CN114438431A - Sintering bearing net for sintering ceramic electronic component and preparation method thereof - Google Patents
Sintering bearing net for sintering ceramic electronic component and preparation method thereof Download PDFInfo
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- CN114438431A CN114438431A CN202210161718.3A CN202210161718A CN114438431A CN 114438431 A CN114438431 A CN 114438431A CN 202210161718 A CN202210161718 A CN 202210161718A CN 114438431 A CN114438431 A CN 114438431A
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- zirconium
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- 238000005245 sintering Methods 0.000 title claims abstract description 126
- 239000000919 ceramic Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 229910052751 metal Inorganic materials 0.000 claims abstract description 103
- 239000002184 metal Substances 0.000 claims abstract description 103
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 74
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000000843 powder Substances 0.000 claims abstract description 39
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 25
- SKERKQMKGVKBEL-UHFFFAOYSA-N [Mg][Ca][Ce] Chemical compound [Mg][Ca][Ce] SKERKQMKGVKBEL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000007921 spray Substances 0.000 claims abstract description 15
- 238000005469 granulation Methods 0.000 claims abstract description 14
- 230000003179 granulation Effects 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims description 55
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 46
- 229910002076 stabilized zirconia Inorganic materials 0.000 claims description 41
- 238000007751 thermal spraying Methods 0.000 claims description 30
- 239000002243 precursor Substances 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 25
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 22
- 239000002562 thickening agent Substances 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000009941 weaving Methods 0.000 claims description 20
- 238000001694 spray drying Methods 0.000 claims description 14
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 13
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 12
- -1 zirconium ions Chemical class 0.000 claims description 12
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 11
- 229910004664 Cerium(III) chloride Inorganic materials 0.000 claims description 11
- 239000001110 calcium chloride Substances 0.000 claims description 11
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 11
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 11
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 10
- 229910001120 nichrome Inorganic materials 0.000 claims description 10
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 10
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 9
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 9
- 238000004080 punching Methods 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- 229910052684 Cerium Inorganic materials 0.000 claims description 7
- 238000010304 firing Methods 0.000 claims description 7
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 6
- 229910001424 calcium ion Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 claims description 3
- RFRMMZAKBNXNHE-UHFFFAOYSA-N 6-[4,6-dihydroxy-5-(2-hydroxyethoxy)-2-(hydroxymethyl)oxan-3-yl]oxy-2-(hydroxymethyl)-5-(2-hydroxypropoxy)oxane-3,4-diol Chemical compound CC(O)COC1C(O)C(O)C(CO)OC1OC1C(O)C(OCCO)C(O)OC1CO RFRMMZAKBNXNHE-UHFFFAOYSA-N 0.000 claims description 3
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 3
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 3
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 3
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 3
- 229920000609 methyl cellulose Polymers 0.000 claims description 3
- 239000001923 methylcellulose Substances 0.000 claims description 3
- 235000010981 methylcellulose Nutrition 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 5
- 239000011247 coating layer Substances 0.000 claims 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 50
- 238000000576 coating method Methods 0.000 abstract description 40
- 239000011248 coating agent Substances 0.000 abstract description 39
- 230000007797 corrosion Effects 0.000 abstract description 18
- 238000005260 corrosion Methods 0.000 abstract description 18
- 230000032683 aging Effects 0.000 abstract description 13
- 230000003647 oxidation Effects 0.000 abstract description 12
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 230000000087 stabilizing effect Effects 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 71
- 229910052759 nickel Inorganic materials 0.000 description 33
- 229910000623 nickel–chromium alloy Inorganic materials 0.000 description 11
- 230000002035 prolonged effect Effects 0.000 description 8
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 6
- 239000011651 chromium Substances 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 6
- 229910000480 nickel oxide Inorganic materials 0.000 description 5
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 230000035882 stress Effects 0.000 description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 238000009954 braiding Methods 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 4
- 238000000280 densification Methods 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- 229910052727 yttrium Inorganic materials 0.000 description 4
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 4
- 230000003712 anti-aging effect Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910006251 ZrOCl2.8H2O Inorganic materials 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229920003086 cellulose ether Polymers 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 238000009499 grossing Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- SZIFAVKTNFCBPC-UHFFFAOYSA-N 2-chloroethanol Chemical compound OCCCl SZIFAVKTNFCBPC-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
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- 239000003792 electrolyte Substances 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
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- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
- C23C4/11—Oxides
-
- 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
- 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
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- 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
- 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
- C04B35/624—Sol-gel processing
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- 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
- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D5/00—Supports, screens, or the like for the charge within the furnace
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- 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
- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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- 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
- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3229—Cerium oxides or oxide-forming salts thereof
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- Chemical & Material Sciences (AREA)
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- Metallurgy (AREA)
- General Engineering & Computer Science (AREA)
- Composite Materials (AREA)
- Coating By Spraying Or Casting (AREA)
Abstract
The application discloses ceramic electronic components sintering is with holding burning net and preparation method thereof, this preparation method of holding burning net is through preparing zirconium sol, zirconium gel and combining the magnesium calcium cerium of spray granulation technology preparation nanometer structure and stabilizing the zirconia powder, and more fine magnesium calcium cerium stabilizes the zirconia powder and is favorable to forming high ageing-resistant coating, and can show the bonding strength and the mechanical properties that improve coating and metal woven net, and simultaneously, magnesium calcium cerium stabilizes the zirconia and own possesses excellent ageing resistance, can improve the ageing resistance of coating, and then improves the corrosion resistance and the oxidation resistance of holding burning net, prolongs the life of holding burning net.
Description
Technical Field
The application relates to the technical field of sintering nets, in particular to a sintering bearing net for sintering ceramic electronic components and a preparation method thereof.
Background
With the development of electronic devices toward miniaturization, lightness, thinness, digitalization and multi-functionalization, ceramic electronic components are more widely used. Generally, a main body of a ceramic electronic component is formed by molding and sintering ceramic powder, and in the sintering process, a molded blank is placed on a sintering plate and is sent into a sintering furnace for sintering.
In the prior art, ceramic setter plates and setter nickel screens coated with zirconia on the surface thereof have been widely used for sintering ceramic electronic components. In comparison, the ceramic setter plates have large thickness and weight, and it is difficult to process vent holes thereon to improve thermal conductivity, resulting in long sintering time, low efficiency, and difficulty in ensuring yield. The sintering nickel net is formed by interweaving a plurality of longitudinal nickel wires arranged in parallel and a plurality of transverse nickel wires, is small in thickness, light in weight, small in processing difficulty and provided with a large number of meshes as air holes, improves heat conductivity and obviously improves sintering efficiency.
However, the problem of insufficient corrosion resistance and oxidation resistance still exists in the use process of the sintering nickel net.
Disclosure of Invention
The application aims to provide a sintering bearing net for sintering ceramic electronic components and a preparation method thereof, and aims to solve the technical problem that the existing sintering bearing nickel net is poor in corrosion resistance and oxidation resistance in the sintering process of the ceramic electronic components.
The second purpose of the application is to provide the sintering bearing net for sintering the ceramic electronic component prepared by the preparation method.
In order to achieve the first purpose, the application provides a preparation method of a sintering bearing net for sintering a ceramic electronic component, which comprises the following steps:
weaving the metal wires to form a metal mesh;
fixing the metal mesh, and heating the metal mesh in vacuum by adopting micro-oxidation treatment;
adding zirconium oxychloride, calcium chloride, magnesium chloride, cerium trichloride and hydrogen peroxide into a solvent, and mixing and heating to obtain zirconium sol;
adding a thickening agent into the zirconium sol, and mixing and stirring to obtain zirconium gel;
atomizing and drying the zirconium gel by adopting a spray granulation process to prepare an aggregate precursor;
sintering the aggregate precursor to prepare magnesium-calcium-cerium stabilized zirconia powder;
and spraying the magnesium-calcium-cerium stabilized zirconia powder onto the metal mesh by adopting a thermal spraying process to obtain the sintering bearing mesh.
Further, the step of weaving the metal wires to form a metal mesh comprises:
weaving a nichrome wire into a metal woven net by using a weaving machine, and folding burrs of the metal woven net on the inner side by using a punching machine, wherein the diameter of the nichrome wire is 0.15-0.6 mm, and the mesh number of the metal woven net is 20-60 meshes.
Further, the step of fixing the metal mesh and heating the metal mesh in vacuum by micro-oxidation treatment comprises:
and clamping two side surfaces of the metal mesh by using aluminum oxide plates, and placing the metal mesh into a vacuum sintering furnace for heat treatment, wherein the internal temperature of the vacuum sintering furnace is 400-800 ℃, and the vacuum degree is 30-1000 Pa.
Further, the step of adding zirconium oxychloride, calcium chloride, magnesium chloride, cerium trichloride and hydrogen peroxide into a solvent, and preparing the zirconium sol by mixing and heating comprises the following steps:
zirconium oxychloride, calcium chloride, magnesium chloride, cerium trichloride, hydrogen peroxide and ethanol are placed in a reaction kettle and stirred for 0.5 hour, then heated to 70 ℃ and continuously stirred until suspension is clear and no bubbles are generated, and then ammonia water is added to adjust the pH value to 5 to prepare zirconium sol;
the step of adding the thickener to the zirconium sol and preparing the zirconium gel by mixing and stirring comprises the following steps:
adding a thickening agent into the zirconium sol, and stirring the zirconium sol for 0.5 hour to obtain zirconium gel.
Further, atomizing and drying the zirconium gel by adopting a spray granulation process to prepare an aggregate precursor; sintering the aggregate precursor to prepare the magnesium-calcium-cerium stabilized zirconia powder, wherein the step of preparing the magnesium-calcium-cerium stabilized zirconia powder comprises the following steps:
putting the zirconium gel into a spray drying tower for spray drying to prepare an aggregate precursor, wherein the temperature in the spray drying tower is 110-300 ℃;
and sintering the aggregate precursor in a sintering furnace to prepare the magnesium-calcium-cerium stabilized zirconia powder, wherein the internal temperature of the sintering furnace is 900-1200 ℃.
Further, the concentration ratio of hydrogen peroxide to zirconium ions is 3: 1-6: 1; the mass ratio of ethanol to hydrogen peroxide is 1: 9-2: 8; the ratio of the total concentration of calcium ions, cerium ions and magnesium ions to the concentration of zirconium ions is 1: 100-10: 100.
further, the hydrogen peroxide is 30 weight percent, and the thickening agent is 0.5-2 weight percent.
The thickener is any one of hydroxyethyl cellulose, methyl cellulose, hydroxypropyl methyl cellulose and hydroxyethyl cellulose ether.
Further, the thermal spraying temperature of the thermal spraying process is 2000-2500 ℃, and the thickness of the coating is 50-100 mu m.
In order to achieve the second purpose, the application also provides a sintering net which is prepared by adopting the preparation method of the sintering net for the ceramic electronic component.
The application has the following beneficial effects: according to the preparation method of the burning-bearing net, the magnesium-calcium-cerium-stabilized zirconia powder with the nano structure is prepared by preparing the zirconium sol, the zirconium gel and combining the spray granulation process, the fine magnesium-calcium-cerium-stabilized zirconia powder is more favorable for forming a high-aging-resistance coating, the bonding strength and the mechanical property of the coating and a metal woven net can be obviously improved, meanwhile, the magnesium-calcium-cerium-stabilized zirconia has excellent aging resistance, the aging resistance of the coating can be improved, the corrosion resistance and the oxidation resistance of the burning-bearing net are further improved, and the service life of the burning-bearing net is prolonged.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art according to the structures shown in the drawings without creative efforts.
FIG. 1 is a flowchart illustrating the steps of one embodiment of a method for making a setter mesh of the present application;
FIG. 2 is an SEM image of an embodiment of a Mg-Ca-Ce stabilized zirconia powder according to the present application;
FIG. 3 is a schematic structural diagram of an embodiment of the load-bearing net of the present application.
The implementation, functional features and advantages of the objectives of the present application will be further explained with reference to the accompanying drawings.
Detailed Description
The present application will be described in further detail with reference to examples and drawings, but the embodiments of the present application are not limited thereto. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the prior art, ceramic setter plates and setter nickel screens coated with zirconia on the surface thereof have been widely used for sintering ceramic electronic components. In comparison, the ceramic setter plates have large thickness and weight, and it is difficult to process vent holes thereon to improve thermal conductivity, resulting in long sintering time, low efficiency, and difficulty in ensuring yield. The sintering nickel net is formed by interweaving a plurality of longitudinal nickel wires arranged in parallel and a plurality of transverse nickel wires, is small in thickness, light in weight, small in processing difficulty and provided with a large number of meshes as air holes, improves heat conductivity and obviously improves sintering efficiency.
However, the problem of insufficient corrosion resistance and oxidation resistance still exists in the use process of the sintering nickel net.
The technical scheme mainly aims to provide a sintering bearing net for sintering ceramic electronic components and a preparation method thereof, and aims to solve the technical problem that the corrosion resistance and the oxidation resistance of the existing sintering bearing nickel net are poor due to the fact that a coating of the sintering bearing nickel net is easy to age and peel off in the sintering process of the ceramic electronic components.
Referring to fig. 1, a method for preparing a sintering support net for sintering a ceramic electronic component provided by the present application includes the following steps:
s10: weaving the metal wires to form a metal mesh;
s20: fixing the metal mesh, and heating the metal mesh in vacuum by adopting micro-oxidation treatment;
s30: adding zirconium oxychloride, calcium chloride, magnesium chloride, cerium trichloride and hydrogen peroxide into a solvent, and mixing and heating to obtain zirconium sol;
s40: adding a thickening agent into the zirconium sol, and mixing and stirring to obtain zirconium gel;
s50: atomizing and drying the zirconium gel by adopting a spray granulation process to prepare an aggregate precursor;
s60: and sintering the aggregate precursor to obtain the magnesium-calcium-cerium stabilized zirconia powder.
S70: and spraying the magnesium-calcium-cerium stabilized zirconia powder onto the metal mesh by adopting a thermal spraying process to obtain the sintering bearing mesh.
In the present application, a magnesium-calcium-cerium composite stabilized zirconia powder having a nano structure and suitable for a thermal spraying process can be prepared using a sol-gel method in combination with spray granulation. The sol-gel process is an effective method for preparing nano powder, the crystal grains of the zirconia powder prepared by the sol-gel process are very fine, and the coating prepared by the sol-gel process can effectively inhibit the aging of zirconia and obviously improve the bonding strength and mechanical property of the coating; meanwhile, compared with yttrium-stabilized zirconia which is commonly used for firing-bearing net coatings, the aging resistance of the zirconia compounded and stabilized by magnesium, calcium and cerium is more excellent, and the aging resistance of the zirconia coating can be promoted by the zirconia compounded and stabilized by magnesium, calcium and cerium. The spray granulation aims at preparing a precursor of a zirconia aggregate, the precursor of the aggregate is sintered to be converted into the magnesium-calcium-cerium stabilized zirconia, and densification is promoted to obtain micron-sized zirconia powder with nano-crystalline grains, so that the micron-sized zirconia powder is suitable for a thermal spraying process.
The existing sintering nickel screen technology also has a technical means that yttrium stabilized zirconia powder is sprayed on the sintering nickel screen by adopting a thermal spraying process so as to form an isolation coating and further improve the oxidation resistance and corrosion resistance of the sintering nickel screen. However, in the use process of the sintering nickel net, the coating is easy to age, and micro or macro microcracks appear on the surface of the coating to cause the coating to peel off, thereby further influencing the corrosion resistance and the oxidation resistance of the sintering nickel net. The preparation method prepares the magnesium-calcium-cerium-stabilized zirconia powder with the nano structure by preparing zirconium sol and zirconium gel and combining a spray granulation process, the fine magnesium-calcium-cerium-stabilized zirconia powder is more beneficial to forming a high anti-aging coating, the bonding strength and the mechanical property of the coating and a metal mesh can be obviously improved, meanwhile, the magnesium-calcium-cerium-stabilized zirconia has excellent anti-aging property, the anti-aging capability of the coating can be improved, the corrosion resistance and the oxidation resistance of the burning net are further improved, and the service life of the burning net is prolonged.
Further, in the present application, the step S10: weaving the metal wires to form the metal mesh comprises:
s11: weaving a nichrome wire into a metal woven net by adopting a weaving machine, and folding burrs of the metal woven net on the inner side by using a punching machine, wherein the diameter of the nichrome wire is 0.15-0.6 mm, and the mesh number of the metal woven net is 20-60 meshes.
In a preferred embodiment of the present application, the diameter of the nichrome wire is specifically 0.3mm, and the mesh number of the metal mesh is 32. Nickel chromium alloy (Cr) is used herein30Ni70) Instead of pure nickel as a matrix material for woven nickel mesh, the addition of chromium in nichrome alloys can significantly improve the corrosion resistance of nickel in oxidizing corrosive media as well as the local corrosion resistance. Therefore, the nickel-chromium alloy is used as the base material, so that the corrosion resistance of the metal mesh in the sintering process can be improved, and the service life of the metal mesh can be prolonged.
Further, in the present application, the step S20: fixing the metal mesh, and carrying out vacuum heating on the metal mesh by adopting micro-oxidation treatment, wherein the vacuum heating comprises the following steps:
s21: and clamping two side surfaces of the metal mesh by using an aluminum oxide plate, and placing the metal mesh into a vacuum sintering furnace for heat treatment, wherein the internal temperature of the vacuum sintering furnace is 400-800 ℃, and the vacuum degree is 30-1000 Pa.
In a preferred embodiment, the temperature in the vacuum sintering furnace is 600 ℃, the vacuum degree is 300Pa, and the micro-oxidation treatment is carried out on the surface of the metal mesh by reserving a trace amount of oxygen. In the application, the internal stress in the metal mesh can be eliminated by fixing the two side surfaces of the metal mesh and then carrying out vacuum heating, so that the metal mesh is prevented from deforming in the thermal spraying process to influence the combination of the coating and the metal mesh, and the combination strength of the coating and the metal mesh can be further improved by micro-oxidation treatment. In the process, the woven metal mesh is placed in two smooth aluminum oxide plates and heated in a vacuum sintering furnace; in the heating process, the internal stress caused by weaving in the metal mesh is gradually eliminated, and the metal mesh cannot deform due to the clamping limiting effect of the aluminum oxide plate and still keeps flat after the internal stress is released. Meanwhile, the oxygen content in the vacuum sintering furnace is regulated and controlled by adjusting the vacuum degree in the vacuum sintering furnace, so that the micro-oxidation treatment on the surface of the metal woven mesh is realized, and the bonding strength between the metal woven mesh and the coating in the thermal spraying process is improved.
It will be understood that the main purpose of the above steps is to limit the metal mesh by means of a flat alumina plate, so that its surface remains flat and cannot be deformed, and therefore, based on this principle, other flattening processes can be used in the process instead of the operation of clamping the alumina plate. In conclusion, the internal stress in the metal mesh is eliminated through the vacuum heating and smoothing process, and the micro-oxidation treatment is carried out, so that the bonding strength of the metal mesh and the zirconia in the thermal spraying process can be improved, and the oxidation resistance and the corrosion resistance of the burning bearing net are further improved.
Further, in the present application, the step S30: adding zirconium oxychloride, calcium chloride, magnesium chloride, cerium trichloride and hydrogen peroxide into a solvent, and mixing and heating to prepare zirconium sol, wherein the zirconium sol comprises the following components:
s31: zirconium oxychloride, calcium chloride, magnesium chloride, cerium trichloride, hydrogen peroxide and ethanol are placed in a reaction kettle and stirred for 0.5 hour, then heated to 70 ℃ and continuously stirred until suspension is clear and no bubbles are generated, and then ammonia water is added to adjust the pH value to 5, so that the zirconium sol is prepared.
In this application, adding a thickener to the zirconium sol to prepare a zirconium gel by mixing and stirring comprises:
s32: adding a thickening agent into the zirconium sol, and stirring the zirconium sol for 0.5 hour to obtain zirconium gel.
Further, in the application, the zirconium gel is atomized and dried by adopting a spray granulation process to prepare an aggregate precursor; sintering the aggregate precursor to prepare the magnesium-calcium-cerium stabilized zirconia powder, wherein the step of preparing the magnesium-calcium-cerium stabilized zirconia powder comprises the following steps:
putting the zirconium gel into a spray drying tower for spray drying to prepare an aggregate precursor, wherein the temperature in the spray drying tower is 110-300 ℃;
and sintering the aggregate precursor in a sintering furnace, wherein the aggregate precursor is converted into magnesium-calcium-cerium stabilized zirconia in the sintering process and densification is promoted to obtain micron-sized zirconia powder with nano-crystalline grains, and the internal temperature of the sintering furnace is 900-1200 ℃. In a preferred embodiment of the present application, the spray drying tower has an internal temperature of 230 ℃ and the sintering furnace has an internal temperature of 1200 ℃.
Further, in step S31, the concentration ratio of hydrogen peroxide to zirconium ions is 3: 1-6: 1; the mass ratio of ethanol to hydrogen peroxide is 1: 9-2: 8; the ratio of the total concentration of calcium ions, cerium ions and magnesium ions to the concentration of zirconium ions is 1: 100-10: 100. in a preferred embodiment of the present application, the concentration ratio of hydrogen peroxide to zirconium ions is 4: 1, the mass ratio of ethanol to hydrogen peroxide is 1: 9, the ratio of the total concentration of calcium ions, cerium ions and magnesium ions to the concentration of zirconium ions is 2: 100.
further, in the step S31, the hydrogen peroxide is 30 wt%, and the thickener is 0.5-2 wt%. In a preferred embodiment of the present application, the thickener is present in an amount of 1 weight percent. However, in other embodiments, the weight percent of the thickener can also be 0.5 or 2. When the weight percentage of the thickener added into the zirconium gel is 0.5, the zirconium gel is relatively diluted, the zirconium gel adopts a spray granulation process, and the particles of the magnesium-calcium-cerium-stabilized zirconia powder obtained after sintering the zirconium gel are relatively small; when the weight percentage of the thickener added into the zirconium gel is 2, the zirconium gel is viscous, the zirconium gel adopts a spray granulation process, and the magnesium-calcium-cerium-stabilized zirconia powder obtained after sintering the zirconium gel has larger particles. In the preparation process, the thickening agent with the weight percentage of 0.5-2 is adopted to obtain the aggregate precursor meeting the granularity condition. FIG. 2 shows an SEM of an example of a Mg-Ca-Ce stabilized zirconia powder according to the present application.
In step S31, the thickener is any one of hydroxyethyl cellulose, methyl cellulose, hydroxypropyl methyl cellulose, and hydroxyethyl cellulose ether. In a preferred embodiment of the present application, hydroxyethyl cellulose is used as the thickener.
The thickener is a hydrophilic high molecular polymer. Can be divided into three categories, natural (such as xanthan gum), semi-natural (such as cellulose ether) and pure synthetic (such as polyacrylamide). In the present application, the hydroxyethyl cellulose is used to thicken the zirconium sol so that it forms a zirconium gel. Hydroxyethyl cellulose (HEC), formula (C)2H6O2) n is a white or light yellow, tasteless and nontoxic fibrous or powdery solid, is prepared by etherification reaction of alkali cellulose and ethylene oxide (or chloroethanol), and belongs to nonionic soluble cellulose ether. Has exceptionally good salt solubility in electrolytes, as HEC has good properties of thickening, suspending, dispersing, emulsifying, binding, film forming, moisture protecting, and providing protective colloids. Has the properties of thickening, suspending, binding, emulsifying, dispersing, moisture retaining and the like, and can prepare solutions with different viscosity ranges.
Further, in the step S70, the thermal spraying temperature of the thermal spraying process is 2000-2500 ℃, and the thickness of the coating is 50-100 μm. In a preferred embodiment of the present application, the thermal spray temperature is 2500 ℃ and the coating thickness is 100 μm.
The technical effects that can be achieved by the technical scheme provided by the application are further illustrated by the comparison experiments of each control group.
Control group 1
The sintering bearing net is prepared by adopting the following preparation method, and the preparation method comprises the following steps:
(1) weaving pure nickel wires into a metal woven net by using a full-automatic metal net weaving machine, and folding burrs of the metal woven net on the inner side by using a punching machine, wherein the diameter of the pure nickel wires is 0.3mm, and the mesh number of the metal woven net is 32 meshes;
(2) clamping two side surfaces of the metal mesh by using an aluminum oxide plate, and placing the metal mesh in a vacuum sintering furnace for heat treatment, wherein the internal temperature of the sintering furnace is 600 ℃, and the vacuum degree is 30-70 Pa;
(3) spraying the yttrium stabilized zirconia (8YSZ) for commercial thermal spraying onto the metal mesh obtained in the step (1) by adopting a thermal spraying process to obtain the burning net, wherein the thermal spraying temperature is 2200 ℃, and the thickness of the zirconia coating is 80 microns.
The experimental results are as follows: the sintering net prepared by the control group 1 is used for sintering the MLCC electronic component, the sintering temperature is 800 ℃, and the heat preservation time is 16h each day. The experimental result shows that the surface of the burning net of the control group obviously becomes green after 4 months, namely the surface of the pure nickel is oxidized into nickel oxide.
Control group 2
The firing bearing net is prepared by the following preparation method, and the preparation method comprises the following steps:
(1) nickel-chromium alloy wire (Cr) using full-automatic metal net braiding machine30Ni70) Weaving to form a metal woven net, and folding burrs of the metal woven net on the inner side by using a punching machine, wherein the diameter of the nichrome wire is 0.3mm, and the mesh number of the metal woven net is 32 meshes;
(2) clamping two side surfaces of the metal mesh by using an aluminum oxide plate, and placing the metal mesh in a vacuum sintering furnace for heat treatment, wherein the internal temperature of the sintering furnace is 600 ℃, and the vacuum degree is 30-70 Pa;
(3) spraying the yttrium stabilized zirconia (8YSZ) for commercial thermal spraying onto the metal mesh obtained in the step (1) by adopting a thermal spraying process to obtain the burning net, wherein the thermal spraying temperature is 2200 ℃, and the thickness of the zirconia coating is 80 microns.
The experimental results are as follows: the sintering net prepared by the control group 2 is used for sintering the MLCC electronic component, the sintering temperature is 800 ℃, and the heat preservation time is 16h each day. The results show that after 5 months, the surface of the burning net obviously becomes green, namely the nickel surface is oxidized into nickel oxide. Compared with the control group 1, the control group 2 adopts the nickel-chromium alloy to replace pure nickel to be used as the nickel net matrix, so that the oxidation resistance and the corrosion resistance of the burning net can be improved, and the service time of the burning net of the control group is prolonged.
Control group 3
The firing bearing net is prepared by the following preparation method, and the preparation method comprises the following steps:
(1) nickel-chromium alloy wire (Cr) using full-automatic metal net braiding machine30Ni70) Weaving a metal woven net, and folding burrs of the metal woven net on the inner side by using a punching machine, wherein the diameter of the nichrome wire is 0.3mm, and the mesh number of the metal woven net is 32 meshes;
(2) clamping two side surfaces of the metal mesh by using an aluminum oxide plate, and placing the metal mesh in a vacuum sintering furnace for heat treatment, wherein the internal temperature of the sintering furnace is 600 ℃, and the vacuum degree is 300-;
(3) spraying the yttrium stabilized zirconia (8YSZ) for commercial thermal spraying onto the metal mesh obtained in the step (1) by adopting a thermal spraying process to obtain the burning net, wherein the thermal spraying temperature is 2200 ℃, and the thickness of the zirconia coating is 80 microns.
The experimental results are as follows: the sintering net prepared by the control group 3 is used for sintering the MLCC electronic component, the sintering temperature is 800 ℃, and the heat preservation time is 16h each day. The results show that after 5.5 months, the surface of the burning net obviously becomes green, namely the nickel surface is oxidized into nickel oxide. Compared with the control group 2, the control group 3 performs micro-oxidation treatment on the surface of the nickel-chromium alloy, so that the bonding strength of the nickel-chromium alloy and the zirconia coating can be improved, the corrosion resistance is enhanced, and the service time of the burning bearing net of the control group is prolonged.
Control group 4
The firing bearing net is prepared by the following preparation method, and the preparation method comprises the following steps:
(1) nickel-chromium alloy (Cr) using full-automatic metal net braiding machine30Ni70) Weaving the wires into a metal woven net, and folding the rough edges of the nickel net on the inner side by using a punching machine, wherein the diameter of the nickel-chromium alloy wires is 0.3mm, and the mesh number of the metal woven net is 32 meshes;
(2) clamping two side surfaces of the metal mesh by using an aluminum oxide plate, and placing the metal mesh in a vacuum sintering furnace for heat treatment, wherein the internal temperature of the sintering furnace is 600 ℃, and the vacuum degree is 300-;
(3) ZrOCl2.8H2O、CaCl2、MgCl2、CeCl3Hydrogen peroxide (H)2O230 wt.%) and ethanol were placed in the reaction kettle and stirred for 0.5H, where n (H)2O2):n(Zr4+)＝4:1，m(C2H5OH):m(H2O2)＝1:9，n(Ca2+):n(Zr4+)＝5:100，n(Mg2+):n(Zr4+) 3: 100. Then raising the temperature to 70 ℃ and continuing stirring until the suspension is clear and no bubbles are generated, and finally adding ammonia water to adjust the pH value to 5 to obtain zirconium sol;
(4) adding 1 wt% of hydroxyethyl cellulose into the zirconium sol, stirring for 0.5h by using an electric stirrer to prepare zirconium gel, and then placing the zirconium gel into a spray drying tower for spray drying, wherein the temperature in the drying tower is 230 ℃, so as to prepare an aggregate precursor;
(5) sintering the aggregate precursor in a sintering furnace to convert the aggregate precursor into magnesium-calcium stabilized zirconia powder and promote densification, wherein the sintering temperature is 1200 ℃;
(6) and (3) spraying the magnesium-calcium stabilized zirconia powder obtained in the step (5) onto the metal mesh obtained in the step (2) by adopting a thermal spraying process to obtain the burning net, wherein the thermal spraying temperature is 2200 ℃, and the zirconia coating is 80 microns.
The experimental results are as follows: the sintering net prepared by the control group 4 is used for sintering the MLCC electronic component, the sintering temperature is 800 ℃, and the heat preservation time is 16h each day. The results show that after 6.5 months, the surface of the burning net obviously becomes green, namely the nickel surface is oxidized into nickel oxide. Compared with a control group 3, the control group 4 uses calcium-magnesium stabilized zirconia powder with a nano structure for thermal spraying, the nano structure can effectively improve the mechanical strength of the coating and the bonding strength of the nickel-chromium alloy and the zirconia coating, the grain refinement can promote the ageing resistance of the zirconia coating, and magnesium and calcium also have a promoting effect on the ageing resistance of the zirconia coating, so that the burning bearing net prepared by the control group has stronger corrosion resistance, and the service time is obviously prolonged.
Control group 5
The firing bearing net is prepared by the following preparation method, and the preparation method comprises the following steps:
(1) nickel-chromium alloy (Cr) using full-automatic metal net braiding machine30Ni70) Weaving the wires into a metal woven net, and folding burrs of the nickel net on the inner side by using a punching machine, wherein the diameter of the nickel wires is 0.3mm, and the mesh number of the metal woven net is 32 meshes;
(2) clamping two side surfaces of the metal mesh by using an aluminum oxide plate, and placing the metal mesh in a vacuum sintering furnace for heat treatment, wherein the internal temperature of the sintering furnace is 600 ℃, and the vacuum degree is 300-;
(3) ZrOCl2.8H2O、CaCl2、MgCl2、CeCl3Hydrogen peroxide (H)2O230 wt.%) and ethanol were placed in the reaction kettle and stirred for 0.5H, where n (H)2O2):n(Zr4+)＝4:1，m(C2H5OH):m(H2O2)＝1:9，n(Ca2+):n(Zr4+)＝4:100，n(Mg2+):n(Zr4+)＝2:100，n(Ce2+):n(Zr4+) 2: 100. Then raising the temperature to 70 ℃ and continuing stirring until the suspension is clear and no bubbles are generated, and finally adding ammonia water to adjust the pH value to 5 to obtain zirconium sol;
(4) adding 1 wt% of hydroxyethyl cellulose into the zirconium sol, stirring for 0.5h by using an electric stirrer to prepare zirconium gel, and then placing the zirconium gel into a spray drying tower for spray drying, wherein the temperature in the drying tower is 230 ℃, so as to prepare an aggregate precursor;
(5) and sintering the aggregate precursor in a sintering furnace to convert the aggregate precursor into magnesium-calcium stabilized zirconia powder and promote densification, wherein the sintering temperature is 1200 ℃. Wherein the microstructure of the magnesium-calcium stabilized zirconia powder is shown in figure 1;
(6) and (3) spraying the magnesium-calcium stabilized zirconia powder obtained in the step (5) onto the metal mesh obtained in the step (2) by adopting a thermal spraying process to obtain the sintering net, wherein the thermal spraying temperature is 2200 ℃, the zirconia coating is 80 microns, and the finally obtained sintering net is specifically shown in figure 2.
The experimental results are as follows: the sintering net prepared by the control group 5 is used for sintering the MLCC electronic component, the sintering temperature is 800 ℃, and the heat preservation time is 16h each day. The results show that after 7 months, the surface of the burning net obviously becomes green, namely the nickel surface is oxidized into nickel oxide. Compared with the control group 4, the control group 5 adds cerium as a stabilizer on the basis of calcium and magnesium, so that the ageing resistance of the zirconia coating is further improved, and the service time of the burning net prepared by the control group is further prolonged.
The preparation method of the sintering-bearing net is simple in preparation process, low in preparation cost and high in yield, and is particularly suitable for sintering and bearing sintering of small ceramic electronic components; the burning bearing net prepared by the preparation method has the advantages of excellent mechanical property, difficult deformation, strong corrosion resistance and long service life. The preparation method comprises the steps of fixing the metal mesh, processing the metal mesh by adopting a vacuum heating and smoothing process, and realizing micro-oxidation treatment on the surface of the metal mesh by using a vacuum sintering furnace, so that the internal stress caused by weaving in the metal mesh is eliminated, the metal mesh is prevented from deforming in the thermal spraying process, the combination of the coating and the metal mesh is further prevented from being influenced, and the combination strength of the coating and the metal mesh can be further improved by the micro-oxidation treatment. In addition, the magnesium-calcium-cerium-stabilized zirconia powder with the nano structure is prepared by preparing zirconium sol and zirconium gel and combining a spray granulation process, the fine magnesium-calcium-cerium-stabilized zirconia powder is more beneficial to forming a high-aging-resistance coating, the bonding strength and the mechanical property of the coating and a metal mesh can be obviously improved, and meanwhile, the magnesium-calcium-cerium-stabilized zirconia has excellent aging resistance, the aging resistance of the coating can be improved, the corrosion resistance and the oxidation resistance of the burning bearing net are further improved, and the service life of the burning bearing net is prolonged.
Referring to fig. 3, in order to achieve the above object, the present application further provides a setter mesh, where the setter mesh is prepared by the method for preparing a setter mesh for sintering a ceramic electronic component, and the concrete structure of the setter mesh refers to the above embodiment.
The above description is only an alternative embodiment of the present application, and not intended to limit the scope of the present application, and all modifications and equivalents of the technical solutions that can be directly or indirectly applied to other related fields without departing from the spirit of the present application are intended to be included in the scope of the present application.
Claims (10)
1. A preparation method of a sintering bearing net for sintering ceramic electronic components is characterized by comprising the following steps:
weaving the metal wires to form a metal mesh;
fixing the metal mesh, and heating the metal mesh in vacuum by adopting micro-oxidation treatment;
adding zirconium oxychloride, calcium chloride, magnesium chloride, cerium trichloride and hydrogen peroxide into a solvent, and mixing and heating to obtain zirconium sol;
adding a thickening agent into the zirconium sol, and mixing and stirring to obtain zirconium gel;
atomizing and drying the zirconium gel by adopting a spray granulation process to prepare an aggregate precursor;
sintering the aggregate precursor to obtain magnesium-calcium-cerium stabilized zirconia powder;
and spraying the magnesium-calcium-cerium stabilized zirconia powder onto the metal mesh by adopting a thermal spraying process to obtain the sintering bearing mesh.
2. The method of claim 1, wherein the step of weaving the metal wires to form the metal mesh comprises:
weaving a nichrome wire into a metal woven net by adopting a weaving machine, and folding burrs of the metal woven net on the inner side by using a punching machine, wherein the diameter of the nichrome wire is 0.15-0.6 mm, and the mesh number of the metal woven net is 20-60 meshes.
3. The method for manufacturing a setter mesh for sintering a ceramic electronic component as set forth in claim 1, wherein the step of fixing the metal mesh and heating the metal mesh in vacuum by means of micro-oxidation treatment includes:
and clamping two side surfaces of the metal mesh by using an aluminum oxide plate, and placing the metal mesh into a vacuum sintering furnace for heat treatment, wherein the internal temperature of the vacuum sintering furnace is 400-800 ℃, and the vacuum degree is 30-1000 Pa.
4. The method for producing a setter screen for firing ceramic electronic components as set forth in claim 1, wherein:
the method comprises the following steps of adding zirconium oxychloride, calcium chloride, magnesium chloride, cerium trichloride and hydrogen peroxide into a solvent, and mixing and heating to prepare zirconium sol: zirconium oxychloride, calcium chloride, magnesium chloride, cerium trichloride, hydrogen peroxide and ethanol are placed in a reaction kettle and stirred for 0.5 hour, then heated to 70 ℃ and continuously stirred until suspension is clear and no bubbles are generated, and then ammonia water is added to adjust the pH value to 5 to prepare zirconium sol;
the step of adding the thickener to the zirconium sol and preparing the zirconium gel by mixing and stirring comprises the following steps: adding a thickening agent into the zirconium sol, and stirring the zirconium sol for 0.5 hour to obtain zirconium gel.
5. The method for preparing the sintering load net for sintering the ceramic electronic component as claimed in claim 4, wherein the zirconium gel is atomized and dried by a spray granulation process to obtain an aggregate precursor; sintering the aggregate precursor to prepare the magnesium-calcium-cerium stabilized zirconia powder, wherein the step of preparing the magnesium-calcium-cerium stabilized zirconia powder comprises the following steps:
putting the zirconium gel into a spray drying tower for spray drying to prepare an aggregate precursor, wherein the temperature in the spray drying tower is 110-300 ℃;
and sintering the aggregate precursor in a sintering furnace to prepare the magnesium-calcium-cerium stabilized zirconia powder, wherein the internal temperature of the sintering furnace is 900-1200 ℃.
6. The method for preparing the setter mesh for sintering the ceramic electronic component as set forth in claim 4, wherein a concentration ratio of hydrogen peroxide to zirconium ions is 3: 1-6: 1; the mass ratio of ethanol to hydrogen peroxide is 1: 9-2: 8; the ratio of the total concentration of calcium ions, cerium ions and magnesium ions to the concentration of zirconium ions is 1: 100-10: 100.
7. the method for preparing the setter mesh for sintering the ceramic electronic component as set forth in claim 4, wherein the hydrogen peroxide is 30 wt%, and the thickener is 0.5-2 wt%.
8. The method for producing a setter mesh for firing ceramic electronic components as set forth in claim 1, wherein the thickener is any one of hydroxyethyl cellulose, methyl cellulose, hydroxypropyl methyl cellulose, and hydroxyethyl cellulose ether.
9. The method for manufacturing a setter mesh for sintering ceramic electronic component as set forth in claim 1, wherein the thermal spraying temperature in the thermal spraying process is 2000 ℃ to 2500 ℃, and the thickness of the coating layer is 50 μm to 100 μm.
10. The sintering setter net for ceramic electronic component manufactured by the manufacturing method as set forth in any one of claims 1 to 9.
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