CN116514569A - Ceramic metallization slurry, preparation method and application thereof - Google Patents
Ceramic metallization slurry, preparation method and application thereof Download PDFInfo
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- CN116514569A CN116514569A CN202310347032.8A CN202310347032A CN116514569A CN 116514569 A CN116514569 A CN 116514569A CN 202310347032 A CN202310347032 A CN 202310347032A CN 116514569 A CN116514569 A CN 116514569A
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- ceramic
- powder
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- metallized
- slurry
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- 239000000919 ceramic Substances 0.000 title claims abstract description 139
- 239000002002 slurry Substances 0.000 title claims abstract description 62
- 238000001465 metallisation Methods 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000000853 adhesive Substances 0.000 claims abstract description 70
- 230000001070 adhesive effect Effects 0.000 claims abstract description 70
- 239000000843 powder Substances 0.000 claims abstract description 53
- 229910052751 metal Inorganic materials 0.000 claims abstract description 45
- 239000002184 metal Substances 0.000 claims abstract description 45
- 239000000839 emulsion Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 18
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims description 21
- 239000011248 coating agent Substances 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 12
- 150000003839 salts Chemical class 0.000 claims description 12
- 238000007650 screen-printing Methods 0.000 claims description 10
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 229920002845 Poly(methacrylic acid) Polymers 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 229920002125 Sokalan® Polymers 0.000 claims description 6
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 6
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 6
- 229920001971 elastomer Polymers 0.000 claims description 6
- 229920002401 polyacrylamide Polymers 0.000 claims description 6
- 239000004584 polyacrylic acid Substances 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 239000005060 rubber Substances 0.000 claims description 6
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 6
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 6
- 229920001909 styrene-acrylic polymer Polymers 0.000 claims description 6
- 229920003169 water-soluble polymer Polymers 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- -1 acrylic ester Chemical class 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 238000003618 dip coating Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 238000004544 sputter deposition Methods 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims 1
- 239000011572 manganese Substances 0.000 claims 1
- 229910052750 molybdenum Inorganic materials 0.000 claims 1
- 239000011733 molybdenum Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 14
- 238000005265 energy consumption Methods 0.000 abstract description 8
- 239000002904 solvent Substances 0.000 abstract description 8
- 239000010410 layer Substances 0.000 description 33
- 239000011230 binding agent Substances 0.000 description 20
- PCEXQRKSUSSDFT-UHFFFAOYSA-N [Mn].[Mo] Chemical compound [Mn].[Mo] PCEXQRKSUSSDFT-UHFFFAOYSA-N 0.000 description 18
- 238000007639 printing Methods 0.000 description 10
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 9
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 9
- 229940116411 terpineol Drugs 0.000 description 9
- 238000007665 sagging Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000001000 micrograph Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 229910000679 solder Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000002344 surface layer Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000004630 mental health Effects 0.000 description 2
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- 230000004048 modification Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
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- 238000004062 sedimentation Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- PSGCQDPCAWOCSH-UHFFFAOYSA-N (4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl) prop-2-enoate Chemical compound C1CC2(C)C(OC(=O)C=C)CC1C2(C)C PSGCQDPCAWOCSH-UHFFFAOYSA-N 0.000 description 1
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 description 1
- WDQMWEYDKDCEHT-UHFFFAOYSA-N 2-ethylhexyl 2-methylprop-2-enoate Chemical compound CCCCC(CC)COC(=O)C(C)=C WDQMWEYDKDCEHT-UHFFFAOYSA-N 0.000 description 1
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 229910000914 Mn alloy Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- IAXXETNIOYFMLW-COPLHBTASA-N [(1s,3s,4s)-4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl] 2-methylprop-2-enoate Chemical compound C1C[C@]2(C)[C@@H](OC(=O)C(=C)C)C[C@H]1C2(C)C IAXXETNIOYFMLW-COPLHBTASA-N 0.000 description 1
- NEIHULKJZQTQKJ-UHFFFAOYSA-N [Cu].[Ag] Chemical compound [Cu].[Ag] NEIHULKJZQTQKJ-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- OIWOHHBRDFKZNC-UHFFFAOYSA-N cyclohexyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1CCCCC1 OIWOHHBRDFKZNC-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229940119545 isobornyl methacrylate Drugs 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229940065472 octyl acrylate Drugs 0.000 description 1
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 238000012858 packaging process Methods 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
- C04B37/023—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
- C04B37/028—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles by means of an interlayer consisting of an organic adhesive, e.g. phenol resin or pitch
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Parts Printed On Printed Circuit Boards (AREA)
Abstract
The invention discloses ceramic metalized slurry, a preparation method and application thereof, and the ceramic metalized slurry comprises the following components: ceramic metal powder and aqueous adhesive emulsion, wherein the mass ratio of the ceramic metal powder to the aqueous adhesive emulsion is (1-2.5): 1, the ceramic metal powder comprises the following components in parts by weight: 66-84 parts of molybdenum powder, 7-16 parts of manganese powder and 8-18 parts of porcelain powder; the aqueous adhesive emulsion comprises an aqueous adhesive and water, wherein the mass ratio of the aqueous adhesive to the water is (0.5-1.5): 1. The ceramic metallization slurry provided by the invention only uses water as a solvent, is environment-friendly, can be well coated at the ambient temperature of 5-60 ℃, does not need to have specific requirements on the production environment, reduces energy consumption and cost, and improves the consistency of products.
Description
Technical Field
The invention relates to the technical field of ceramic packaging, in particular to ceramic metalized slurry, and a preparation method and application thereof.
Background
Oxide ceramics or nitride ceramics are widely used for packaging electronic current and power components. In the packaging process, the ceramic surface generally needs to be metallized first, most of the prior art is to carry out molybdenum-manganese metallization on the ceramic surface first, and then, the ceramic surface is welded with a metal piece by adopting solder after being coated with nickel. Wherein, the molybdenum-manganese metallization is obtained by preparing molybdenum-manganese slurry in terpineol solvent and then carrying out high-temperature treatment. The process mainly has the following problems: the use of a large amount of terpineol not only increases the production cost of the slurry, but also has a special smell, which can seriously affect the health of production workers. In addition, because terpineol is thicker, the slurry is prepared at the temperature of 60-100 ℃ and the printing is performed at about 60 ℃ so as to ensure that the slurry has certain fluidity and can be leveled on the surface of the ceramic.
Disclosure of Invention
The invention provides ceramic metallization slurry, a preparation method and application thereof, and aims to solve the technical problems that the conventional molybdenum-manganese metallization process has high temperature requirements and is not environment-friendly.
According to one aspect of the present invention, there is provided a ceramic metallizing slurry comprising the following components: ceramic metal powder and aqueous adhesive emulsion, wherein the mass ratio of the ceramic metal powder to the aqueous adhesive emulsion is (1-2.5): 1,
the ceramic metal powder comprises the following components in parts by weight: 66-84 parts of molybdenum powder, 7-16 parts of manganese powder and 8-18 parts of porcelain powder; the aqueous adhesive emulsion comprises an aqueous adhesive and water, wherein the mass ratio of the aqueous adhesive to the water is (0.5-1.5) 1, and the aqueous adhesive is one or a combination of more of acrylic ester aqueous adhesives, styrene-butadiene rubber emulsion aqueous adhesives, styrene-acrylic rubber emulsion aqueous adhesives or aqueous adhesives prepared from water-soluble polymers such as polyacrylic acid and salts thereof, polymethacrylic acid and salts thereof, sodium carboxymethyl cellulose, polyacrylamide and polyvinyl alcohol.
Further, the particle size of the molybdenum powder and the manganese powder is 0.1-5 microns.
According to another aspect of the present invention, there is also provided a method for preparing the above ceramic metallization paste, comprising: mixing molybdenum powder, manganese powder and porcelain powder, adding water-based adhesive and water, and stirring at normal temperature until the viscosity of the slurry is 2000-4500 mPa.s.
According to yet another aspect of the present invention, there is also provided a metallized ceramic article comprising a ceramic article and a metallized layer overlying the ceramic article, the metallized layer being made of the ceramic metallization paste described above.
Further, the composition of the ceramic powder in the ceramic metallization paste is consistent with or close to the composition of the ceramic part.
Further, the porcelain powder comprises Al 2 O 3 、SiO 2 CaO, mgO and MnO 2 One or more combinations thereof.
Further, the ceramic metallization slurry is coated on the surface of the ceramic part in a screen printing, point coating, spray coating, roll coating, dip coating or sputtering mode, and a metallization layer is obtained after drying and sintering.
Further, the coating temperature is 5 to 60 ℃.
Further, the drying temperature is 40-80 ℃ and the drying time is 20-60min.
Further, the sintering temperature is 1480-1580 ℃ and the heat preservation time is 60-90min.
The invention has the following beneficial effects:
the slurry provided by the invention only uses water as a solvent, the water is colorless and odorless, and the slurry does not harm the physical and mental health of production workers in the drying process, so that the slurry is environment-friendly and the solvent cost is reduced. In addition, as the physical and chemical properties such as viscosity and the like of the water are less influenced by temperature compared with terpineol, the slurry preparation can be carried out at normal temperature, and the slurry can be well coated at the environmental temperature of 5-60 ℃ (such as the printing temperature of screen printing coating can be selected), so that specific requirements on the production environment are not needed, the energy consumption and the cost can be reduced, and the consistency of products is improved.
In addition to the objects, features and advantages described above, the present invention has other objects, features and advantages. The present invention will be described in further detail with reference to the drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is a sagging experiment chart of example 1 of the present invention;
FIG. 2 is a graph showing the results of the viscosity test of example 1 of the present invention;
FIG. 3 is a surface view of the metallized layer of example 1 of the present invention after drying;
FIG. 4 is a scanning electron microscope image of a metallized ceramic according to example 1 of the invention;
FIG. 5 is a surface view of the metallized layer of example 2 of the present invention after drying;
FIG. 6 is a scanning electron microscope image of a metallized ceramic according to example 2 of the invention;
FIG. 7 is a surface view of the metallized layer of example 3 of the present invention after drying;
FIG. 8 is a scanning electron microscope image of a metallized ceramic according to example 3 of the invention;
FIG. 9 is a surface view of the metallized layer of example 4 of the present invention after drying;
FIG. 10 is a scanning electron microscope image of a metallized ceramic according to example 4 of the invention;
FIG. 11 is a surface view of the metallized layer of comparative example 1 after drying;
FIG. 12 is a scanning electron microscope image of the metallized ceramic of comparative example 1;
fig. 13 is a graph showing the results of tensile test experiments after the metallized ceramic parts of examples 1 to 4 and comparative example 1 are packaged.
Detailed Description
In order to make the objects, technical solutions and advantageous technical effects of the present invention clearer, the present invention will be further described in detail with reference to examples. It should be understood that the examples described in this specification are for the purpose of illustrating the invention only and are not intended to limit the invention.
For simplicity, only a few numerical ranges are explicitly disclosed herein. However, any lower limit may be combined with any upper limit to form a range not explicitly recited; and any lower limit may be combined with any other lower limit to form a range not explicitly recited, and any upper limit may be combined with any other upper limit to form a range not explicitly recited. Furthermore, each point or individual value between the endpoints of the range is included within the range, although not explicitly recited. Thus, each point or individual value may be combined as a lower or upper limit on itself with any other point or individual value or with other lower or upper limit to form a range that is not explicitly recited.
In the description herein, unless otherwise indicated, "above" and "below" are intended to include the present number, "one or more" means two or more, and "one or more" means two or more.
A first aspect of the present invention provides a ceramic metallizing slurry comprising the following components: ceramic metal powder and aqueous adhesive emulsion, wherein the mass ratio of the ceramic metal powder to the aqueous adhesive emulsion is (1-2.5): 1,
the ceramic metal powder comprises the following components in parts by weight: 66-84 parts of molybdenum powder, 7-16 parts of manganese powder and 8-18 parts of porcelain powder; the aqueous adhesive emulsion comprises an aqueous adhesive and water, wherein the mass ratio of the aqueous adhesive to the water is (0.5-1.5) 1, and the aqueous adhesive is one or a combination of more of acrylic ester aqueous adhesives, styrene-butadiene rubber emulsion aqueous adhesives, styrene-acrylic rubber emulsion aqueous adhesives or aqueous adhesives prepared from water-soluble polymers such as polyacrylic acid and salts thereof, polymethacrylic acid and salts thereof, sodium carboxymethyl cellulose, polyacrylamide and polyvinyl alcohol.
The mass ratio of the ceramic metal powder to the aqueous adhesive emulsion is (1-2.5): 1, for example, the mass ratio of ceramic metal powder to aqueous binder emulsion is 1:1, 1.2:1, 1.5:1, 1.8:1, 2: 1. 2.2:1 or 2.5:1, etc., the mass ratio of the ceramic metal powder to the aqueous binder emulsion may also be in any combination of the above values. When the mass ratio of the ceramic metal powder to the aqueous adhesive emulsion is less than 1:1, the adhesive is too much to be added, and cracking carbon is easy to remain in the molybdenum-manganese metal layer during high-temperature treatment, so that the subsequent welding strength is affected; when the mass ratio of the ceramic metal powder to the aqueous adhesive emulsion is more than 2.5:1, the addition amount of the aqueous adhesive emulsion is too small, a stable slurry system cannot be formed, and the bonding strength of the coating can be reduced.
The ceramic metal powder comprises the following components in parts by weight: 66-84 parts of molybdenum powder, 7-16 parts of manganese powder and 8-18 parts of porcelain powder, wherein the molybdenum powder can be 66 parts, 68 parts, 70 parts, 75 parts, 80 parts or 84 parts, and the like, and the mass parts of the molybdenum powder can be any combination range of the numerical values. The manganese powder may be 7 parts, 10 parts, 12 parts, 15 parts, 16 parts, or the like, and the mass parts of the manganese powder may be any combination of the above values. The ceramic powder can be 8 parts, 10 parts, 12 parts, 15 parts or 18 parts, etc., and the mass parts of the ceramic powder can be any combination range of the above values.
The mass ratio of the aqueous binder to the water is (0.5-1.5): 1, for example, the mass ratio of the binder to the water is 0.5:1, 0.8:1, 1:1, 1.2:1, 1.5:1, etc., and the mass ratio of the binder to the water may be any combination range of the above values.
In the embodiment of the invention, the aqueous adhesive is one or a combination of more of acrylic ester aqueous adhesive, styrene-butadiene rubber emulsion aqueous adhesive, styrene-acrylic rubber emulsion aqueous adhesive or aqueous adhesive prepared from water-soluble polymer polyacrylic acid and salt thereof, polymethacrylic acid and salt thereof, sodium carboxymethyl cellulose, polyacrylamide and polyvinyl alcohol. In some embodiments, the aqueous binder is an acrylic aqueous binder, for example, methyl acrylate, ethyl acrylate, n-butyl acrylate, t-butyl acrylate, octyl acrylate, vinyl acetate, isobornyl acrylate, methyl methacrylate, ethyl methacrylate, n-butyl methacrylate, 2-ethylhexyl methacrylate, cyclohexyl methacrylate, isobornyl methacrylate, hydroxyethyl methacrylate, hydroxypropyl methacrylate, epoxypropyl methacrylate, and the like.
In some embodiments, the aqueous binder is a styrene-butadiene rubber emulsion aqueous binder. In other embodiments, the aqueous binder is a mixed binder of a styrene-acrylic rubber emulsion-based aqueous binder and a styrene-butadiene rubber emulsion-based aqueous binder.
In other embodiments, the aqueous binder is an aqueous binder prepared from the water-soluble polymers polyacrylic acid and salts thereof, polymethacrylic acid and salts thereof, sodium carboxymethyl cellulose, polyacrylamide, polyvinyl alcohol, and the like.
In some embodiments, the aqueous adhesive is prepared as follows: adding 40 parts by mass of acrylamide and distilled water into a reaction container, stirring and dissolving, wherein the rotating speed is 200r/min; introducing nitrogen; heating to 60 ℃, and then adding 60 parts by mass of butyl acrylate to the temperature to be constant at 60 ℃; then adding initiator ammonium persulfate to initiate reaction, taking out precipitate after reacting for 10 hours, adding ammonia water to neutralize pH to 6.5-9, and obtaining the aqueous adhesive.
The slurry provided by the invention only uses water as a solvent, the water is colorless and odorless, and the slurry does not harm the physical and mental health of production workers in the drying process, so that the slurry is environment-friendly and the solvent cost is reduced. Compared with terpineol, the water has smaller intermolecular friction force, lower viscosity and smaller influence on the physical and chemical properties such as slurry viscosity and the like due to temperature. In addition, the ceramic metal powder is hydrophilic, a large number of hydrophilic groups are also arranged in the structure of the binder, and according to the similar principle of compatibility, the hydrophilic groups of the binder are easier to interact with the surface of the ceramic metal powder in a water solvent system compared with a terpineol system. Therefore, under the synergistic effect of low-viscosity solvent characteristics and similar compatibility principles, the slurry preparation can be carried out at normal temperature, and can be well coated (such as screen printing coating printing temperature can be selected) for printing at the ambient temperature of 5-60 ℃, so that specific requirements on the production environment are not needed, the energy consumption and the cost can be reduced, and the product consistency is improved.
The terpineol is sticky, the viscosity of the terpineol is greatly influenced by temperature, and the melting point is about 30 ℃, so that the thermal movement of material molecules is often enhanced at the temperature of 60-100 ℃ when the molybdenum-manganese slurry is prepared, the interaction between a binder group and ceramic metal powder is promoted, and the process is also performed at about 60 ℃ when printing, so that better slurry fluidity is obtained, and the slurry can be ensured to be leveled on the ceramic surface.
In an embodiment of the invention, the molybdenum powder and manganese powder have a particle size of 0.1-5 microns. When the particle size is lower than 0.1 micron, the manufacturing cost of the nano material is very high, the nano material is easy to agglomerate and not easy to store, and even the safety risk of explosion is brought; when the particle size is higher than 5 microns, the quality is heavy, the stability of the slurry is poor, sedimentation is easy to occur, and the normal-temperature preparation and normal-temperature printing of the slurry are not facilitated.
An embodiment of the second aspect of the present invention provides a method for preparing the ceramic metallization paste, including: mixing molybdenum powder, manganese powder and porcelain powder, adding water-based adhesive and water, and stirring at normal temperature until the viscosity of the slurry is 2000-4500 mPa.s. Too low viscosity can cause easy sedimentation of the slurry and easy overflow during coating; when the viscosity is too high, the fluidity of the slurry is poor, the slurry cannot be scraped at normal temperature, and the coating is easy to crack.
The preparation method of the ceramic metalized slurry provided by the invention can be carried out at normal temperature, can simplify the production process, reduce the energy consumption and save the production cost.
Embodiments of the third aspect of the present invention provide a metallized ceramic article comprising a ceramic article and a metallized layer overlying the ceramic article, the metallized layer being made from the ceramic metallization paste.
The ceramic powder in the ceramic metallization slurry has a composition consistent with or close to that of the ceramic part. The ceramic powder can form glass phase to fill the gaps of the molybdenum-manganese metal layer at high temperature, and has excellent compatibility due to the consistency of the glass phase and the ceramic body, so that the bonding force and compactness between the molybdenum-manganese metal layer and the ceramic body are improved. The ceramic material is not limited to alumina ceramics, aluminum nitride ceramics, silicon carbide ceramics, silicon nitride ceramics, dielectric ceramics, piezoelectric ceramics, and the like.
In some embodiments, the porcelain powder comprises Al 2 O 3 、SiO 2 CaO, mgO and MnO 2 One or more combinations thereof.
In the embodiment of the invention, the ceramic metallization slurry is coated on the surface of the ceramic in a mode of screen printing, point coating, spray coating, roll coating, dip coating or sputtering, and a metallization layer is obtained after drying and sintering.
In an embodiment of the invention, the coating temperature is 5 to 60 ℃.
The slurry can be coated at an ambient temperature of 5-60 ℃, for example, screen printing is used for coating at 5-60 ℃, specific requirements on production environment are not needed, energy consumption and cost can be reduced, and product consistency is improved.
In the embodiment of the invention, the drying temperature in the step (2) is 40-80 ℃ and the drying time is 20-60min. Too short a time will not dry, too long a time will not have obvious benefits on the drying effect, but will increase energy consumption and reduce production efficiency.
In the embodiment of the invention, the sintering temperature in the step (2) is 1480-1580 ℃ and the heat preservation time is 60-90min. The ceramic metal powder is subjected to chemical change in the temperature range, and the heat preservation is carried out for more than 60 minutes, so that the chemical change is more sufficient, the metallization effect is not obviously beneficial for a long time, but the energy consumption is increased and the production efficiency is reduced.
The ceramic metalized slurry provided by the invention can be prepared at normal temperature, can be well coated at the ambient temperature of 5-60 ℃, does not need to have specific requirements on the production environment, can reduce energy consumption and cost, and improves the consistency of products.
Examples
The following examples more particularly describe the disclosure of the present application, which are intended as illustrative only, since numerous modifications and variations within the scope of the disclosure will be apparent to those skilled in the art. Unless otherwise indicated, all parts, percentages, and ratios reported in the examples below are by weight, and all reagents used in the examples are commercially available or were obtained synthetically according to conventional methods and can be used directly without further treatment, as well as the instruments used in the examples.
Example 1
The embodiment provides a ceramic metallization paste comprising the following components: the ceramic metal powder and the aqueous adhesive emulsion have the mass ratio of 1.5:1,
the ceramic metal powder comprises the following components in parts by weight: 70 parts of molybdenum powder, 15 parts of manganese powder and 15 parts of porcelain powder; the aqueous adhesive emulsion comprises an aqueous adhesive and water, wherein the mass ratio of the aqueous adhesive to the water is 1:1, and the aqueous adhesive is styrene-butadiene rubber emulsion aqueous adhesive.
The preparation method for preparing the metallized ceramic part by using the raw materials comprises the following steps:
(1) Preparation of ceramic metallization slurry: mixing molybdenum powder, manganese powder and ceramic powder according to the raw material components, adding an aqueous adhesive and water, and stirring at normal temperature to obtain ceramic metallization slurry; the viscosity of the ceramic metallization slurry is 4086 mPa.s.
Firstly, performing sagging performance test on the obtained ceramic metalized slurry, wherein the test method is to make the slurry naturally flow down after the slurry is stuck by a spoon, observe the flowing down state of the slurry, if the slurry is in a uniform fine pulling wire shape, the sagging performance is good, and if the slurry is in a thick line flowing down or in a drop shape and intermittently flowing down, the sagging performance is poor, the ceramic metalized slurry cannot be uniformly spread on the surface to be coated to be uneven during printing, the result is shown in figure 1, and the result shows that: the slurry is in a fine string shape when sagging at 60 ℃, which indicates that the slurry has good sagging degree. When the temperature is reduced to 40 ℃ and even 5 ℃, the slurry still presents a tiny string shape when sagging, which indicates that the sagging performance of the slurry is less affected by the temperature.
Next, the obtained ceramic metalized slurry was subjected to a viscosity test by referring to a rotational viscosimeter method in national standard GB/T13217.4-2020, the results are shown in fig. 2, and the results show that: at 60 ℃, the viscosity of the paste is about-3400 mPas, the viscosity starts to rise slowly with the temperature drop, and when the temperature drops to 5 ℃, the viscosity of the paste rises to-4500 mPas, and the viscosity of the paste is not greatly changed as a whole, so that the paste is suitable for the subsequent printing process.
(2) The printing process comprises the following steps: the obtained ceramic metalized slurry is coated on the end face of an alumina ceramic tube (particularly a ceramic sealing ring for a power type lithium ion battery) at the temperature of 5 ℃ in a screen printing mode, wherein a screen is 200 meshes, and then the ceramic metalized ceramic part is obtained through drying and sintering treatment. The drying temperature in the step (2) is 60 ℃, the drying time is 40 minutes, the sintering temperature in the step (2) is 1500 ℃, and the heat preservation time is 75 minutes.
Fig. 3 is a surface view of the dried metallized layer, and it can be seen from fig. 1 that the surface of the metallized layer is uniform and flat.
FIG. 4 is a Scanning Electron Microscope (SEM) image of a metallized ceramic part, wherein FIG. 4 (left) is a front SEM image of a molybdenum manganese metal layer, which shows that the surface is flat and no grooves are seen; fig. 4 (right) is a cross-sectional SEM image of a molybdenum-manganese metal layer, showing that the surface layer is relatively uniform in thickness, on the order of about 10-12 microns.
Example 2
This example is different from example 1 in that the temperature at the time of screen printing coating is 60℃and the other is the same as example 1.
Fig. 5 is a surface view of the dried metallized layer, and it can be seen from fig. 5 that the surface of the metallized layer is uniform and flat.
FIG. 6 is a Scanning Electron Microscope (SEM) view of a metallized ceramic part, wherein FIG. 6 (left) is a front SEM view of a molybdenum manganese metal layer, which shows that the surface is flat and no grooves are seen; fig. 6 (right) is a cross-sectional SEM image of a molybdenum-manganese metal layer, showing that the surface layer is relatively uniform in thickness, on the order of about 10-12 microns.
From examples 1-2, it was found that the ceramic metallization paste was applied and dried to the end face of an alumina ceramic tube using screen printing techniques at 5 ℃ and 60 ℃ and that the coatings were very flat and free of grooves without significant differences. Further, SEM tests were performed on the cross section after the formation of the molybdenum-manganese metallization layer by high temperature treatment, and it was also found that: the coating microstructures of the two are not obviously different, relatively dense molybdenum-manganese alloy grains are formed, the thickness of the molybdenum-manganese layer is about 10-12 microns, and obvious differences of the coating thickness, flatness and microstructure caused by the change of printing coating temperature are avoided.
Example 3
The embodiment provides a ceramic metallization paste comprising the following components: the ceramic metal powder and the aqueous adhesive emulsion have the mass ratio of 1:1,
the ceramic metal powder comprises the following components in parts by weight: 68 parts of molybdenum powder, 7 parts of manganese powder and 10 parts of porcelain powder; the aqueous adhesive emulsion comprises an aqueous adhesive and water, wherein the mass ratio of the aqueous adhesive to the water is 0.5:1, and the aqueous adhesive is a mixed adhesive of styrene-acrylic rubber emulsion aqueous adhesive and styrene-butadiene rubber emulsion aqueous adhesive.
The above raw materials were used to prepare metallized ceramic parts, and the ceramic parts and metallized ceramic parts were prepared in the same manner as in example 1.
Fig. 7 is a surface view of the dried metallized layer, and it can be seen from fig. 7 that the surface of the metallized layer is uniform and flat.
Fig. 8 is a Scanning Electron Microscope (SEM) image of a metallized ceramic, wherein fig. 8 is a cross-sectional SEM image of a molybdenum manganese metal layer, and the thickness of the surface layer is relatively uniform, about 10-12 microns.
Example 4
The embodiment provides a ceramic metallization paste comprising the following components: the ceramic metal powder and the aqueous adhesive emulsion have the mass ratio of 2.5:1,
the ceramic metal powder comprises the following components in parts by weight: 84 parts of molybdenum powder, 10 parts of manganese powder and 18 parts of porcelain powder; the aqueous adhesive emulsion comprises an aqueous adhesive and water, wherein the mass ratio of the aqueous adhesive to the water is 1.5:1, and the aqueous adhesive is prepared from water-soluble polymer polyacrylic acid and salts thereof, polymethacrylic acid and salts thereof, sodium carboxymethyl cellulose, polyacrylamide and polyvinyl alcohol.
The above raw materials were used to prepare metallized ceramic parts, and the ceramic parts and metallized ceramic parts were prepared in the same manner as in example 1.
Fig. 9 is a surface view of the dried metallized layer, and it can be seen from fig. 9 that the surface of the metallized layer is uniform and flat.
FIG. 10 is a Scanning Electron Microscope (SEM) image of a metallized ceramic article with a relatively uniform surface layer thickness, no grooves, and a thickness of about 10-12 microns.
Comparative example 1
(1) Mixing 70 parts of molybdenum powder, 15 parts of manganese powder and 15 parts of ceramic powder to obtain ceramic metal powder;
(2) Adding 4 parts of ethyl cellulose into 100 parts of terpineol at 60 ℃ and stirring to form a binder solution;
(3) Adding 10 parts of ceramic metal powder and 3 parts of binder solution into a ball milling tank, and stirring and ball milling for 24 hours at 60 ℃ to obtain uniform slurry, wherein the viscosity of the ceramic metal slurry is 5000 mPa.s;
the temperature at the time of screen printing coating was 5 DEG C
The remainder of the procedure was the same as in example 1, and the ceramic member used was the same as in example 1, to obtain a metallized ceramic member.
Fig. 11 is a surface view of the dried metallization layer, and it can be seen from fig. 1 that the surface of the metallization layer presents distinct grooves.
Fig. 12 is a Scanning Electron Microscope (SEM) image of a metallized ceramic part, showing that surface grooves and cracks are evident and that the strength is extremely low after welding with metal.
The metallized ceramic pieces and the metal pieces prepared in examples 1 to 4 and comparative example 1 were packaged by the following method:
(1) Electroplating the molybdenum-manganese metallized ceramic piece to deposit an electrodeposited nickel layer with the thickness of about 3-5 microns on the surface of the molybdenum-manganese metal layer in an electroplating mode;
(2) And (3) taking a silver-copper solder sheet with the thickness of 0.08mm as a solder, placing the solder between the metallized ceramic piece and the metal piece to be soldered, and performing high-temperature soldering at the temperature of about 850 ℃ in vacuum or inert atmosphere or reducing atmosphere to realize packaging.
The packages of examples 1 to 3 and comparative example 1 were subjected to a weld strength test, the test method being based on the national industry standard (JC/T2681-2022), the weld strengths of the metallized ceramic and the metal of examples 1 to 3 after the package were 130MPa and above (the strengths of examples 1 and 2 are based on FIG. 13), and the weld strength of comparative example 1 was only 81MPa.
While the present application has been described with reference to a preferred embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the present application, and in particular, the technical features mentioned in the various embodiments may be combined in any manner as long as there is no structural conflict. The present application is not limited to the specific embodiments disclosed herein, but encompasses all technical solutions falling within the scope of the claims.
Claims (10)
1. A ceramic metallizing slurry comprising the following components: ceramic metal powder and aqueous adhesive emulsion, wherein the mass ratio of the ceramic metal powder to the aqueous adhesive emulsion is (1-2.5): 1,
the ceramic metal powder comprises the following components in parts by weight: 66-84 parts of molybdenum powder, 7-16 parts of manganese powder and 8-18 parts of porcelain powder; the aqueous adhesive emulsion comprises an aqueous adhesive and water, wherein the mass ratio of the aqueous adhesive to the water is (0.5-1.5) 1, and the aqueous adhesive is one or a combination of more of acrylic ester aqueous adhesives, styrene-butadiene rubber emulsion aqueous adhesives, styrene-acrylic rubber emulsion aqueous adhesives or aqueous adhesives prepared from water-soluble polymers such as polyacrylic acid and salts thereof, polymethacrylic acid and salts thereof, sodium carboxymethyl cellulose, polyacrylamide and polyvinyl alcohol.
2. The ceramic metallization paste of claim 1, wherein the molybdenum and manganese powders have a particle size of 0.1-5 microns.
3. A method of preparing the ceramic metallizing slurry according to claim 1 or 2, comprising: mixing molybdenum powder, manganese powder and porcelain powder, adding water-based adhesive and water, and stirring at normal temperature until the viscosity of the slurry is 2000-4500 mPa.s.
4. A metallized ceramic article comprising a ceramic article and a metallized layer overlying the ceramic article, the metallized layer being made from the ceramic metallization paste of claim 1 or 2.
5. The metallized ceramic article according to claim 4, wherein the composition of the ceramic powder in the ceramic metallization paste is consistent with or near the composition of the ceramic article.
6. The metallized ceramic according to claim 5, wherein said ceramic powder comprises Al 2 O 3 、SiO 2 CaO, mgO and MnO 2 One or more combinations thereof.
7. The metallized ceramic according to claim 4, wherein said ceramic metallized slurry is applied to the surface of said ceramic by screen printing, spot coating, spray coating, roll coating, dip coating or sputtering, and is baked and sintered to provide a metallized layer.
8. The metallized ceramic according to claim 7, wherein said coating temperature is between 5 and 60 ℃.
9. The metallized ceramic according to claim 7, wherein said drying temperature is 40-80 ℃ and drying time is 20-60min.
10. The metallized ceramic according to claim 7, wherein said sintering temperature is 1480-1580 ℃ and holding time is 60-90min.
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