CN111925752B - Adhesive for high-temperature photoelectric semiconductor material and preparation method thereof - Google Patents
Adhesive for high-temperature photoelectric semiconductor material and preparation method thereof Download PDFInfo
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- CN111925752B CN111925752B CN202010647857.8A CN202010647857A CN111925752B CN 111925752 B CN111925752 B CN 111925752B CN 202010647857 A CN202010647857 A CN 202010647857A CN 111925752 B CN111925752 B CN 111925752B
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- 239000000853 adhesive Substances 0.000 title claims abstract description 96
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 96
- 239000004065 semiconductor Substances 0.000 title claims abstract description 75
- 239000000463 material Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000000839 emulsion Substances 0.000 claims abstract description 72
- 239000002562 thickening agent Substances 0.000 claims abstract description 64
- 239000000945 filler Substances 0.000 claims abstract description 60
- 239000002270 dispersing agent Substances 0.000 claims abstract description 57
- 229920002689 polyvinyl acetate Polymers 0.000 claims abstract description 55
- 239000011118 polyvinyl acetate Substances 0.000 claims abstract description 55
- 239000002904 solvent Substances 0.000 claims abstract description 49
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 239000013530 defoamer Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 112
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 97
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 97
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 75
- 239000011863 silicon-based powder Substances 0.000 claims description 67
- 239000002518 antifoaming agent Substances 0.000 claims description 52
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical group CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 claims description 34
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 18
- 229920000570 polyether Polymers 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- 239000001087 glyceryl triacetate Substances 0.000 claims description 17
- 235000013773 glyceryl triacetate Nutrition 0.000 claims description 17
- 230000001965 increasing effect Effects 0.000 claims description 17
- 229960002622 triacetin Drugs 0.000 claims description 17
- 239000003973 paint Substances 0.000 claims description 16
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- 230000008961 swelling Effects 0.000 claims description 16
- 229910021485 fumed silica Inorganic materials 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 12
- 230000005693 optoelectronics Effects 0.000 claims description 6
- 125000005375 organosiloxane group Chemical group 0.000 claims description 4
- 239000013538 functional additive Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 75
- 238000000576 coating method Methods 0.000 abstract description 75
- 238000004519 manufacturing process Methods 0.000 abstract description 14
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- 238000000227 grinding Methods 0.000 description 31
- 238000000034 method Methods 0.000 description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 25
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 25
- 235000010234 sodium benzoate Nutrition 0.000 description 25
- 239000004299 sodium benzoate Substances 0.000 description 25
- 239000004575 stone Substances 0.000 description 22
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- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 14
- 239000010439 graphite Substances 0.000 description 14
- 229910002804 graphite Inorganic materials 0.000 description 14
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- 238000003825 pressing Methods 0.000 description 2
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- 238000005086 pumping Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 208000010392 Bone Fractures Diseases 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 1
- 206010017076 Fracture Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011335 coal coke Substances 0.000 description 1
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- 238000007580 dry-mixing Methods 0.000 description 1
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- 238000011068 loading method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
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- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
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- 239000003381 stabilizer Substances 0.000 description 1
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- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J131/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid, or of a haloformic acid; Adhesives based on derivatives of such polymers
- C09J131/02—Homopolymers or copolymers of esters of monocarboxylic acids
- C09J131/04—Homopolymers or copolymers of vinyl acetate
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
- H01L21/56—Encapsulations, e.g. encapsulation layers, coatings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to the technical field of semiconductor material processing, in particular to an adhesive for a high-temperature photoelectric semiconductor material and a preparation method thereof. The raw materials for preparing the adhesive comprise the following components: 25-50 parts of polyvinyl acetate emulsion, 40-60 parts of filler, 0-1.0 part of thickener, 1-3.5 parts of functional assistant, 0.1-0.8 part of dispersant, 0.1-0.8 part of defoamer and 3-12 parts of solvent. The adhesive for the high-temperature photoelectric semiconductor material has higher bonding strength to a millstone, does not crack or break again after being used for a plurality of times after being used for brushing and repairing damaged parts of a coating, obviously prolongs the service life, can improve the degree of 180 heats/pieces from the traditional 100 heats/pieces, and does not reduce the yield in the production of semiconductor products after being repaired.
Description
Technical Field
The invention relates to the technical field of semiconductor material processing, in particular to an adhesive for a high-temperature photoelectric semiconductor material and a preparation method thereof.
Background
Semiconductor materials are essential materials for the production of semiconductor devices, and are the basis for semiconductor device applications, which determine and support the state and development of the overall semiconductor electronics. One of the most important of the semiconductor materials at present is the semiconductor epitaxial material, which usually comprises many layers, including substrate material, buffer layer (n-type, p-type or intrinsic semiconductor material), active region, contact layer (p-type or n-type), and its application range includes microelectronics, optoelectronic device circuits, such as LED, LD, PD, IC, etc. The methods for preparing semiconductor epitaxial materials are various, wherein the MOCVD method is the main means for preparing compound epitaxial materials, especially photoelectronic materials in the industry at present. Among them, a graphite tray for loading a substrate sheet used in MOCVD epitaxial growth is an important component in MOCVD equipment. In order to avoid the corrosive effect of gases such as ammonia gas and hydrogen gas on graphite, a graphite tray used in the epitaxial growth of group III nitride is generally coated with a uniform protective layer on the surface of the graphite tray. The requirement on the uniformity, consistency and heat conductivity of the protective layer in the epitaxial growth of the material is very high, however, the coating on the surface of the stone grinding disc is easy to crack and other damage phenomena in the use process, so that a large amount of graphite dust exists in the reaction chamber, the normal processing of the photoelectric material is influenced, and the production yield of the product is remarkably reduced. Therefore, the damaged part of the coating on the surface of the stone grinding disc needs to be repaired, so that the surface of the stone grinding disc is always in a uniform and flat state.
Chinese patent CN201010033965 discloses a method for metal organic chemistryA lining tray of a deposition device and a manufacturing process thereof are disclosed, wherein components such as silicon carbide, carbon, boron or boride are mixed in a dry mode, and then a blank body is formed by adopting a dry pressing forming process; carrying out high-temperature vacuum sintering on the blank; and grinding the sintered blank to form the lining tray. However, the processing method is complex, the firing process can be performed after dry mixing, dry pressing and forming process, numerical control processing process and the like, the production cost is high, and the effect is low. Chinese patent CN201210374319 discloses a method for preparing a silicon carbide coating on the surface of graphite. The method comprises the steps of firstly heating solid silicon materials in a high-temperature graphitization furnace to form silicon vapor, directly reacting the silicon vapor with carbon on the surface layer of a graphite matrix to form a layer of CVR silicon carbide coating, and then introducing trichloromethylsilane (CH) into a CVD furnace3SiCl3MTS) is adopted, a CVD silicon carbide coating is cracked on the CVR silicon carbide coating at a high temperature by using a CVD process, so that the pores of the CVR silicon carbide coating are effectively filled, and the bonding strength is improved. However, since the reaction between the silicon vapor and the solid carbon on the surface of the graphite substrate is random, the thickness, uniformity, etc. of the coating are not well controlled, and the coating needs to be subjected to post-planarization treatment again. Moreover, when the damaged portion of the coating surface is repaired in the same manner as the original coating preparation method, silicon atoms or crystals are deposited on the undamaged portion, resulting in unnecessary waste. Therefore, the conventional technology has no technical scheme for repairing and reusing the coating on the surface of the millstone, and the conventional method for preparing the silicon carbide coating on the surface of the millstone is not suitable for repairing the breakage of the coating.
Disclosure of Invention
In view of the above technical problems, a first aspect of the present invention provides an adhesive for a high-temperature optoelectronic semiconductor material, wherein the raw materials for preparing the adhesive comprise the following components: 25-50 parts of polyvinyl acetate emulsion, 40-60 parts of filler, 0-1.0 part of thickener, 1-3.5 parts of functional assistant, 0.1-0.8 part of dispersant, 0.1-0.8 part of defoamer and 3-12 parts of solvent.
As a preferable technical scheme of the invention, the filler is silicon powder and/or silicon carbide.
As a preferable technical scheme of the invention, the particle size of the silicon powder is not higher than 50 microns.
As a preferred technical scheme of the present invention, the weight ratio of the silicon carbide to the silicon powder is 1: (3-5).
In a preferred embodiment of the present invention, the grain size of the silicon carbide is not greater than 50 μm.
As a preferable technical scheme, the functional auxiliary agent is glyceryl triacetate.
As a preferable technical scheme, the defoaming agent is polyether modified organic siloxane emulsion.
As a preferable technical scheme of the invention, the polyether modified organic siloxane emulsion contains gas phase silicon dioxide.
As a preferable technical scheme of the invention, the pH value of the dispersing agent is not lower than 7.0.
The second aspect of the present invention provides a method for preparing the adhesive for high-temperature optoelectronic semiconductor material, which comprises the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a functional assistant, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 2-5 min at 180-220 rpm, then increasing the stirring speed to 1200-1800 rpm, and stirring for 15-30 min;
(4) and (3) adding the thickening agent in the step (1), and stirring for 10-20 min to obtain the water-based paint.
Has the advantages that: compared with the traditional process, when the adhesive for the high-temperature photoelectric semiconductor material is used for repairing the damaged part of the millstone, the filler is connected to the surface of the millstone in a chemical bonding mode to repair the coating, so that the thermal mismatch and the resource waste when the silicon carbide coating is prepared on the surface of the graphite matrix by directly adopting a chemical vapor deposition process in the traditional method are effectively avoided, the bonding strength of the silicon carbide coating on the surface of the graphite disk is improved, the repaired coating is less prone to secondary cracking or damage, and the phenomenon of secondary cracking or damage does not occur after the damaged part of the coating is brushed and repaired for many times. And the fluidity of the components of the adhesive is improved by regulating and controlling the components and the proportion of the filler, the functional assistant, the defoaming agent, the dispersing agent and the like in the adhesive, so that the adhesive can effectively flow into a smooth and cloudy coating, and meanwhile, the denaturation of the adhesive can be effectively improved, so that the adhesive can also hang on the edge of a stone grinding disc well, and the microstructure uniformity and consistency of a repaired coating obtained by heat treatment can be improved. Meanwhile, under the action of the components such as polyvinyl acetate emulsion, a dispersing agent, a defoaming agent and the like, silicon powder and silicon carbide in the adhesive system are fully dispersed and uniformly coated on the damaged part of the coating, and in the heat treatment process of the coating, the silicon carbide in the system is uniformly filled in a cavity formed by the reaction of the silicon powder and carbon on the surface of the stone mill, so that the density of the repaired coating is improved. And because the reaction between the silicon powder and the carbon on the surface of the stone grinding disc and the deposition repair of the silicon carbide in the adhesive component are carried out simultaneously, the silicon carbide formed by the reaction is beneficial to inducing the arrangement and the deposition direction of the silicon carbide filler in the adhesive at the damaged part of the coating, so that the microstructure of the silicon carbide filler in the adhesive is consistent with that of the original coating, the thermal mismatch caused by the difference of the microstructure between the repair coating and the original coating is avoided, and the great difference of the performances of the thermal conductivity, the expansion capacity and the like in the using process is avoided, thereby influencing the normal production of the semiconductor material, obviously improving the service life, improving the traditional 100 heats/wafer level to 180 heats/wafer level, and not reducing the yield in the production of the semiconductor product after the repair.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
The words "preferred", "preferably", "further", "more preferred", and the like, in the present invention, refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
The invention provides an adhesive for a high-temperature photoelectric semiconductor material, which is prepared from the following raw materials in parts by weight: 25-50 parts of polyvinyl acetate emulsion, 40-60 parts of filler, 0-1.0 part of thickener, 1-3.5 parts of functional assistant, 0.1-0.8 part of dispersant, 0.1-0.8 part of defoamer and 3-12 parts of solvent.
In some embodiments, the filler is silicon powder and/or silicon carbide.
The use method of the adhesive for the high-temperature photoelectric semiconductor material is not specially limited, the adhesive for the high-temperature photoelectric semiconductor material can be arranged at the cracking or damage part of the surface coating of the millstone by adopting the modes of spraying, brushing and the like, the brushing thickness can be 3-25 micrometers, the adjustment is carried out according to the thickness of the original coating, then the millstone is placed in a graphitization furnace, the vacuum pumping is carried out, the oxidizing gas such as oxygen in the furnace is removed, the vacuum degree is 100-1000 Pa, and the heat treatment is carried out for 30-90 minutes at 1400 ℃.
The uniformity and consistency of the silicon carbide coating on the surface of the stone grinding disc are crucial to the photoelectric performance of semiconductor materials, but the uniformity and consistency are influenced by the breakage of the surface coating. If the millstone is directly replaced, great waste and sharp increase of production cost are caused, and on one hand, complicated process flow is needed to repair the cracking and damage of the coating according to the traditional preparation method of the millstone silicon carbide coating, so that the production cost is improved, and on the other hand, the thickness of the coating at the repaired part and the uniformity, consistency and the like between the thickness of the coating and the original coating cannot be well controlled, so that the heat conduction is not uniform, and the normal production of semiconductor products is influenced. The applicant finds that the adhesive is prepared by adding the filler into the polyvinyl acetate emulsion, the prepared adhesive is coated on the damaged part of the millstone as required, and then the heat treatment is carried out in the graphitization furnace at 1400 ℃, because the filler contains silicon powder, the silicon powder is vaporized into silicon steam under the conditions of vacuum pumping and high temperature in the graphitization furnace, the silicon steam reacts with carbon on the surface of the damaged part of the millstone to generate silicon carbide, and the damaged or cracked part is filled and repaired, so that the coating uniformity, the consistency and the like on the surface of the graphite disk are improved. The filler such as silicon powder is coated on the cracked and damaged parts in a liquid form, so that the thickness and uniformity of the coating are easy to adjust, and the coating with the thickness of 3-20 micrometers can be generally coated as required and then subjected to heat treatment. In addition, because the repair coating obtains through chemical vapor reaction with the carbon atom on stone mill surface in this application, is connected through chemical bonding between coating and the stone mill to make the bonding strength between repair coating and the stone mill higher, the coating after repairing is more difficult to secondary fracture or damage, helps improving the life of stone mill, makes its life-span promote to 160 ~ 180 heats/piece from original 100 heats/piece.
The silicon powder (Microsilica or Silica Fume) in the invention, also called Microsilica, is known as "Silica Fume", and is a component which is well known to those skilled in the art, and is obtained by collecting and treating smoke dust escaping with waste gas in the process of smelting industrial silicon and ferrosilicon at high temperature by an industrial electric furnace through a special collecting device. The silicon carbide (SiC) is also called carborundum, is prepared by smelting quartz sand, petroleum coke (or coal coke), wood chips (salt is required when producing green silicon carbide) and other raw materials at high temperature by a resistance furnace, and is a well-known component for the technical personnel in the field.
In some preferred embodiments, the silicon powder has a particle size of no greater than 50 microns.
Further, the particle size of the silicon powder is not higher than 30 microns.
Further preferably, the weight ratio of the silicon carbide to the silicon powder is 1: (3-5).
Preferably, the weight ratio of the silicon carbide to the silicon powder is 1: 4.8.
further, the particle size of the silicon carbide is not greater than 50 microns.
Preferably, the particle size of the silicon carbide is 40-50 microns. The silicon carbide in the invention can be selected from green silicon carbide micropowder of a Zibo Zichuan new grinding material grinding tool factory.
The applicant found in the course of completing the present invention that although the filler in the adhesive can be chemically bonded to the surface of the graphite disk by means provided by the present application to repair the coating, the bonding strength to the surface of the graphite disk is improved. However, the adhesive also contains components such as polyvinyl acetate emulsion, glyceryl triacetate and solvent, which are vaporized in the heat treatment process of the coating, so that holes are formed in the original position of the coating, which affects the density of the repaired coating, even pores are formed on the surface or inside of the coating, the uniformity and the heat conduction consistency of the coating are seriously reduced, and the photoelectric performance of the photoelectric semiconductor product and the yield of the product are directly affected. The applicant finds that when a certain amount of silicon powder and silicon carbide are added into the adhesive for the high-temperature photoelectric semiconductor material as fillers, the uniformity and the density of the repair coating are improved, and the problem of uneven heat conduction of the repair coating is solved, so that the yield of semiconductor products is remarkably improved from about 90% to 98% or above. The applicant speculates that the silicon powder and the silicon carbide in the adhesive system are fully dispersed and uniformly coated on the damaged part of the coating under the action of components such as polyvinyl acetate emulsion, a dispersing agent, a defoaming agent and the like, and the silicon carbide in the system is uniformly filled in a cavity formed by the reaction of the silicon powder and carbon on the surface of a stone grinding disc in the heat treatment process of the coating, so that the compactness of the repair coating is improved. And because the reaction between the silicon powder and the carbon on the surface of the stone grinding disc and the deposition repair of the silicon carbide in the adhesive component are carried out simultaneously, the silicon carbide formed by the reaction is beneficial to inducing the arrangement and the deposition direction of the silicon carbide filler in the adhesive at the damaged part of the coating, so that the microstructure of the silicon carbide filler in the adhesive is consistent with that of the original coating, the thermal mismatch caused by the difference of the microstructures between the repair coating and the original coating is avoided, and the large difference of the performances of the thermal conductivity, the expansion capacity and the like in the use process is avoided, thereby influencing the normal production of the semiconductor material.
The applicant finds that the grain sizes and the weight ratio of the silicon powder and the silicon carbide in the adhesive for the high-temperature photoelectric semiconductor material have important relation on the comprehensive performance of the repaired coating. When the weight ratio of the silicon carbide to the silicon powder is 1: (3-5), when the particle size of the silicon powder is smaller than 50 microns, all the performances of the millstone after repairing the damaged coating are obviously improved, the yield of the produced photoelectric semiconductor product is obviously improved, and the degree before damage can be basically achieved. Particularly, on the premise that silicon powder and silicon carbide with specific particle size and proportion are adopted according to the conditions, when green silicon carbide with the particle size of 40-50 microns is used, the repaired stone grinding disc has the most remarkable effect of improving the yield of semiconductor products. Probably, under the conditions, the reaction between the silicon powder and the carbon on the surface of the stone grinding disc and the ordered arrangement and deposition of the silicon carbide in the adhesive reach the optimal balance, so that the silicon powder can fully react with the carbon on the surface of the stone grinding disc to form a silicon carbide coating, and simultaneously, the silicon carbide in the adhesive can just fill gaps formed by the reaction of the silicon powder, so that the silicon powder becomes compact and uniform. When the particle sizes of the silicon carbide and the silicon powder are too large or too small, the sizes of the cavity and the gap formed on the silicon carbide coating formed by the reaction of the silicon powder and the carbon on the surface of the stone grinding disc are not matched with the size of the silicon carbide in the adhesive, and the gaps cannot be fully filled, so that the heat conduction stability and uniformity of the silicon carbide coating are influenced.
In some embodiments, the functional additive is glyceryl triacetate.
In some embodiments, the defoamer is a polyether modified organosiloxane emulsion.
Further, the polyether modified organosiloxane emulsion includes fumed silica.
Further, the solid content of the defoaming agent is 15-30 wt%.
Further, the solid content of the defoaming agent was 20 wt%. In the invention, the de-foaming agent can be selected from 1488.
In some embodiments, the pH of the dispersant is not less than 7.0.
Further, the pH value of the dispersant is not higher than 9.0.
More preferably, the pH of the dispersant is 8.5. The dispersant of the present invention may be 760W.
The thickener in the invention is a component for adjusting the consistency of the adhesive, and the specific components are not particularly limited, and various thickeners known to those skilled in the art can be selected, including but not limited to hydroxyethyl cellulose.
The polyvinyl acetate emulsion is a milky viscous liquid prepared by polymerizing vinyl acetate monomers under the action of materials such as an initiator, a protective adhesive and the like. In some embodiments, the polyvinyl acetate emulsion has a solids content of 25 to 50 wt%; further, the viscosity of the polyvinyl acetate emulsion is 8000-18000 mPa.s. The polyvinyl acetate emulsion of the present invention can be commercially available, for example, WX-505 of Star light Synthesis materials, Inc. of West lake; or biochemical SD-40.
The solvent used in the present invention is a component for dissolving or dispersing other components in the adhesive, and can be selected from solvents known to those skilled in the art, including but not limited to water, isopropanol, propylene glycol, etc.
Under the premise of not affecting the comprehensive performance of the adhesive, other various auxiliary agents known by persons skilled in the art can be added, including but not limited to bactericides (such as sodium benzoate and the like), stabilizers and the like.
The applicant finds that the stable leveling of the adhesive at the damaged part forms a uniform coating, and the physical and chemical parameters of components such as a dispersing agent, a defoaming agent, polyvinyl acetate and the like in the adhesive are closely related. The compactness, uniformity and consistency of the repair coating require that the adhesive has excellent leveling property and is leveled into a uniform coating. However, because the coating of the stone grinding disc is cracked and the damaged position is uncertain, when the stone grinding disc is damaged at the edge of the stone grinding disc, the adhesive for the high-temperature photoelectric semiconductor material has good fluidity and can not hang well, so that the edge and the center of the repairing coating are uneven or uneven, the stone grinding disc can not conduct heat uniformly after the repairing coating is carried out, and the photoelectric effect of the semiconductor material is influenced. The applicant finds that the addition of glyceryl triacetate as a functional auxiliary agent to the adhesive under the interaction between an alkaline dispersant, a defoaming agent and the like is helpful for improving the fluidity of the adhesive components, so that the adhesive can effectively flow into a smooth and cloudy coating, and meanwhile, the denaturation of the adhesive components can be effectively improved, so that the adhesive components can also hang well at the edge of a stone mill, and the microstructure uniformity and consistency of a repaired coating obtained by heat treatment can be improved.
The second aspect of the present invention provides a method for preparing the adhesive for high-temperature optoelectronic semiconductor material, which comprises the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a functional assistant, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 2-5 min at 180-220 rpm, then increasing the stirring speed to 1200-1800 rpm, and stirring for 15-30 min;
(4) and (3) adding the thickening agent in the step (1), and stirring for 10-20 min to obtain the water-based paint.
Examples
Example 1: the adhesive for the high-temperature photoelectric semiconductor material is provided, and the preparation raw materials of the adhesive comprise the following components: 36 parts of polyvinyl acetate emulsion, 50 parts of filler, 1.0 part of thickening agent, 2.0 parts of functional assistant, 0.5 part of dispersing agent, 0.4 part of defoaming agent and 10 parts of solvent.
The solvent is deionized water; the polyvinyl acetate emulsion is WX-505 of Star light synthetic Material Co., Ltd, West lake; the filler is a mixture of silicon powder and silicon carbide, and the weight ratio of the silicon carbide to the silicon powder is 1: 4.8, selecting the green silicon carbide micro powder of a Zibo Zichuan new abrasive grinding tool factory, wherein the average grain diameter of the silicon powder is 30 microns, and the grain diameter of the silicon carbide is 40-50 microns; the thickening agent is hydroxyethyl cellulose; the functional auxiliary agent is glyceryl triacetate; the pH value of the dispersing agent is 8.5, and the German height of 760W is selected; the defoaming agent is polyether modified organic siloxane emulsion containing fumed silica, and the German height 1488 is selected.
The preparation method of the adhesive for the high-temperature photoelectric semiconductor material comprises the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a functional assistant, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 4min at 200 r/min, then increasing the stirring speed to 1500 r/min, and stirring for 25 min;
(4) adding the thickening agent in the step (1), and stirring for 15min to obtain the water-based paint.
Example 2: the adhesive for the high-temperature photoelectric semiconductor material is provided, and the preparation raw materials of the adhesive comprise the following components: 36 parts of polyvinyl acetate emulsion, 50 parts of filler, 1.0 part of thickening agent, 2.0 parts of functional assistant, 0.5 part of dispersing agent, 0.4 part of defoaming agent, 10 parts of solvent and 0.1 part of sodium benzoate.
The solvent is propylene glycol; the polyvinyl acetate emulsion is SD-40 in the chemical industry of Hadamard; the filler is a mixture of silicon powder and silicon carbide, and the weight ratio of the silicon carbide to the silicon powder is 1: 4.8, selecting the green silicon carbide micro powder of a Zibo Zichuan new abrasive grinding tool factory, wherein the average grain diameter of the silicon powder is 30 microns, and the grain diameter of the silicon carbide is 40-50 microns; the thickening agent is hydroxyethyl cellulose; the functional auxiliary agent is glyceryl triacetate; the pH value of the dispersing agent is 8.5, and the German height of 760W is selected; the defoaming agent is polyether modified organic siloxane emulsion containing fumed silica, and the German height 1488 is selected.
The preparation method of the adhesive for the high-temperature photoelectric semiconductor material comprises the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a functional assistant, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent, sodium benzoate and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 4min at 200 r/min, then increasing the stirring speed to 1500 r/min, and stirring for 25 min;
(4) adding the thickening agent in the step (1), and stirring for 15min to obtain the water-based paint.
Example 3: the adhesive for the high-temperature photoelectric semiconductor material is provided, and the preparation raw materials of the adhesive comprise the following components: 48 parts of polyvinyl acetate emulsion, 50 parts of filler, 0.4 part of thickening agent, 1.6 parts of functional assistant, 0.3 part of dispersing agent, 0.3 part of defoaming agent, 10 parts of solvent and 0.1 part of sodium benzoate.
The solvent is propylene glycol; the polyvinyl acetate emulsion is SD-40 in the chemical industry of Hadamard; the filler is a mixture of silicon powder and silicon carbide, and the weight ratio of the silicon carbide to the silicon powder is 1: 4.8, selecting the green silicon carbide micro powder of a Zibo Zichuan new abrasive grinding tool factory, wherein the average grain diameter of the silicon powder is 30 microns, and the grain diameter of the silicon carbide is 40-50 microns; the thickening agent is hydroxyethyl cellulose; the functional auxiliary agent is glyceryl triacetate; the pH value of the dispersing agent is 8.5, and the German height of 760W is selected; the defoaming agent is polyether modified organic siloxane emulsion containing fumed silica, and the German height 1488 is selected.
The preparation method of the adhesive for the high-temperature photoelectric semiconductor material comprises the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a functional assistant, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent, sodium benzoate and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 4min at 200 r/min, then increasing the stirring speed to 1500 r/min, and stirring for 25 min;
(4) adding the thickening agent in the step (1), and stirring for 15min to obtain the water-based paint.
Example 4: the adhesive for the high-temperature photoelectric semiconductor material is provided, and the preparation raw materials of the adhesive comprise the following components: 25 parts of polyvinyl acetate emulsion, 50 parts of filler, 1.0 part of thickening agent, 1.8 parts of functional assistant, 0.6 part of dispersing agent, 0.5 part of defoaming agent, 10 parts of solvent and 0.1 part of sodium benzoate.
The solvent is propylene glycol; the polyvinyl acetate emulsion is SD-40 in the chemical industry of Hadamard; the filler is a mixture of silicon powder and silicon carbide, and the weight ratio of the silicon carbide to the silicon powder is 1: 4.8, selecting the green silicon carbide micro powder of a Zibo Zichuan new abrasive grinding tool factory, wherein the average grain diameter of the silicon powder is 30 microns, and the grain diameter of the silicon carbide is 40-50 microns; the thickening agent is hydroxyethyl cellulose; the functional auxiliary agent is glyceryl triacetate; the pH value of the dispersing agent is 8.5, and the German height of 760W is selected; the defoaming agent is polyether modified organic siloxane emulsion containing fumed silica, and the German height 1488 is selected.
The preparation method of the adhesive for the high-temperature photoelectric semiconductor material comprises the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a functional assistant, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent, sodium benzoate and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 4min at 200 r/min, then increasing the stirring speed to 1500 r/min, and stirring for 25 min;
(4) adding the thickening agent in the step (1), and stirring for 15min to obtain the water-based paint.
Example 5: the adhesive for the high-temperature photoelectric semiconductor material is provided, and the preparation raw materials of the adhesive comprise the following components: 36 parts of polyvinyl acetate emulsion, 50 parts of filler, 1.0 part of thickening agent, 2.0 parts of functional assistant, 0.5 part of dispersing agent, 0.4 part of defoaming agent, 10 parts of solvent and 0.1 part of sodium benzoate.
The solvent is propylene glycol; the polyvinyl acetate emulsion is SD-40 in the chemical industry of Hadamard; the filler is silicon powder, and the average particle size of the silicon powder is 30 microns; the thickening agent is hydroxyethyl cellulose; the functional auxiliary agent is glyceryl triacetate; the pH value of the dispersing agent is 8.5, and the German height of 760W is selected; the defoaming agent is polyether modified organic siloxane emulsion containing fumed silica, and the German height 1488 is selected.
The preparation method of the adhesive for the high-temperature photoelectric semiconductor material comprises the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a functional assistant, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent, sodium benzoate and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 4min at 200 r/min, then increasing the stirring speed to 1500 r/min, and stirring for 25 min;
(4) adding the thickening agent in the step (1), and stirring for 15min to obtain the water-based paint.
Example 6: provides a high-temperature photoelectric semiconductorThe adhesive for the material comprises the following raw materials in parts by weight: 36 parts of polyvinyl acetate emulsion, 50 parts of filler, 1.0 part of thickening agent, 2.0 parts of functional assistant, 0.5 part of dispersing agent, 0.4 part of defoaming agent, 10 parts of solvent and 0.1 part of sodium benzoate.
The solvent is propylene glycol; the polyvinyl acetate emulsion is SD-40 in the chemical industry of Hadamard; the filler is silicon carbide, the particle size of the silicon carbide is 40-50 microns, and the green silicon carbide micro powder of a catabol catalpi new abrasive grinding tool factory is selected; the thickening agent is hydroxyethyl cellulose; the functional auxiliary agent is glyceryl triacetate; the pH value of the dispersing agent is 8.5, and the German height of 760W is selected; the defoaming agent is polyether modified organic siloxane emulsion containing fumed silica, and the German height 1488 is selected.
The preparation method of the adhesive for the high-temperature photoelectric semiconductor material comprises the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a functional assistant, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent, sodium benzoate and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 4min at 200 r/min, then increasing the stirring speed to 1500 r/min, and stirring for 25 min;
(4) adding the thickening agent in the step (1), and stirring for 15min to obtain the water-based paint.
Example 7: the adhesive for the high-temperature photoelectric semiconductor material is provided, and the preparation raw materials of the adhesive comprise the following components: 36 parts of polyvinyl acetate emulsion, 50 parts of filler, 1.0 part of thickening agent, 2.0 parts of functional assistant, 0.5 part of dispersing agent, 0.4 part of defoaming agent, 10 parts of solvent and 0.1 part of sodium benzoate.
The solvent is propylene glycol; the polyvinyl acetate emulsion is SD-40 in the chemical industry of Hadamard; the filler is a mixture of silicon powder and silicon carbide, and the weight ratio of the silicon carbide to the silicon powder is 1: 4.8, selecting green silicon carbide micro powder of a Zibo Zichuan new abrasive grinding tool factory, wherein the average grain diameter of the silicon powder is 80 microns, and the grain diameter of the silicon carbide is 40-50 microns; the thickening agent is hydroxyethyl cellulose; the functional auxiliary agent is glyceryl triacetate; the pH value of the dispersing agent is 8.5, and the German height of 760W is selected; the defoaming agent is polyether modified organic siloxane emulsion containing fumed silica, and the German height 1488 is selected.
The preparation method of the adhesive for the high-temperature photoelectric semiconductor material comprises the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a functional assistant, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent, sodium benzoate and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 4min at 200 r/min, then increasing the stirring speed to 1500 r/min, and stirring for 25 min;
(4) adding the thickening agent in the step (1), and stirring for 15min to obtain the water-based paint.
Example 8: the adhesive for the high-temperature photoelectric semiconductor material is provided, and the preparation raw materials of the adhesive comprise the following components: 36 parts of polyvinyl acetate emulsion, 50 parts of filler, 1.0 part of thickening agent, 2.0 parts of functional assistant, 0.5 part of dispersing agent, 0.4 part of defoaming agent, 10 parts of solvent and 0.1 part of sodium benzoate.
The solvent is propylene glycol; the polyvinyl acetate emulsion is SD-40 in the chemical industry of Hadamard; the filler is a mixture of silicon powder and silicon carbide, and the weight ratio of the silicon carbide to the silicon powder is 1: 4.8, selecting the green silicon carbide micro powder of a Zibo Zichuan new abrasive grinding tool factory, wherein the average grain diameter of the silicon powder is 30 microns, and the grain diameter of the silicon carbide is 100-120 microns; the thickening agent is hydroxyethyl cellulose; the functional auxiliary agent is glyceryl triacetate; the pH value of the dispersing agent is 8.5, and the German height of 760W is selected; the defoaming agent is polyether modified organic siloxane emulsion containing fumed silica, and the German height 1488 is selected.
The preparation method of the adhesive for the high-temperature photoelectric semiconductor material comprises the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a functional assistant, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent, sodium benzoate and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 4min at 200 r/min, then increasing the stirring speed to 1500 r/min, and stirring for 25 min;
(4) adding the thickening agent in the step (1), and stirring for 15min to obtain the water-based paint.
Example 9: the adhesive for the high-temperature photoelectric semiconductor material is provided, and the preparation raw materials of the adhesive comprise the following components: 36 parts of polyvinyl acetate emulsion, 50 parts of filler, 1.0 part of thickening agent, 2.0 parts of functional assistant, 0.5 part of dispersing agent, 0.4 part of defoaming agent, 10 parts of solvent and 0.1 part of sodium benzoate.
The solvent is propylene glycol; the polyvinyl acetate emulsion is SD-40 in the chemical industry of Hadamard; the filler is a mixture of silicon powder and silicon carbide, and the weight ratio of the silicon carbide to the silicon powder is 1: 0.8, selecting the green silicon carbide micro powder of a Zibo Zichuan new abrasive grinding tool factory, wherein the average grain diameter of the silicon powder is 30 microns, and the grain diameter of the silicon carbide is 40-50 microns; the thickening agent is hydroxyethyl cellulose; the functional auxiliary agent is glyceryl triacetate; the pH value of the dispersing agent is 8.5, and the German height of 760W is selected; the defoaming agent is polyether modified organic siloxane emulsion containing fumed silica, and the German height 1488 is selected.
The preparation method of the adhesive for the high-temperature photoelectric semiconductor material comprises the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a functional assistant, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent, sodium benzoate and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 4min at 200 r/min, then increasing the stirring speed to 1500 r/min, and stirring for 25 min;
(4) adding the thickening agent in the step (1), and stirring for 15min to obtain the water-based paint.
Example 10: provides an adhesive for high-temperature photoelectric semiconductor material, and the adhesiveThe preparation raw materials comprise the following components: 36 parts of polyvinyl acetate emulsion, 50 parts of filler, 1.0 part of thickening agent, 0.5 part of dispersing agent, 0.4 part of defoaming agent, 10 parts of solvent and 0.1 part of sodium benzoate.
The solvent is propylene glycol; the polyvinyl acetate emulsion is SD-40 in the chemical industry of Hadamard; the filler is a mixture of silicon powder and silicon carbide, and the weight ratio of the silicon carbide to the silicon powder is 1: 4.8, selecting the green silicon carbide micro powder of a Zibo Zichuan new abrasive grinding tool factory, wherein the average grain diameter of the silicon powder is 30 microns, and the grain diameter of the silicon carbide is 40-50 microns; the thickening agent is hydroxyethyl cellulose; the pH value of the dispersing agent is 8.5, and the German height of 760W is selected; the defoaming agent is polyether modified organic siloxane emulsion containing fumed silica, and the German height 1488 is selected.
The preparation method of the adhesive for the high-temperature photoelectric semiconductor material comprises the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent, sodium benzoate and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 4min at 200 r/min, then increasing the stirring speed to 1500 r/min, and stirring for 25 min;
(4) adding the thickening agent in the step (1), and stirring for 15min to obtain the water-based paint.
Example 11: the adhesive for the high-temperature photoelectric semiconductor material is provided, and the preparation raw materials of the adhesive comprise the following components: 36 parts of polyvinyl acetate emulsion, 50 parts of filler, 1.0 part of thickening agent, 2.0 parts of functional assistant, 0.5 part of dispersing agent, 0.4 part of defoaming agent, 10 parts of solvent and 0.1 part of sodium benzoate.
The solvent is propylene glycol; the polyvinyl acetate emulsion is SD-40 in the chemical industry of Hadamard; the filler is a mixture of silicon powder and silicon carbide, and the weight ratio of the silicon carbide to the silicon powder is 1: 8, selecting the silicon green carbide micro powder of a Zibo zichuan new abrasive grinding tool factory, wherein the average grain diameter of the silicon powder is 30 microns, and the grain diameter of the silicon carbide is 40-50 microns; the thickening agent is hydroxyethyl cellulose; the functional auxiliary agent is glyceryl triacetate; the pH value of the dispersing agent is 8.5, and the German height of 760W is selected; the defoaming agent is polyether modified organic siloxane emulsion containing fumed silica, and the German height 1488 is selected.
The preparation method of the adhesive for the high-temperature photoelectric semiconductor material comprises the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a functional assistant, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent, sodium benzoate and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 4min at 200 r/min, then increasing the stirring speed to 1500 r/min, and stirring for 25 min;
(4) adding the thickening agent in the step (1), and stirring for 15min to obtain the water-based paint.
Example 12: the adhesive for the high-temperature photoelectric semiconductor material is provided, and the preparation raw materials of the adhesive comprise the following components: 36 parts of polyvinyl acetate emulsion, 50 parts of filler, 1.0 part of thickening agent, 2.0 parts of functional assistant, 0.5 part of dispersing agent, 0.4 part of defoaming agent, 10 parts of solvent and 0.1 part of sodium benzoate.
The solvent is propylene glycol; the polyvinyl acetate emulsion is SD-40 in the chemical industry of Hadamard; the filler is a mixture of silicon powder and silicon carbide, and the weight ratio of the silicon carbide to the silicon powder is 1: 4.8, selecting the green silicon carbide micro powder of a Zibo Zichuan new abrasive grinding tool factory, wherein the average grain diameter of the silicon powder is 30 microns, and the grain diameter of the silicon carbide is 40-50 microns; the thickening agent is hydroxyethyl cellulose; the functional auxiliary agent is glyceryl triacetate; the dispersant is BYK-170; the defoaming agent is polyether modified organic siloxane emulsion containing fumed silica, and the German height 1488 is selected.
The preparation method of the adhesive for the high-temperature photoelectric semiconductor material comprises the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a functional assistant, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent, sodium benzoate and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 4min at 200 r/min, then increasing the stirring speed to 1500 r/min, and stirring for 25 min;
(4) adding the thickening agent in the step (1), and stirring for 15min to obtain the water-based paint.
Example 13: the adhesive for the high-temperature photoelectric semiconductor material is provided, and the preparation raw materials of the adhesive comprise the following components: 36 parts of polyvinyl acetate emulsion, 50 parts of filler, 1.0 part of thickening agent, 2.0 parts of functional assistant, 0.5 part of dispersing agent, 0.4 part of defoaming agent, 10 parts of solvent and 0.1 part of sodium benzoate.
The solvent is propylene glycol; the polyvinyl acetate emulsion is SD-40 in the chemical industry of Hadamard; the filler is a mixture of silicon powder and silicon carbide, and the weight ratio of the silicon carbide to the silicon powder is 1: 4.8, selecting the green silicon carbide micro powder of a Zibo Zichuan new abrasive grinding tool factory, wherein the average grain diameter of the silicon powder is 30 microns, and the grain diameter of the silicon carbide is 40-50 microns; the thickening agent is hydroxyethyl cellulose; the functional auxiliary agent is glyceryl triacetate; the pH value of the dispersing agent is 8.5, and the German height of 760W is selected; the defoaming agent is a mineral oil defoaming agent, and Solvay Rhodoline DF 642NI is selected.
The preparation method of the adhesive for the high-temperature photoelectric semiconductor material comprises the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a functional assistant, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent, sodium benzoate and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 4min at 200 r/min, then increasing the stirring speed to 1500 r/min, and stirring for 25 min;
(4) adding the thickening agent in the step (1), and stirring for 15min to obtain the water-based paint.
Uniformly coating the high-temperature photoelectric semiconductor material on the damaged part on the surface of a millstone by using an adhesive, wherein the thickness is about 12 microns, then placing the millstone in a graphitization furnace, vacuumizing, removing oxidizing gases such as oxygen in the furnace to achieve the vacuum degree of 800Pa, performing heat treatment at 1400 ℃ for 60 minutes, then using the repaired millstone in the production of the semiconductor material, observing that graphite in a reaction cavity is subjected to powder falling after the millstone is used for 120 times/piece, and evaluating 1-4 grades according to the powder falling degree, wherein the grade 1 has no powder falling and no dust; the 4-grade powder falling condition is serious, and obvious dust exists; the powder dropping conditions of the grade 2 and the grade 3 are obviously increased in turn.
Further, the service life of the repaired millstone in the production of semiconductor (LED) materials (after 80 heats/piece, three consecutive failures occurred in the product, and the service life was determined to have been reached) and the average yield of semiconductor products when 120 heats/piece were used in the repaired millstone were observed, and the results are shown in the following table.
Table 1 results of performance testing
From the results, the adhesive for the high-temperature photoelectric semiconductor material has higher bonding strength to the millstone, does not crack or break again after being used for many times after the damaged part of the coating is brushed and repaired, has obviously prolonged service life, can be improved to 180 heats/piece from the traditional 100 heats/piece, and does not reduce the yield in the production of semiconductor products after being repaired.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art may modify or change the technical content disclosed above into an equivalent embodiment with equivalent changes, but all those simple modifications, equivalent changes and modifications made on the above embodiment according to the technical spirit of the present invention still belong to the protection scope of the present invention.
Claims (8)
1. The adhesive for the high-temperature photoelectric semiconductor material is characterized by comprising the following raw materials in parts by weight: 25-50 parts of polyvinyl acetate emulsion, 40-60 parts of filler, 0-1.0 part of thickener, 1-3.5 parts of functional assistant, 0.1-0.8 part of dispersant, 0.1-0.8 part of defoamer and 3-12 parts of solvent;
the filler is silicon powder and silicon carbide; the weight ratio of the silicon carbide to the silicon powder is 1: (3-5).
2. The adhesive for high-temperature photoelectric semiconductor material according to claim 1, wherein the particle size of the silicon powder is not higher than 50 μm.
3. The adhesive for high-temperature optoelectronic semiconductor material as claimed in claim 1, wherein the grain size of the silicon carbide is not more than 50 μm.
4. The adhesive for high-temperature photoelectric semiconductor material according to claim 1, wherein the functional additive is triacetin.
5. The adhesive for high-temperature photoelectric semiconductor materials as claimed in claim 1, wherein the defoaming agent is polyether modified organosiloxane emulsion.
6. The adhesive for high-temperature photoelectric semiconductor materials according to claim 5, wherein the polyether modified organosiloxane emulsion contains fumed silica.
7. The adhesive for high-temperature optoelectronic semiconductor material according to any one of claims 1 to 6, wherein the pH value of the dispersant is not less than 7.0.
8. The preparation method of the adhesive for the high-temperature photoelectric semiconductor material according to any one of claims 1 to 7, characterized by comprising the following steps:
(1) adding the thickener with the formula amount into 1/5 weight of solvent, stirring and swelling;
(2) sequentially adding a filler, a functional assistant, a polyvinyl acetate emulsion, a dispersing agent, a defoaming agent and a residual solvent into a stirring tank;
(3) stirring the stirring tank for 2-5 min at 180-220 rpm, then increasing the stirring speed to 1200-1800 rpm, and stirring for 15-30 min;
(4) and (3) adding the thickening agent in the step (1), and stirring for 10-20 min to obtain the water-based paint.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106867431A (en) * | 2017-02-25 | 2017-06-20 | 苏州大乘环保建材有限公司 | Aqueous, environmental protective plastic cement race track adhesive and preparation method thereof |
| CN111349412A (en) * | 2020-05-09 | 2020-06-30 | 山东美登新材料技术有限公司 | Environment-friendly adhesive and preparation method and application thereof |
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| CN100575439C (en) * | 2006-04-17 | 2009-12-30 | 张恩天 | Environment friendly heat resistant adhesive for energy saving lamp holder |
| CN108251026A (en) * | 2017-12-29 | 2018-07-06 | 重庆蓝兔塑胶制品有限公司 | A kind of adhesive |
| JP6790032B2 (en) * | 2018-09-06 | 2020-11-25 | 日東電工株式会社 | Adhesive sheet |
| CN110423576A (en) * | 2019-07-10 | 2019-11-08 | 东莞市冠力胶业有限公司 | A kind of high viscosity water resistance glue and its preparation process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106867431A (en) * | 2017-02-25 | 2017-06-20 | 苏州大乘环保建材有限公司 | Aqueous, environmental protective plastic cement race track adhesive and preparation method thereof |
| CN111349412A (en) * | 2020-05-09 | 2020-06-30 | 山东美登新材料技术有限公司 | Environment-friendly adhesive and preparation method and application thereof |
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