing is 1500～1550 ℃.
3. according to claim 1 is the method for feedstock production cristobalite material with the quartz crucible, it is characterized in that described surperficial removal of impurities is to adopt physics or chemical process to remove the impurity on described quartz crucible surface, and this impurity comprises ash, sila matter.
4. according to claim 3 is the method for feedstock production cristobalite material with the quartz crucible, it is characterized in that described physical method is an impurity of removing the quartz crucible surface by mechanical grinding or sandblast.
5. according to claim 3 is the method for feedstock production cristobalite material with the quartz crucible, it is characterized in that described chemical process is to adopt chemical solution to soak to remove the impurity on quartz crucible surface, has fluorochemicals in the described chemical solution.
6. according to claim 5 is the method for feedstock production cristobalite material with the quartz crucible, it is characterized in that described fluorochemicals is hydrofluoric acid or hydrogen fluoride ammonia.
According to claim 1～6 each described be the method for feedstock production cristobalite material with the quartz crucible, it is characterized in that described high purity cristobalite material is powder or piece material, the size range of cristobalite powder is 1～1000 micron, and cristobalite piece material is of a size of 1～200 millimeter.
8. according to claim 7 is the method for feedstock production cristobalite material with the quartz crucible, it is characterized in that described fragmentation, grinds and sieving technology employing dry method or wet method.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100385592A CN101531368B (en) | 2009-04-10 | 2009-04-10 | Method for preparing cristobalite material by taking quartz crucible as raw material |
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| CN2009100385592A CN101531368B (en) | 2009-04-10 | 2009-04-10 | Method for preparing cristobalite material by taking quartz crucible as raw material |
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| CN101531368A CN101531368A (en) | 2009-09-16 |
| CN101531368B true CN101531368B (en) | 2011-06-22 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145339B (en) * | 2013-03-20 | 2015-06-03 | 江苏中硅工程材料有限公司 | Quartz ceramic material and application for same |
| CN104773991B (en) * | 2015-03-27 | 2016-08-31 | 武汉理工大学 | A kind of enhancing crack resistance type mold materials and forming method thereof |
| CN107282035B (en) * | 2016-04-12 | 2019-12-24 | 中国石油化工股份有限公司 | Cristobalite and preparation method and application thereof |
| CN107445168B (en) * | 2017-06-16 | 2020-03-31 | 江苏大学 | Method for recycling fused quartz crucible after polycrystalline silicon ingot casting |
| CN107324344A (en) * | 2017-06-16 | 2017-11-07 | 江苏大学 | A kind of method that utilization polycrystalline silicon ingot casting fused silica crucible prepares cristobalite micro mist |
| CN109052417B (en) * | 2018-09-11 | 2019-07-26 | 安徽科技学院 | A kind of synthetic method of high-purity low-temperature phase cristobalite |
| CN109336379B (en) * | 2018-11-30 | 2021-10-01 | 湖北新华光信息材料有限公司 | Sulfur glass waste residue recycling method and obtained glass |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6106610A (en) * | 1997-09-30 | 2000-08-22 | Heraeus Quarzglas Gmbh & Co. Kg | Quartz glass crucible for producing silicone single crystal and method for producing the crucible |
| US6302957B1 (en) * | 1999-10-05 | 2001-10-16 | Sumitomo Metal Industries, Ltd. | Quartz crucible reproducing method |
| CN101041548A (en) * | 2007-03-05 | 2007-09-26 | 中国地质大学（武汉） | Method for preparing cristobalite by calcining quartz |
-
2009
- 2009-04-10 CN CN2009100385592A patent/CN101531368B/en not_active Ceased
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6106610A (en) * | 1997-09-30 | 2000-08-22 | Heraeus Quarzglas Gmbh & Co. Kg | Quartz glass crucible for producing silicone single crystal and method for producing the crucible |
| US6302957B1 (en) * | 1999-10-05 | 2001-10-16 | Sumitomo Metal Industries, Ltd. | Quartz crucible reproducing method |
| CN101041548A (en) * | 2007-03-05 | 2007-09-26 | 中国地质大学（武汉） | Method for preparing cristobalite by calcining quartz |
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