CN113045308A - Ceramic-plastic composite and preparation method and application thereof - Google Patents
Ceramic-plastic composite and preparation method and application thereof Download PDFInfo
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- CN113045308A CN113045308A CN201911399390.3A CN201911399390A CN113045308A CN 113045308 A CN113045308 A CN 113045308A CN 201911399390 A CN201911399390 A CN 201911399390A CN 113045308 A CN113045308 A CN 113045308A
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- ceramic
- plastic
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- zirconia
- plastic composite
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- 239000002131 composite material Substances 0.000 title claims abstract description 80
- 229920003023 plastic Polymers 0.000 title claims abstract description 80
- 239000004033 plastic Substances 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 116
- 239000000919 ceramic Substances 0.000 claims abstract description 84
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 22
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011787 zinc oxide Substances 0.000 claims abstract description 7
- 239000002002 slurry Substances 0.000 claims description 54
- 239000000843 powder Substances 0.000 claims description 52
- 239000011159 matrix material Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 17
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000002270 dispersing agent Substances 0.000 claims description 12
- 239000011347 resin Substances 0.000 claims description 11
- 229920005989 resin Polymers 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000011230 binding agent Substances 0.000 claims description 10
- 238000007788 roughening Methods 0.000 claims description 10
- -1 polybutylene terephthalate Polymers 0.000 claims description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 229920002125 Sokalan® Polymers 0.000 claims description 8
- 239000003365 glass fiber Substances 0.000 claims description 8
- 238000001746 injection moulding Methods 0.000 claims description 8
- 239000004584 polyacrylic acid Substances 0.000 claims description 8
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 8
- 238000012986 modification Methods 0.000 claims description 7
- 230000004048 modification Effects 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims description 5
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 239000004952 Polyamide Substances 0.000 claims description 5
- 239000004734 Polyphenylene sulfide Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 5
- 239000004917 carbon fiber Substances 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- 239000002557 mineral fiber Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 5
- 229920002647 polyamide Polymers 0.000 claims description 5
- 229920000069 polyphenylene sulfide Polymers 0.000 claims description 5
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 229920002678 cellulose Polymers 0.000 claims description 4
- 239000001913 cellulose Substances 0.000 claims description 4
- 229910052731 fluorine Inorganic materials 0.000 claims description 4
- 239000011737 fluorine Substances 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 239000011698 potassium fluoride Substances 0.000 claims description 2
- 235000003270 potassium fluoride Nutrition 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 239000011775 sodium fluoride Substances 0.000 claims description 2
- 235000013024 sodium fluoride Nutrition 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 description 14
- 238000012360 testing method Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 7
- 238000005469 granulation Methods 0.000 description 6
- 230000003179 granulation Effects 0.000 description 6
- 239000002612 dispersion medium Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 238000005238 degreasing Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 238000007373 indentation Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
Classifications
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/14—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/486—Fine ceramics
- C04B35/488—Composites
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
- C04B41/48—Macromolecular compounds
- C04B41/488—Other macromolecular compounds obtained otherwise than by reactions only involving unsaturated carbon-to-carbon bonds
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/53—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
- C04B41/5338—Etching
- C04B41/5353—Wet etching, e.g. with etchants dissolved in organic solvents
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/82—Coating or impregnation with organic materials
- C04B41/83—Macromolecular compounds
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/91—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics involving the removal of part of the materials of the treated articles, e.g. etching
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- Polymers & Plastics (AREA)
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- Injection Moulding Of Plastics Or The Like (AREA)
Abstract
The invention relates to the field of ceramic-plastic composite materials, and discloses a ceramic-plastic composite body and a preparation method and application thereof. A ceramic-plastic composite comprising: the composite zirconia ceramic comprises 90-99 wt% of zirconia and 1-10 wt% of at least one auxiliary agent selected from zinc oxide, silicon oxide, aluminum oxide and titanium oxide based on the total weight of the composite zirconia ceramic. The bonding strength of the ceramic and the plastic in the ceramic-plastic composite can reach more than 25 MPa.
Description
Technical Field
The invention relates to the field of ceramic-plastic composite materials, in particular to a ceramic-plastic composite body and a preparation method and application thereof.
Background
The zirconia ceramic is an inorganic nonmetal multiphase crystalline material, has the appearance characteristics of being mild and moist like jade, excellent mechanical properties, wear resistance, high temperature resistance, corrosion resistance, high insulation, biocompatibility and good optical properties, but has the defects of high dielectric constant, high density and high hardness, so that the zirconia ceramic is difficult to directly process and post-process. In the prior art, the problem is solved by adopting a combined body of zirconia ceramics and plastics, but the bonding force between the zirconia ceramics and the plastics is insufficient due to the difference of the material characteristics of the zirconia ceramics and the plastics, so that the stability of the combined body is influenced.
Disclosure of Invention
The invention aims to overcome the problem of bonding between ceramics and plastics in a ceramic-plastic composite body, and provides a ceramic-plastic composite body, and a preparation method and application thereof.
In order to achieve the above object, a first aspect of the present invention provides a ceramic plastic composite body comprising: the composite zirconia ceramic comprises 90-99 wt% of zirconia and 1-10 wt% of at least one auxiliary agent selected from zinc oxide, silicon oxide, aluminum oxide and titanium oxide based on the total weight of the composite zirconia ceramic.
Preferably, the bonding strength between the composite zirconia ceramic and the plastic is 25MPa or more, preferably 30MPa or more, and more preferably 35 to 45 MPa.
The second aspect of the present invention provides a method for preparing a ceramic-plastic composite, comprising:
(1) preparing powder slurry containing zirconium oxide and an auxiliary agent, wherein the auxiliary agent is selected from at least one of zinc oxide, silicon oxide, aluminum oxide and titanium oxide;
(2) carrying out modification treatment on the powder slurry and a dispersant to obtain modified slurry;
(3) mixing the modified slurry with a binder, and granulating the obtained mixture to obtain composite zirconia ceramic powder;
(4) forming and sintering the ceramic powder to obtain a ceramic matrix;
(5) carrying out surface roughening treatment on the ceramic matrix to form a contact surface; injection molding a plastic material onto the contact surface to form a ceramic-plastic composite;
based on the total amount of the powder slurry, the content of zirconia in the powder slurry is 90-99 wt%, and the content of the auxiliary agent is 1-10 wt%.
In a third aspect, the present invention provides a ceramic-plastic composite obtained by the preparation method of the present invention.
The invention provides an application of the ceramic-plastic composite body in communication electronic products.
Through the technical scheme, the invention provides the ceramic-plastic composite body formed by combining the composite zirconia ceramic containing the auxiliary agent with the plastic material in a specific content, wherein the bonding strength of the ceramic and the plastic can reach more than 20 MPa.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The present invention provides in a first aspect a ceramic-plastic composite body comprising: the composite zirconia ceramic comprises 90-99 wt% of zirconia and 1-10 wt% of at least one auxiliary agent selected from zinc oxide, silicon oxide, aluminum oxide and titanium oxide based on the total weight of the composite zirconia ceramic.
In some embodiments of the invention, the provided composite zirconia ceramics are employed to achieve improved bond strength with plastics. Preferably, the composite zirconia ceramic contains 94-98 wt% zirconia and 2-6 wt% of the auxiliary agent.
In some embodiments of the present invention, a plastic that can be combined with the zirconia ceramic may be selected. Preferably, the plastic comprises a resin and a modifying material; the resin is selected from at least one of polyphenylene sulfide, polybutylene terephthalate and polyamide, and the modifying material is selected from at least one of glass fiber, carbon fiber and mineral fiber.
The ceramic-plastic composite provided by the invention has good bonding strength between ceramics and plastics. In some embodiments of the invention, the bond strength can be determined by pulling through a universal tester. Preferably, the bonding strength between the composite zirconia ceramic and the plastic is 25MPa or more, preferably 30MPa or more, and more preferably 35 to 45 MPa.
The second aspect of the present invention provides a method for preparing a ceramic-plastic composite, comprising:
(1) preparing powder slurry containing zirconium oxide and an auxiliary agent, wherein the auxiliary agent is selected from at least one of zinc oxide, silicon oxide, aluminum oxide and titanium oxide;
(2) carrying out modification treatment on the powder slurry and a dispersant to obtain modified slurry;
(3) mixing the modified slurry with a binder, and granulating the obtained mixture to obtain composite zirconia ceramic powder;
(4) forming and sintering the ceramic powder to obtain a ceramic matrix;
(5) carrying out surface roughening treatment on the ceramic matrix to form a contact surface; injection molding a plastic material onto the contact surface to form a ceramic-plastic composite;
based on the total amount of the powder slurry, the content of zirconia in the powder slurry is 90-99 wt%, and the content of the auxiliary agent is 1-10 wt%.
In some embodiments of the present invention, preferably, the content of the zirconia in the powder slurry is 94 to 98 wt%, and the content of the auxiliary agent is 2 to 6 wt%. The optimization of each component in the powder slurry can ensure that the contact surface formed by the ceramic matrix obtained by compounding a plurality of oxides with zirconia after the surface roughening treatment has an improved more proper contact angle, thereby being beneficial to enhancing the bonding strength of ceramics and plastics in the finally obtained ceramic-plastic composite.
In the step (1) of the production method provided by the present invention, water may be used as a dispersion medium in the preparation of the powder slurry. The solid content of the powder slurry may be 25 to 50 wt%, preferably 30 to 40 wt%.
In the step (2) of the present invention, the dispersant may modify the slurry. Preferably, the process of the modification treatment comprises: and ball milling and dispersing the powder slurry and a dispersing agent for 0.5-10h, and then sanding for 1-10 h.
In some embodiments of the present invention, preferably, the dispersant is selected from one or more of sodium dodecylbenzenesulfonate, cetyltrimethylammonium bromide, polyacrylic acid, and polyethylene glycol; preferably, the amount of the dispersant is 0.1-5 wt% of the powder slurry. Wherein the polyacrylic acid may have an average molecular weight of 500-. The dispersants are all commercially available.
The addition of the binder in the step (3) of the invention is beneficial to obtaining the composite zirconia ceramic powder through subsequent granulation. Preferably, the binder is selected from one or more of polyvinyl alcohol, cellulose and polyacrylic acid; preferably, the binder is used in an amount of 2 to 6 wt% of the modified slurry. Further, the polyvinyl alcohol may be 5000-20000 in average molecular weight. The cellulose may be 5000-. The polyacrylic acid may have an average molecular weight of 5000-. The binders are all commercially available.
In the present invention, the granulation may be spray granulation.
In the step (4) of the present invention, the molding may be performed by dry pressing and isostatic pressing the powder. The sintering process can be carried out at 1450-1490 ℃ for 2-4 h.
In step (5) of the present invention, surface treatment of the ceramic base is performed to bond with the plastic material. The process of surface roughening treatment comprises the following steps: soaking the surface of the ceramic matrix in an acid solution of at least one of phosphoric acid, hydrochloric acid, nitric acid and sulfuric acid for 10s-20h at 25-70 ℃, then soaking in hydrofluoric acid or a mixed solution of a fluorine-containing substance and one or more of phosphoric acid, hydrochloric acid, nitric acid and sulfuric acid for 10s-20h, and then washing with water; preferably, the fluorine-containing species comprises one or more of ammonium fluoride, potassium fluoride, sodium fluoride and ammonium bifluoride. The surface of the ceramic matrix is treated by acid liquor, and then etched and formed holes are further formed on the surface of the ceramic matrix by acid solution containing fluoride ions.
In some embodiments of the invention, preferably, the plastic comprises a resin and a modifying material; the resin is selected from at least one of polyphenylene sulfide, polybutylene terephthalate and polyamide, and the modifying material is selected from at least one of glass fiber, carbon fiber and mineral fiber. Among them, polyphenylene sulfide, polybutylene terephthalate, polyamide, glass fiber, carbon fiber and mineral fiber are not particularly limited and are commercially available.
In some embodiments of the present invention, preferably, the plastic contains 40 to 80 wt% of the resin and 20 to 60 wt% of the modifying material, based on the total amount of the plastic.
In some embodiments of the present invention, the plastic may be formed on the contact surface by injection molding, so as to achieve bonding with the ceramic substrate. The injection molding conditions may include a pressure of 80 to 140MPa and a mold temperature of 60 to 150 ℃.
In a third aspect, the present invention provides a ceramic-plastic composite obtained by the preparation method of the present invention. The ceramic mass composite may have the features described above.
The invention provides an application of the ceramic-plastic composite body in communication electronic products. The method can be applied to wristwatches, mobile phones and notebook computers.
The present invention will be described in detail below by way of examples. In the following examples and comparative examples,
bonding strength test of ceramic plastic composite: the test conditions were: processing the ceramic-plastic composite into 3mm multiplied by 12mm multiplied by 40mm sample strips by adopting a universal testing machine, and the speed is as follows: 5 mm/min.
And (3) measuring the hardness of the ceramic: a hardness meter and an indentation method (a diamond pressure head, a force of 10kg and a pressure test time of 15 s);
determination of ceramic fracture toughness Kic toughness: a hardness meter and an indentation method (a diamond pressure head, a force of 10kg and a pressure test time of 15 s);
the oxide powder, dispersant and binder are all commercially available.
Example 1
According to the composition shown in table 1, powder slurry containing zirconia and an auxiliary agent is prepared by taking water as a dispersion medium, and the solid content of the powder slurry is 30 wt%; then, adding polyacrylic acid (with the average molecular weight of 1000) accounting for 0.1 wt% of the powder slurry into the powder slurry, performing ball milling dispersion for 5 hours, and then performing sand milling for 6 hours to obtain modified slurry;
adding 6 wt% of polyacrylic acid (with average molecular weight of 10000) in the modified slurry into the modified slurry, mixing, and performing spray granulation on the obtained mixture to obtain the composite zirconia ceramic powder.
And (3) carrying out static pressure forming on the powder, and then sintering for 2h at 1490 ℃ to obtain the ceramic matrix.
Carrying out surface roughening treatment on the ceramic matrix: the surface of the ceramic substrate was immersed in 10 wt% hydrochloric acid at 40 ℃ for 2 hours, then immersed in a mixed solution of 30 wt% ammonium bifluoride and 50 wt% hydrochloric acid at 60 ℃ for 600 seconds, and then the ceramic substrate was washed with water to obtain a contact surface.
A plastic containing 60 wt% of polybutylene terephthalate and 40 wt% of glass fiber was molded on the contact surface by injection molding to obtain a composite zirconia ceramic-plastic composite. The composite was subjected to performance testing and the results are shown in table 1.
Example 2
According to the composition shown in table 1, powder slurry containing zirconia and an auxiliary agent is prepared by taking water as a dispersion medium, and the solid content of the powder slurry is 40 wt%; adding 1 wt% of hexadecyl trimethyl ammonium bromide of the powder slurry into the powder slurry, performing ball milling dispersion for 1h, and performing sand milling for 4h to obtain modified slurry;
adding 5 wt% of cellulose (with average molecular weight of 10000) in the modified slurry into the modified slurry, mixing, and performing spray granulation on the obtained mixture to obtain the composite zirconia ceramic powder.
And (3) carrying out static pressure forming on the powder, and then sintering at 1470 ℃ for 2h to obtain the ceramic matrix.
Carrying out surface roughening treatment on the ceramic matrix: the surface of the ceramic substrate was immersed in 30 wt% sulfuric acid at room temperature for 600 seconds, then immersed in a mixed solution of 10 wt% ammonium bifluoride and 20 wt% sulfuric acid at 40 ℃ for 6000 seconds, and then the ceramic substrate was washed with water to obtain a contact surface.
And molding plastic containing 80 wt% of polybutylene terephthalate and 20 wt% of glass fiber to the contact surface through injection molding to obtain the composite zirconia ceramic-plastic composite. The composite was subjected to performance testing and the results are shown in table 1.
Example 3
According to the composition shown in table 1, preparing powder slurry containing zirconium oxide and an auxiliary agent by using water as a dispersion medium, wherein the solid content of the powder slurry is 35 wt%, then adding 2 wt% of sodium dodecyl sulfate of the powder slurry, according to the composition shown in table 1, preparing the powder slurry containing zirconium oxide and the auxiliary agent by using water as the dispersion medium, wherein the solid content of the powder slurry is subjected to ball milling dispersion for 2 hours, and then performing sand milling for 6 hours to obtain modified slurry;
adding 5 wt% of polyvinyl alcohol (with the average molecular weight of 5000) in the modified slurry into the modified slurry, mixing, and performing spray granulation on the obtained mixture to obtain the composite zirconia ceramic powder.
And carrying out static pressure forming on the powder, and then sintering at 1450 ℃ for 4h to obtain the ceramic matrix.
Carrying out surface roughening treatment on the ceramic matrix: the surface of the ceramic substrate was immersed in 25 wt% nitric acid at 25 ℃ for 30min, and then immersed in 20 wt% hydrofluoric acid at 25 ℃ for 40 min.
A plastic containing 70 wt% of polybutylene terephthalate and 30 wt% of glass fiber was molded on the contact surface by injection molding to obtain a composite zirconia ceramic-plastic composite. The composite was subjected to performance testing and the results are shown in table 1.
Examples 4 to 16
A composite zirconia ceramic-plastic composite was prepared by following the procedure of example 1 except that the composition of the powder slurry was replaced with the composition shown in Table 1. The composites were subjected to performance testing and the results are shown in table 1.
Example 17
The process of example 2 was followed, except that the ceramic matrix was subjected to a surface roughening treatment: the surface of the ceramic substrate was immersed in a mixed solution of ammonium bifluoride at a concentration of 10 wt% and sulfuric acid at 20 wt% at 40 ℃ for 6000 s. The composite was subjected to performance testing and the results are shown in table 1.
Comparative example 1
A composite zirconia ceramic-plastic composite was prepared by following the procedure of example 1 except that the composition of the powder slurry was replaced with the composition shown in Table 1. The composites were subjected to performance testing and the results are shown in table 1.
Comparative example 2
A zirconia ceramic substrate was prepared according to the composition shown in table 1, and a clean surface was obtained after mechanical polishing, degreasing and degreasing.
The zirconia ceramic matrix is put into acid solution of 20 percent sulfuric acid, corroded for 2400s at the temperature of 80 ℃, washed clean by water and dried. Forming a nano-scale roughened surface on the zirconia ceramic matrix.
The zirconia ceramic matrix with the roughened surface is placed in an injection mold, and the same plastic as in example 2 is injection molded to the roughened surface by the method of example 2, so as to obtain the composite zirconia ceramic plastic composite. The composite was subjected to performance testing and the results are shown in table 1.
Comparative example 3
A zirconia ceramic substrate was prepared according to the composition shown in table 1, and a clean surface was obtained after mechanical polishing, degreasing and degreasing.
Putting the zirconia ceramic matrix into 10 wt% hydrofluoric acid solution, corroding the zirconia ceramic matrix for 300s at 65 ℃, washing with water and drying. Forming a nano-scale roughened surface on the zirconia ceramic matrix.
The zirconia ceramic matrix with the roughened surface is placed in an injection mold, and the same plastic as in example 2 is injection molded to the roughened surface by the method of example 2, so as to obtain the composite zirconia ceramic plastic composite. The composite was subjected to performance testing and the results are shown in table 1.
TABLE 1
TABLE 1 (continuation)
TABLE 1 (continuation)
TABLE 1 (continuation)
TABLE 1 (continuation)
As can be seen from the results of the above examples, comparative examples, and table 1, the ceramic plastic composite provided by the present invention has high bonding strength between the ceramic substrate and the plastic; examples 1 to 14 further preferably contain an auxiliary agent in an amount to further improve the bonding strength between the ceramic substrate and the plastic in the ceramic-plastic composite provided; it can be seen from examples 2 and 17 that the bonding strength between the ceramic substrate and the plastic can be improved by treating the surface of the ceramic substrate with the preferred two-step process. The additive content of comparative example 1 was too high and comparative examples 2 and 3 were free of additive, and the bonding strength of the ceramic substrate and the plastic was significantly reduced.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (12)
1. A ceramic-plastic composite comprising: the composite zirconia ceramic comprises 90-99 wt% of zirconia and 1-10 wt% of at least one auxiliary agent selected from zinc oxide, silicon oxide, aluminum oxide and titanium oxide based on the total weight of the composite zirconia ceramic.
2. The ceramic-plastic composite of claim 1, wherein the composite zirconia ceramic contains 94-98 wt% zirconia and 2-6 wt% of the adjunct.
3. The ceramic-plastic composite of claim 1 or 2, wherein the plastic comprises a resin and a modifying material; the resin is selected from at least one of polyphenylene sulfide, polybutylene terephthalate and polyamide, and the modifying material is selected from at least one of glass fiber, carbon fiber and mineral fiber;
preferably, the plastic contains 40 to 80 wt% of the resin and 20 to 60 wt% of the modifying material, based on the total amount of the plastic.
4. The ceramic-plastic composite body according to any one of claims 1 to 3, wherein the bonding strength between the composite zirconia ceramic and the plastic is 25MPa or more, preferably 30MPa or more, and more preferably 35 to 45 MPa.
5. A method of making a ceramic-plastic composite comprising:
(1) preparing powder slurry containing zirconium oxide and an auxiliary agent, wherein the auxiliary agent is selected from at least one of zinc oxide, silicon oxide, aluminum oxide and titanium oxide;
(2) carrying out modification treatment on the powder slurry and a dispersant to obtain modified slurry;
(3) mixing the modified slurry with a binder, and granulating the obtained mixture to obtain composite zirconia ceramic powder;
(4) forming and sintering the ceramic powder to obtain a ceramic matrix;
(5) carrying out surface roughening treatment on the ceramic matrix to form a contact surface; injection molding a plastic material onto the contact surface to form a ceramic-plastic composite;
based on the total amount of the powder slurry, the content of zirconia in the powder slurry is 90-99 wt%, and the content of the auxiliary agent is 1-10 wt%.
6. The preparation method according to claim 5, wherein the content of zirconia in the powder slurry is 94-98 wt%, and the content of the auxiliary agent is 2-6 wt%.
7. The production method according to claim 5 or 6, wherein, in the step (2), the dispersant is selected from one or more of sodium dodecylbenzenesulfonate, cetyltrimethylammonium bromide, polyacrylic acid, and polyethylene glycol; preferably, the amount of the dispersant is 0.1-5 wt% of the powder slurry;
preferably, the process of the modification treatment comprises: and ball milling and dispersing the powder slurry and a dispersing agent for 0.5-10h, and then sanding for 1-10 h.
8. The production method according to any one of claims 5 to 7, wherein in the step (3), the binder is selected from one or more of polyvinyl alcohol, cellulose and polyacrylic acid; preferably, the amount of the binder is 2-6 wt% of the powder slurry.
9. The production method according to any one of claims 5 to 8, wherein the surface roughening treatment in step (5) comprises: soaking the surface of the ceramic matrix in an acid solution of at least one of phosphoric acid, hydrochloric acid, nitric acid and sulfuric acid for 10s-20h at 25-70 ℃, then soaking in hydrofluoric acid or a mixed solution of a fluorine-containing substance and one or more of phosphoric acid, hydrochloric acid, nitric acid and sulfuric acid for 10s-20h, and then washing with water;
preferably, the fluorine-containing species comprises one or more of ammonium fluoride, potassium fluoride, sodium fluoride and ammonium bifluoride.
10. The production method according to any one of claims 5 to 9, wherein the plastic comprises a resin and a modifying material; the resin is selected from at least one of polyphenylene sulfide, polybutylene terephthalate and polyamide, and the modifying material is selected from at least one of glass fiber, carbon fiber and mineral fiber;
preferably, the plastic contains 40 to 80 wt% of the resin and 20 to 60 wt% of the modifying material, based on the total amount of the plastic.
11. A ceramic-plastic composite obtained by the method of any one of claims 5 to 10.
12. Use of a ceramic-plastic composite according to any one of claims 1 to 4 and 11 in telecommunications electronics.
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