CN114538948A - Metal transition layer suitable for welding zirconia ceramic and metal and preparation method thereof - Google Patents
Metal transition layer suitable for welding zirconia ceramic and metal and preparation method thereof Download PDFInfo
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- CN114538948A CN114538948A CN202011334674.7A CN202011334674A CN114538948A CN 114538948 A CN114538948 A CN 114538948A CN 202011334674 A CN202011334674 A CN 202011334674A CN 114538948 A CN114538948 A CN 114538948A
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 63
- 239000002184 metal Substances 0.000 title claims abstract description 62
- 239000000919 ceramic Substances 0.000 title claims abstract description 40
- 230000007704 transition Effects 0.000 title claims abstract description 25
- 238000003466 welding Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000006263 metalation reaction Methods 0.000 title description 2
- 239000000843 powder Substances 0.000 claims abstract description 57
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011248 coating agent Substances 0.000 claims abstract description 15
- 238000000576 coating method Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 10
- 239000011230 binding agent Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000007747 plating Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical group [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000001856 Ethyl cellulose Substances 0.000 claims description 3
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical group CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 3
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 3
- 229920001249 ethyl cellulose Polymers 0.000 claims description 3
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 238000007649 pad printing Methods 0.000 claims description 3
- 238000007650 screen-printing Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 229940116411 terpineol Drugs 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000001465 metallisation Methods 0.000 abstract description 5
- 238000005219 brazing Methods 0.000 description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 5
- 229910001928 zirconium oxide Inorganic materials 0.000 description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- -1 fully stirring Substances 0.000 description 4
- 239000011224 oxide ceramic Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010344 co-firing Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910000833 kovar Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 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
- C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a metal transition layer suitable for welding zirconia ceramics and metal and a preparation method thereof, wherein 60-80 parts of Mo powder or 50-65 parts of tungsten powder, 5-30 parts of Mn powder and 2-20 parts of SiO powder are calculated according to parts by weight2Powder and 0.5-4 parts of ZrO2Mixing 0.5-5 parts of Ti powder and 0.5-3 parts of Cr powder to obtain metalized powder; uniformly mixing the metallization powder and a binder, and coating the mixture on the surface of the sintered zirconia ceramic; sintering the zirconia ceramic coated with the metalized powder under the protection of reducing atmosphere; and plating a nickel layer on the metal layer formed after sintering to obtain the metal transition layer. The product obtained by the method has high reliability, high air tightness, high welding strength, low cost and controllable quality.
Description
Technical Field
The invention belongs to the field of ceramic sealing, and particularly relates to a metal transition layer suitable for welding zirconia ceramic and metal and a preparation method thereof.
Background
Because the surface structure of the ceramic material is different from that of the metal material, welding cannot wet the surface of the ceramic material and cannot act with the surface of the ceramic material to form firm adhesion, so that sealing between the ceramic and the metal is a special process method, namely a metallization method, and a metal film is firmly adhered to the surface of the ceramic material so as to realize welding between the ceramic and the metal.
In the prior art, the problems of low strength and low reliability exist in the welding of zirconia ceramics and metals.
Disclosure of Invention
The technical problem to be solved by the present invention is to overcome the above mentioned disadvantages and drawbacks in the background art, and to provide a metal transition layer suitable for welding zirconia ceramics and metal and a method for preparing the same, so as to improve the welding strength and reliability.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of a metal transition layer suitable for welding zirconia ceramics and metal comprises the following steps:
(1) 60-80 parts of Mo powder or 50-65 parts of tungsten powder, 5-30 parts of Mn powder and 2-20 parts of SiO by weight2Powder and 0.5-4 parts of ZrO2Mixing 0.5-5 parts of Ti powder and 0.5-3 parts of Cr powder to obtain metalized powder;
(2) uniformly mixing the metallized powder obtained in the step (1) with a binder, and coating the mixture on the surface of the sintered zirconia ceramic;
(3) sintering the zirconia ceramic coated with the metalized powder under the protection of reducing atmosphere;
(4) and plating a nickel layer on the metal layer formed after sintering to obtain the metal transition layer.
Further, the binder is ethyl cellulose, terpineol or stearic acid.
Further, the coating adopts a screen printing, pad printing, spraying or pen coating mode.
Further, the reducing atmosphere is hydrogen or a nitrogen-hydrogen mixed gas.
Further, the sintering temperature is 1200-1450 ℃.
Further, the thickness of the nickel layer is 2-6 microns.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, different elements are added to be matched with the zirconia ceramic to induce the elements in the zirconia ceramic, so that low-temperature migration and eutectic melting of the elements are realized, an anchoring effect between the elements is achieved, the surface metal layer and the zirconia ceramic are migrated and permeated with each other, and a firm metal transition layer is formed. The product obtained by brazing the zirconia ceramic covering the metal transition layer and the metal has the advantages of high reliability, high air tightness, high welding strength, low cost, controllable quality and capability of realizing batch production.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments below.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
The preparation method of the metal transition layer suitable for welding the zirconia ceramics and the metal comprises the following steps:
1) preparing the metallized powder from 60-80 parts of Mo powder or 50-65 parts of high-purity metal tungsten powder, 5-30 parts of Mn powder and 2-20 parts of SiO by weight2Powder and 0.5-4 parts of ZrO20.5-5 parts of Ti powder and 0.5-3 parts of Cr powder are put into a mixer and fully mixed. By Mn, SiO2Ti and Cr can induce the glass phases of the zirconia ceramic body and the metal layer to mutually migrate and penetrate at the temperature lower than the sintering temperature of the ceramic, and ZrO2The stress of the bonding layer of the metal layer and the zirconia ceramic layer can be reduced.
2) Adding a proper amount of organic binder (such as ethyl cellulose, terpineol or stearic acid) into the prepared metalized powder, fully stirring, coating the mixture on the surface of the cleaned sintered zirconia ceramic in a screen printing, pad printing, spraying or pen coating mode, and drying. Compared with the method of coating metal slurry on the zirconia ceramic green body and co-firing the zirconia ceramic green body and the zirconia ceramic, the method has the advantages of high green body strength, no product deformation and controllable quality.
3) The zirconia ceramic coated with the metallization powder is sintered at 1200-1450 ℃ under the protection of reducing atmosphere (hydrogen or mixed gas of hydrogen and nitrogen with the content of more than 30%). The reducing atmosphere avoids the oxidation of metal elements in the metal coating during sintering, and the thickness of the metal layer is half of that of the original coating paste due to the eutectic infiltration reaction of the elements during sintering, and the metal layer mainly comprises molybdenum, tungsten and zirconium oxide wrapped by glass phase.
4) Plating a nickel layer with the thickness of 2-6 microns on the sintered metal layer, wherein the nickel layer is mainly convenient for solder to flow away during welding, and thus the high-strength metal transition layer suitable for brazing with metal is obtained.
The zirconium oxide ceramic covered with the metal transition layer is brazed with metal (such as oxygen-free copper, stainless steel, kovar alloy, iron and the like), the welding strength can reach 80-90Mpa, and the air tightness can reach 10-12Pa·m3And s. The weld strength was measured using SUST electronic Universal tester CMT-4304, accuracy grade 0.5, maximum test force 30 KN. The air tightness is measured by a helium mass spectrometer leak detector of a Chinese medical science instrument.
Example 1:
the preparation method of the metal transition layer suitable for welding the zirconia ceramic and the metal comprises the following steps:
1) the metallized powder is prepared from 65 parts of Mo powder, 8 parts of Mn powder and 5 parts of SiO powder2Powder, 1 part of ZrO21 part of Ti powder and 1 part of Cr powder are put into a mixer and fully mixed.
2) Adding a proper amount of organic binder into the prepared metalized powder, fully stirring, coating the mixture on the surface of the cleaned sintered zirconia ceramic, and drying.
3) The zirconia ceramic coated with the metallization powder is sintered at 1250 ℃ under the protection of a reducing atmosphere.
4) And plating a nickel layer with the thickness of 5 microns on the sintered metal layer to obtain the high-strength metal transition layer suitable for brazing with metal.
Brazing the zirconium oxide ceramic covered with the metal transition layer with oxygen-free copper, wherein the welding strength reaches 86Mpa, and the air tightness reaches 10-12Pa·m3/s。
Example 2:
the preparation method of the metal transition layer suitable for welding zirconia ceramic and metal of the embodiment comprises the following steps:
1) the metallized powder is prepared from (by weight parts) Mo powder 75, Mn powder 25, and SiO 152Powder, 3 parts of ZrO23 parts of Ti powder and 2 parts of Cr powder are put into a mixer and fully mixed.
2) Adding a proper amount of organic binder into the prepared metalized powder, fully stirring, coating the mixture on the surface of the cleaned sintered zirconia ceramic, and drying.
3) And sintering the zirconia ceramic coated with the metalized powder at 1400 ℃ under the protection of a reducing atmosphere.
4) And plating a nickel layer with the thickness of 5 microns on the sintered metal layer to obtain the high-strength metal transition layer suitable for brazing with metal.
Brazing the zirconium oxide ceramic covered with the metal transition layer and the stainless steel, wherein the welding strength reaches 90Mpa, and the air tightness reaches 10-12Pa·m3/s。
Example 3:
the preparation method of the metal transition layer suitable for welding the zirconia ceramic and the metal comprises the following steps:
1) the metallized powder is prepared from (by weight parts) high-purity tungsten powder 60, Mn powder 15, and SiO 102Powder, 2 parts of ZrO23 parts of Ti powder and 1.5 parts of Cr powder are put into a mixer and fully mixed.
2) Adding a proper amount of organic binder into the prepared metalized powder, fully stirring, coating the mixture on the surface of the cleaned sintered zirconia ceramic, and drying.
3) The zirconia ceramic coated with the metallization powder is sintered at 1350 ℃ under the protection of a reducing atmosphere.
4) And plating a nickel layer with the thickness of 5 microns on the sintered metal layer to obtain the high-strength metal transition layer suitable for brazing with metal.
Brazing the zirconium oxide ceramic covered with the metal transition layer and the stainless steel, wherein the welding strength reaches 88Mpa, and the air tightness reaches 10-12Pa·m3/s。
The foregoing is considered as illustrative of the preferred embodiments of the invention and is not to be construed as limiting the invention in any way. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention should fall within the protection scope of the technical scheme of the present invention, unless the technical spirit of the present invention departs from the content of the technical scheme of the present invention.
Claims (7)
1. A preparation method of a metal transition layer suitable for welding zirconia ceramics and metal is characterized by comprising the following steps:
(1) 60-80 parts of Mo powder or 50-65 parts of tungsten powder, 5-30 parts of Mn powder and 2-20 parts of SiO by weight2Powder and 0.5-4 parts of ZrO2Mixing 0.5-5 parts of Ti powder and 0.5-3 parts of Cr powder to obtain metalized powder;
(2) uniformly mixing the metallized powder obtained in the step (1) with a binder, and coating the mixture on the surface of the sintered zirconia ceramic;
(3) sintering the zirconia ceramic coated with the metalized powder under the protection of reducing atmosphere;
(4) and plating a nickel layer on the metal layer formed after sintering to obtain the metal transition layer.
2. The method according to claim 1, wherein the binder is ethyl cellulose, terpineol, or stearic acid.
3. The method according to claim 1 or 2, wherein the coating is performed by screen printing, pad printing, spraying or pen coating.
4. The method according to claim 1, wherein the reducing atmosphere is hydrogen gas or a mixed gas of nitrogen and hydrogen.
5. The method as claimed in claim 1 or 4, wherein the sintering temperature is 1200-1450 ℃.
6. The method of claim 1, wherein the nickel layer has a thickness of 2 to 6 microns.
7. A metal transition layer suitable for welding zirconia ceramics and metals, which is prepared by the method of any one of claims 1 to 6.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011334674.7A CN114538948A (en) | 2020-11-24 | 2020-11-24 | Metal transition layer suitable for welding zirconia ceramic and metal and preparation method thereof |
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| CN202011334674.7A CN114538948A (en) | 2020-11-24 | 2020-11-24 | Metal transition layer suitable for welding zirconia ceramic and metal and preparation method thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4729504A (en) * | 1985-06-01 | 1988-03-08 | Mizuo Edamura | Method of bonding ceramics and metal, or bonding similar ceramics among themselves; or bonding dissimilar ceramics |
| CN1887814A (en) * | 2006-07-16 | 2007-01-03 | 常熟市银洋陶瓷器件有限公司 | Powder for ceramic metallizing paste and its prepn |
| CN103102180A (en) * | 2013-02-22 | 2013-05-15 | 浙江亚通金属陶瓷有限公司 | Metallized surface of zirconia ceramic and preparation method |
| CN109604859A (en) * | 2018-11-30 | 2019-04-12 | 湖南人文科技学院 | Preparation method, ceramics and its packaging method of the solder paste of ceramic package |
| CN110171981A (en) * | 2019-05-31 | 2019-08-27 | 景德镇景华特种陶瓷有限公司 | A kind of ceramic metallizing paste, preparation method and applications |
| CN110563484A (en) * | 2019-08-26 | 2019-12-13 | 泰州市光明电子材料有限公司 | Ceramic surface metallization process |
-
2020
- 2020-11-24 CN CN202011334674.7A patent/CN114538948A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4729504A (en) * | 1985-06-01 | 1988-03-08 | Mizuo Edamura | Method of bonding ceramics and metal, or bonding similar ceramics among themselves; or bonding dissimilar ceramics |
| CN1887814A (en) * | 2006-07-16 | 2007-01-03 | 常熟市银洋陶瓷器件有限公司 | Powder for ceramic metallizing paste and its prepn |
| CN103102180A (en) * | 2013-02-22 | 2013-05-15 | 浙江亚通金属陶瓷有限公司 | Metallized surface of zirconia ceramic and preparation method |
| CN109604859A (en) * | 2018-11-30 | 2019-04-12 | 湖南人文科技学院 | Preparation method, ceramics and its packaging method of the solder paste of ceramic package |
| CN110171981A (en) * | 2019-05-31 | 2019-08-27 | 景德镇景华特种陶瓷有限公司 | A kind of ceramic metallizing paste, preparation method and applications |
| CN110563484A (en) * | 2019-08-26 | 2019-12-13 | 泰州市光明电子材料有限公司 | Ceramic surface metallization process |
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Application publication date: 20220527 |