CN116286145A - Crucible inner surface release agent for ingot casting and preparation method thereof - Google Patents
Crucible inner surface release agent for ingot casting and preparation method thereof Download PDFInfo
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- CN116286145A CN116286145A CN202310302972.5A CN202310302972A CN116286145A CN 116286145 A CN116286145 A CN 116286145A CN 202310302972 A CN202310302972 A CN 202310302972A CN 116286145 A CN116286145 A CN 116286145A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000005266 casting Methods 0.000 title claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 43
- 239000011268 mixed slurry Substances 0.000 claims abstract description 38
- 239000011230 binding agent Substances 0.000 claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 29
- 239000002253 acid Substances 0.000 claims abstract description 28
- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 28
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 23
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 23
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000006082 mold release agent Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 6
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 32
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 32
- 239000004310 lactic acid Substances 0.000 claims description 16
- 235000014655 lactic acid Nutrition 0.000 claims description 16
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000002002 slurry Substances 0.000 abstract description 22
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract description 10
- 230000015271 coagulation Effects 0.000 abstract description 2
- 238000005345 coagulation Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 15
- 239000000126 substance Substances 0.000 description 11
- 230000000694 effects Effects 0.000 description 10
- 150000002148 esters Chemical class 0.000 description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 239000005350 fused silica glass Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000012798 spherical particle Substances 0.000 description 4
- 238000000889 atomisation Methods 0.000 description 3
- 230000003628 erosive effect Effects 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 229920005591 polysilicon Polymers 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M163/00—Lubricating compositions characterised by the additive being a mixture of a compound of unknown or incompletely defined constitution and a non-macromolecular compound, each of these compounds being essential
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B7/00—Moulds; Cores; Mandrels
- B28B7/38—Treating surfaces of moulds, cores, or mandrels to prevent sticking
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/061—Carbides; Hydrides; Nitrides
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/10—Compounds containing silicon
- C10M2201/105—Silica
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/02—Hydroxy compounds
- C10M2207/021—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
- C10M2207/124—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms containing hydroxy groups; Ethers thereof
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/287—Partial esters
- C10M2207/289—Partial esters containing free hydroxy groups
- C10M2207/2895—Partial esters containing free hydroxy groups used as base material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/04—Detergent property or dispersant property
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/18—Anti-foaming property
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/36—Release agents or mold release agents
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Ceramic Engineering (AREA)
- Mechanical Engineering (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a mold release agent for the inner surface of a crucible for cast ingots and a preparation method thereof, wherein the mold release agent comprises, by weight, 30-40 parts of silicon nitride, 10-20 parts of silica sol, 5-10 parts of fatty alcohol, 5-10 parts of weak acid, 10-20 parts of binder and 20-30 parts of water. Firstly, mixing silicon nitride, silica sol and water, and grinding and stirring to obtain a mixed slurry I; and then adding a binder, weak acid and fatty alcohol into the mixed slurry I, and continuously stirring to obtain mixed slurry II, namely the release agent. According to the mold release agent for the inner surface of the crucible for the cast ingot and the preparation method thereof, weak acid and fatty alcohol are added into raw materials, and the binder and a specific process in the preparation process are combined, so that the mold release agent prepared by the mold release agent is high in stability, free of limitation of using temperature, suitable in pH value of prepared slurry, free of coagulation on the surface of the crucible, smooth and fine in surface of a polycrystalline silicon ingot of the cast ingot, and suitable for large-scale industrial production.
Description
Technical Field
The invention relates to the technical field of polycrystalline silicon ingots, in particular to a release agent for the inner surface of a crucible for ingots and a preparation method thereof.
Background
In the preparation process of the polycrystalline silicon ingot, a fused quartz crucible is an important container which is necessary to be adopted in the stage of the polycrystalline silicon ingot, a silicon material is cast into a polycrystalline silicon ingot through the processes of melting, crystal growth, annealing and cooling in the crucible, and the polycrystalline silicon ingot is cut into silicon wafers according to technical requirements, so that the polycrystalline silicon ingot becomes a base material for producing and manufacturing solar cells.
At present, the release agent on the inner surface of the fused quartz crucible is mainly prepared into slurry by adding silicon nitride and silica sol and water, and then the release agent is sprayed when the fused quartz crucible is heated to 80-100 ℃. The slurry prepared by the preparation method is easy to have bubbles, so that the slurry forms poor pinholes after being coagulated on the surface of the crucible, and the slurry is easy to be rapidly coagulated into spherical particles after being sprayed on the surface of the crucible, so that the surface roughness of the silicon ingot is particularly large.
Disclosure of Invention
The invention provides a release agent for the inner surface of a crucible for ingot casting and a preparation method thereof, which are not limited by temperature, and can effectively avoid the risk of sticking the crucible to the ingot, so that the surface of a silicon ingot is smooth and fine.
In order to achieve the above purpose, the present invention provides the following technical solutions: the inner surface release agent for the crucible for the ingot comprises silicon nitride, silica sol, water, fatty alcohol, weak acid and a binder.
As a preferable scheme, the mold release agent for the inner surface of the crucible for casting ingot comprises the following raw materials in parts by weight: 30-40 parts of silicon nitride, 10-20 parts of silica sol, 5-10 parts of fatty alcohol, 5-10 parts of weak acid, 10-20 parts of binder and 20-30 parts of water. The weak acid can adjust the pH value of the release agent, so that the release agent slurry has better dispersibility and atomization effect, and the slurry is prevented from being coagulated into spherical particles on the surface of the crucible; the fatty alcohol can disperse and defoam bubbles in the release agent slurry, so that the slurry is prevented from forming needle hole defects after being coagulated on the surface of the crucible; the binder can stabilize the binding slurry and reduce its flow.
As a preferable scheme, the mold release agent for the inner surface of the crucible for casting ingot comprises the following raw materials in parts by weight: 34 parts of silicon nitride, 16 parts of silica sol, 8 parts of fatty alcohol, 8 parts of weak acid, 15 parts of binder and 23 parts of water.
Preferably, the fatty alcohol is n-octanol.
Preferably, the weak acid is lactic acid.
The invention also provides a preparation method of the inner surface release agent of the crucible for ingot casting, which comprises the following steps:
s1, mixing silicon nitride, silica sol and water, and grinding and stirring to obtain mixed slurry I;
s2, adding a binder, weak acid and fatty alcohol into the mixed slurry I, and continuously stirring to obtain mixed slurry II, namely the release agent.
According to the preferred scheme, the mold release agent for the inner surface of the crucible comprises, by weight, 30-40 parts of silicon nitride, 10-20 parts of silica sol, 5-10 parts of fatty alcohol, 5-10 parts of weak acid, 10-20 parts of binder and 20-30 parts of water;
the preparation method of the release agent on the inner surface of the crucible comprises the following steps:
s1, mixing the silicon nitride, silica sol and water, grinding and stirring for 30-40 minutes to obtain mixed slurry I;
s2, sequentially adding a binder, weak acid and fatty alcohol into the first mixed slurry, and continuously stirring for 8-10 minutes to obtain a second mixed slurry, namely the release agent.
S2, through mixing the weak acid substance and the fatty alcohol, the weak acid substance and the fatty alcohol can be reacted to generate ester substances, so that the stability of the mixed slurry II is further ensured, the flow ductility is further reduced, and the release agent can be sprayed on the surface of the crucible at normal temperature. And the generated ester substances enable the molding effect of the release agent to be better, and can isolate the erosion effect of external feed liquid on the crucible.
As a preferable scheme, the adhesive, weak acid and fatty alcohol are added into the first mixed slurry and continuously stirred to obtain the second mixed slurry, wherein the stirring mode is that an ultrasonic stirrer is adopted for stirring, and the ultrasonic stirrer is adopted for stirring, so that the adhesive can be prevented from agglomerating.
The mold release agent for the inner surface of the crucible for the cast ingot and the preparation method thereof have the following beneficial effects: lactic acid and n-octanol are added into the raw materials, and the pH value of the silicon nitride slurry is neutralized by the lactic acid, so that the slurry has better dispersibility and atomization effect, and the slurry is prevented from being coagulated into spherical particles on the surface of a crucible; by utilizing the good defoaming effect of n-octanol, the slurry is prevented from forming bad pinholes after being coagulated on the surface of the crucible, so that the surface of the polysilicon ingot of the ingot is smooth and fine. The produced ester substance can make the release agent more stable through the reaction of lactic acid and n-octanol, the molding effect is good, and the ester substance and the adhesive have isolated effect on external erosion, and meanwhile, the integral ductility of the release agent is reduced through the cooperation of the ester substance and the adhesive, so that the use of the release agent is not limited by temperature.
Detailed Description
Other advantages and advantages of the present invention will become readily apparent to those skilled in the art from the following detailed description, wherein it is shown and described only a part, but not all, of the practice of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention discloses a release agent for the inner surface of a crucible for an ingot and a preparation method thereof, wherein the release agent for the inner surface of the crucible for the ingot comprises the following raw materials in parts by weight: 30-40 parts of silicon nitride, 10-20 parts of silica sol, 5-10 parts of fatty alcohol, 5-10 parts of weak acid, 10-20 parts of binder and 20-30 parts of water, and the preparation method comprises the following steps:
s1, mixing silicon nitride, silica sol and water, grinding and stirring for 30-40 minutes to thoroughly stir to obtain mixed slurry I;
s2, sequentially adding a binder, weak acid and fatty alcohol into the first mixed slurry, and continuously stirring for 8-10 minutes to obtain a second mixed slurry, namely the release agent.
In S2, the binder stabilizes the binder slurry and reduces its flowability.
Since silicon nitride is generally alkaline, the pH value of the mixed slurry I can be adjusted by adding weak acid into the mixed slurry I, so that the slurry has better dispersibility and atomization effect, and the slurry is prevented from being coagulated into spherical particles on the surface of the crucible. And can not adopt strong acid substances to prevent corrosion to the crucible. As the weak acid, lactic acid, citric acid and the like are usually used.
By adding the fatty alcohol to the mixed slurry one, the fatty alcohol can disperse and defoam the bubbles in the mixed slurry one, and prevent the slurry from forming pinholes after coagulation on the crucible surface. The fatty alcohol can be n-octanol, ethanol, etc.
In S2, the stirring mode is ultrasonic stirring, and the ultrasonic stirrer is used for stirring, so that the caking of the binder can be prevented.
In the invention, the weak acid substance and the fatty alcohol are mixed to react to generate the ester substance, so that the stability of the mixed slurry II is further ensured, the flow ductility is further reduced, and the release agent can be sprayed on the surface of the crucible at normal temperature. In addition, the molding effect of the mold release agent is better through the generated ester substances, and the erosion effect of the external feed liquid on the crucible can be isolated.
Lactic acid and n-octanol are subjected to slow weak esterification reaction at normal temperature, complete reaction does not occur, and a part of lactic acid and n-octanol are reserved, so that the slurry is dispersed and defoamed.
The present invention will be further described in conjunction with the following examples, which are also to be understood as being merely illustrative of the present invention and not limiting the scope of the present invention, and some insubstantial modifications and variations will be within the scope of the invention as described above by those skilled in the art. The specific process parameters and the like described below are also merely examples of suitable ranges, i.e., one skilled in the art can make a suitable selection from the description herein and are not intended to be limited to the specific values described below.
Example 1
The embodiment discloses a preparation method of a release agent for the inner surface of a crucible for ingot casting, which comprises the following steps:
s1, mixing 30 parts by weight of silicon nitride, 20 parts by weight of silica sol and 30 parts by weight of water, and grinding and stirring for 30 minutes to obtain a first mixed slurry;
s2, taking 5 parts by weight of n-octanol, 10 parts by weight of lactic acid and 20 parts by weight of binder for standby, adding the binder, lactic acid and n-octanol into the mixed slurry I, and carrying out ultrasonic stirring for 10 minutes to obtain mixed slurry II, namely the release agent. The binder used in this example was GH-2 type high purity binder manufactured by Yoshike electronics technologies Co.
Example two
The embodiment discloses a preparation method of a release agent for the inner surface of a crucible for ingot casting, which comprises the following steps:
s1, mixing 40 parts by weight of silicon nitride, 10 parts by weight of silica sol and 20 parts by weight of water, and grinding and stirring for 40 minutes to obtain mixed slurry I;
s2, 10 parts by weight of n-octanol, 5 parts by weight of lactic acid and 10 parts by weight of binder are taken for standby, the binder, lactic acid and n-octanol are added into the mixed slurry I for ultrasonic stirring, the stirring time is 8 minutes, and the mixed slurry II is obtained, namely the release agent. The binder used in this example was GH-2 type high purity binder manufactured by Yoshike electronics technologies Co.
Example III
The embodiment discloses a preparation method of a release agent for the inner surface of a crucible for ingot casting, which comprises the following steps:
s1, mixing 34 parts by weight of silicon nitride, 16 parts by weight of silica sol and 23 parts by weight of water, and grinding and stirring for 35 minutes to obtain a mixed slurry I;
s2, 8 parts by weight of n-octanol, 8 parts by weight of lactic acid and 15 parts by weight of binder are taken for standby, the binder, lactic acid and n-octanol are added into the mixed slurry I for ultrasonic stirring, the stirring time is 10 minutes, and the mixed slurry II is obtained, namely the release agent. The binder used in this example was GH-2 type high purity binder manufactured by Yoshike electronics technologies Co.
Example IV
This example differs from example three in that n-octanol is replaced with ethanol, and other raw materials, components, and methods of preparation are the same as example three.
Example five
This example differs from example three in that lactic acid is replaced with citric acid, and other raw materials, components and methods of preparation are the same as example three.
Comparative example one
The difference between the first comparative example and the third comparative example is that n-octanol is not added in the comparative example, and other raw materials, components and preparation methods are the same as those of the third comparative example.
Comparative example two
The difference between the second comparative example and the third comparative example is that lactic acid was not added in the present comparative example, and other raw materials, components and preparation methods were the same as those of the third comparative example.
Comparative example three
The difference between the comparative example III and the example III is that the ultrasonic stirring is not adopted in the S2, but the common stirring mode is adopted, and other raw materials and preparation methods are the same as those of the example III.
Comparative example four
The fourth comparative example uses the existing release agent, and the ingredients of the release agent are silicon nitride, silica sol and water.
Nine mold release agents provided in examples one, two, three, four, five, and one, two, three, four were sampled in equal amounts and measured for the following performance parameters, respectively:
1. use temperature
2. pH value of slurry
3. Ductility of flow
And further measuring the polysilicon ingot cast by the fused quartz crucible adopting the nine release agents, wherein the specific measurement item is the roughness of the surface of the silicon ingot, and a measuring tool adopts a roughness meter.
See table 1 for test results:
table 1 test results of nine release agents
According to the table, the detection results of the examples and the comparative examples show that the release agent for the inner surface of the crucible for the ingot and the preparation method thereof provided by the invention have the advantages that the stability of the release agent prepared by the invention is strong, the release agent is not limited by the use temperature, the pH value of the prepared slurry is proper, the slurry is not condensed on the surface of the crucible, and the surface of the polysilicon ingot of the ingot is smooth and fine, so that the release agent is suitable for large-scale industrial production.
While the invention has been described in detail in the foregoing general description and specific examples, it will be apparent to those skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed. The embodiments of the present invention described above do not limit the scope of the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the scope of the present invention as set forth in the appended claims.
Claims (8)
1. The inner surface release agent for the crucible for the ingot casting comprises silicon nitride, silica sol and water, and is characterized by further comprising fatty alcohol, weak acid and a binder.
2. The mold release agent for the inner surface of the crucible according to claim 1, which comprises the following raw materials in parts by weight: 30-40 parts of silicon nitride, 10-20 parts of silica sol, 5-10 parts of fatty alcohol, 5-10 parts of weak acid, 10-20 parts of binder and 20-30 parts of water.
3. The mold release agent for the inner surface of the crucible according to claim 1, which comprises the following raw materials in parts by weight: 34 parts of silicon nitride, 16 parts of silica sol, 8 parts of fatty alcohol, 8 parts of weak acid, 15 parts of binder and 23 parts of water.
4. The crucible inner surface release agent according to claim 1, wherein the fatty alcohol is n-octanol.
5. The crucible inner surface release agent according to claim 1, wherein the weak acid is lactic acid.
6. The method for producing the mold release agent for the inner surface of the crucible for ingot casting according to any one of claims 1 to 5, comprising the steps of:
mixing silicon nitride, silica sol and water, and grinding and stirring to obtain mixed slurry I;
and adding a binder, weak acid and fatty alcohol into the first mixed slurry, and continuously stirring to obtain a second mixed slurry, namely the release agent.
7. The method for preparing the mold release agent for the inner surface of the crucible for the ingot casting according to claim 6, wherein the mold release agent for the inner surface of the crucible comprises the following raw materials, by weight, 30-40 parts of silicon nitride, 10-20 parts of silica sol, 5-10 parts of fatty alcohol, 5-10 parts of weak acid, 10-20 parts of binder and 20-30 parts of water;
the preparation method of the release agent on the inner surface of the crucible comprises the following steps:
mixing the silicon nitride, silica sol and water, grinding and stirring for 30-40 minutes to obtain a first mixed slurry;
and sequentially adding a binder, weak acid and fatty alcohol into the first mixed slurry, and continuously stirring to obtain a second mixed slurry, namely the release agent.
8. The method for producing an ingot casting crucible inner surface mold release agent according to claim 6, wherein the first mixed slurry is mixed with a binder, a weak acid and a fatty alcohol continuously to obtain a second mixed slurry, and the second mixed slurry is stirred by an ultrasonic stirrer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310302972.5A CN116286145B (en) | 2023-03-27 | 2023-03-27 | Crucible inner surface release agent for ingot casting and preparation method thereof |
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| CN202310302972.5A CN116286145B (en) | 2023-03-27 | 2023-03-27 | Crucible inner surface release agent for ingot casting and preparation method thereof |
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| CN116286145B CN116286145B (en) | 2024-07-23 |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004338185A (en) * | 2003-05-14 | 2004-12-02 | Fuji Photo Film Co Ltd | Polylactic acid resin molded product and its manufacturing method |
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| JP2004338185A (en) * | 2003-05-14 | 2004-12-02 | Fuji Photo Film Co Ltd | Polylactic acid resin molded product and its manufacturing method |
| WO2004110671A2 (en) * | 2003-06-13 | 2004-12-23 | Leibniz-Institut Für Neue Materialien Gemeinnützige Gmbh | Antiadhesive high temperature layers |
| US20090159230A1 (en) * | 2006-08-30 | 2009-06-25 | Kyocera Corporation | Mold Forming and Molding Method |
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| US20130068925A1 (en) * | 2011-09-20 | 2013-03-21 | Chung-Hou Tony Hsiao | Photovoltaic Ingot Mold Release |
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