CN117304624A - Composition, method and sealed product for preparing vacuum sealing material - Google Patents
Composition, method and sealed product for preparing vacuum sealing material Download PDFInfo
- Publication number
- CN117304624A CN117304624A CN202210709221.0A CN202210709221A CN117304624A CN 117304624 A CN117304624 A CN 117304624A CN 202210709221 A CN202210709221 A CN 202210709221A CN 117304624 A CN117304624 A CN 117304624A
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- CN
- China
- Prior art keywords
- fluororubber
- tetrafluoroethylene
- composition
- vinylidene fluoride
- initial monomer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000000203 mixture Substances 0.000 title claims abstract description 22
- 239000003566 sealing material Substances 0.000 title claims abstract description 16
- 229920001973 fluoroelastomer Polymers 0.000 claims abstract description 43
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- 239000000654 additive Substances 0.000 claims abstract description 19
- 230000000996 additive effect Effects 0.000 claims abstract description 18
- 229920001971 elastomer Polymers 0.000 claims abstract description 17
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 10
- 239000011737 fluorine Substances 0.000 claims abstract description 10
- 238000007789 sealing Methods 0.000 claims abstract description 10
- 239000000178 monomer Substances 0.000 claims description 25
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 22
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 21
- -1 polytrifluoroethylene, tetrafluoroethylene Polymers 0.000 claims description 19
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 15
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 11
- 229920001577 copolymer Polymers 0.000 claims description 9
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 9
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 9
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical class C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims description 6
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 claims description 6
- 229920006169 Perfluoroelastomer Polymers 0.000 claims description 5
- 150000004985 diamines Chemical class 0.000 claims description 4
- 239000004973 liquid crystal related substance Substances 0.000 claims description 4
- 229920005862 polyol Polymers 0.000 claims description 4
- 150000003077 polyols Chemical class 0.000 claims description 4
- 239000004065 semiconductor Substances 0.000 claims description 4
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 3
- PYGXAGIECVVIOZ-UHFFFAOYSA-N Dibutyl decanedioate Chemical compound CCCCOC(=O)CCCCCCCCC(=O)OCCCC PYGXAGIECVVIOZ-UHFFFAOYSA-N 0.000 claims description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 3
- 239000005977 Ethylene Substances 0.000 claims description 3
- 239000006057 Non-nutritive feed additive Substances 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 239000008029 phthalate plasticizer Substances 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- 238000009472 formulation Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 description 7
- 239000002131 composite material Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- 230000003749 cleanliness Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 210000002381 plasma Anatomy 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000001020 plasma etching Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- WRXCBRHBHGNNQA-UHFFFAOYSA-N (2,4-dichlorobenzoyl) 2,4-dichlorobenzenecarboperoxoate Chemical compound ClC1=CC(Cl)=CC=C1C(=O)OOC(=O)C1=CC=C(Cl)C=C1Cl WRXCBRHBHGNNQA-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 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 description 1
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical class C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 description 1
- 125000004203 4-hydroxyphenyl group Chemical group [H]OC1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 102100027446 Acetylserotonin O-methyltransferase Human genes 0.000 description 1
- 229930185605 Bisphenol Natural products 0.000 description 1
- 101000936718 Homo sapiens Acetylserotonin O-methyltransferase Proteins 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 150000001454 anthracenes Chemical class 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
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000002790 naphthalenes Chemical class 0.000 description 1
- 239000012766 organic filler Substances 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 125000000864 peroxy group Chemical group O(O*)* 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920002493 poly(chlorotrifluoroethylene) Polymers 0.000 description 1
- 239000005023 polychlorotrifluoroethylene (PCTFE) polymer Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/16—Homopolymers or copolymers or vinylidene fluoride
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1339—Gaskets; Spacers; Sealing of cells
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Nonlinear Science (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mathematical Physics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a composition, a method and a sealing product for preparing a vacuum sealing material, which belong to the field of rubber preparation, wherein the composition for preparing the vacuum sealing material comprises the following components: at least 50% to not more than 95% by weight of a fluororubber; at least 3% to no more than 50% by weight of fluorothermoplastic additive; at least 2% to not more than 5% by weight of a vulcanizing agent, wherein the fluorine content of the fluorine-containing rubber is greater than 69%. By the treatment scheme disclosed by the invention, the preparation cost is remarkably reduced and the production timeliness is improved.
Description
Technical Field
The invention relates to the field of rubber preparation, in particular to a composition, a method and a sealing product for preparing a vacuum sealing material.
Background
With the improvement of the technology in the semiconductor and liquid crystal panel industries, the requirements on the cleaning degree in the process reaction cavity are continuously improved. Rubber products are used as important sealing parts in the process reaction cavity, and for rubberThe content and the cleanliness of the etched precipitate of the glue body are also more and more severely required. Whereas conventional fluororubbers are generally filled with inorganic metal oxides, e.g. carbon black, baSO 4 (barium sulfate), siO 2 (silica), tiO 2 (titanium dioxide) and the like. However, when these rubber sealing materials are in the bombardment state of high-energy plasmas, a certain amount of etching precipitates are generated, the products in the process reaction in the cavity are polluted, and the process with high cleanliness requirements cannot meet the requirements of the process on the internal environment of the cavity, so that the conventional vacuum sealing materials cannot meet the use requirements of customers at present.
Disclosure of Invention
Accordingly, in order to overcome the above-described disadvantages of the prior art, the present invention provides a composition, method and sealed product for preparing a vacuum sealing material.
In order to achieve the above object, the present invention provides a composition for preparing a vacuum sealing material, comprising: at least 50% to not more than 95% by weight of a fluororubber; at least 3% to no more than 50% by weight of fluorothermoplastic additive; at least 2% to not more than 5% by weight of a vulcanizing agent, wherein the fluorine content of the fluorine-containing rubber is greater than 69%.
In one embodiment, the fluororubber is at least one of fluororubber system with initial monomer containing vinylidene fluoride, perfluoroelastomer rubber without carbon-hydrogen bond, fluororubber obtained by copolymerizing propylene and tetrafluoroethylene with initial monomer.
In one embodiment, the initial monomer comprises vinylidene fluoride and the fluororubber system is any one of the following: the initial monomer is a fluororubber system of vinylidene fluoride and hexafluoropropylene, and the molar ratio is 45% -85%:15% -55%; the initial monomer is fluororubber system of vinylidene fluoride, tetrafluoroethylene and hexafluoropropylene, the mole ratio is 35% -85%:0-30%:15% -45%; the initial monomer is fluororubber system of vinylidene fluoride, tetrafluoroethylene and fluorinated vinyl ether, the mol ratio is 50% -80%:0-20%:5-50%; the initial monomer is fluororubber system of vinylidene fluoride, tetrafluoroethylene and propylene, the mol ratio is 35% -85%:0-30%:0-20%; the initial monomer is fluororubber system of vinylidene fluoride, tetrafluoroethylene, ethylene and fluorinated vinyl ether, the mol ratio is 35% -85%:0-30%:0-20%:5-20%.
In one embodiment, the molar ratio of the propylene to the tetrafluoroethylene is 20% to 30%.
In one embodiment, the fluorothermoplastic additive is at least one of polytrifluoroethylene, tetrafluoroethylene and hexafluoropropylene copolymer, polytetrafluoroethylene, tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer, tetrafluoroethylene and perfluoromethyl vinyl ether copolymer, PPVE modified polytetrafluoroethylene.
In one embodiment, the vulcanizing agent is at least one of a diamine curative, a peroxide sulfide, and a polyol-based vulcanizing agent.
In one embodiment, the composition further comprises a processing aid that is at least one of a phthalate plasticizer, dioctyl phthalate, dibutyl sebacate, zinc stearate, sodium stearate, polyethylene wax.
A method of making a vacuum sealing material comprising: fully mixing the fluororubber and the fluorothermoplastic additive in the composition proportion at 50-320 ℃; adding vulcanizing agent below 60deg.C, mixing, and pressing to obtain final product.
The sealing product is applied to a semiconductor or liquid crystal panel and is characterized by being prepared by the method.
Compared with the prior art, the invention has the advantages that: the physical mixing method of the fluorothermoplastic additive is directly adopted, so that the preparation cost can be obviously reduced, the production timeliness can be improved, even if inorganic metal oxide is added in the preparation process, the fluorothermoplastic additive can avoid etching precipitates even if the prepared product is in the bombardment state of high-energy plasma, the service life and cleanliness of the prepared vacuum sealing component are improved, the wear resistance of the product is obviously improved, and the product has excellent performances in the aspects of plasma etching resistance and the like.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present disclosure, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present disclosure, and other drawings may be obtained according to these drawings without inventive effort to a person of ordinary skill in the art.
Fig. 1 is a flow chart of a method for preparing a vacuum sealing material according to an embodiment of the present invention.
Detailed Description
Embodiments of the present disclosure are described in detail below with reference to the accompanying drawings.
Other advantages and effects of the present disclosure will become readily apparent to those skilled in the art from the following disclosure, which describes embodiments of the present disclosure by way of specific examples. It will be apparent that the described embodiments are merely some, but not all embodiments of the present disclosure. The disclosure may be embodied or practiced in other different specific embodiments, and details within the subject specification may be modified or changed from various points of view and applications without departing from the spirit of the disclosure. It should be noted that the following embodiments and features in the embodiments may be combined with each other without conflict. All other embodiments, which can be made by one of ordinary skill in the art without inventive effort, based on the embodiments in this disclosure are intended to be within the scope of this disclosure.
It is noted that various aspects of the embodiments are described below within the scope of the following claims. It should be apparent that the aspects described herein may be embodied in a wide variety of forms and that any specific structure and/or function described herein is merely illustrative. Based on the present disclosure, one skilled in the art will appreciate that one aspect described herein may be implemented independently of any other aspect, and that two or more of these aspects may be combined in various ways. For example, an apparatus may be implemented and/or a method practiced using any number of the aspects set forth herein. In addition, such apparatus may be implemented and/or such methods practiced using other structure and/or functionality in addition to one or more of the aspects set forth herein.
It should also be noted that the illustrations provided in the following embodiments merely illustrate the basic concepts of the disclosure by way of illustration, and only the components related to the disclosure are shown in the drawings and are not drawn according to the number, shape and size of the components in actual implementation, and the form, number and proportion of the components in actual implementation may be arbitrarily changed, and the layout of the components may be more complicated.
In addition, in the following description, specific details are provided in order to provide a thorough understanding of the examples. However, it will be understood by those skilled in the art that the aspects may be practiced without these specific details.
As shown in fig. 1, an embodiment of the present disclosure provides a method for preparing a vacuum sealing material, including the steps of:
thoroughly mixing the fluororubber and fluorothermoplastic additive at 50 ℃ to 320 ℃ by plastication;
adding vulcanizing agent below 60deg.C, mixing, and pressing to obtain final product. The finished product can be subsequently prepared into gaskets of hoses, pipes, O-rings and other cross-sectional shapes according to the requirements. The spacer may be applied to a semiconductor or liquid crystal panel.
The above-described process may be carried out using any known blending plastication technique, including continuous, batch, and semi-continuous techniques. Specific implementation equipment may include, but is not limited to, internal mixers, twin rolls, triple rolls, homogenizers, high speed dispersers, single screws, twin screws, and the like.
Embodiments of the present disclosure also provide a composition for preparing a vacuum sealing material, including: at least 50% to not more than 95% by weight of a fluororubber; at least 3% to no more than 50% by weight of fluorothermoplastic additive; at least 2% to not more than 5% by weight of a vulcanizing agent, wherein the fluorine content of the fluorine-containing rubber is greater than 69%.
According to the method, a physical mixing method of the fluorothermoplastic additive is directly adopted, so that the preparation cost can be obviously reduced, the production timeliness can be improved, even if inorganic metal oxides are added in the preparation process, the fluorothermoplastic additive can avoid etching precipitates even if the prepared product is in a high-energy plasma bombardment state, the service life and cleanliness of the prepared vacuum sealing component are improved, the wear resistance of the product is obviously improved, and the product is excellent in plasma etching resistance and the like.
In one embodiment, the fluororubber is at least one of a fluororubber system in which the initial monomer comprises vinylidene fluoride, a perfluoroelastomer rubber containing no carbon-hydrogen bonds, and a fluororubber obtained by copolymerizing propylene and tetrafluoroethylene with the initial monomer.
In one embodiment, the initial monomer comprises vinylidene fluoride in a fluororubber system of any one of the following:
the initial monomer is a fluororubber system of vinylidene fluoride and hexafluoropropylene, and the molar ratio is 45% -85%:15% -55%;
the initial monomer is fluororubber system of vinylidene fluoride, tetrafluoroethylene and hexafluoropropylene, the mole ratio is 35% -85%:0-30%:15% -45%;
the initial monomer is fluororubber system of vinylidene fluoride, tetrafluoroethylene and fluorinated vinyl ether, the mol ratio is 50% -80%:0-20%:5-50%;
the initial monomer is fluororubber system of vinylidene fluoride, tetrafluoroethylene and propylene, the mol ratio is 35% -85%:0-30%:0-20%;
the initial monomer is fluororubber system of vinylidene fluoride, tetrafluoroethylene, ethylene and fluorinated vinyl ether, the mol ratio is 35% -85%:0-30%:0-20%:5-20.
In one embodiment, the hydrogen atoms on all carbon atoms in the perfluoroelastomer rubber are replaced with fluorine atoms, having a structure that is extremely stable to high temperatures and chemicals. The perfluoroelastomer rubber may be DuPontSeries products, or Daikin and Ausimont as the perfluoro products of the supplier.
In one embodiment, the molar ratio of propylene to tetrafluoroethylene is 20% to 30%.
In some embodiments, at least 5% to no more than 50% by weight of the fluororesin additive may be used, based on the total mass of the incorporated components. More preferably, at least 5%, 10%, 15%, 20% or 25% of the fluororesin additive is used. In one embodiment, the fluorothermoplastic additive is at least one of PCTFE (polytrifluoroethylene), FEP (tetrafluoroethylene and hexafluoropropylene copolymer), PTFE (polytetrafluoroethylene), PFA (tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer; fusible polytetrafluoroethylene), MFA (tetrafluoroethylene and perfluoromethyl vinyl ether copolymer), TFM (PPVE modified polytetrafluoroethylene). TFM is formed by copolymerizing TFE, mainly comprising PTFE, with PPVE monomer added in an amount of 0.1% by mass during suspension polymerization. The fluorothermoplastic additive may be mixed with the fluororubber as solid particles, powder or emulsion.
In some embodiments, at least 1% and no more than 5% by weight of vulcanizing agent based on the total mass of the incorporated components may be used. In some embodiments, at least 0.8%, 1%, 1.5%, 1.65%, or 2% of the vulcanizing agent is used. In one embodiment, the vulcanizing agent is at least one of a diamine curative, a peroxide sulfide, and a polyol-based vulcanizing agent. The diamine curing agent may be Dia-1. The peroxide curing agent may be an organic peroxide-containing agent such as 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane, 2, 4-dichloro benzoyl peroxide, di-t-butyl peroxide, and the like. The polyol vulcanizing agent may include an aromatic polyhydroxy compound, an aliphatic polyhydroxy compound, a phenol resin, or the like. The aromatic polyhydroxy compounds may be di-, tri-, tetra-hydroxy benzenes, naphthalenes and anthracenes, and bisphenols, and the aliphatic polyhydroxy compounds may be fluorine-based aliphatic diols such as 1, 6-tetrahydro-octafluoro diol and 2- (4-alkylphenyl) -2 (4-hydroxyphenyl).
In one embodiment, the composition further comprises a processing aid that is at least one of a phthalate plasticizer, dioctyl phthalate, dibutyl sebacate, zinc stearate, sodium stearate, polyethylene wax.
In one embodiment, the composition further comprises a cure accelerator and/or filler, which may include, but is not limited to, a divalent metal oxide or hydroxide, such as Ca (OH) 2 (calcium hydroxide), mgO (magnesium oxide), caO (calcium oxide), znO (zinc oxide), and the like. Fillers include, but are not limited to, inorganic and organic fillers such as barium sulfate, zinc sulfide, carbon black, titanium dioxide, clay, silica, talc, and the like.
Example 1
Fluororubber: threo P959
Fluorothermoplastic additives: tianshi wax powder (PTFE-1005)
Other auxiliary agents: carbon black N990 (Kenkobo), cross-linking agent TAIC (Ackesu), vulcanizing agent Bispenta-101 (Ackesu).
Examples one to three
Preparation step of fluorine-containing composite component sample
Step one: and (5) mixing the components. The preparation of the Send bar P930 (peroxy) ternary fluororubber was carried out by adding it to an internal mixer, raising the temperature to 80℃and plasticating it for 5 minutes, and then raising the temperature of the internal mixer to 120 ℃. Gradually adding the PTFE emulsion into an internal mixer, and lowering the top bolt for 30-60 minutes, wherein the rotor speed of the internal mixer is 40r/min.
Step two: and (5) adding an auxiliary agent. And then taking out the mixed PTFE ternary fluororubber composite material, plasticating for 5 minutes on a double-roller wheel, gradually adding a cross-linking agent and a vulcanizing agent, starting water circulation after the cross-linking agent and the vulcanizing agent are added, and then continuously mixing the PTFE ternary fluororubber composite material on the double-roller wheel for 30 minutes to obtain a sheet.
Step three: and (5) preforming. The PTFE ternary fluororubber composite material from which the sheet is obtained is put into a preforming machine, and a rubber strip is extruded in the preforming machine at 80 degrees.
Step four: and (5) post-treating the rubber strip. After the rubber strip is parked for 16 hours, the rubber strip is cut into corresponding sizes, after the flat vulcanizing machine is vulcanized at 170 degrees for 300 seconds, the finished product is taken out to correct burrs, and then the finished product is baked at 230 degrees for 4 hours in a vacuum oven.
And when the finished product obtained after the steps are finished, making a relevant physical property test report of PTFE ternary fluororubber on a universal testing machine, performing a simulation test of an actual use environment in a plasma environment, observing the powder discharge condition of a sample, and calculating the weight reduction rate.
Among them, the difference between examples one to three is the weight fraction difference of the added PTFE emulsion (fluorothermoplastic additive) in the whole composition system.
Physical property test Standard of sample
The vacuum sealing composite material containing fluororubber is molded and used for measuring physical properties after a post-treatment process, and the sample is restored to a room temperature state before testing.
Tensile strength, elongation at break, as determined by ASMT D412C, the samples used were prepared according to the example standards.
Hardness was measured according to ASTM 2240 using a VICTOR LX-A-Y type durometer.
An O-ring having a circular cross-sectional area was prepared from the compounded sample mold and subjected to a compression set test according to the method of ASTM-D395 (B).
Test conditions are simulated by the actual use environment of the sample
As can be seen from the comparison of the data, the sealing material and the prepared sealing ring product have excellent actual measurement performance and comprehensive performance compared with the prior comparative example.
The foregoing is merely specific embodiments of the disclosure, but the protection scope of the disclosure is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the disclosure are intended to be covered by the protection scope of the disclosure. Therefore, the protection scope of the present disclosure shall be subject to the protection scope of the claims.
Claims (9)
1. A composition for preparing a vacuum sealing material, comprising:
at least 50% to not more than 95% by weight of a fluororubber;
at least 3% to no more than 50% by weight of fluorothermoplastic additive;
at least 2% to not more than 5% by weight of a vulcanizing agent,
wherein the fluorine content of the fluorine-containing rubber is more than 69%.
2. The composition of claim 1, wherein the fluororubber is at least one of a fluororubber system wherein the initial monomer comprises vinylidene fluoride, a perfluoroelastomer rubber having no carbon-hydrogen bond, and a fluororubber obtained by copolymerizing propylene and tetrafluoroethylene using the initial monomer.
3. The composition of claim 2, wherein the fluororubber system of the initial monomer comprising vinylidene fluoride is any of the following:
the initial monomer is a fluororubber system of vinylidene fluoride and hexafluoropropylene, and the molar ratio is 45% -85%:15-55%;
the initial monomer is fluororubber system of vinylidene fluoride, tetrafluoroethylene and hexafluoropropylene, the mole ratio is 35% -85%:0-30%:15% -45%;
the initial monomer is fluororubber system of vinylidene fluoride, tetrafluoroethylene and fluorinated vinyl ether, the mol ratio is 50% -80%:0-20%:5% -50%;
the initial monomer is fluororubber system of vinylidene fluoride, tetrafluoroethylene and propylene, the mol ratio is 35% -85%:0-30%:0-20%;
the initial monomer is fluororubber system of vinylidene fluoride, tetrafluoroethylene, ethylene and fluorinated vinyl ether, the mol ratio is 35% -85%:0-30%:0-20%:5% -20%.
4. The composition of claim 2, wherein the molar ratio of propylene to tetrafluoroethylene is 20% to 30%.
5. The composition of claim 1 wherein the fluorothermoplastic additive is at least one of polytrifluoroethylene, tetrafluoroethylene and hexafluoropropylene copolymers, polytetrafluoroethylene, tetrafluoroethylene-perfluoroalkyl vinyl ether copolymers, tetrafluoroethylene and perfluoromethyl vinyl ether copolymers, PPVE modified polytetrafluoroethylene.
6. The composition of claim 1, wherein the vulcanizing agent is at least one of a diamine curative, a peroxide sulfide, and a polyol-based vulcanizing agent.
7. The composition of claim 1, further comprising a processing aid that is at least one of a phthalate plasticizer, dioctyl phthalate, dibutyl sebacate, zinc stearate, sodium stearate, polyethylene wax.
8. A method for preparing a vacuum sealing material, comprising:
thoroughly mixing the fluororubber and fluorothermoplastic additive according to the composition formulation of any one of claims 1 to 7 at 50 ℃ to 320 ℃;
adding vulcanizing agent below 60deg.C, mixing, and pressing to obtain final product.
9. A sealing product applied to a semiconductor or liquid crystal panel, which is characterized in that the sealing product prepared by the method of claim 8.
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