CN117226710A - Wax-free pad for single-sided polishing planarization of wafer and preparation process thereof - Google Patents
Wax-free pad for single-sided polishing planarization of wafer and preparation process thereof Download PDFInfo
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- CN117226710A CN117226710A CN202311232207.7A CN202311232207A CN117226710A CN 117226710 A CN117226710 A CN 117226710A CN 202311232207 A CN202311232207 A CN 202311232207A CN 117226710 A CN117226710 A CN 117226710A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
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- 239000003822 epoxy resin Substances 0.000 claims abstract description 37
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 37
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 27
- 239000004917 carbon fiber Substances 0.000 claims abstract description 27
- 239000000945 filler Substances 0.000 claims abstract description 26
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 30
- 229910052582 BN Inorganic materials 0.000 claims description 27
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical class N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 25
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
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- 229910052581 Si3N4 Inorganic materials 0.000 claims description 8
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- 239000000843 powder Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 125000003545 alkoxy group Chemical group 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 6
- 238000007334 copolymerization reaction Methods 0.000 claims description 6
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- 239000012153 distilled water Substances 0.000 claims description 6
- 239000005543 nano-size silicon particle Substances 0.000 claims description 6
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- 238000010992 reflux Methods 0.000 claims description 6
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- 238000001291 vacuum drying Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
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- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 3
- XVEASTGLHPVZNA-UHFFFAOYSA-N 3,4-dichlorobut-1-ene Chemical compound ClCC(Cl)C=C XVEASTGLHPVZNA-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 3
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- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims description 3
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Landscapes
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention discloses a wax-free pad for single-sided polishing planarization of a wafer and a preparation process thereof, and belongs to the technical field of wax-free pads. The wax-free pad for single-sided polishing planarization of the wafer comprises a base chassis and an adsorption layer, wherein the adsorption layer is clamped on the base chassis, and the base chassis is made of the following materials in parts by weight: 30-40 parts of modified epoxy resin, 10-30 parts of carbon fiber, 10-20 parts of filler and 20-30 parts of curing agent, wherein the adsorption layer is made of polyurethane foaming material. The invention solves the problem of easy abrasion during the existing high-resistance polishing, and the wax-free pad for single-sided polishing planarization of the wafer and the preparation process thereof provided by the invention use the liquid chloroprene-hydroxyethyl methacrylate copolymer to modify the epoxy resin, so that the toughness of the epoxy resin is improved, and simultaneously, lignin sulfonate is added in the modified epoxy resin, so that the wax-free pad has stronger adsorptivity and reduces the adsorption or adhesion of the wax-free pad to polishing liquid.
Description
Technical Field
The invention relates to the technical field of wax-free pads, in particular to a wax-free pad for single-sided polishing planarization of a wafer and a preparation process thereof.
Background
The existing wax-free polishing process adopts an integrated template, a special template is ordered according to the specification of a silicon wafer to be processed, the silicon wafer is directly placed into a wafer placing hole of the template for polishing, the silicon wafers with different specifications can be polished after being matched with the sizes of the wafer placing holes with the same specifications, once the thickness of the silicon wafer is different from the depth of the wafer placing hole, the silicon wafer is very likely to slide out from the wafer placing hole in the processing process to cause broken wafers or even rollover.
Chinese patent publication No. CN112873074B discloses a method for producing a wax-free pad for polishing, the wax-free pad comprises a base chassis, a wafer placing hole, a clamping pad and a wax-free adsorption pad, at least one wafer placing hole is provided on the surface of the base chassis, the wax-free adsorption pad for adsorbing wafers is provided in the wafer placing hole, and at least one layer of clamping pad is provided between the wax-free adsorption pad and the inner bottom of the wafer placing hole.
The invention solves the problem that the wax-free polishing process adopts an integrated template in the background technology, but in the patent, epoxy resin and polyurethane prepolymer are utilized to react to produce composite resin, and the composite resin is used as an adhesive layer, so that the adhesive layer has high viscosity, is easy to wear during high-resistance polishing, causes poor flatness and influences the planarization of wafer polishing.
Disclosure of Invention
The invention aims to provide a wax-free pad for single-sided polishing planarization of a wafer and a preparation process thereof, wherein the toughness of epoxy resin is improved, and lignin sulfonate is added into modified epoxy resin, so that the wax-free pad has strong anti-adsorption property and strong thermal stability, and further, the stability of the wax-free pad is improved during polishing, the adsorption or adhesion of the wax-free pad to polishing liquid is reduced, and the problems in the background art are solved.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the wax-free pad for single-sided polishing planarization of the wafer comprises a base chassis and an adsorption layer, wherein the adsorption layer is clamped on the base chassis, and the base chassis is made of the following materials in parts by weight: 30-40 parts of modified epoxy resin, 10-30 parts of carbon fiber, 10-20 parts of filler and 20-30 parts of curing agent, wherein the adsorption layer is made of polyurethane foaming material.
Preferably, the base chassis is provided with a wafer groove, a clamping groove is formed in the position, close to the bottom, of the wafer groove, and clamping holes are uniformly distributed in the bottom of the wafer groove.
Preferably, the outer wall of the lower end of the adsorption layer is connected with a clamping edge, the clamping edge is of a conical structure with a large upper end opening, the clamping edge is clamped with the wafer groove, and the lower surface of the adsorption layer is provided with a clamping column matched with the clamping hole.
Preferably, the preparation method of the modified epoxy resin comprises the following steps:
dehydrochlorination of 3, 4-dichloro butene-1 under the action of alkali, rectification until the purity is more than 98%, then copolymerization reaction with hydroxyethyl methacrylate, placing a monomer, a molecular weight regulator, a solvent and an initiator into a three-mouth bottle or a stainless steel pressure-resistant reaction bottle, copolymerization reaction under nitrogen flow, and vacuum distillation after termination of the reaction to obtain a liquid chloroprene-hydroxyethyl methacrylate copolymer;
adding the obtained liquid chloroprene-hydroxyethyl methacrylate copolymer, epoxy resin and lignin sulfonate into a mixing mill for mixing for 20min to obtain the modified epoxy resin.
Preferably, the filler is made of the following materials in parts by weight: 10-16 parts of modified silicon nitride and 12-24 parts of aluminum oxide coated hexagonal boron nitride.
Preferably, the preparation method of the modified silicon nitride comprises the following steps:
uniformly mixing new alkoxy tri (p-aminophenoxy) zirconate and a solvent at 55-65 ℃, wherein the addition of the new alkoxy tri (p-aminophenoxy) zirconate is 40-70wt% of nano silicon nitride, then adding nano silicon nitride, magnetically stirring and refluxing for 20-30 hours at 65-85 ℃, centrifugally separating an obtained reflux system, centrifugally washing with absolute ethyl alcohol, and finally drying and grinding the obtained substance to obtain the modified silicon nitride.
Preferably, the preparation method of the aluminum oxide coated hexagonal boron nitride comprises the following steps:
mixing hexagonal boron nitride powder with the particle size of 10-30nm and a dispersing agent with distilled water to prepare hexagonal boron nitride suspension with the particle size of 3-8g/L, wherein the adding amount of the dispersing agent is 3-5% of the mass of hexagonal boron nitride;
adding an acetic acid-sodium acetate buffer solution with the pH value of 4.5, performing ultrasonic dispersion, stirring and heating to 30-40 ℃, slowly dripping an aluminum nitrate solution with the Al3+ concentration of 0.1-0.2mol/L, slowly dripping ammonia water to adjust the pH value to 7.0-7.5, and keeping the temperature of 30-40 ℃ for reacting for 1.5-2.5h after dripping;
and then standing for aging, precipitating, filtering, cleaning, centrifuging and vacuum drying to obtain hexagonal boron nitride composite powder with aluminum hydroxide coated on the surface, and vacuum calcining to obtain aluminum oxide coated hexagonal boron nitride composite powder with the particle size of 20-50 nm.
The invention provides a preparation process of a wax-free pad for single-sided polishing and planarization of a wafer, which comprises the following steps:
s1: adding modified epoxy resin into a reaction kettle, adding filler and curing agent, stirring at 70-110 ℃ for 3-6 hours, then paving the pretreated carbon fiber material into a mold, and carrying out injection molding, curing and forming on the stirred and mixed material to obtain a base chassis;
s2: injection molding the polyurethane foaming material, demolding, preparing an adsorption layer, and roughening the clamping column;
s3: and assembling the adsorption layer with the base chassis to prepare the wax-free pad.
Preferably, the pretreatment method of the carbon fiber comprises the following steps:
soaking carbon fiber in acetone solution for 30-40min, taking out, oven drying, soaking in 70% concentrated nitric acid for 50-60min, taking out, soaking and washing with distilled water for 3-5 times, and vacuum drying at 100deg.C for 12 hr; the carbon fibers are blown into a state of being uniformly distributed in the three-dimensional direction by utilizing air flow, so that the carbon fibers are mutually overlapped to form a net shape.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the liquid chloroprene-hydroxyethyl methacrylate copolymer is used for modifying the epoxy resin, so that the toughness of the epoxy resin is improved, and simultaneously, the lignin sulfonate is added in the modified epoxy resin, so that the modified epoxy resin has stronger adsorptivity and stronger thermal stability, and further, the stability of the wax-free pad is improved during polishing, and the adsorption or adhesion of the wax-free pad to polishing liquid is reduced;
2. according to the invention, the modified silicon nitride and the aluminum oxide are used for coating the hexagonal boron nitride in the filler, so that the whole strength of the base chassis is improved, the base chassis is not easy to deform, the wear resistance is improved, the integrity of the base chassis can be ensured during polishing, the aluminum oxide coated hexagonal boron nitride effectively improves the lubricating property and the thermal shock resistance of a ceramic material, the antifriction and wear resistance effects are realized, and further the planarization of a polished wafer is ensured during polishing;
3. according to the invention, double-layer clamping is carried out through the base chassis and the adsorption layer through the clamping edges and the clamping columns, the elasticity of the adsorption layer is utilized for installation, under the condition that the friction coefficient of the base chassis is low, the clamping columns are utilized for improving the connection firmness, and meanwhile, the clamping columns ensure the whole flatness of the adsorption layer and improve the adsorption firmness;
4. the invention is also provided with the netlike carbon fiber material, improves the integrity of the base chassis, improves the tensile property of the base chassis and avoids the tearing and breaking of the base chassis.
Drawings
FIG. 1 is an overall cross-sectional view of a wax-free mat of the present invention.
In the figure: 1. a base chassis; 11. a wafer groove; 111. a clamping groove; 112. a clamping hole; 2. an adsorption layer; 21. a clamping edge; 22. and (5) clamping the column.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. 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.
Embodiment one:
in order to solve the problem that the flatness is poor and the planarization of wafer polishing is affected due to the abrasion during the polishing with high viscosity and high resistance of the existing composite resin as an adhesive layer, referring to fig. 1, the present embodiment provides the following technical scheme:
the utility model provides a no wax pad for wafer single face polishing planarization, including base chassis 1 and adsorbed layer 2, the block has adsorbed layer 2 on the base chassis 1, the wafer recess 11 has been seted up on the base chassis 1, the position that wafer recess 11 is close to the bottom has been seted up the block groove 111, the block hole 112 of evenly distributed has been seted up to the tank bottom of wafer recess 11, be connected with block limit 21 on the outer wall of adsorbed layer 2 lower extreme, block limit 21 is the toper structure that the upper end opening is big, block limit 21 and wafer recess 11 block, adsorbed layer 2's lower surface is provided with block hole 112 assorted block post 22.
Specifically, the adsorption layer 2 is clamped with the wafer groove 11, the clamping edge 21 deforms under the pushing force, the adsorption layer 2 is pushed to the bottom of the wafer groove 11, the clamping edge 21 is clamped with the wafer groove 11, the clamping column 22 is clamped with the clamping hole 112 in an interference manner, and the adsorption layer 2 and the base chassis 1 are doubly fixed.
The base chassis 1 is made of the following materials in parts by weight: 30 parts of modified epoxy resin, 30 parts of carbon fiber, 10 parts of filler and 20 parts of curing agent, and the adsorption layer 2 is made of polyurethane foam materials.
The preparation method of the modified epoxy resin comprises the following steps:
dehydrochlorination of 3, 4-dichloro butene-1 under the action of alkali, rectification until the purity is more than 98%, then copolymerization reaction with hydroxyethyl methacrylate, placing a monomer, a molecular weight regulator, a solvent and an initiator into a three-mouth bottle or a stainless steel pressure-resistant reaction bottle, copolymerization reaction under nitrogen flow, and vacuum distillation after termination of the reaction to obtain a liquid chloroprene-hydroxyethyl methacrylate copolymer;
adding the obtained liquid chloroprene-hydroxyethyl methacrylate copolymer, epoxy resin and lignin sulfonate into a mixing mill for mixing for 20min to obtain the modified epoxy resin.
The filler is prepared from the following materials in parts by weight: 10 parts of modified silicon nitride and 23 parts of aluminum oxide coated hexagonal boron nitride.
The preparation method of the modified silicon nitride comprises the following steps:
uniformly mixing new alkoxy tri (p-aminophenoxy) zirconate and a solvent at 61 ℃, wherein the addition amount of the new alkoxy tri (p-aminophenoxy) zirconate is 48wt% of nano silicon nitride, then adding the nano silicon nitride, magnetically stirring and refluxing for 25 hours at 78 ℃, centrifugally separating an obtained reflux system, centrifugally washing with absolute ethyl alcohol, and finally drying and grinding the obtained substance to obtain the modified silicon nitride.
The preparation method of the aluminum oxide coated hexagonal boron nitride comprises the following steps:
mixing hexagonal boron nitride powder with the particle size of 10-30nm and a dispersing agent into distilled water to prepare hexagonal boron nitride suspension with the particle size of 6g/L, wherein the adding amount of the dispersing agent is 4% of the mass of hexagonal boron nitride;
adding an acetic acid-sodium acetate buffer solution with the pH value of 4.5, performing ultrasonic dispersion, stirring and heating to 32 ℃, slowly dropwise adding an aluminum nitrate solution with the Al3+ concentration of 0.1mol/L, slowly dropwise adding ammonia water to adjust the pH value to 7.0, and keeping the temperature of 35 ℃ for 2h after dropwise adding;
and then standing for aging, precipitating, filtering, cleaning, centrifuging and vacuum drying to obtain hexagonal boron nitride composite powder with aluminum hydroxide coated on the surface, and vacuum calcining to obtain aluminum oxide coated hexagonal boron nitride composite powder with the particle size of 20-50 nm.
In order to better demonstrate the preparation flow of the wax-free pad for single-sided polishing and planarization of a wafer, the embodiment now provides a preparation process of the wax-free pad for single-sided polishing and planarization of a wafer, which comprises the following steps:
step one: adding the modified epoxy resin into a reaction kettle, adding a filler and a curing agent, stirring for 4 hours at 100 ℃, and pretreating carbon fibers:
soaking carbon fiber in acetone solution for 35min, taking out, oven drying, soaking in 70% concentrated nitric acid for 60min, taking out, soaking in distilled water for 4 times, and vacuum drying at 100deg.C for 12 hr;
blowing the carbon fibers into a state of being uniformly distributed in a three-dimensional direction by utilizing air flow, so that the carbon fibers are mutually overlapped to form a net shape;
then paving the pretreated carbon fiber material into a mould, and carrying out injection molding, solidification and molding on the stirred and mixed material to obtain a base chassis 1;
step two: injection molding the polyurethane foaming material, demolding to prepare an adsorption layer 2, and roughening the clamping column 22;
step three: the adsorption layer 2 and the base chassis 1 are assembled to form the wax-free pad.
Embodiment two:
the wax-free pad for single-sided polishing and planarization of a wafer comprises a base chassis 1 and an adsorption layer 2, wherein the adsorption layer 2 is clamped on the base chassis 1, and the base chassis 1 and the adsorption layer 2 have the same structure as in the first embodiment.
The base chassis 1 is made of the following materials in parts by weight: 30 parts of modified epoxy resin, 30 parts of carbon fiber, 15 parts of filler and 20 parts of curing agent, and the adsorption layer 2 is made of polyurethane foam materials.
The filler is prepared from the following materials in parts by weight: 12 parts of modified silicon nitride and 20 parts of aluminum oxide coated hexagonal boron nitride.
Embodiment III:
the wax-free pad for single-sided polishing and planarization of a wafer comprises a base chassis 1 and an adsorption layer 2, wherein the adsorption layer 2 is clamped on the base chassis 1, and the base chassis 1 and the adsorption layer 2 have the same structure as in the first embodiment.
The base chassis 1 is made of the following materials in parts by weight: 30 parts of modified epoxy resin, 30 parts of carbon fiber, 10 parts of filler and 20 parts of curing agent, and the adsorption layer 2 is made of polyurethane foam materials.
The filler is prepared from the following materials in parts by weight: 16 parts of modified silicon nitride and 15 parts of aluminum oxide coated hexagonal boron nitride.
Embodiment four:
the wax-free pad for single-sided polishing and planarization of a wafer comprises a base chassis 1 and an adsorption layer 2, wherein the adsorption layer 2 is clamped on the base chassis 1, and the base chassis 1 and the adsorption layer 2 have the same structure as in the first embodiment.
The base chassis 1 is made of the following materials in parts by weight: 35 parts of modified epoxy resin, 30 parts of carbon fiber, 15 parts of filler and 20 parts of curing agent, and the adsorption layer 2 is made of polyurethane foam materials.
The filler is prepared from the following materials in parts by weight: 16 parts of modified silicon nitride and 15 parts of aluminum oxide coated hexagonal boron nitride.
Comparative example one:
a wax-free pad for single-sided polishing and planarization of a wafer comprises a base chassis 1 and an adsorption layer 2, wherein the adsorption layer 2 is clamped on the base chassis 1, and the structures of the base chassis 1 and the adsorption layer 2 are the same as those of the first embodiment.
The base chassis 1 is made of the following materials in parts by weight: 30 parts of epoxy resin, 30 parts of carbon fiber, 10 parts of filler and 20 parts of curing agent, and the adsorption layer 2 is made of polyurethane foam materials.
The filler is prepared from the following materials in parts by weight: 10 parts of modified silicon nitride and 23 parts of aluminum oxide coated hexagonal boron nitride.
Comparative example two:
a wax-free pad for single-sided polishing and planarization of a wafer comprises a base chassis 1 and an adsorption layer 2, wherein the adsorption layer 2 is clamped on the base chassis 1, and the structures of the base chassis 1 and the adsorption layer 2 are the same as those of the first embodiment.
The base chassis 1 is made of the following materials in parts by weight: 30 parts of modified epoxy resin, 30 parts of carbon fiber, 10 parts of filler and 20 parts of curing agent, and the adsorption layer 2 is made of polyurethane foam materials.
The filler is prepared from the following materials in parts by weight: 10 parts of silicon nitride and 23 parts of aluminum oxide.
Comparative example three:
a wax-free pad for single-sided polishing and planarization of a wafer comprises a base chassis 1 and an adsorption layer 2, wherein the adsorption layer 2 is clamped on the base chassis 1, a wafer groove 11 is formed in the base chassis 1, the adsorption layer 2 is directly clamped with the wafer groove 11, and in the comparative example, a clamping edge 21 and a clamping column 22 at the lower end of the adsorption layer 2 are removed.
The base chassis 1 is made of the following materials in parts by weight: 30 parts of modified epoxy resin, 30 parts of carbon fiber, 10 parts of filler and 20 parts of curing agent, and the adsorption layer 2 is made of polyurethane foam materials.
The filler is prepared from the following materials in parts by weight: 10 parts of modified silicon nitride and 23 parts of aluminum oxide coated hexagonal boron nitride.
In order to better demonstrate the preparation flow of the wax-free pad for single-sided polishing and planarization of a wafer, the embodiment now provides a preparation process of the wax-free pad for single-sided polishing and planarization of a wafer, which comprises the following steps:
step one: adding modified epoxy resin into a reaction kettle, adding filler and curing agent, stirring at 100 ℃ for 4 hours, then paving the pretreated carbon fiber material into a mold, and performing injection molding, curing and forming on the stirred and mixed material to obtain a base chassis 1;
step two: injection molding the polyurethane foaming material, demolding to prepare an adsorption layer 2, and roughening the bottom of the adsorption layer 2;
step three: the adsorption layer 2 and the base chassis 1 are assembled to form the wax-free pad.
The base chassis 1 obtained in the examples and comparative examples was subjected to abrasion resistance, tensile resistance, and maximum working temperature, wherein the abrasion resistance was tested in accordance with the specification of QB/T2726-2005, and the test condition was 1000g under load with a CS-10 grinding wheel, 1000 revolutions was tested, and the grade was evaluated: stage 1: it is obvious that; 2 stages: the method is obvious; 3 stages: can be distinguished; 4 stages: difficult to distinguish; 5 stages: can not be distinguished; the tensile property adopts a GB/T10120-2013 metal material tensile stress relaxation test method, a pressure detection device is applied, under normal temperature conditions, the experimental conditions adopt 1MPa, the occurrence condition of cracks is checked, and the grade is rated: stage 1: it is obvious that; 2 stages: the method is obvious; 3 stages: can be distinguished; 4 stages: difficult to distinguish; 5 stages: the friction coefficient was indistinguishable from a 45 steel pair, and the test results are shown below.
| Example 1 | Example two | Example III | Example IV | Comparative example one | Comparative example two | |
| Wear resistance | 5 | 5 | 5 | 5 | 3 | 4 |
| Tensile properties | 5 | 5 | 5 | 5 | 4 | 4 |
| Coefficient of friction | 0.34 | 0.32 | 0.33 | 0.34 | 0.55 | 0.52 |
As can be seen from the above table, the base chassis 1 prepared in examples one to four had little difference in abrasion resistance, tensile properties, and frictional force of the surface, while in comparative example one, a common epoxy resin was used, and in comparative example two, silicon nitride and aluminum oxide were used as fillers, so that the base chassis 1 prepared in examples one and two had higher abrasion resistance, tensile properties than examples, and the base chassis 1 prepared in comparative example one and comparative example two had a higher frictional coefficient of the surface than examples, indicating that the surface of the base chassis 1 prepared in comparative example one and comparative example two was more prone to residue of polishing liquid or polishing powder, while the surface of the base chassis 1 prepared in example one was smoother, and the processed wafer was flattened more.
The peel force test is performed on the adsorption layer 2 without the wax pad obtained in the first embodiment and the third embodiment and the base chassis 1, the data of the first embodiment is 35N, the data of the third embodiment is 6N, it can be seen that the adsorption layer 2 without the wax pad obtained in the first embodiment is more tightly installed than the adsorption layer 2 without the wax pad obtained in the third embodiment, which indicates that the clamping edge 21 and the clamping column 22 improve the integral connection firmness of the adsorption layer 2.
To sum up: according to the wax-free pad for single-sided polishing planarization of the wafer and the preparation process thereof, the liquid chloroprene-hydroxyethyl methacrylate copolymer is used for modifying the epoxy resin, so that the toughness of the epoxy resin is improved, and simultaneously, lignin sulfonate is added in the modified epoxy resin, so that the wax-free pad has stronger adsorptivity and stronger thermal stability, and further, the stability of the wax-free pad is improved during polishing, and the adsorption or adhesion of the wax-free pad to polishing liquid is reduced; the modified silicon nitride and the aluminum oxide are used for coating the hexagonal boron nitride in the filler, the whole strength of the base chassis 1 is improved by the modified silicon nitride, so that the base chassis is not easy to deform, the wear resistance is improved, the integrity of the base chassis can be ensured during polishing, the aluminum oxide coated hexagonal boron nitride effectively improves the lubricating property and the thermal shock resistance of a ceramic material, the antifriction and wear resistance effects are realized, and further the polished wafer planarization is ensured during polishing; the base chassis 1 and the adsorption layer 2 are clamped in a double-layer manner through the clamping edges 21 and the clamping columns 22, the elasticity of the adsorption layer 2 is utilized for installation, the clamping columns 22 are utilized for improving the connection firmness under the condition that the friction coefficient of the base chassis 1 is low, and meanwhile, the clamping columns 22 ensure the flatness of the whole adsorption layer 2, so that the adsorption firmness is improved.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A wax-free pad for single-sided polishing planarization of a wafer, comprising a base chassis (1) and an adsorption layer (2), characterized in that: the base chassis (1) is clamped with an adsorption layer (2), and the base chassis (1) is made of the following materials in parts by weight: 30-40 parts of modified epoxy resin, 10-30 parts of carbon fiber, 10-20 parts of filler and 20-30 parts of curing agent, wherein the adsorption layer (2) is made of polyurethane foaming material.
2. A wax-free pad for single-sided polishing planarization of a wafer as recited in claim 1, wherein: the base chassis (1) is provided with a wafer groove (11), a clamping groove (111) is formed in the position, close to the bottom, of the wafer groove (11), and clamping holes (112) are uniformly distributed in the bottom of the wafer groove (11).
3. A wax-free pad for single-sided polishing planarization of a wafer as recited in claim 2, wherein: the outer wall of the lower end of the adsorption layer (2) is connected with a clamping edge (21), the clamping edge (21) is of a conical structure with a large upper end opening, the clamping edge (21) is clamped with the wafer groove (11), and the lower surface of the adsorption layer (2) is provided with a clamping column (22) matched with the clamping hole (112).
4. A wax-free pad for single-sided polishing planarization of a wafer as recited in claim 3, wherein: the preparation method of the modified epoxy resin comprises the following steps:
dehydrochlorination of 3, 4-dichloro butene-1 under the action of alkali, rectification until the purity is more than 98%, then copolymerization reaction with hydroxyethyl methacrylate, placing a monomer, a molecular weight regulator, a solvent and an initiator into a three-mouth bottle or a stainless steel pressure-resistant reaction bottle, copolymerization reaction under nitrogen flow, and vacuum distillation after termination of the reaction to obtain a liquid chloroprene-hydroxyethyl methacrylate copolymer;
adding the obtained liquid chloroprene-hydroxyethyl methacrylate copolymer, epoxy resin and lignin sulfonate into a mixing mill for mixing for 20min to obtain the modified epoxy resin.
5. A wax-free pad for single-sided polishing planarization of a wafer as recited in claim 4, wherein: the filler is prepared from the following materials in parts by weight: 10-16 parts of modified silicon nitride and 12-24 parts of aluminum oxide coated hexagonal boron nitride.
6. A wax-free pad for single-sided polishing planarization of a wafer as recited in claim 5, wherein: the preparation method of the modified silicon nitride comprises the following steps:
uniformly mixing new alkoxy tri (p-aminophenoxy) zirconate and a solvent at 55-65 ℃, wherein the addition of the new alkoxy tri (p-aminophenoxy) zirconate is 40-70wt% of nano silicon nitride, then adding nano silicon nitride, magnetically stirring and refluxing for 20-30 hours at 65-85 ℃, centrifugally separating an obtained reflux system, centrifugally washing with absolute ethyl alcohol, and finally drying and grinding the obtained substance to obtain the modified silicon nitride.
7. A wax-free pad for wafer single-sided polish planarization as in claim 6, wherein: the preparation method of the aluminum oxide coated hexagonal boron nitride comprises the following steps:
mixing hexagonal boron nitride powder with the particle size of 10-30nm and a dispersing agent with distilled water to prepare hexagonal boron nitride suspension with the particle size of 3-8g/L, wherein the adding amount of the dispersing agent is 3-5% of the mass of hexagonal boron nitride;
adding an acetic acid-sodium acetate buffer solution with the pH value of 4.5, performing ultrasonic dispersion, stirring and heating to 30-40 ℃, slowly dripping an aluminum nitrate solution with the Al3+ concentration of 0.1-0.2mol/L, slowly dripping ammonia water to adjust the pH value to 7.0-7.5, and keeping the temperature of 30-40 ℃ for reacting for 1.5-2.5h after dripping;
and then standing for aging, precipitating, filtering, cleaning, centrifuging and vacuum drying to obtain hexagonal boron nitride composite powder with aluminum hydroxide coated on the surface, and vacuum calcining to obtain aluminum oxide coated hexagonal boron nitride composite powder with the particle size of 20-50 nm.
8. A process for preparing a wax-free pad for single-sided polishing planarization of a wafer as recited in claim 7, comprising the steps of:
s1: adding modified epoxy resin into a reaction kettle, adding filler and curing agent, stirring at 70-110 ℃ for 3-6 hours, then paving the pretreated carbon fiber material into a mold, and carrying out injection molding, curing and forming on the stirred and mixed material to obtain a base chassis (1);
s2: injection molding the polyurethane foaming material, demolding, preparing an adsorption layer (2), and roughening the clamping column (22);
s3: and assembling the adsorption layer (2) with the base chassis (1) to prepare the wax-free pad.
9. The process for preparing a wax-free pad for single-sided polishing planarization of a wafer of claim 8, wherein: the pretreatment method of the carbon fiber comprises the following steps:
soaking carbon fiber in acetone solution for 30-40min, taking out, oven drying, soaking in 70% concentrated nitric acid for 50-60min, taking out, soaking and washing with distilled water for 3-5 times, and vacuum drying at 100deg.C for 12 hr;
the carbon fibers are blown into a state of being uniformly distributed in the three-dimensional direction by utilizing air flow, so that the carbon fibers are mutually overlapped to form a net shape.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117720751A (en) * | 2024-02-06 | 2024-03-19 | 广州傲群刷业科技有限公司 | High-durability chemical mechanical polishing polyurethane material and polishing cleaning brush preparation process thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117720751A (en) * | 2024-02-06 | 2024-03-19 | 广州傲群刷业科技有限公司 | High-durability chemical mechanical polishing polyurethane material and polishing cleaning brush preparation process thereof |
| CN117720751B (en) * | 2024-02-06 | 2024-05-10 | 广州傲群刷业科技有限公司 | High-durability chemical mechanical polishing polyurethane material and polishing cleaning brush preparation process thereof |
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