CN114085437A - Mold moistening glue with durable mold moistening capability for semiconductor packaging mold - Google Patents
Mold moistening glue with durable mold moistening capability for semiconductor packaging mold Download PDFInfo
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- CN114085437A CN114085437A CN202111476890.XA CN202111476890A CN114085437A CN 114085437 A CN114085437 A CN 114085437A CN 202111476890 A CN202111476890 A CN 202111476890A CN 114085437 A CN114085437 A CN 114085437A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/066—LDPE (radical process)
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Abstract
The invention discloses a mold lubricating adhesive with durable mold lubricating capability for a semiconductor packaging mold, which is used for solving the problems of poor lubricating effect, insufficient durability and easy migration of a mold lubricating agent of the mold lubricating adhesive in the existing semiconductor packaging industry; the mold lubricant is characterized in that a mold lubricant is grafted on the surface of reinforcing agent silicon dioxide through chemical reaction to enhance the anti-migration characteristic and the durable lubricating effect of the reinforcing agent silicon dioxide, and then a compound mold lubricant is prepared in an optimized proportion to play the synergistic effect of the compound mold lubricant, so that the durable lubricating protection of a semiconductor packaging mold is realized, and the service life of the mold is prolonged; the invention provides a mold lubricating adhesive with durable mold lubricating capability, which mainly comprises the following raw materials in parts by mass: 100 parts of unvulcanized rubber, 5-25 parts of polyolefin, 15-45 parts of silicon dioxide, 0.8-12 parts of surface bridging agent, 18-72 parts of adsorbent, 10-55 parts of mold lubricant, 0.5-4 parts of anti-aging agent, 1.5-8.6 parts of colorant, 0.4-2.5 parts of vulcanizing agent and 0.2-3 parts of vulcanization accelerator. The compound mold lubricant in the mold lubricant can play a synergistic role, plays a role in lubricating and protecting a mold after semiconductor packaging, and has migration resistance and improved lubricating durability to the mold.
Description
Technical Field
The invention relates to a mold moistening glue with durable mold moistening capability, and belongs to the field of preparation of high polymer materials.
Background
The semiconductor packaging industry commonly uses epoxy plastic packaging materials to package chips, the epoxy resin plays a role in protecting the chips after being cured, but after a certain amount of epoxy resin is packaged, scale is generated on the surface of a packaging mold, so that the surface of a product is dark, and a mucosa phenomenon appears in severe cases. Therefore, the mold must be cleaned periodically. The existing method for cleaning the die mainly comprises a liquid cleaning agent, a melamine die cleaning material and die cleaning rubber, and the die cleaning rubber can soften epoxy resin dirt remained on the surface of the die in situ, has strong dissolving capacity on scale deposit and is more and more widely applied. No matter which kind of clearance method, after the mould clearance, because of the easy production sticking of dry and astringent in mould surface, thereby the difficult drawing of patterns of goods influences product quality, need use the emollient to carry out the moist mould before shifting into production and prevent the sticking, plays protection and lubrication action to the mould simultaneously, makes the epoxy plastic-sealed spare change from the type, prolongs the active service life of packaging mold simultaneously. With the development of the semiconductor packaging industry, the demand and the requirement for the mold lubricant of the semiconductor packaging mold are higher and higher.
The mold moistening rubber is a rubber material processed by adding components such as a lubricant, a flow modifier, a release agent and the like into synthetic rubber, and is widely used as a mold moistening material of a packaging mold due to the advantages of simple and convenient processing, high mold moistening efficiency, rapid transfer to production and the like. Chinese patent publication No. CN112430366A discloses a mold moistening glue containing molybdenum disulfide, which is characterized in that the main raw materials are as follows: 100 parts of unvulcanized rubber, 30-55 parts of silicon dioxide, 5-20 parts of molybdenum disulfide powder, 15-22 parts of a release agent, 1-8 parts of a coloring agent, 0.3-6 parts of a processing aid, 1-3 parts of a vulcanization accelerator and 0.5-8 parts of a vulcanizing agent, and the molybdenum disulfide particles and wax in the release agent are utilized to generate a synergistic effect to lubricate a mold. At present, the mold release agent components in the mold moistening glue, such as paraffin, polysiloxane, low molecular weight fatty alcohol ester and the like, can migrate and be extracted in the using process, particularly, the mold can be polluted at high temperature, the continuous mold moistening capacity of the mold moistening glue is still required to be further improved, the mold moistening interval time is short after the mold is moistened and washed for the next time, and the durable mold moistening capacity of the mold moistening glue is insufficient. Reports on the improvement of the mold moistening capability and the optimization of the mold moistening effect of the mold moistening glue are quite lacking.
Disclosure of Invention
The invention aims to provide a preparation method of a mold lubricating adhesive with durable mold lubricating capability aiming at the defects of the prior art, which is characterized in that a mold lubricating agent is grafted on the surface of silicon dioxide by utilizing a chemical reaction to enhance the anti-migration characteristic and the durable lubricating effect of the silicon dioxide, and then a compound mold lubricating agent is prepared in an optimized proportion to play the synergistic effect of the compound mold lubricating agent, so that the durable lubricating protection of a semiconductor packaging mold is realized, and the service life of the mold is prolonged.
In order to improve the durable mold moistening capability of the mold moistening glue, the technical scheme adopted by the invention is as follows: a mold moistening glue with durable mold moistening capability comprises the following raw materials in parts by weight: 100 parts of unvulcanized rubber, 5-25 parts of polyolefin, 15-45 parts of silicon dioxide, 0.8-12 parts of surface bridging agent, 18-72 parts of adsorbent, 10-55 parts of mold lubricant, 0.5-4 parts of anti-aging agent, 1.5-8.6 parts of colorant, 0.4-2.5 parts of vulcanizing agent and 0.2-3 parts of vulcanization accelerator. The unvulcanized rubber is a mixed rubber composed of butadiene rubber and ethylene propylene diene monomer, and comprises the following components in percentage by mass: 65-95% of butadiene rubber and 5-35% of ethylene propylene diene monomer. The polyolefinIs any one of linear low density polyethylene, high density polyethylene, atactic polypropylene and isotactic polypropylene. The specific surface area of the silicon dioxide is 80-220 m2A fumed silica powder having a particle size of from 10 to 70 nm per g. The surface modifier is any one of gamma-glycidoxypropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-chloropropyltriethoxysilane and gamma-chloropropyltrimethoxysilane. The adsorbent is any one of zeolite molecular sieves 3A, 4A, 5A and 13X with the size of 2-8 μm. The mold lubricant is compounded by two or more of stearoyl monoethanolamine, cocoyl monoethanolamine, oleamide, ethylene bisoleamide, erucamide and oxidized polyethylene wax. The anti-aging agent is any one of 2-mercaptobenzimidazole, 2,2, 4-trimethyl-1, 2-dihydroquinoline polymer, N-phenyl-2-naphthylamine, 2, 6-di-tert-butyl-p-cresol, 2,2' -methylenebis (4-methyl-6-tert-butylphenol) and N-phenyl-alpha-naphthylamine. The colorant is one or two of titanium dioxide, zinc oxide and molybdenum disulfide. The vulcanizing agent is any one of sulfur, di-tert-butyl cumyl peroxide, 2, 5-di-tert-butyl peroxy-2, 5-dimethyl hexane and trimethylolpropane triacrylate. The vulcanization accelerator is any one of 2-mercaptobenzothiazole, N-cyclohexyl-2-benzothiazole sulfonamide, tetramethylthiuram disulfide, zinc di-N-butyldithiocarbamate, triallyl isocyanurate and trimethylolpropane triacrylate.
The preparation method of the mold moistening glue with durable mold moistening capacity comprises the following steps:
preparation of anti-migration mold lubricant grafted silica:
adding 15-45 parts of silicon dioxide into 400-4500 parts of deionized water, ultrasonically dispersing for 0.5-2 h, heating to 50-95 ℃, adding 0.8-12 parts of surface bridging agent, violently stirring, refluxing, keeping reacting for 0.5-6 h, filtering after the reaction is finished, and carrying out vacuum drying at 50-80 ℃ to obtain a solid product; and dissolving the solid product in 300-1200 parts of absolute ethanol, heating to 80 ℃, adding 10-55 parts of mold lubricant, uniformly stirring, refluxing, keeping the reaction for 0.5-4 h, filtering after the reaction is finished, and drying in vacuum at 50-80 ℃ to obtain the anti-migration mold lubricant grafted silicon dioxide product.
Preparing a mold moistening glue with durable mold moistening capacity:
plasticating unvulcanized rubber on an open mill for 3 min at room temperature, then sequentially adding an anti-migration mold lubricant grafted silicon dioxide, an adsorbent, an anti-aging agent and a coloring agent, uniformly mixing, then adding a vulcanizing agent and a vulcanization accelerator, uniformly mixing, performing triangular wrapping, thinly passing, then discharging, performing tabletting by a calender and cutting into strip-shaped products to obtain the mold lubricant with durable mold moistening capability; the vulcanization conditions of the rinsing die are that the vulcanization temperature is 155-.
By adopting the technical scheme, the invention provides the mold lubricating glue with durable mold lubricating capability, the mold lubricating agent in the mold lubricating glue is grafted on the surface of silicon dioxide, the anti-migration characteristic and the durable lubricating effect of the silicon dioxide are enhanced, and meanwhile, the compounded mold lubricating agent plays a synergistic effect and plays a role in durable lubricating and protecting a mold after semiconductor packaging.
Detailed Description
The present invention is further described in the following by specific examples, which are only used for further illustration of the present invention and are not to be construed as limiting the scope of the present invention, and those skilled in the art can make non-essential modifications to the present invention based on the above disclosure, and all other examples obtained without creative efforts will fall within the scope of the present invention.
Example 1
The method comprises the following steps: adding 30 parts of silicon dioxide into 2000 parts of deionized water, performing ultrasonic dispersion for 1 hour, heating to 85 ℃, adding 3 parts of gamma-glycidyl ether oxypropyl trimethoxy silane, stirring vigorously, refluxing, keeping the reaction for 4 hours, filtering after the reaction is finished, and performing vacuum drying at 60 ℃ to obtain a solid product; dissolving the solid product in 600 parts of absolute ethyl alcohol, heating to 80 ℃, adding 27 parts of a mold lubricant, namely 12 parts of oleamide, 2 parts of erucamide, 3 parts of stearoyl monoethanolamine and 10 parts of ethylene bis-oleamide, uniformly stirring, refluxing, keeping the reaction for 3 hours, filtering after the reaction is finished, and performing vacuum drying at 50 ℃ to obtain the anti-migration mold lubricant grafted silicon dioxide product.
Step two: adding 75 parts of butadiene rubber and 25 parts of ethylene propylene diene monomer rubber into an internal mixer, melting and blending at 130 ℃, adding 10 parts of high-density polyethylene, mixing for 3 min, and discharging; plasticating for 3 min on an open mill, sequentially adding the anti-migration mold lubricant grafted silica, 28 parts of molecular sieve 3A, 2 parts of 2-mercaptobenzimidazole and 2 parts of molybdenum disulfide, uniformly mixing, then adding 1 part of di-tert-butyl cumene peroxide and 0.5 part of triallyl isocyanurate, uniformly mixing, performing triangular bag making, thinning, discharging, tabletting by a calender, and cutting into strip-shaped products to obtain the mold lubricant; the mold lubricant is placed on a packaging mold, the vulcanization condition is that the vulcanization temperature is 165 ℃, the vulcanization pressure is 10 MPa, and the vulcanization time is 3 min, then the mold is opened, the adhesive tape is taken down, a demolding lubricating layer is formed on the surface of the semiconductor packaging mold, the demolding of an epoxy plastic packaging part is facilitated, the mold lubricant is good in durable mold lubrication effect, the tensile strength of the vulcanized mold lubricant is 11.2 MPa, and the elongation at break is 462%.
Example 2
The method comprises the following steps: adding 40 parts of silicon dioxide into 3000 parts of deionized water, performing ultrasonic dispersion for 1.5 h, heating to 70 ℃, adding 6 parts of gamma-aminopropyltriethoxysilane, violently stirring, refluxing, keeping reaction for 6 h, filtering after the reaction is finished, and performing vacuum drying at 65 ℃ to obtain a solid product; dissolving the solid product in 500 parts of absolute ethyl alcohol, heating to 60 ℃, adding 35 parts of mold lubricant of 18 parts of oleamide, 5 parts of erucamide and 12 parts of cocoyl monoethanolamine, stirring uniformly, refluxing, keeping reacting for 4 hours, filtering after the reaction is finished, and drying in vacuum at 50 ℃ to obtain the anti-migration mold lubricant grafted silicon dioxide product.
Step two: adding 85 parts of butadiene rubber and 15 parts of ethylene propylene diene monomer rubber into an internal mixer, melting and blending at 120 ℃, adding 16 parts of low-density polyethylene, mixing for 4 min, and discharging; plasticating for 3 min on an open mill, sequentially adding 5 parts of the anti-migration mold lubricant grafted silicon dioxide, 33 parts of molecular sieve 4A, 1.5 parts of 2, 6-di-tert-butyl-p-cresol, 2 parts of molybdenum disulfide and 3 parts of titanium dioxide, uniformly mixing, then adding 1.3 parts of 2, 5-di-tert-butyl peroxide-2, 5-dimethylhexane and 0.3 part of sulfur, uniformly mixing, performing triangular packaging, blanking after thinning, tabletting by a calender and cutting into strip-shaped products to obtain the mold lubricant; the mold lubricant is placed on a packaging mold, the vulcanization condition is that the vulcanization temperature is 175 ℃, the vulcanization pressure is 12 MPa, and the vulcanization time is 5 min, then the mold is opened, the adhesive tape is taken down, a demolding lubricating layer is formed on the surface of the semiconductor packaging mold, the demolding of an epoxy plastic packaging part is facilitated, the mold lubricant is good in durable mold lubrication effect, the tensile strength of the vulcanized mold lubricant is 10.6 MPa, and the elongation at break is 522%.
Example 3
The method comprises the following steps: adding 50 parts of silicon dioxide into 4000 parts of deionized water, performing ultrasonic dispersion for 2 hours, heating to 80 ℃, adding 10 parts of gamma-chloropropyltriethoxysilane, violently stirring, performing reflux reaction for 6 hours, filtering after the reaction is finished, and performing vacuum drying at 60 ℃ to obtain a solid product; dissolving the solid product in 800 parts of absolute ethyl alcohol, heating to 70 ℃, adding 46 parts of oleic acid amide, 4 parts of cocoyl monoethanolamine and 16 parts of oxidized polyethylene wax, stirring uniformly, refluxing, keeping reacting for 4 hours, filtering after the reaction is finished, and drying in vacuum at 50 ℃ to obtain the anti-migration mold lubricant grafted silicon dioxide product.
Step two: adding 95 parts of butadiene rubber and 5 parts of ethylene propylene diene monomer rubber into an internal mixer, melting and blending at 125 ℃, adding 12 parts of atactic polypropylene, mixing for 4 min, and discharging; plasticating for 3 min on an open mill, sequentially adding 9 parts of the anti-migration mold lubricant grafted silicon dioxide, 50 parts of molecular sieve 5A, 1.5 parts of N-phenyl-2-naphthylamine, 3 parts of molybdenum disulfide and 6 parts of titanium dioxide, uniformly mixing, then adding 3 parts of 2, 5-di-tert-butyl peroxy-2, 5-dimethylhexane and 0.8 part of N-cyclohexyl-2-benzothiazole sulfenamide, uniformly mixing, performing triangular packaging, thinly passing, blanking, and tabletting by a calender to obtain a strip-shaped product so as to obtain the cutting mold lubricant; the mold lubricant is placed on a packaging mold, the vulcanization condition is that the vulcanization temperature is 180 ℃, the vulcanization pressure is 13 MPa, the vulcanization time is 4 min, then the mold is opened, the adhesive tape is taken down, a demolding lubricating layer is formed on the surface of the semiconductor packaging mold, the demolding of an epoxy plastic packaging part is facilitated, the mold lubricant is good in durable mold lubrication effect, the tensile strength of the vulcanized mold lubricant is 11.4 MPa, and the elongation at break is 573%.
Example 4
The method comprises the following steps: adding 22 parts of silicon dioxide into 2200 parts of deionized water, performing ultrasonic dispersion for 1 hour, heating to 80 ℃, adding 4 parts of gamma-chloropropyltrimethoxysilane, vigorously stirring, refluxing, keeping the reaction for 3 hours, filtering after the reaction is finished, and performing vacuum drying at 70 ℃ to obtain a solid product; dissolving the solid product in 400 parts of absolute ethyl alcohol, heating to 60 ℃, adding 18 parts of a mold lubricant of 2 parts of cocoyl monoethanolamine, 4 parts of stearoyl monoethanolamine and 12 parts of oleamide, stirring uniformly, refluxing, keeping reacting for 4 hours, filtering after the reaction is finished, and drying in vacuum at 60 ℃ to obtain the anti-migration mold lubricant grafted silicon dioxide product.
Step two: adding 65 parts of butadiene rubber and 35 parts of ethylene propylene diene monomer rubber into an internal mixer, melting and blending at 125 ℃, adding 6 parts of linear low-density polyethylene, mixing for 3 min, and discharging; plasticating for 3 min on an open mill, sequentially adding the anti-migration mold lubricant grafted silicon dioxide, 18 parts of molecular sieve 13X, 3 parts of 2,2' -methylenebis (4-methyl-6-tert-butylphenol) and 3 parts of molybdenum disulfide, uniformly mixing, then adding 1.8 parts of di-tert-butyl cumene peroxide and 1.5 parts of zinc di-n-butyldithiocarbamate, uniformly mixing, performing triangular bag making, sheet discharging after thin passing, and cutting into strip-shaped products after sheet pressing by a calender to obtain the mold lubricant; the mold lubricant is placed on a packaging mold, the vulcanization condition is that the vulcanization temperature is 180 ℃, the vulcanization pressure is 12 MPa, and the vulcanization time is 6 min, then the mold is opened, the adhesive tape is taken down, a demolding lubricating layer is formed on the surface of the semiconductor packaging mold, the epoxy plastic packaging member is favorably released, the mold lubricating effect is good, the tensile strength of the vulcanized mold lubricating adhesive is 9.7 MPa, and the elongation at break is 386%.
The above description is the preferred embodiment of the present invention, and it is within the scope of the appended claims to cover all modifications of the invention which may occur to those skilled in the art without departing from the spirit and scope of the invention.
Claims (10)
1. The mold moistening glue with durable mold moistening capability is characterized by comprising the following main raw materials in parts by mass:
100 parts of unvulcanized rubber, 5-25 parts of polyolefin, 15-45 parts of silicon dioxide, 0.8-12 parts of surface bridging agent, 18-72 parts of adsorbent, 10-55 parts of mold lubricant, 0.5-4 parts of anti-aging agent, 1.5-8.6 parts of colorant, 0.4-2.5 parts of vulcanizing agent and 0.2-3 parts of vulcanization accelerator.
2. The mold lubricating gel with durable mold lubricating capability according to claim 1, characterized in that: the unvulcanized rubber is a mixed rubber composed of butadiene rubber and ethylene propylene diene monomer, and mainly comprises the following components in percentage by mass: 65-95% of butadiene rubber and 5-35% of ethylene propylene diene monomer.
3. The mold lubricating gel with durable mold lubricating capability according to claim 1, characterized in that: the polyolefin is any one of linear low-density polyethylene, high-density polyethylene, atactic polypropylene and isotactic polypropylene.
4. The mold lubricating gel with durable mold lubricating capability according to claim 1, characterized in that: the specific surface area of the silicon dioxide is 80-220 m2A fumed silica powder having a particle size of from 10 to 70 nm per g.
5. The mold lubricating gel with durable mold lubricating capability according to claim 1, characterized in that: the surface modifier is any one of gamma-glycidoxypropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-chloropropyltriethoxysilane and gamma-chloropropyltrimethoxysilane.
6. The mold lubricating gel with durable mold lubricating capability according to claim 1, characterized in that: the adsorbent is any one of zeolite molecular sieves 3A, 4A, 5A and 13X with the size of 2-8 mu m.
7. The mold lubricating gel with durable mold lubricating capability according to claim 1, characterized in that: the mold lubricant is compounded by two or more of stearoyl monoethanolamine, cocoyl monoethanolamine, oleamide, ethylene bisoleamide, erucamide and oxidized polyethylene wax.
8. The mold lubricating gel with durable mold lubricating capability according to claim 1, characterized in that: the anti-aging agent is any one of 2-mercaptobenzimidazole, 2,2, 4-trimethyl-1, 2-dihydroquinoline polymer, N-phenyl-2-naphthylamine, 2, 6-di-tert-butyl-p-cresol, 2,2' -methylenebis (4-methyl-6-tert-butylphenol) and N-phenyl-alpha-naphthylamine.
9. The mold lubricating gel with durable mold lubricating capability according to claim 1, characterized in that: the colorant is one or two of titanium dioxide, zinc oxide and molybdenum disulfide.
10. The mold lubricating gel with durable mold lubricating capability according to claim 1, characterized in that: the vulcanizing agent is any one of sulfur, di-tert-butyl cumyl peroxide, 2, 5-di-tert-butyl peroxy-2, 5-dimethyl hexane and trimethylolpropane triacrylate; the vulcanization accelerator is any one of 2-mercaptobenzothiazole, N-cyclohexyl-2-benzothiazole sulfonamide, tetramethyl thiuram disulfide, zinc di-N-butyl dithiocarbamate, triallyl isocyanurate and trimethylolpropane triacrylate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111476890.XA CN114085437A (en) | 2021-12-06 | 2021-12-06 | Mold moistening glue with durable mold moistening capability for semiconductor packaging mold |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111476890.XA CN114085437A (en) | 2021-12-06 | 2021-12-06 | Mold moistening glue with durable mold moistening capability for semiconductor packaging mold |
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| CN114085437A true CN114085437A (en) | 2022-02-25 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202111476890.XA Withdrawn CN114085437A (en) | 2021-12-06 | 2021-12-06 | Mold moistening glue with durable mold moistening capability for semiconductor packaging mold |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114736442A (en) * | 2022-04-15 | 2022-07-12 | 池州市鼎弘半导体科技有限公司 | Mould moistening rubber strip without sodium ions |
-
2021
- 2021-12-06 CN CN202111476890.XA patent/CN114085437A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114736442A (en) * | 2022-04-15 | 2022-07-12 | 池州市鼎弘半导体科技有限公司 | Mould moistening rubber strip without sodium ions |
| CN114736442B (en) * | 2022-04-15 | 2024-02-02 | 池州市鼎弘半导体科技有限公司 | Sodium ion-free mold wetting adhesive tape |
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