CN116694005A - High-temperature-resistant perfluoroether rubber composition and preparation method and application thereof - Google Patents
High-temperature-resistant perfluoroether rubber composition and preparation method and application thereof Download PDFInfo
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- CN116694005A CN116694005A CN202310844028.2A CN202310844028A CN116694005A CN 116694005 A CN116694005 A CN 116694005A CN 202310844028 A CN202310844028 A CN 202310844028A CN 116694005 A CN116694005 A CN 116694005A
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 205
- 229920001774 Perfluoroether Polymers 0.000 title claims abstract description 133
- UJMWVICAENGCRF-UHFFFAOYSA-N oxygen difluoride Chemical compound FOF UJMWVICAENGCRF-UHFFFAOYSA-N 0.000 title claims abstract description 133
- 239000000203 mixture Substances 0.000 title claims abstract description 96
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 57
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 45
- 238000012545 processing Methods 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000004065 semiconductor Substances 0.000 claims abstract description 28
- 238000004073 vulcanization Methods 0.000 claims description 108
- 239000006229 carbon black Substances 0.000 claims description 90
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 66
- 239000006057 Non-nutritive feed additive Substances 0.000 claims description 41
- 238000003490 calendering Methods 0.000 claims description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 40
- 239000000945 filler Substances 0.000 claims description 40
- 238000002156 mixing Methods 0.000 claims description 40
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 33
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 33
- 238000007599 discharging Methods 0.000 claims description 32
- MSTZGVRUOMBULC-UHFFFAOYSA-N 2-amino-4-[2-(3-amino-4-hydroxyphenyl)-1,1,1,3,3,3-hexafluoropropan-2-yl]phenol Chemical compound C1=C(O)C(N)=CC(C(C=2C=C(N)C(O)=CC=2)(C(F)(F)F)C(F)(F)F)=C1 MSTZGVRUOMBULC-UHFFFAOYSA-N 0.000 claims description 28
- 230000001105 regulatory effect Effects 0.000 claims description 17
- 238000005516 engineering process Methods 0.000 claims description 15
- 239000000498 cooling water Substances 0.000 claims description 13
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 12
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 229920000642 polymer Polymers 0.000 claims description 6
- 239000000178 monomer Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000006835 compression Effects 0.000 claims 2
- 238000007906 compression Methods 0.000 claims 2
- 230000032683 aging Effects 0.000 abstract description 34
- 238000005530 etching Methods 0.000 abstract description 7
- 230000001590 oxidative effect Effects 0.000 abstract description 7
- 238000012360 testing method Methods 0.000 description 26
- 238000003825 pressing Methods 0.000 description 14
- 238000000748 compression moulding Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 238000005979 thermal decomposition reaction Methods 0.000 description 11
- 238000004227 thermal cracking Methods 0.000 description 10
- 238000004513 sizing Methods 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 6
- 229910021485 fumed silica Inorganic materials 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- 239000000806 elastomer Substances 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 229920002313 fluoropolymer Polymers 0.000 description 2
- 239000004811 fluoropolymer Substances 0.000 description 2
- 229920002725 thermoplastic elastomer Polymers 0.000 description 2
- 239000004636 vulcanized rubber Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000003878 thermal aging Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/18—Amines; Quaternary ammonium compounds with aromatically bound amino groups
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
- C08K2003/2213—Oxides; Hydroxides of metals of rare earth metal of cerium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/80—Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
- Y02T10/86—Optimisation of rolling resistance, e.g. weight reduction
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention relates to the technical field of rubber compositions, in particular to a high-temperature-resistant perfluoroether rubber composition, and a preparation method and application thereof. The high temperature resistant perfluoro ether rubber composition is prepared with perfluoro ether rubber 80-120 weight portions, stuffing 15-25 weight portions, cross-linking agent 1.0-2.5 weight portions and processing assistant 0.5-1.5 weight portions. The high temperature resistant perfluoroether rubber composition solves the problems of uneven surface, poor thermal oxidative aging performance and poor thermal stability of a rubber product prepared by vulcanizing domestic perfluoroether rubber raw rubber, and can obtain a sealing product with flat surface and excellent thermal oxidative aging performance. The sealing product prepared by adopting the high-temperature-resistant perfluoroether rubber composition disclosed by the invention does not influence an etching process and the product process yield in the semiconductor industry in the use process.
Description
Technical Field
The invention relates to the technical field of rubber compositions, in particular to a high-temperature-resistant perfluoroether rubber composition, and a preparation method and application thereof.
Background
Along with the development and transition of the age, the semiconductor industry has a significant position in modern life, the fluorine-containing polymer elastomer can meet the requirements of the processing fields of materials, equipment, chips, packaging and the like related to the semiconductor industry on high temperature resistance of sealing products used by the fluorine-containing polymer elastomer, and the variety and content of introduced metal ions need to be avoided or reduced as much as possible in the process of manufacturing procedures of the semiconductor industry; with the rapid development of the semiconductor industry, the requirements on processing equipment are higher and higher, and the high temperature resistance of materials adopted for sealing products is also improved, the high temperature resistance of the sealing products is generally improved by modifying the fluorine-containing polymer structure, and the high temperature resistance of the sealing products is further improved; the high temperature resistance of the seal product can also be improved by adding filler and processing aid to the fluoropolymer.
In order to improve the high temperature resistance, mechanical property and processing property of the fluoropolymer elastomer at present, processing aids such as magnesium oxide, calcium hydroxide, lead oxide and the like are usually added in the formula, and metals such as magnesium, calcium or lead and the like are introduced into the processing aids, so that the success rate of an etching process can be influenced, and the yield of the product process in the semiconductor industry can be reduced. The Chinese patent with the patent application number of CN202111536744.1 discloses a perfluoroether rubber composition, a preparation method and application thereof, wherein the perfluoroether rubber composition prepared by adopting perfluoroether rubber produced by foreign manufacturers and HT290 (fatty acid derivative and wax mixture) as a processing aid is applicable to the industries of semiconductors, photovoltaics, food and medicines and the like with high cleanliness, low precipitation of particles and low metal ion content.
At present, the perfluoroether rubber is a neck material of a semiconductor industry chain, and the quality of the domestic perfluoroether rubber is quite different from that of the imported perfluoroether rubber. In order to improve the safety of the Chinese semiconductor industry chain as soon as possible, under the condition that the structure of the domestic perfluoroether rubber is not changed, the formula and the process are subjected to technical breakthrough, and the high-temperature resistant material which does not influence the etching process and the product process yield in the semiconductor industry is provided, so that the main technical problem to be solved at present is provided.
Disclosure of Invention
In order to solve the problems, the first aspect of the invention provides a high-temperature-resistant perfluoroether rubber composition, which comprises, by weight, 80-120 parts of perfluoroether rubber raw rubber, 15-25 parts of filler, 1.0-2.5 parts of cross-linking agent and 0.5-1.5 parts of processing aid; the perfluoro ether rubber raw rubber comprises tetrafluoroethylene-perfluoroalkyl vinyl ether-vulcanization point monomer polymer; the processing aid is cerium oxide; the particle size of the processing aid is less than or equal to 300nm; the filler is selected from one or two of carbon black and white carbon black.
Further, the high temperature resistant perfluoroether rubber composition comprises, by weight, 100 parts of perfluoroether rubber raw rubber, 15-25 parts of filler, 1.0-2.5 parts of cross-linking agent and 0.5-1.5 parts of processing aid.
Preferably, the perfluoroether rubber green is a tetrafluoroethylene-perfluoroalkyl vinyl ether-cure site monomer polymer;
preferably, the cure site monomer is preferably a CN-CSM cure site monomer.
In one embodiment, the perfluoroether rubber is FFKM-A, FFKM-B.
theFFKM-AhasamanufacturerofMitsuKagakuCo.
The FFKM-B has a manufacturer of Mitsu Kagaku Co.
Further, the carbon black is N990 thermal decomposition carbon black.
Further, the white carbon black is gas phase white carbon black N20.
Preferably, the cross-linking agent is selected from one or more of 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane, triallyl isocyanurate, 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane.
The CAS number of the 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane is 83558-87-6.
The triallyl isocyanurate has a CAS number of 1025-15-6.
The CAS number of the 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane is 78-63-7.
In order to solve the problems of uneven surface, poor thermal oxidative aging performance and poor thermal stability of a rubber product prepared by vulcanizing domestic perfluoroether rubber raw rubber, the inventor finds that the rubber product prepared by vulcanizing the domestic perfluoroether rubber raw rubber, a filler, a cross-linking agent and cerium oxide is flat in surface and excellent in thermal oxidative aging performance and thermal stability after being matched with 100 parts of the perfluoroether rubber raw rubber, 15-25 parts of the filler, 1.0-2.5 parts of the cross-linking agent and 0.5-2.0 parts of cerium oxide, in particular when the particle size of cerium oxide is less than or equal to 300 nm.
In order to solve the problems that the high temperature-resistant perfluoroether rubber composition does not affect the etching process and the product process yield in the semiconductor industry, the inventor finds that cerium oxide is adopted as a processing aid in the experimental process, the high temperature resistance of a product can be improved, and the semiconductor processing etching process is not affected, probably because the polishing agent adopted in semiconductor processing equipment contains cerium oxide, the high temperature-resistant perfluoroether rubber composition prepared by the application contains cerium oxide and can not cause the problem of introducing new metal ions, and the sealing product prepared by adopting the high temperature-resistant perfluoroether rubber composition can be used for a long time at 300 ℃.
The second aspect of the application provides a method for preparing a high temperature resistant perfluoroether rubber composition, comprising the steps of:
s1, adding perfluoroether rubber raw rubber into an internal mixer for banburying, adding filler for banburying to obtain master batch, carrying out thin-pass triangular bag opening on the master batch on an open mill, adjusting the roll gap of the open mill for calendaring and sheet discharging, and standing the prepared master batch for more than 12 hours for later use;
s2, putting the parked masterbatch into an open mill for calendering and softening, wrapping a roll of the masterbatch, adding a processing aid for mixing, adding a cross-linking agent for mixing after mixing uniformly, and regulating the roll gap of the open mill for calendering and discharging sheets for standby after standing for more than 12 hours.
Preferably, in the step S2, cooling water is introduced into the open mill, the roll gap of the open mill is adjusted to be 0.6-1.0mm, and then the parked masterbatch is put into the open mill for calendering and softening.
Further, the preparation method of the high-temperature-resistant perfluoroether rubber composition comprises the following steps:
s1, setting the temperature of an internal mixer to 90-120 ℃, putting perfluoroether rubber raw rubber into a banburying chamber for banburying for 120s until torque is stable after the temperature of the internal mixer is stable, putting filler into the banburying chamber through a feed inlet, putting down an upper plug for banburying for 2-10min to obtain master batch, and discharging rubber from the master batch, wherein the rubber discharge temperature is controlled at 130-160 ℃; putting the master batch on an open mill with the roll spacing of 0.1-0.5mm, opening a triangular bag for 10 times, adjusting the roll spacing to 2.0mm, calendaring out sheets, and standing the prepared master batch for more than 12 hours for later use.
S2, introducing cooling water into an open mill, adjusting the roll gap of the open mill to be 0.6-1.0mm, putting the parked masterbatch on the open mill for calendering and softening, wrapping the masterbatch, gradually adding a processing aid for mixing, after the processing aid is completely mixed with sizing materials, uniformly mixing the sizing materials by a left cutter and a right cutter for 5 times, uniformly mixing, adding a cross-linking agent for mixing, turning the left rubber cutting and the right rubber cutting, adjusting the roll gap of the open mill to be 0.2mm for 5-10 times, continuously adjusting the roll gap of the open mill to be 1.0mm, calendering and discharging sheets, and parking for more than 12 hours for later use.
In order to obtain the sealing product with stable mechanical properties, the inventor finds that the processing aid, the filler and the cross-linking agent can be uniformly dispersed in the raw perfluoroether rubber in the experimental process, and the inventor finds that the perfluoroether rubber composition with the raw material uniform dispersion characteristic can be obtained by adopting the preparation method in the experimental process, so that the mechanical properties of the sealing product are further stabilized.
The invention provides an application of a high-temperature-resistant perfluoroether rubber composition, which is applied to the technical field of semiconductor industry processing by preparing a sealing product through primary mould pressing vulcanization and secondary vulcanization.
Preferably, the sealing article is a seal.
Preferably, the vulcanization temperature of the one-stage mould pressing vulcanization is 150-190 ℃, the vulcanization time is 5-15min, and the vulcanization pressure is 10-20MPa.
Further, the high temperature-resistant perfluoroether rubber composition is placed in a mold, the mold is placed in a flat vulcanizing machine for one-stage compression molding vulcanization to obtain one-stage vulcanized product, the one-stage vulcanized product is placed in an oven for two-stage vulcanization after being parked for 12 hours, and a sealing product is prepared and applied to the technical field of semiconductor industry processing.
The vulcanization temperature of the one-stage mould pressing vulcanization is 150-190 ℃, the vulcanization time is 5-15min, and the vulcanization pressure is 10-20MPa.
The processing technology of the secondary vulcanization is that the primary vulcanization product is placed in an oven, the temperature of the oven is uniformly heated to 200 ℃ from 25 ℃, the temperature is kept at 200 ℃ for 8 hours, the temperature is then increased to 290 ℃ according to the heating rate of 10 ℃ per hour, the temperature is kept at 290 ℃ for 12-24 hours, and then the temperature is slowly reduced to 25 ℃, and the sealing product is taken out for standby.
Drawings
Fig. 1 is a photograph of the O-ring prepared in example 3 under a microscope.
Fig. 2 is a photograph of the O-ring prepared in example 10 under a microscope.
Fig. 3 is a photograph of the O-ring prepared in example 8 under a microscope.
Fig. 4 is a photograph of the O-ring prepared in example 9 under a microscope.
Advantageous effects
1. The high temperature resistant perfluoroether rubber composition solves the problems of uneven surface, poor thermal oxidative aging performance and poor thermal stability of a rubber product prepared by vulcanizing domestic perfluoroether rubber raw rubber, and can obtain a sealing product with flat surface and excellent thermal oxidative aging performance.
2. The sealing product prepared by adopting the high-temperature-resistant perfluoroether rubber composition disclosed by the invention does not influence an etching process and the product process yield in the semiconductor industry in the use process.
3. By adopting the processing technology defined in the invention for processing, the processing aid, the filler and the cross-linking agent can be uniformly dispersed in the raw perfluoroether rubber, so that the perfluoroether rubber composition with the characteristic of uniformly dispersing raw materials can be obtained, and the mechanical properties of the sealing product are further stabilized.
4. The invention discovers that cerium oxide with specific particle size is used as a processing aid, so that the problems of uneven surface, poor thermal oxidative aging performance and poor thermal stability of a rubber product prepared by vulcanizing domestic perfluoro ether rubber raw rubber can be solved, and the semiconductor processing etching process is not influenced.
Detailed Description
Example 1
The first aspect of the embodiment provides a high-temperature-resistant perfluoroether rubber composition, which comprises, by weight, 100 parts of perfluoroether rubber raw rubber, 20 parts of filler and 1.5 parts of cross-linking agent.
theperfluoroetherrubberrawrubberisFFKM-A.
The cross-linking agent is 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane.
The filler is carbon black.
The carbon black is thermal cracking carbon black N990.
theFFKM-AhasamanufacturerofMitsuKagakuCo.
The manufacturer of the thermal decomposition carbon black N990 is cabot in the United states.
The CAS number of the 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane is 83558-87-6.
The second aspect of the present embodiment provides a method for preparing a high temperature resistant perfluoroether rubber composition, comprising the steps of:
s1, setting the temperature of an internal mixer at 110 ℃, after the temperature of the internal mixer is stable, putting perfluoroether rubber raw rubber into a banburying chamber, banburying for 120s until torque is stable, putting filler into the banburying chamber through a feed inlet, putting down an upper plug, banburying for 5min to obtain master batch, and discharging the obtained master batch at 140 ℃; and (3) placing the master batch on an open mill with the roll spacing of 0.2mm, carrying out thin-pass triangular bag opening for 10 times, adjusting the roll spacing to 2.0mm, calendaring to obtain sheets, and standing the prepared master batch for more than 12 hours for later use.
S2, cooling water is introduced into an open mill, after the roll gap of the open mill is adjusted to be 1.0mm, the parked masterbatch is put into the open mill for calendaring and softening, the masterbatch is wrapped by rolls, cross-linking agents are gradually added for mixing, left and right rubber cuts are turned over for mixing, the high temperature resistant perfluoroether rubber composition is prepared after uniform mixing, the roll gap of the open mill is adjusted to be 0.2mm for 10 times, the roll gap of the open mill is continuously adjusted to be 1.0mm, calendaring and sheet discharging are carried out, and the open mill is parked for more than 12 hours for standby.
In a third aspect, the embodiment provides an application of a high-temperature-resistant perfluoroether rubber composition, the high-temperature-resistant perfluoroether rubber composition is placed in a mold, the mold is placed in a flat vulcanizing machine for one-stage compression molding vulcanization to obtain one-stage vulcanized product, the one-stage vulcanized product is parked for 12 hours, and then the one-stage vulcanized product is placed in an oven for two-stage vulcanization to prepare a sealing product, so that the sealing product is applied to the technical field of semiconductor industry processing.
The vulcanization temperature of the one-stage mould pressing vulcanization is 170 ℃, the vulcanization time is 10min, and the vulcanization pressure is 15MPa.
The processing technology of the secondary vulcanization is that the primary vulcanization product is placed in an oven, the temperature of the oven is uniformly heated to 200 ℃ from 25 ℃, the temperature is kept at 200 ℃ for 8 hours, the temperature is then increased to 290 ℃ according to the heating rate of 10 ℃ per hour, the temperature is kept at 290 ℃ for 12-24 hours, and then the temperature is slowly reduced to 25 ℃, and the sealing product is taken out for standby.
Example 2
The first aspect of the embodiment provides a high-temperature-resistant perfluoroether rubber composition, which comprises, by weight, 100 parts of perfluoroether rubber raw rubber, 15 parts of filler and 1 part of cross-linking agent.
theperfluoroetherrubberrawrubberisFFKM-A.
The cross-linking agent is 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane.
The filler is carbon black.
The carbon black is thermal cracking carbon black N990.
theFFKM-AhasamanufacturerofMitsuKagakuCo.
The manufacturer of the thermal decomposition carbon black N990 is cabot in the United states.
The CAS number of the 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane is 83558-87-6.
The second aspect of the present embodiment provides a method for preparing a high temperature resistant perfluoroether rubber composition, comprising the steps of:
S1, setting the temperature of an internal mixer at 110 ℃, after the temperature of the internal mixer is stable, putting perfluoroether rubber raw rubber into a banburying chamber, banburying for 120s until torque is stable, putting filler into the banburying chamber through a feed inlet, putting down an upper plug, banburying for 5min to obtain master batch, and discharging the obtained master batch at 140 ℃; and (3) placing the master batch on an open mill with the roll spacing of 0.2mm, carrying out thin-pass triangular bag opening for 10 times, adjusting the roll spacing to 2.0mm, calendaring to obtain sheets, and standing the prepared master batch for more than 12 hours for later use.
S2, cooling water is introduced into an open mill, after the roll gap of the open mill is adjusted to be 1.0mm, the parked masterbatch is put into the open mill for calendaring and softening, the masterbatch is wrapped by rolls, cross-linking agents are gradually added for mixing, left and right rubber cuts are turned over for mixing, the high temperature resistant perfluoroether rubber composition is prepared after uniform mixing, the roll gap of the open mill is adjusted to be 0.2mm for 10 times, the roll gap of the open mill is continuously adjusted to be 1.0mm, calendaring and sheet discharging are carried out, and the open mill is parked for more than 12 hours for standby.
In a third aspect, the embodiment provides an application of a high-temperature-resistant perfluoroether rubber composition, the high-temperature-resistant perfluoroether rubber composition is placed in a mold, the mold is placed in a flat vulcanizing machine for one-stage compression molding vulcanization to obtain one-stage vulcanized product, the one-stage vulcanized product is parked for 12 hours, and then the one-stage vulcanized product is placed in an oven for two-stage vulcanization to prepare a sealing product, so that the sealing product is applied to the technical field of semiconductor industry processing.
The vulcanization temperature of the one-stage mould pressing vulcanization is 170 ℃, the vulcanization time is 10min, and the vulcanization pressure is 15MPa.
The processing technology of the secondary vulcanization is that the primary vulcanization product is placed in an oven, the temperature of the oven is uniformly heated to 200 ℃ from 25 ℃, the temperature is kept at 200 ℃ for 8 hours, the temperature is then increased to 290 ℃ according to the heating rate of 10 ℃ per hour, the temperature is kept at 290 ℃ for 12-24 hours, and then the temperature is slowly reduced to 25 ℃, and the sealing product is taken out for standby.
Example 3
The first aspect of the embodiment provides a high-temperature-resistant perfluoroether rubber composition, which comprises, by weight, 100 parts of perfluoroether rubber raw rubber, 20 parts of filler, 1.5 parts of cross-linking agent and 1 part of processing aid.
theperfluoroetherrubberrawrubberisFFKM-A.
The cross-linking agent is 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane.
The processing aid is cerium oxide.
The filler is carbon black.
The carbon black is thermal cracking carbon black N990.
theFFKM-AhasamanufacturerofMitsuKagakuCo.
The manufacturer of the thermal decomposition carbon black N990 is cabot in the United states.
The CAS number of the 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane is 83558-87-6.
The manufacturer of cerium oxide is Shanghai mao nano technology Co., ltd, and the grain size is 200nm.
The second aspect of the present embodiment provides a method for preparing a high temperature resistant perfluoroether rubber composition, comprising the steps of:
s1, setting the temperature of an internal mixer at 110 ℃, after the temperature of the internal mixer is stable, putting perfluoroether rubber raw rubber into a banburying chamber, banburying for 120s until torque is stable, putting filler into the banburying chamber through a feed inlet, putting down an upper plug, banburying for 5min to obtain master batch, and discharging the obtained master batch at 140 ℃; and (3) placing the master batch on an open mill with the roll spacing of 0.2mm, carrying out thin-pass triangular bag opening for 10 times, adjusting the roll spacing to 2.0mm, calendaring to obtain sheets, and standing the prepared master batch for more than 12 hours for later use.
S2, introducing cooling water into an open mill, regulating the roll gap of the open mill to be 1.0mm, putting the parked masterbatch into the open mill for calendering and softening, gradually adding a processing aid into a masterbatch roller for mixing, after the processing aid is completely mixed with sizing materials, respectively 5 times of left and right cutters for mixing uniformly, adding a cross-linking agent for mixing, turning left and right rubber cuts, regulating the roll gap of the open mill to be 0.2mm for 10 times, continuously regulating the roll gap of the open mill to be 1.0mm, calendering and discharging sheets, and standing for more than 12 hours for later use.
In a third aspect, the embodiment provides an application of a high-temperature-resistant perfluoroether rubber composition, the high-temperature-resistant perfluoroether rubber composition is placed in a mold, the mold is placed in a flat vulcanizing machine for one-stage compression molding vulcanization to obtain one-stage vulcanized product, the one-stage vulcanized product is parked for 12 hours, and then the one-stage vulcanized product is placed in an oven for two-stage vulcanization to prepare a sealing product, so that the sealing product is applied to the technical field of semiconductor industry processing.
The vulcanization temperature of the one-stage mould pressing vulcanization is 170 ℃, the vulcanization time is 10min, and the vulcanization pressure is 15MPa.
The processing technology of the secondary vulcanization is that the primary vulcanization product is placed in an oven, the temperature of the oven is uniformly heated to 200 ℃ from 25 ℃, the temperature is kept at 200 ℃ for 8 hours, the temperature is then increased to 290 ℃ according to the heating rate of 10 ℃ per hour, the temperature is kept at 290 ℃ for 12-24 hours, and then the temperature is slowly reduced to 25 ℃, and the sealing product is taken out for standby.
Example 4
The first aspect of the embodiment provides a high-temperature-resistant perfluoroether rubber composition, which comprises, by weight, 100 parts of perfluoroether rubber raw rubber, 20 parts of filler and 1 part of cross-linking agent.
theperfluoroetherrubberrawrubberisFFKM-A.
The filler is a composition of carbon black and white carbon black, and the mass ratio of the carbon black to the white carbon black is 3:1.
The carbon black is thermal cracking carbon black N990.
The white carbon black is gas phase white carbon black N20.
The cross-linking agent is 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane.
theFFKM-AhasamanufacturerofMitsuKagakuCo.
The manufacturer of the thermal decomposition carbon black N990 is cabot in the United states.
The manufacturer of the fumed silica N20 is German Yingchuang-Degusai.
The CAS number of the 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane is 83558-87-6.
The second aspect of the present embodiment provides a method for preparing a high temperature resistant perfluoroether rubber composition, comprising the steps of:
s1, setting the temperature of an internal mixer at 110 ℃, after the temperature of the internal mixer is stable, putting perfluoroether rubber raw rubber into a banburying chamber, banburying for 120 seconds until torque is stable, putting weighed white carbon black into the banburying chamber through a feed inlet at one time, putting down an upper top bolt, banburying for 5 minutes, lifting the upper top bolt, slowly adding the weighed carbon black into the banburying chamber, putting down the upper top bolt, continuously banburying for 5 minutes, discharging rubber, and controlling the rubber discharging temperature at 140 ℃; and (3) placing the master batch on an open mill with the roll spacing of 0.2mm, carrying out thin-pass triangular bag opening for 10 times, adjusting the roll spacing to 2.0mm, calendaring to obtain sheets, and standing the prepared master batch for more than 12 hours for later use.
S2, cooling water is introduced into an open mill, after the roll gap of the open mill is adjusted to be 1.0mm, the parked masterbatch is put into the open mill for calendaring and softening, the masterbatch is wrapped by rolls, cross-linking agents are gradually added for mixing, left and right rubber cuts are turned over for mixing, the high temperature resistant perfluoroether rubber composition is prepared after uniform mixing, the roll gap of the open mill is adjusted to be 0.2mm for 10 times, the roll gap of the open mill is continuously adjusted to be 1.0mm, calendaring and sheet discharging are carried out, and the open mill is parked for more than 12 hours for standby.
In a third aspect, the embodiment provides an application of a high-temperature-resistant perfluoroether rubber composition, the high-temperature-resistant perfluoroether rubber composition is placed in a mold, the mold is placed in a flat vulcanizing machine for one-stage compression molding vulcanization to obtain one-stage vulcanized product, the one-stage vulcanized product is parked for 12 hours, and then the one-stage vulcanized product is placed in an oven for two-stage vulcanization to prepare a sealing product, so that the sealing product is applied to the technical field of semiconductor industry processing.
The vulcanization temperature of the one-stage mould pressing vulcanization is 170 ℃, the vulcanization time is 10min, and the vulcanization pressure is 15MPa.
The processing technology of the secondary vulcanization is that the primary vulcanization product is placed in an oven, the temperature of the oven is uniformly heated to 200 ℃ from 25 ℃, the temperature is kept at 200 ℃ for 8 hours, the temperature is then increased to 290 ℃ according to the heating rate of 10 ℃ per hour, the temperature is kept at 290 ℃ for 12-24 hours, and then the temperature is slowly reduced to 25 ℃, and the sealing product is taken out for standby.
Example 5
The first aspect of the embodiment provides a high-temperature-resistant perfluoroether rubber composition, which comprises, by weight, 100 parts of perfluoroether rubber raw rubber, 20 parts of filler, 1 part of cross-linking agent and 0.5 part of processing aid.
theperfluoroetherrubberrawrubberisFFKM-A.
The filler is a composition of carbon black and white carbon black, and the mass ratio of the carbon black to the white carbon black is 3:1.
The carbon black is thermal cracking carbon black N990.
The white carbon black is gas phase white carbon black N20.
The cross-linking agent is 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane.
The processing aid is cerium oxide.
theFFKM-AhasamanufacturerofMitsuKagakuCo.
The manufacturer of the thermal decomposition carbon black N990 is cabot in the United states.
The manufacturer of the fumed silica N20 is German Yingchuang-Degusai.
The CAS number of the 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane is 83558-87-6.
The manufacturer of cerium oxide is Shanghai mao nano technology Co., ltd, and the grain size is 200nm.
The second aspect of the present embodiment provides a method for preparing a high temperature resistant perfluoroether rubber composition, comprising the steps of:
s1, setting the temperature of an internal mixer at 110 ℃, after the temperature of the internal mixer is stable, putting perfluoroether rubber raw rubber into a banburying chamber, banburying for 120 seconds until torque is stable, putting weighed white carbon black into the banburying chamber through a feed inlet at one time, putting down an upper top bolt, banburying for 5 minutes, lifting the upper top bolt, slowly adding the weighed carbon black into the banburying chamber, putting down the upper top bolt, continuously banburying for 5 minutes, discharging rubber, and controlling the rubber discharging temperature at 140 ℃; and (3) placing the master batch on an open mill with the roll spacing of 0.2mm, carrying out thin-pass triangular bag opening for 10 times, adjusting the roll spacing to 2.0mm, calendaring to obtain sheets, and standing the prepared master batch for more than 12 hours for later use.
S2, introducing cooling water into an open mill, regulating the roll gap of the open mill to be 1.0mm, putting the parked masterbatch into the open mill for calendering and softening, gradually adding a processing aid into a masterbatch roller for mixing, after the processing aid is completely mixed with sizing materials, respectively 5 times of left and right cutters for mixing uniformly, adding a cross-linking agent for mixing, turning left and right rubber cuts, regulating the roll gap of the open mill to be 0.2mm for 10 times, continuously regulating the roll gap of the open mill to be 1.0mm, calendering and discharging sheets, and standing for more than 12 hours for later use.
In a third aspect, the embodiment provides an application of a high-temperature-resistant perfluoroether rubber composition, the high-temperature-resistant perfluoroether rubber composition is placed in a mold, the mold is placed in a flat vulcanizing machine for one-stage compression molding vulcanization to obtain one-stage vulcanized product, the one-stage vulcanized product is parked for 12 hours, and then the one-stage vulcanized product is placed in an oven for two-stage vulcanization to prepare a sealing product, so that the sealing product is applied to the technical field of semiconductor industry processing.
The vulcanization temperature of the one-stage mould pressing vulcanization is 170 ℃, the vulcanization time is 10min, and the vulcanization pressure is 15MPa.
The processing technology of the secondary vulcanization is that the primary vulcanization product is placed in an oven, the temperature of the oven is uniformly heated to 200 ℃ from 25 ℃, the temperature is kept at 200 ℃ for 8 hours, the temperature is then increased to 290 ℃ according to the heating rate of 10 ℃ per hour, the temperature is kept at 290 ℃ for 12-24 hours, and then the temperature is slowly reduced to 25 ℃, and the sealing product is taken out for standby.
Example 6
The first aspect of the embodiment provides a high-temperature-resistant perfluoroether rubber composition, which comprises, by weight, 100 parts of perfluoroether rubber raw rubber, 20 parts of filler, 1 part of cross-linking agent and 1 part of processing aid.
theperfluoroetherrubberrawrubberisFFKM-A.
The filler is a composition of carbon black and white carbon black, and the mass ratio of the carbon black to the white carbon black is 3:1.
The carbon black is thermal cracking carbon black N990.
The white carbon black is gas phase white carbon black N20.
The cross-linking agent is 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane.
The processing aid is cerium oxide.
theFFKM-AhasamanufacturerofMitsuKagakuCo.
The manufacturer of the thermal decomposition carbon black N990 is cabot in the United states.
The manufacturer of the fumed silica N20 is German Yingchuang-Degusai.
The CAS number of the 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane is 83558-87-6.
The manufacturer of cerium oxide is Shanghai mao nano technology Co., ltd, and the grain size is 200nm.
The second aspect of the present embodiment provides a method for preparing a high temperature resistant perfluoroether rubber composition, comprising the steps of:
s1, setting the temperature of an internal mixer at 110 ℃, after the temperature of the internal mixer is stable, putting perfluoroether rubber raw rubber into a banburying chamber, banburying for 120 seconds until torque is stable, putting weighed white carbon black into the banburying chamber through a feed inlet at one time, putting down an upper top bolt, banburying for 5 minutes, lifting the upper top bolt, slowly adding the weighed carbon black into the banburying chamber, putting down the upper top bolt, continuously banburying for 5 minutes, discharging rubber, and controlling the rubber discharging temperature at 140 ℃; and (3) placing the master batch on an open mill with the roll spacing of 0.2mm, carrying out thin-pass triangular bag opening for 10 times, adjusting the roll spacing to 2.0mm, calendaring to obtain sheets, and standing the prepared master batch for more than 12 hours for later use.
S2, introducing cooling water into an open mill, regulating the roll gap of the open mill to be 1.0mm, putting the parked masterbatch into the open mill for calendering and softening, gradually adding a processing aid into a masterbatch roller for mixing, after the processing aid is completely mixed with sizing materials, respectively 5 times of left and right cutters for mixing uniformly, adding a cross-linking agent for mixing, turning left and right rubber cuts, regulating the roll gap of the open mill to be 0.2mm for 10 times, continuously regulating the roll gap of the open mill to be 1.0mm, calendering and discharging sheets, and standing for more than 12 hours for later use.
In a third aspect, the embodiment provides an application of a high-temperature-resistant perfluoroether rubber composition, the high-temperature-resistant perfluoroether rubber composition is placed in a mold, the mold is placed in a flat vulcanizing machine for one-stage compression molding vulcanization to obtain one-stage vulcanized product, the one-stage vulcanized product is parked for 12 hours, and then the one-stage vulcanized product is placed in an oven for two-stage vulcanization to prepare a sealing product, so that the sealing product is applied to the technical field of semiconductor industry processing.
The vulcanization temperature of the one-stage mould pressing vulcanization is 170 ℃, the vulcanization time is 10min, and the vulcanization pressure is 15MPa.
The processing technology of the secondary vulcanization is that the primary vulcanization product is placed in an oven, the temperature of the oven is uniformly heated to 200 ℃ from 25 ℃, the temperature is kept at 200 ℃ for 8 hours, the temperature is then increased to 290 ℃ according to the heating rate of 10 ℃ per hour, the temperature is kept at 290 ℃ for 12-24 hours, and then the temperature is slowly reduced to 25 ℃, and the sealing product is taken out for standby.
Example 7
The first aspect of the embodiment provides a high-temperature-resistant perfluoroether rubber composition, which comprises, by weight, 100 parts of perfluoroether rubber raw rubber, 20 parts of filler, 1 part of cross-linking agent and 2 parts of processing aid.
theperfluoroetherrubberrawrubberisFFKM-A.
The filler is a composition of carbon black and white carbon black, and the mass ratio of the carbon black to the white carbon black is 3:1.
The carbon black is thermal cracking carbon black N990.
The white carbon black is gas phase white carbon black N20.
The cross-linking agent is 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane.
The processing aid is cerium oxide.
theFFKM-AhasamanufacturerofMitsuKagakuCo.
The manufacturer of the thermal decomposition carbon black N990 is cabot in the United states.
The manufacturer of the fumed silica N20 is German Yingchuang-Degusai.
The CAS number of the 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane is 83558-87-6.
The manufacturer of cerium oxide is Shanghai mao nano technology Co., ltd, and the grain size is 200nm.
The second aspect of the present embodiment provides a method for preparing a high temperature resistant perfluoroether rubber composition, comprising the steps of:
s1, setting the temperature of an internal mixer at 110 ℃, after the temperature of the internal mixer is stable, putting perfluoroether rubber raw rubber into a banburying chamber, banburying for 120 seconds until torque is stable, putting weighed white carbon black into the banburying chamber through a feed inlet at one time, putting down an upper top bolt, banburying for 5 minutes, lifting the upper top bolt, slowly adding the weighed carbon black into the banburying chamber, putting down the upper top bolt, continuously banburying for 5 minutes, discharging rubber, and controlling the rubber discharging temperature at 140 ℃; and (3) placing the master batch on an open mill with the roll spacing of 0.2mm, carrying out thin-pass triangular bag opening for 10 times, adjusting the roll spacing to 2.0mm, calendaring to obtain sheets, and standing the prepared master batch for more than 12 hours for later use.
S2, introducing cooling water into an open mill, regulating the roll gap of the open mill to be 1.0mm, putting the parked masterbatch into the open mill for calendering and softening, gradually adding a processing aid into a masterbatch roller for mixing, after the processing aid is completely mixed with sizing materials, respectively 5 times of left and right cutters for mixing uniformly, adding a cross-linking agent for mixing, turning left and right rubber cuts, regulating the roll gap of the open mill to be 0.2mm for 10 times, continuously regulating the roll gap of the open mill to be 1.0mm, calendering and discharging sheets, and standing for more than 12 hours for later use.
In a third aspect, the embodiment provides an application of a high-temperature-resistant perfluoroether rubber composition, the high-temperature-resistant perfluoroether rubber composition is placed in a mold, the mold is placed in a flat vulcanizing machine for one-stage compression molding vulcanization to obtain one-stage vulcanized product, the one-stage vulcanized product is parked for 12 hours, and then the one-stage vulcanized product is placed in an oven for two-stage vulcanization to prepare a sealing product, so that the sealing product is applied to the technical field of semiconductor industry processing.
The vulcanization temperature of the one-stage mould pressing vulcanization is 170 ℃, the vulcanization time is 10min, and the vulcanization pressure is 15MPa.
The processing technology of the secondary vulcanization is that the primary vulcanization product is placed in an oven, the temperature of the oven is uniformly heated to 200 ℃ from 25 ℃, the temperature is kept at 200 ℃ for 8 hours, the temperature is then increased to 290 ℃ according to the heating rate of 10 ℃ per hour, the temperature is kept at 290 ℃ for 12-24 hours, and then the temperature is slowly reduced to 25 ℃, and the sealing product is taken out for standby.
Example 8
The first aspect of the embodiment provides a high-temperature-resistant perfluoroether rubber composition, which comprises, by weight, 100 parts of perfluoroether rubber raw rubber, 23 parts of filler and 2.5 parts of cross-linking agent.
The perfluoro ether rubber raw rubber is FFKM-B.
The filler is a composition of carbon black and white carbon black, and the mass ratio of the carbon black to the white carbon black is 20:3.
The carbon black is thermal cracking carbon black N990.
The white carbon black is gas phase white carbon black N20.
The cross-linking agent is a combination of triallyl isocyanurate and 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane, and the weight ratio of the triallyl isocyanurate to the 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane is 1.5:1.
The FFKM-B has a manufacturer of Mitsu Kagaku Co.
The manufacturer of the thermal decomposition carbon black N990 is cabot in the United states.
The manufacturer of the fumed silica N20 is German Yingchuang-Degusai.
The triallyl isocyanurate has a CAS number of 1025-15-6.
The CAS number of the 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane is 78-63-7.
The second aspect of the present embodiment provides a method for preparing a high temperature resistant perfluoroether rubber composition, comprising the steps of:
S1, setting the temperature of an internal mixer at 110 ℃, after the temperature of the internal mixer is stable, putting perfluoroether rubber raw rubber into a banburying chamber, banburying for 120 seconds until torque is stable, putting weighed white carbon black into the banburying chamber through a feed inlet at one time, putting down an upper top bolt, banburying for 5 minutes, lifting the upper top bolt, slowly adding the weighed carbon black into the banburying chamber, putting down the upper top bolt, continuously banburying for 5 minutes, discharging rubber, and controlling the rubber discharging temperature at 140 ℃; and (3) placing the master batch on an open mill with the roll spacing of 0.2mm, carrying out thin-pass triangular bag opening for 10 times, adjusting the roll spacing to 2.0mm, calendaring to obtain sheets, and standing the prepared master batch for more than 12 hours for later use.
S2, cooling water is introduced into an open mill, after the roll gap of the open mill is adjusted to be 1.0mm, the parked masterbatch is put into the open mill for calendaring and softening, the masterbatch is wrapped by rolls, cross-linking agents are gradually added for mixing, left and right rubber cuts are turned over for mixing, the high temperature resistant perfluoroether rubber composition is prepared after uniform mixing, the roll gap of the open mill is adjusted to be 0.2mm for 10 times, the roll gap of the open mill is continuously adjusted to be 1.0mm, calendaring and sheet discharging are carried out, and the open mill is parked for more than 12 hours for standby.
In a third aspect, the embodiment provides an application of a high-temperature-resistant perfluoroether rubber composition, the high-temperature-resistant perfluoroether rubber composition is placed in a mold, the mold is placed in a flat vulcanizing machine for one-stage compression molding vulcanization to obtain one-stage vulcanized product, the one-stage vulcanized product is parked for 12 hours, and then the one-stage vulcanized product is placed in an oven for two-stage vulcanization to prepare a sealing product, so that the sealing product is applied to the technical field of semiconductor industry processing.
The vulcanization temperature of the one-stage mould pressing vulcanization is 170 ℃, the vulcanization time is 10min, and the vulcanization pressure is 15MPa.
The processing technology of the secondary vulcanization is that the primary vulcanization product is placed in an oven, the temperature of the oven is uniformly heated to 200 ℃ from 25 ℃, the temperature is kept at 200 ℃ for 8 hours, the temperature is then increased to 290 ℃ according to the heating rate of 10 ℃ per hour, the temperature is kept at 290 ℃ for 12-24 hours, and then the temperature is slowly reduced to 25 ℃, and the sealing product is taken out for standby.
Example 9
The first aspect of the embodiment provides a high-temperature-resistant perfluoroether rubber composition, which comprises, by weight, 100 parts of perfluoroether rubber raw rubber, 23 parts of filler, 2.5 parts of cross-linking agent and 1 part of processing aid.
The perfluoro ether rubber raw rubber is FFKM-B.
The filler is a composition of carbon black and white carbon black, and the mass ratio of the carbon black to the white carbon black is 20:3.
The carbon black is thermal cracking carbon black N990.
The white carbon black is gas phase white carbon black N20.
The cross-linking agent is a combination of triallyl isocyanurate and 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane, and the weight ratio of the triallyl isocyanurate to the 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane is 1.5:1.
The processing aid is cerium oxide.
The FFKM-B has a manufacturer of Mitsu Kagaku Co.
The manufacturer of the thermal decomposition carbon black N990 is cabot in the United states.
The manufacturer of the fumed silica N20 is German Yingchuang-Degusai.
The manufacturer of cerium oxide is Shanghai mao nano technology Co., ltd, and the grain size is 200nm.
The triallyl isocyanurate has a CAS number of 1025-15-6.
The CAS number of the 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane is 78-63-7.
The second aspect of the present embodiment provides a method for preparing a high temperature resistant perfluoroether rubber composition, comprising the steps of:
s1, setting the temperature of an internal mixer at 110 ℃, after the temperature of the internal mixer is stable, putting perfluoroether rubber raw rubber into a banburying chamber, banburying for 120 seconds until torque is stable, putting weighed white carbon black into the banburying chamber through a feed inlet at one time, putting down an upper top bolt, banburying for 5 minutes, lifting the upper top bolt, slowly adding the weighed carbon black into the banburying chamber, putting down the upper top bolt, continuously banburying for 5 minutes, discharging rubber, and controlling the rubber discharging temperature at 140 ℃; and (3) placing the master batch on an open mill with the roll spacing of 0.2mm, carrying out thin-pass triangular bag opening for 10 times, adjusting the roll spacing to 2.0mm, calendaring to obtain sheets, and standing the prepared master batch for more than 12 hours for later use.
S2, introducing cooling water into an open mill, regulating the roll gap of the open mill to be 1.0mm, putting the parked masterbatch into the open mill for calendering and softening, gradually adding a processing aid into a masterbatch roller for mixing, after the processing aid is completely mixed with sizing materials, respectively 5 times of left and right cutters for mixing uniformly, adding a cross-linking agent for mixing, turning left and right rubber cuts, regulating the roll gap of the open mill to be 0.2mm for 10 times, continuously regulating the roll gap of the open mill to be 1.0mm, calendering and discharging sheets, and standing for more than 12 hours for later use.
In a third aspect, the embodiment provides an application of a high-temperature-resistant perfluoroether rubber composition, the high-temperature-resistant perfluoroether rubber composition is placed in a mold, the mold is placed in a flat vulcanizing machine for one-stage compression molding vulcanization to obtain one-stage vulcanized product, the one-stage vulcanized product is parked for 12 hours, and then the one-stage vulcanized product is placed in an oven for two-stage vulcanization to prepare a sealing product, so that the sealing product is applied to the technical field of semiconductor industry processing.
The vulcanization temperature of the one-stage mould pressing vulcanization is 170 ℃, the vulcanization time is 10min, and the vulcanization pressure is 15MPa.
The processing technology of the secondary vulcanization is that the primary vulcanization product is placed in an oven, the temperature of the oven is uniformly heated to 200 ℃ from 25 ℃, the temperature is kept at 200 ℃ for 8 hours, the temperature is then increased to 290 ℃ according to the heating rate of 10 ℃ per hour, the temperature is kept at 290 ℃ for 12-24 hours, and then the temperature is slowly reduced to 25 ℃, and the sealing product is taken out for standby.
Example 10
The first aspect of the embodiment provides a high-temperature-resistant perfluoroether rubber composition, which comprises, by weight, 100 parts of perfluoroether rubber raw rubber, 20 parts of filler and 1 part of cross-linking agent.
theperfluoroetherrubberrawrubberisFFKM-A.
The cross-linking agent is 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane.
The filler is carbon black.
The carbon black is thermal cracking carbon black N990.
theFFKM-AhasamanufacturerofMitsuKagakuCo.
The manufacturer of the thermal decomposition carbon black N990 is cabot in the United states.
The CAS number of the 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane is 83558-87-6.
The second aspect of the present embodiment provides a method for preparing a high temperature resistant perfluoroether rubber composition, comprising the steps of:
s1, setting the temperature of an internal mixer at 110 ℃, after the temperature of the internal mixer is stable, putting perfluoroether rubber raw rubber into a banburying chamber, banburying for 120s until torque is stable, putting filler into the banburying chamber through a feed inlet, putting down an upper plug, banburying for 5min to obtain master batch, and discharging the obtained master batch at 140 ℃; and (3) placing the master batch on an open mill with the roll spacing of 0.2mm, carrying out thin-pass triangular bag opening for 10 times, adjusting the roll spacing to 2.0mm, calendaring to obtain sheets, and standing the prepared master batch for more than 12 hours for later use.
S2, cooling water is introduced into an open mill, after the roll gap of the open mill is adjusted to be 1.0mm, the parked masterbatch is put into the open mill for calendaring and softening, the masterbatch is wrapped by rolls, cross-linking agents are gradually added for mixing, left and right rubber cuts are turned over for mixing, the high temperature resistant perfluoroether rubber composition is prepared after uniform mixing, the roll gap of the open mill is adjusted to be 0.2mm for 10 times, the roll gap of the open mill is continuously adjusted to be 1.0mm, calendaring and sheet discharging are carried out, and the open mill is parked for more than 12 hours for standby.
In a third aspect, the embodiment provides an application of a high-temperature-resistant perfluoroether rubber composition, the high-temperature-resistant perfluoroether rubber composition is placed in a mold, the mold is placed in a flat vulcanizing machine for one-stage compression molding vulcanization to obtain one-stage vulcanized product, the one-stage vulcanized product is parked for 12 hours, and then the one-stage vulcanized product is placed in an oven for two-stage vulcanization to prepare a sealing product, so that the sealing product is applied to the technical field of semiconductor industry processing.
The vulcanization temperature of the one-stage mould pressing vulcanization is 170 ℃, the vulcanization time is 10min, and the vulcanization pressure is 15MPa.
The processing technology of the secondary vulcanization is that the primary vulcanization product is placed in an oven, the temperature of the oven is uniformly heated to 200 ℃ from 25 ℃, the temperature is kept at 200 ℃ for 8 hours, the temperature is then increased to 290 ℃ according to the heating rate of 10 ℃ per hour, the temperature is kept at 290 ℃ for 12-24 hours, and then the temperature is slowly reduced to 25 ℃, and the sealing product is taken out for standby.
The sealing products prepared in examples 1-10 were O-ring seals.
Performance testing
1. Appearance surface evaluation
The O-shaped sealing rings prepared in examples 1-10 were observed under the same magnification of a microscope, and whether the surfaces of the O-shaped sealing rings were flat or not and whether protrusions and pits were present or not were recorded, and the test results are shown in Table 1. The external appearance of the O-shaped sealing ring prepared in the embodiment 3 is shown in fig. 1, and the external appearance of the O-shaped sealing ring prepared in the embodiment 10 is shown in fig. 2.
2. Mechanical property test
The high temperature-resistant perfluoroether rubber compositions prepared in examples 1-10 are prepared according to the processing technology of one-stage compression molding vulcanization and two-stage vulcanization in the application method of the high temperature-resistant perfluoroether rubber composition, test standard samples are prepared after vulcanization, the test hardness, tensile strength and elongation at break are tested, 10 test samples in each example are respectively tested during the test, the maximum value and the minimum value are removed, the average value is taken, and the test results are shown in table 1.
Hardness testing was performed according to GB/T531.1-2008 method for testing indentation hardness of vulcanized rubber or thermoplastic rubber part 1 Shore durometer (Shore hardness).
The tensile strength and elongation at break were tested according to GB/T528-2009 test for tensile stress and strain properties of vulcanized rubber or thermoplastic rubber.
3. Thermal performance testing
Taking the high temperature-resistant perfluoroether rubber compositions prepared in examples 3, 4, 6, 8, 9 and 10, preparing a test standard sample piece according to a processing technology of one-stage mould pressing vulcanization and two-stage vulcanization in an application method of the high temperature-resistant perfluoroether rubber composition, placing the standard sample piece in a thermal aging box at 300 ℃ for 70 hours, taking out the test sample piece, standing at 25 ℃ for 24 hours, and then testing the mass change rate, the hardness change rate, the tensile strength change rate and the elongation at break change rate, wherein 10 test samples of each example are respectively tested, removing the maximum value and the minimum value, taking an average value, and the test results are shown in Table 2; and the aging coefficients of the tests performed in examples 3, 8, and 10 were calculated, and the results are shown in Table 2.
The mass change rate (%) is the ratio of the mass difference between the standard sample before and after heat aging to the mass of the standard sample before heat aging.
The hardness change rate (%) is the ratio of the difference in hardness between the standard sample before heat aging and after heat aging to the hardness of the standard sample before heat aging.
The tensile strength change rate (%) is the ratio of the tensile strength difference between the standard sample before heat aging and after heat aging to the tensile strength of the standard sample before heat aging.
The elongation at break change (%) is the ratio of the difference in elongation at break between the standard sample before heat aging and after heat aging to the elongation at break of the standard sample before heat aging.
The aging coefficient defines the ratio of the performance value of the sample after aging to the performance value before aging. The typical values of the properties before and after aging are usually tensile products (equal to the product of tensile strength and elongation at break), expressed as:
σ1, σ2: tensile strength of test specimen before and after aging, MPa
η1, η2: elongation at break of test specimen before and after aging%
When the aging coefficient is higher than 0.85, the samples after aging have use value, and the higher the value is, the better the aging resistance is.
4. Plasma resistance test
Treatment of gas O using plasma 2 The mass loss rate, O, of the perfluororubber products with surface tack free prepared in examples 1 to 5 after 60 minutes was tested at a temperature of 100℃and a power of 800w 2 The vacuum degree set at the time of the test as the plasma processing gas was 15mtorr, and the gas flow rates of the plasma processing gas were all set to 80sccm; the sealing products prepared in examples 4, 6, 8 and 9 were taken to obtain 10 sealing products, the maximum value and the minimum value were removed, the average value was taken, and the test results are shown in Table 2.
TABLE 1
As can be seen from fig. 1 and 2, the O-ring of fig. 1 has a flat surface without protrusions and depressions; the O-ring in fig. 2 has an uneven surface with protrusions and depressions. It can be seen that when the high temperature resistant perfluoroether rubber composition does not contain the processing aid cerium oxide, the prepared O-shaped sealing ring has uneven surface and has the problems of protrusions and pits; when the high temperature resistant perfluoroether rubber composition contains the processing aid cerium oxide, the prepared O-shaped sealing ring has a flat surface and no protrusions or pits.
As can be seen from the test data in table 1, the high temperature resistant perfluoroether rubber compositions prepared by changing the amount of the crosslinking agent or the amount of the filler in examples 1 and 2 have no significant difference in physical and mechanical properties, and also have the problem of surface defects, so that the problem that the surface defects cannot be improved by changing the amount of the crosslinking agent or the amount of the filler can be seen; it can be seen from the test results of example 4 that changing the kind of filler also does not improve the surface defects of the product; as can be seen from examples 3 and 10, the physical and mechanical properties of the product were substantially unchanged or slightly reduced after 1 part of cerium oxide was added in example 3, and the surface defects of the product were significantly improved and the surface protrusions and pits were effectively improved when the product was observed under a microscope.
Example 5 used 0.5 parts cerium oxide, example 6 used 1 part cerium oxide; in example 4, no cerium oxide was used, and it can be seen from the test data in Table 1 that the physical and mechanical properties of the product were substantially unchanged or slightly reduced after 0.5 part of cerium oxide and 1 part of cerium oxide were added to the high temperature resistant perfluoroether rubber composition, while the surface defects thereof were effectively improved; however, when 2 parts of cerium oxide was used as in example 7, the physical and mechanical properties of the product prepared from the high temperature-resistant perfluoroether rubber composition were greatly lowered.
TABLE 2
As can be seen from the test results in Table 2, when 1 part of cerium oxide is added in example 3, the physical and mechanical properties of the product are basically unchanged or slightly reduced, but the aging coefficient is obviously increased, which indicates that the high-temperature aging resistance is greatly improved.
Examples 8 and 9 used a peroxide system as the crosslinking system, and the physical and mechanical properties were reduced but still far above the lower limit of use after addition of cerium oxide, while the aging coefficient of example 8 was already below 0.85, indicating that the product was not useful. However, the aging coefficient of example 9 is much higher than 0.85, and the high-temperature aging resistance is significantly improved. From this, it can be seen that the high temperature aging resistance after cerium oxide addition is effectively improved. Meanwhile, after cerium oxide is added in the embodiment 6 and the embodiment 9, the quality loss of the antioxidant plasma is improved to a certain extent compared with that of the antioxidant plasma without cerium oxide.
Claims (10)
1. The high temperature resistant perfluoroether rubber composition is characterized in that the preparation raw materials comprise 80-120 parts by weight of perfluoroether rubber raw rubber, 15-25 parts by weight of filler, 1.0-2.5 parts by weight of cross-linking agent and 0.5-1.5 parts by weight of processing aid;
the processing aid is cerium oxide.
2. The high temperature resistant perfluoroether rubber composition according to claim 1, wherein said perfluoroether rubber raw rubber comprises tetrafluoroethylene-perfluoroalkyl vinyl ether-vulcanizing point monomer polymer.
3. The high temperature resistant perfluoroether rubber composition according to claim 1, wherein the processing aid has a particle size of 300nm or less.
4. The high temperature resistant perfluoroether rubber composition according to claim 1, wherein the filler is one or both of carbon black and white carbon black.
5. The high temperature resistant perfluoroether rubber composition according to claim 1, wherein the crosslinking agent is selected from one or more of 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane, triallyl isocyanurate, 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane.
6. The method for producing a high temperature resistant perfluoroether rubber composition according to any one of claims 1 to 5, comprising the steps of:
S1, adding perfluoroether rubber raw rubber into an internal mixer for banburying, adding filler for banburying to obtain master batch, carrying out thin-pass triangular bag opening on the master batch on an open mill, adjusting the roll gap of the open mill for calendaring and sheet discharging, and standing the prepared master batch for more than 12 hours for later use;
s2, putting the parked masterbatch into an open mill for calendering and softening, wrapping a roll of the masterbatch, adding a processing aid for mixing, adding a cross-linking agent for mixing after mixing uniformly, and regulating the roll gap of the open mill for calendering and discharging sheets for standby after standing for more than 12 hours.
7. The method for preparing a high temperature resistant perfluoroether rubber composition according to claim 6, wherein in S2, cooling water is introduced into an open mill, and after the roll gap of the open mill is adjusted to 0.6-1.0mm, the parked masterbatch is put into the open mill for calendering and softening.
8. The use of the high temperature-resistant perfluoroether rubber composition according to any one of claims 1 to 5, wherein the high temperature-resistant perfluoroether rubber composition is used in the technical field of semiconductor industry processing by preparing a sealing product through one-stage compression vulcanization and two-stage vulcanization.
9. The use of the high temperature resistant perfluoroether rubber composition according to claim 8, wherein the one-stage compression vulcanization has a vulcanization temperature of 150℃to 190℃and a vulcanization time of 5 to 15 minutes and a vulcanization pressure of
10-20MPa。
10. The use of the high temperature resistant perfluoroether rubber composition according to claim 8, wherein the processing technology of the secondary vulcanization is that the primary vulcanization product is placed in an oven, the temperature of the oven is uniformly raised from 25 ℃ to 200 ℃, the temperature is kept at 200 ℃ for 5-10h, the temperature is raised to 290 ℃ according to the heating rate of 5-15 ℃ per hour, the temperature is kept at 290 ℃ for 12-24h, the temperature is lowered to 25 ℃, and the sealing product is taken out for standby.
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| CN117304625A (en) * | 2023-09-19 | 2023-12-29 | 上海芯密科技有限公司 | Fluororubber composition capable of effectively reducing adhesion with metal and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001164115A (en) * | 1999-12-06 | 2001-06-19 | Shin Etsu Chem Co Ltd | Fluororubber composition |
| CN101307165A (en) * | 2007-05-18 | 2008-11-19 | 上海道氟化工科技有限公司 | Heat resisting fluororubber composition and sulfidization molding products thereof |
| CN104356562A (en) * | 2013-10-30 | 2015-02-18 | 东莞市长安东阳光铝业研发有限公司 | Fluororubber rubber compound and preparation method thereof |
| WO2023004585A1 (en) * | 2021-07-27 | 2023-02-02 | Solvay Specialty Polymers Italy S.P.A. | Fluoroelastomer composition |
-
2023
- 2023-07-10 CN CN202310844028.2A patent/CN116694005A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001164115A (en) * | 1999-12-06 | 2001-06-19 | Shin Etsu Chem Co Ltd | Fluororubber composition |
| CN101307165A (en) * | 2007-05-18 | 2008-11-19 | 上海道氟化工科技有限公司 | Heat resisting fluororubber composition and sulfidization molding products thereof |
| CN104356562A (en) * | 2013-10-30 | 2015-02-18 | 东莞市长安东阳光铝业研发有限公司 | Fluororubber rubber compound and preparation method thereof |
| WO2023004585A1 (en) * | 2021-07-27 | 2023-02-02 | Solvay Specialty Polymers Italy S.P.A. | Fluoroelastomer composition |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117304625A (en) * | 2023-09-19 | 2023-12-29 | 上海芯密科技有限公司 | Fluororubber composition capable of effectively reducing adhesion with metal and preparation method thereof |
| CN117304625B (en) * | 2023-09-19 | 2024-05-17 | 上海芯密科技有限公司 | Fluororubber composition capable of effectively reducing adhesion with metal and preparation method thereof |
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