Method for producing fused silica ceramic crucible

A technology of fused silica and ceramic crucibles, applied in glass manufacturing equipment, manufacturing tools, glass molding and other directions, can solve the problems of low stiffness, difficult to control curing time, long drying cycle, etc., to simplify the operation process, save energy and production. time, the effect of ensuring uniformity

Inactive Publication Date: 2011-05-18
SHANGHAI JIAO TONG UNIV
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AI-Extracted Technical Summary

Problems solved by technology

But this method has certain defects
First of all, the ceramic green body obtained by gel injection molding has the elasticity similar to rubber, but the rigidity is low. Due to the large size of the crucible green body, it is difficult to control the deformation of the crucible due to the weight of the crucible before it is completely dried; Secondly, during the process of vacuuming and degassing the quartz ceramic slurry, due to ...
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Abstract

The invention relates to a method for producing a fused silica ceramic crucible, which belongs to the technical field of a nonmetallic material. The method comprises the steps of: blending fused silica ceramic powder with a grain composition and a premix liquid to prepare a sizing agent, and then carrying out vacuum defoaming, pouring, curing, demoulding, drying and sintering to produce a silica ceramic crucible. In the method, the fused silica ceramic powder with a grain composition is used as a raw material, and thus the produced crucible has a uniform organizational structure, excellent thermal shock resistance, high temperature resistance and chemical stability and can meet the process requirements for the production of polysilicon. The method has the advantages of simple process, short production period and low cost and is suitable for industrialized application.

Application Domain

Technology Topic

Examples

  • Experimental program(3)

Example Embodiment

[0018] Example 1
[0019] The first step is to prepare particle-graded fused silica ceramic powder
[0020] According to 100Kg of fused silica ceramic powder, weigh 5Kg of quartz powder with a particle size of 0.1μm~1.0μm, 45Kg of quartz powder with a particle size of 0.1μm~1.0μm, and 55Kg of fused silica powder with a particle size of 10μm~100μm. Dry mixing is carried out in the mixer, and the mixing time is 5 hours to obtain the fused silica ceramic mixed powder used for making the crucible, which is ready for use.
[0021] The second step is to prepare the premix
[0022] The premix is ​​prepared according to 100Kg. The preferred formula is as follows: 35Kg of ethyl silicate, 30Kg of absolute ethanol, 2.5Kg of isopropanol, 10Kg of propylene glycol methyl ether, 22Kg of acidic silica sol, 0.5Kg of hydrochloric acid, and add the above chemical reagents to the mixing tank , Adopt a strong stirring method to mix the above chemical reagents uniformly to obtain a mixed solution, and adopt a cooling method to control the temperature of the mixed solution between 7-11°C. The mixed solution obtained through the above process is a premixed solution and is ready for use.
[0023] The third step is to prepare the curing agent
[0024] Prepare the curing agent according to 10Kg, weigh 3Kg of di-n-butylamine and 7Kg of absolute ethanol, add to the mixing tank, mix evenly, and use it as the curing agent for use.
[0025] The fourth step, the production of the green crucible
[0026] Weigh 20 kg of the premix prepared in the second step, put it into a ball mill equipped with a vacuum device, and then add 80Kg of the fused silica ceramic powder prepared in the first step, ball mill and mix for 12 hours, vacuum degas for 30 minutes, and then add it to the 100g of curing agent prepared in three steps, continue to stir for 2 minutes, pour it into the mold, keep it at room temperature for about 30 minutes, the slurry will solidify into a blank; after the blank is demolded, place it on a horizontal platform, about 12 hours later, The green body is completely dried; the dried green body is put into a sintering furnace, heated to 1350℃ at a heating rate of 0.5℃/min, kept at this temperature for 1h, and cooled to room temperature along with the furnace to obtain a fused silica ceramic crucible.

Example Embodiment

[0027] Example 2
[0028] The first step is to prepare particle-graded fused silica ceramic powder
[0029] According to 100Kg of fused silica ceramic powder, weigh the quartz powder with a particle size of 0.1μm~1.0μm to 10Kg, the quartz powder with a particle size of 0.1μm~1.0μm to 45Kg, and the fused silica powder with a particle size of 10μm~100μm to weigh 45Kg. Dry mixing is carried out in the mixer, and the mixing time is 3 hours to obtain the fused silica ceramic mixed powder used for making the crucible, which is ready for use.
[0030] The second step is to prepare the premix
[0031] The premix is ​​prepared according to 100Kg. The preferred formula is as follows: 35Kg of ethyl silicate, 30Kg of absolute ethanol, 2.5Kg of isopropanol, 10Kg of propylene glycol methyl ether, 22Kg of acidic silica sol, 0.5Kg of hydrochloric acid, and add the above chemical reagents to the mixing tank , Adopt a strong stirring method to mix the above chemical reagents uniformly to obtain a mixed solution, and adopt a cooling method to control the temperature of the mixed solution between 7-11°C. The mixed solution obtained through the above process is a premixed solution and is ready for use.
[0032] The third step is to prepare the curing agent
[0033] Prepare the curing agent according to 10Kg, weigh 3Kg of di-n-butylamine and 7Kg of absolute ethanol, add to the mixing tank, mix evenly, and use it as the curing agent for use.
[0034] The fourth step, the production of the green crucible
[0035] Weigh 35 kg of the premix prepared in the second step, put it into a ball mill equipped with a vacuum device, then add 65Kg of the fused silica ceramic powder prepared in the first step, ball mill and mix for 6 hours, vacuum deaerate for 20 minutes, and then add it to the 350g of curing agent prepared in three steps, continue to stir for 1.5 minutes, inject into the mold, keep at room temperature for about 20 minutes, the slurry will solidify into a blank; after the blank is demolded, put it on a horizontal platform, about 18 hours later, The green body is completely dried; the dried green body is put into a sintering furnace, heated to 1250℃ at a heating rate of 2.5℃/min, kept at this temperature for 12h, and cooled to room temperature along with the furnace to obtain a fused silica ceramic crucible.

Example Embodiment

[0036] Example 3
[0037] The first step is to prepare particle-graded fused silica ceramic powder
[0038] According to 100Kg of fused silica ceramic powder, weigh 20Kg of quartz powder with a particle size of 0.1μm~1.0μm, 60Kg of quartz powder with a particle size of 0.1μm~1.0μm, and 20Kg of fused silica powder with a particle size of 10μm~100μm. Dry mixing is carried out in the mixer, and the mixing time is 2 hours to obtain the fused silica ceramic mixed powder used to make the crucible, which is ready for use.
[0039] The second step is to prepare the premix
[0040] The premix is ​​prepared according to 100Kg. The preferred formula is as follows: 35Kg of ethyl silicate, 30Kg of absolute ethanol, 2.5Kg of isopropanol, 10Kg of propylene glycol methyl ether, 22Kg of acidic silica sol, 0.5Kg of hydrochloric acid, and add the above chemical reagents to the mixing tank , Adopt a strong stirring method to mix the above chemical reagents uniformly to obtain a mixed solution, and adopt a cooling method to control the temperature of the mixed solution between 7-11°C. The mixed solution obtained through the above process is a premixed solution and is ready for use.
[0041] The third step is to prepare the curing agent
[0042] Prepare the curing agent according to 10Kg, weigh 3Kg of di-n-butylamine and 7Kg of absolute ethanol, add to the mixing tank, mix evenly, and use it as the curing agent for use.
[0043] The fourth step, the production of the green crucible
[0044] Weigh 50 kg of the premix prepared in the second step, put it into a ball mill equipped with a vacuum device, and then add 50Kg of the fused silica ceramic powder prepared in the first step, ball mill and mix for 1 hour, vacuum degas for 5 minutes, and then add it to the 1000g of curing agent prepared in three steps, continue to stir for 1 minute, inject into the mold, keep at room temperature for about 5 minutes, the slurry will solidify into a blank; after the blank is demolded, put it on a horizontal platform, about 24 hours later, The green body is completely dried; the dried green body is put into a sintering furnace, heated to 1150℃ at a heating rate of 5℃/min, kept at this temperature for 24h, and cooled to room temperature along with the furnace to obtain a fused silica ceramic crucible.
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