CN102260902B - Method for preparing quartz crucible coating - Google Patents
Method for preparing quartz crucible coating Download PDFInfo
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- CN102260902B CN102260902B CN 201110198592 CN201110198592A CN102260902B CN 102260902 B CN102260902 B CN 102260902B CN 201110198592 CN201110198592 CN 201110198592 CN 201110198592 A CN201110198592 A CN 201110198592A CN 102260902 B CN102260902 B CN 102260902B
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- quartz crucible
- coating
- barium
- barium hydroxide
- hydroxide solution
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Abstract
The invention provides a method for preparing a quartz crucible coating. The method comprises the following steps of: (a) preparing a barium hydroxide solution, wherein the weight ratio of barium hydroxide to water in the barium hydroxide solution is 1:(46-52); and (b) heating a quartz crucible till the temperature is above 200 DEG C, uniformly spraying the barium hydroxide solution on the inner wall and the upper opening of the quartz crucible, and forming a barium hydroxide coating on the inner wall and the upper opening of the quartz crucible after spraying. According to the method, the barium hydroxide formed on the surface of the crucible is reacted with carbon dioxide in air to form barium carbonate; when the quartz crucible is heated on a mono-crystal furnace, the barium carbonate is decomposed into barium oxide; the barium oxide is reacted with the quartz crucible to form barium metasilicate; a barium metasilicate layer can be used for protecting the quartz crucible; mono-crystal silicon can be prevented from reacting with the quartz crucible in a high-temperature drawing process; the service life and the long crystal yield of the quartz crucible are improved; furthermore,the intensity of the quartz crucible can also be increased; and the high-temperature softening phenomenon is reduced.
Description
Technical field
The present invention relates to photovoltaic module and make field, particularly a kind of preparation method of quartz crucible coating.
Background technology
Along with adding of process of industrialization, conventional energy resourcess such as coal, oil and natural gas are exhausted day by day, and a series of environmental issues are also followed appearance.Therefore, traditional fossil energy has been difficult to satisfy the demand of modern industry, and the environmental problem of its generation has also constituted threat to people's survival environment.Sun power is developed gradually in the world fast as a kind of reproducible green energy resource.Increasingly mature along with solar energy generation technology, solar cell is obtained widespread use at numerous areas such as industry, agricultural and space flight.
Solar cell is the device that luminous energy is changed into electric energy by photovoltaic effect or Photochemical effects.At present, according to the difference of material therefor, solar cell can be divided into: silicon solar cell, compound film solar cell and polymer multi-layer modified electrode solar cell, organic solar batteries and nano-crystalline solar battery.Wherein, the silicon solar cell development is the most ripe, occupies an leading position in application.Crystal-silicon solar cell is divided into single crystal silicon solar cell and polycrystalline silicon solar cell again.With respect to polycrystalline silicon solar cell, monocrystalline silicon battery has high conversion rate, so single crystal silicon solar cell is used comparatively extensive.
Vertical pulling method is the main production method of silicon single crystal, the quartz crucible subsidiary material that are absolutely necessary in the crystal pulling process.Quartz crucible at high temperature has the crystal that trend becomes silicon-dioxide, and this process is called crystallization.Crystallization usually occurs in the top layer of quartz crucible, and according to Chinese silica glass industry standard regulation, the semiconductor industry silica glass is incubated 6 hours down at 1400 ℃ ± 5 ℃, and the crystallization of the mean thickness of crystallization layer within 100 μ m is to belong to normal.But, serious crystallization is very big to pulling influence, might destroy the original coating of crucible inwall during inner wall of quartz crucible generation crystallization, this will cause bubble layer and molten silicon below the coating to react, cause part particulate state silicon oxide to enter in the molten silicon, feasible crystalline structure of growing morphs and can't normally grow brilliant.In addition, crystallization is with the original thickness of attenuate quartz crucible, and the intensity that has reduced crucible causes the distortion of quartz crucible easily.
In recent years, along with the increase of charging capacity, the crystal pulling time is corresponding prolongation also, and the crystallization of existing quartz crucible is also serious all the more, causes when crystal pulling quartz crucible can occur can't reaching existing time requirement work-ing life thus and the situation that causes leaking material takes place; And if the subsidiary extremely small impurity in quartz crucible surface, also will cause monocrystalline to interrupt rib in process of growth, influence yield rate.
In order to prolong the work-ing life of quartz crucible, improve yield rate, employing is arranged in quartz crucible surface preparation coating in the prior art, make it form tight zone as be coated with one deck glass sand on the quartz crucible surface, prevent from reacting with quartz crucible in the silicon single crystal high temperature pulling process.The inventor considers to go out one deck hydrated barta coating in quartz crucible surface uniform preparation, is used for preventing that silicon single crystal high temperature pulling process and quartz crucible from reacting.
Summary of the invention
The preparation method that the technical problem that the present invention solves is to provide a kind of quartz crucible coating uses this method to go out the hydrated barta coating in the quartz crucible surface preparation, improves work-ing life and the long brilliant yield of quartz crucible.
In view of this, the invention provides a kind of preparation method of quartz crucible coating, comprising:
A), the configuration barium hydroxide solution, the weight ratio of hydrated barta and water is 1 in the described barium hydroxide solution: (46~52);
B), quartz crucible is heated to more than 200 ℃, described barium hydroxide solution evenly is sprayed at the inwall of described quartz crucible and suitable for reading, the spraying described inner wall of quartz crucible in back and surface suitable for reading form the hydrated barta coating.
Preferably, the density of described hydrated barta coating is 0.65 * 10
-4G/cm
2~0.96 * 10
-4G/cm
2
Preferably, the weight ratio of hydrated barta and water is 1 in the described barium hydroxide solution: (48~52).
Preferably, the quantity for spray of barium hydroxide solution is (18.5~21.5) g/20 inch quartz crucible among the step b.
Preferably, among the step b quartz crucible is heated to 290 ℃~310 ℃.
Preferably, described step b is specially:
B1), take out after quartz crucible being placed baking oven internal heating to 290 ℃~310 ℃;
B2), described barium hydroxide solution evenly is sprayed at the inwall of described quartz crucible and suitable for reading, the spraying described inner wall of quartz crucible in back and last interruption-forming hydrated barta coating in 1.5~3min.
Preferably, described step a carries out under protection of inert gas.
Preferably, described step b carries out under protection of inert gas.
The invention provides a kind of preparation method of quartz crucible coating, comprise the steps: to dispose barium hydroxide solution, the weight ratio of hydrated barta and water is 1 in the described barium hydroxide solution: (46~52); Quartz crucible is heated to more than 200 ℃, described barium hydroxide solution evenly is sprayed at the inwall of described quartz crucible and suitable for reading, the spraying described inner wall of quartz crucible in back and surface suitable for reading form the hydrated barta coating.By such scheme as can be known, the present invention adopts spraying method barium hydroxide solution to be sprayed to the inwall of quartz crucible of heat and suitable for reading, because the quartz crucible temperature is higher, therefore barium hydroxide solution touches the water evaporation in the solution behind the crucible surface, hydrated barta is stayed crucible inwall and surface suitable for reading, forms the hydrated barta coating.The hydrated barta that forms can form barium carbonate with the carbon dioxide in air reaction, when this kind quartz crucible when single crystal growing furnace is heated, barium carbonate can be decomposed to form barium oxide, barium oxide can form barium silicate with the quartz crucible reaction again.Therefore, final quartz crucible surface forms the fine and close small barium silicate cristobalite crystallizing layer of one deck, and quartz crucible is played a protective role, and prevents from reacting with quartz crucible in the silicon single crystal high temperature pulling process, improves work-ing life and the long brilliant yield of quartz crucible; In addition, it can also increase the quartzy intensity of crucible just, reduces the hot mastication phenomenon.
Description of drawings
Figure 1 shows that the quartz crucible structural representation that scribbles the hydrated barta coating provided by the invention.
Embodiment
In order further to understand the present invention, be described below in conjunction with the preferred embodiment of the invention of embodiment, but should be appreciated that these describe just to further specifying the features and advantages of the present invention, rather than to the restriction of claim of the present invention.
The embodiment of the invention discloses a kind of preparation method of hydrated barta coating, comprising:
A), the configuration barium hydroxide solution, the weight ratio of hydrated barta and water is 1 in the described barium hydroxide solution: (46~52);
B), quartz crucible is heated to more than 200 ℃, described barium hydroxide solution evenly is sprayed at the inwall of described quartz crucible and suitable for reading, the spraying described inner wall of quartz crucible in back and surface suitable for reading form the hydrated barta coating.
The present invention adopts spraying coating process at the working face of quartz crucible, be suitable for reading and inwall prepares the hydrated barta coating, obtain the quartz crucible that scribbles the hydrated barta coating shown in Figure 1, this quartz crucible comprises the hydrated barta coating 2 on matrix crucible 1 and coating and matrix crucible inwall and surface suitable for reading.The hydrated barta that forms can form barium carbonate with the carbon dioxide in air reaction, when this kind quartz crucible when single crystal growing furnace is heated, barium carbonate can be decomposed to form barium oxide, barium oxide can form barium silicate with the quartz crucible reaction again.Because the existence of barium silicate is arranged, make the quartz crucible surface can form the fine and close small cristobalite crystallization of one deck, this small cristobalite crystallization is difficult to be infiltrated by melted silicon and peel off.Therefore, barium silicate can play a protective role to quartz crucible, prevents from reacting with quartz crucible in the silicon single crystal high temperature pulling process; In addition, it can also increase the quartzy intensity of crucible just, reduces the hot mastication phenomenon.
Select hydrated barta to be as the reason of coating: with respect to barium silicate or barium carbonate, hydrated barta has higher solubleness in water, and therefore above-mentioned quartz crucible can adopt spraying method to prepare coating.Select the reason of spraying method to be that quantity for spray is easy to control, can control the amount of hydrated barta on the quartz crucible by the control quantity for spray.Before spraying, need earlier quartz crucible to be heated to more than 200 ℃, preferably be heated to 290 ℃~310 ℃; As early as possible the sodium hydroxide solution that configures is sprayed at the inwall of quartz crucible and suitable for reading then, because this moment, the quartz crucible temperature was higher, the moisture that therefore is sprayed in the sodium hydroxide solution on quartz crucible surface can evaporate, and forms the hydrated barta coating thus.
Consider that the quartz crucible crucible is in the taking-up process, and temperature all can reduce in spraying process, therefore the present invention controls Heating temperature and the spray time of quartz crucible, to guarantee that quartz crucible all can keep its temperature more than 200 ℃ in spraying process, avoid the quartz crucible temperature low excessively, making barium hydroxide solution contact back moisture with quartz crucible can not evaporate fully, the sagging phenomenon occurs, causes hydrated barta coat-thickness skewness thus.Step b preferably carries out in the following manner thus:
B1), take out after quartz crucible being placed baking oven internal heating to 290 ℃~310 ℃;
B2), described barium hydroxide solution evenly is sprayed at the inwall of described quartz crucible and suitable for reading, the spraying described inner wall of quartz crucible in back and last interruption-forming hydrated barta coating in 1.5~3min.
Preferred, quartz crucible cleaned earlier carry out hot spraying again.Most preferred, quartz crucible is heated to 295 ℃~305 ℃, and the control spray time is 1.5~3min.
According to the method described above can be in crucible inwall and the hydrated barta coating of preparing suitable for reading, the density of hydrated barta is low excessively, and then the hydrated barta coating is difficult to realize the provide protection to quartz crucible if thickness is thin excessively; If hydrated barta density is too high, and then its thickness is blocked up easily peels off in the quartz crucible surface, causes monocrystalline to interrupt rib in process of growth, influences yield rate.For this reason, to control the density of hydrated barta coating be 0.65 * 10 in the present invention
-4G/cm
2~0.96 * 10
-4G/cm
2For this reason, the middle hydrated barta of selected control hydrogen manufacturing barium oxide solution of the present invention and the weight ratio of water are 1: (46~52) preferably are controlled to be 1: (48~52).If hydrated barta content is low excessively in the barium hydroxide solution, then easily cause the situation of above-mentioned cover light; As if the hydrated barta too high levels, then be difficult to control homogeneity and the consumption of quantity for spray in the spraying process, cause coating inhomogeneous or too thick thus, the situation that part is peeled off easily takes place during use.The quantity for spray of barium hydroxide solution is preferably (18.5~21.5) g/20 inch quartz crucible.
The arrangement step of barium hydroxide solution, namely step a preferably carries out under protection of inert gas, and this is because hydrated barta easily and the carbon dioxide in air formation barium carbonate sediment that reacts, influences the homogeneity that sprays in the spraying process.In like manner, the spraying coating process of barium hydroxide solution, namely step b also carries out in rare gas element.
By such scheme as can be known, the present invention adopts spraying method barium hydroxide solution to be sprayed to the inwall of quartz crucible of heat and suitable for reading, because the quartz crucible temperature is higher, therefore barium hydroxide solution touches the water evaporation in the solution behind the crucible surface, hydrated barta is stayed crucible inwall and surface suitable for reading, forms the hydrated barta coating.The hydrated barta that forms can form barium carbonate with the carbon dioxide in air reaction, when this kind quartz crucible when single crystal growing furnace is heated, barium carbonate can be decomposed to form barium oxide, barium oxide can form barium silicate with the quartz crucible reaction again.Therefore, final quartz crucible surface forms the fine and close small barium silicate cristobalite crystallizing layer of one deck, and quartz crucible is played a protective role, and prevents from reacting with quartz crucible in the silicon single crystal high temperature pulling process, improves work-ing life and the long brilliant yield of quartz crucible; In addition, it can also increase the quartzy intensity of crucible just, reduces the hot mastication phenomenon.
In order further to understand the present invention, below in conjunction with embodiment the preparation method of quartz crucible coating provided by the invention is described, protection scope of the present invention is not limited by the following examples.
1, takes by weighing 50g deionized water and 1g hydrated barta respectively with electronic scale, in nitrogen atmosphere, hydrated barta is dissolved in the deionized water, obtain barium hydroxide solution;
2, place baking oven to heat 20 inches quartz crucibles, be heated to and take out after 300 ℃ immediately with the barium hydroxide solution of spray gun in inner wall of quartz crucible and even spraying step 1 configuration suitable for reading, keep the solution no sag phenomenon on the crucible inwall in the spraying process, the quantity for spray of every crucible is 20.4g/20 inch crucible, and spraying coating process is finished in 2min.The quartz crucible surface forms the hydrated barta coating, and the density of hydrated barta is 0.8 * 10
-4G/cm
2
1, takes by weighing 48g deionization 1g hydrated barta respectively with electronic scale, hydrated barta is dissolved in the deionized water, obtain barium hydroxide solution;
2, place baking oven to heat 20 inches quartz crucibles, take out after being heated to 290 ℃, immediately with the barium hydroxide solution of spray gun in inner wall of quartz crucible and even spraying step 1 configuration suitable for reading, keep the solution no sag phenomenon on the crucible inwall in the spraying process, the quantity for spray of every crucible is 19.6g/20 inch crucible, and spraying coating process is finished in 1.5min.The quartz crucible surface forms the hydrated barta coating, and the density of hydrated barta is 0.8 * 10
-4G/cm
2
Embodiment 3
1, takes by weighing 52g deionization 1g hydrated barta respectively with electronic scale, hydrated barta is dissolved in the deionized water, obtain barium hydroxide solution;
2, place baking oven to heat 20 inches quartz crucibles, take out after being heated to 310 ℃, immediately with the barium hydroxide solution of spray gun in inner wall of quartz crucible and even spraying step 1 configuration suitable for reading, keep the solution no sag phenomenon on the crucible inwall in the spraying process, the quantity for spray of every crucible is 21.1g/20 inch crucible, and spraying coating process is finished in 3min.The quartz crucible surface forms the hydrated barta coating, and the density of hydrated barta is 0.8 * 10
-4G/cm
2
The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be apparent concerning those skilled in the art, and defined General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments herein.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the wideest scope consistent with principle disclosed herein and features of novelty.
Claims (5)
1. the preparation method of a quartz crucible coating, described quartz crucible coating prepares in accordance with the following methods:
A), the configuration barium hydroxide solution, the weight ratio of hydrated barta and water is 1:(48~52 in the described barium hydroxide solution);
B), quartz crucible is heated to more than 200 ℃, described barium hydroxide solution evenly is sprayed at the inwall of described quartz crucible and suitable for reading, the quantity for spray of described barium hydroxide solution is (18.5~21.5) g/20 inch quartz crucible, the spraying described inner wall of quartz crucible in back and surface suitable for reading form the hydrated barta coating, and the density of described hydrated barta coating is 0.65 * 10
-4G/cm
2~0.96 * 10
-4G/cm
2
2. preparation method according to claim 1 is characterized in that, among the step b quartz crucible is heated to 290 ℃~310 ℃.
3. preparation method according to claim 2 is characterized in that, described step b is specially:
B1), take out after quartz crucible being placed baking oven internal heating to 290 ℃~310 ℃;
B2), in 1.5~3min, described barium hydroxide solution evenly is sprayed at the inwall of described quartz crucible and suitable for reading, the spraying described inner wall of quartz crucible in back and last interruption-forming hydrated barta coating.
4. preparation method according to claim 1 is characterized in that, described step a carries out under protection of inert gas.
5. preparation method according to claim 1 is characterized in that, described step b carries out under protection of inert gas.
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JP5509189B2 (en) | 2011-12-26 | 2014-06-04 | ジルトロニック アクチエンゲゼルシャフト | Method for producing single crystal silicon |
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WO2017017258A1 (en) * | 2015-07-30 | 2017-02-02 | Basf Se | Process for manufacture of nox storage materials |
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CN108018600A (en) * | 2016-10-28 | 2018-05-11 | 上海新昇半导体科技有限公司 | Monocrystal growing furnace heat shielding and its manufacture method |
TWI651283B (en) * | 2017-04-28 | 2019-02-21 | 友達晶材股份有限公司 | Crucible structure and manufacturing method thereof and silicon crystal structure and manufacturing method thereof |
CN107099842A (en) * | 2017-05-10 | 2017-08-29 | 宁夏协鑫晶体科技发展有限公司 | The preparation method of monocrystalline silicon |
CN107460538B (en) * | 2017-07-19 | 2019-02-01 | 内蒙古中环光伏材料有限公司 | A method of it improves and throws monocrystalline silicon crystal forming rate again |
CN109811401A (en) * | 2017-11-20 | 2019-05-28 | 上海新昇半导体科技有限公司 | A kind of crucible device for long crystalline substance |
CN108531980B (en) * | 2018-05-29 | 2020-12-11 | 宁夏富乐德石英材料有限公司 | Improved quartz crucible and method for making same |
CN115142121B (en) * | 2021-03-31 | 2023-06-20 | 晶科能源股份有限公司 | Method for improving crystal yield of re-cast monocrystalline silicon and monocrystalline silicon preparation device |
CN115368155B (en) * | 2022-07-22 | 2023-07-25 | 湖南晶碳新材料有限公司 | Preparation method and application of composite material crucible for Czochralski silicon single crystal |
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CN1448685A (en) * | 2002-03-29 | 2003-10-15 | 日本超精石英株式会社 | Surface modified quartz glass crucible and its modification process |
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