CN108329023B - Preparation method of zinc oxide based nano composite powder resistance card - Google Patents
Preparation method of zinc oxide based nano composite powder resistance card Download PDFInfo
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- CN108329023B CN108329023B CN201810180412.6A CN201810180412A CN108329023B CN 108329023 B CN108329023 B CN 108329023B CN 201810180412 A CN201810180412 A CN 201810180412A CN 108329023 B CN108329023 B CN 108329023B
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- zinc oxide
- composite powder
- nano composite
- based nano
- salt
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 173
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 86
- 239000000843 powder Substances 0.000 title claims abstract description 64
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000001354 calcination Methods 0.000 claims abstract description 20
- 238000000227 grinding Methods 0.000 claims abstract description 17
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- 238000005507 spraying Methods 0.000 claims abstract description 13
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 238000000576 coating method Methods 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims description 29
- 239000002184 metal Substances 0.000 claims description 29
- 150000003839 salts Chemical class 0.000 claims description 27
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- 239000012153 distilled water Substances 0.000 claims description 23
- 239000000243 solution Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 239000008139 complexing agent Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 9
- 235000006408 oxalic acid Nutrition 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 150000003751 zinc Chemical class 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000003607 modifier Substances 0.000 claims description 6
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 5
- 150000001462 antimony Chemical class 0.000 claims description 5
- 150000001621 bismuth Chemical class 0.000 claims description 5
- 150000001844 chromium Chemical class 0.000 claims description 5
- 150000001868 cobalt Chemical class 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 159000000003 magnesium salts Chemical class 0.000 claims description 5
- 150000002696 manganese Chemical class 0.000 claims description 5
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 5
- 239000001393 triammonium citrate Substances 0.000 claims description 5
- 235000011046 triammonium citrate Nutrition 0.000 claims description 5
- 150000003746 yttrium Chemical class 0.000 claims description 5
- 150000003608 titanium Chemical class 0.000 claims description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 3
- 229920000053 polysorbate 80 Polymers 0.000 claims description 3
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 238000000498 ball milling Methods 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 abstract description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 abstract description 8
- 238000005469 granulation Methods 0.000 abstract description 7
- 230000003179 granulation Effects 0.000 abstract description 6
- 238000009826 distribution Methods 0.000 abstract description 5
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 4
- 150000004706 metal oxides Chemical class 0.000 abstract description 4
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 238000003980 solgel method Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 239000000306 component Substances 0.000 description 8
- 239000002131 composite material Substances 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- QYIGOGBGVKONDY-UHFFFAOYSA-N 1-(2-bromo-5-chlorophenyl)-3-methylpyrazole Chemical compound N1=C(C)C=CN1C1=CC(Cl)=CC=C1Br QYIGOGBGVKONDY-UHFFFAOYSA-N 0.000 description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 2
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 description 2
- 229940009827 aluminum acetate Drugs 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 2
- WYYQVWLEPYFFLP-UHFFFAOYSA-K chromium(3+);triacetate Chemical compound [Cr+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WYYQVWLEPYFFLP-UHFFFAOYSA-K 0.000 description 2
- 229940011182 cobalt acetate Drugs 0.000 description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 2
- JVLRYPRBKSMEBF-UHFFFAOYSA-K diacetyloxystibanyl acetate Chemical compound [Sb+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JVLRYPRBKSMEBF-UHFFFAOYSA-K 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 2
- 239000011654 magnesium acetate Substances 0.000 description 2
- 235000011285 magnesium acetate Nutrition 0.000 description 2
- 229940069446 magnesium acetate Drugs 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 229940071125 manganese acetate Drugs 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- NFSAPTWLWWYADB-UHFFFAOYSA-N n,n-dimethyl-1-phenylethane-1,2-diamine Chemical compound CN(C)C(CN)C1=CC=CC=C1 NFSAPTWLWWYADB-UHFFFAOYSA-N 0.000 description 2
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 2
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical compound [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 description 2
- 239000004246 zinc acetate Substances 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- INNSZZHSFSFSGS-UHFFFAOYSA-N acetic acid;titanium Chemical compound [Ti].CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O INNSZZHSFSFSGS-UHFFFAOYSA-N 0.000 description 1
- 229910000410 antimony oxide Inorganic materials 0.000 description 1
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 description 1
- JRLDUDBQNVFTCA-UHFFFAOYSA-N antimony(3+);trinitrate Chemical compound [Sb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JRLDUDBQNVFTCA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 231100000045 chemical toxicity Toxicity 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000000887 hydrating effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 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
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 239000012856 weighed raw material Substances 0.000 description 1
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- C04B35/453—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 zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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Abstract
The invention discloses a preparation method of a zinc oxide-based nano composite powder resistor disc, which comprises the steps of preparing zinc oxide-based nano composite powder, containing water, tabletting, sintering, cleaning a grinding sheet, spraying aluminum and coating insulating glaze on the side surface, thereby finally obtaining the zinc oxide-based nano composite powder resistor disc. The zinc oxide-containing metal oxides prepared by the chemical sol-gel method are all nano-level powder, all components are uniformly mixed, and the particle size distribution of particles is small, so that the potential gradient, the through-current capacity and the large-current impact resistance of the zinc oxide resistance chip are improved; the preparation of the zinc oxide resistance card does not need ball milling and granulation processes, so that the cost can be saved, the production efficiency is improved, and the batch production is facilitated; according to the invention, polyvinyl alcohol as an adhesive is not added, the rough blank prepared by tabletting can keep good strength, cracks can not occur during calcination, the production cost is reduced, and the method is environment-friendly.
Description
Technical Field
The invention belongs to the technical field of high-voltage electrical sensitive ceramic materials, and relates to a preparation method of a zinc oxide-based nano composite powder resistor disc.
Background
The zinc oxide resistance card is a multi-component metal oxide polycrystalline semiconductor ceramic, which takes zinc oxide (ZnO) as a main raw material and is added with a plurality of metal oxide components (Bi)2O3、MnO2、Co2O3、Cr2O3、Sb2O3、SiO2、TiO2Etc.) are prepared by typical ceramic material processes. The zinc oxide resistor disc is used as a core component of the arrester, and the performance of the zinc oxide resistor disc directly influences the performance of a zinc oxide arrester product. The zinc oxide arrester resistance card for the extra-high voltage level is owned by only a few countries at present due to complex technology and high manufacturing cost, and companies with the capacity of producing the extra-high voltage zinc oxide arrester and the high-voltage sensitive voltage gradient valve plate abroad comprise: japanese TMT&D (combined by Mitsubishi, Toshiba in 2002) and Hitachi, Russian Federation, GE, OB, Sweden ABB, England EMP. In order to accelerate the development of the power industry in China, get rid of the dependence on foreign technologies, and develop the zinc oxide resistance card with high circulation capacity and high voltage gradient, the zinc oxide resistance card has practical significance.
The research finds that the main reason influencing the current capacity of the resistor disc is that the microscopic uneven structure inside the resistor disc causes the uneven distribution of current, and the heat generated thereby causes the formation of internal thermal stress, so that the resistor disc is broken down or burst. The voltage gradient of the resistive sheet is related to the size of the grain diameter of the grains composing the resistive sheet, and the smaller the grain diameter of the grains is, the larger the voltage gradient of the resistive sheet is.
The production process flow of the existing zinc oxide resistance card is as follows: batching, grinding, granulating, hydrating, tabletting, sintering, cleaning a grinding sheet and spraying aluminum on the side surface insulating layer to finally obtain the zinc oxide resistance card, and has the disadvantages of complex process, long production period and low production efficiency; the ball milling process is generally adopted, the particle size of the ball milled particles is large, the mixing effect is poor, and nano-scale raw material powder is difficult to obtain; furthermore, it is necessary to add polyvinyl alcohol, a binder which decomposes the CO obtained during sintering, to the slurry during granulation2、H2O and carbon black, and the reaction product of the catalyst,the porosity of the zinc oxide resistance card is increased, and the uniformity of the internal structure of the resistance card is reduced; meanwhile, the production cost is increased, and the polyvinyl alcohol has chemical toxicity, so that the safety production of operators is not facilitated, and the environment is polluted.
Disclosure of Invention
The invention aims to provide a preparation method of a zinc oxide-based nano composite powder resistor disc, and the prepared zinc oxide resistor disc has the advantages of uniform components, small particle size, low cost, environmental friendliness, high voltage gradient, strong flow capacity and the like.
The invention relates to a preparation method of a zinc oxide-based nano composite powder resistor disc, which comprises the following steps:
(1) preparing a mixture of a plurality of metal salts including zinc salt into an aqueous solution, dripping a surface modifier into the aqueous solution, and uniformly stirring to obtain a metal salt mixed solution;
(2) dissolving a complexing agent in absolute ethyl alcohol to prepare absolute ethyl alcohol solution of the complexing agent, dripping the metal salt mixed solution into the absolute ethyl alcohol solution of the complexing agent, stirring at a set temperature to fully dissolve the metal salt mixed solution, then preserving heat, and filtering to obtain white gel;
(3) washing the white gel, drying, putting the white gel into a tubular furnace, calcining at a set temperature, washing the obtained product, and drying to obtain zinc oxide-based nano composite powder;
(4) water content: adding a predetermined amount of distilled water into the zinc oxide-based nano composite powder, and fully and uniformly stirring;
(5) tabletting: putting the powder containing water into a tablet press to press into a sheet rough blank;
(6) and (3) sintering: calcining the rough blank in a muffle furnace;
(7) grinding and cleaning: grinding two end faces of the resistance card, and cleaning the resistance card by using distilled water;
(8) spraying aluminum and coating insulating glaze on the side surfaces: and spraying aluminum electrodes on two end surfaces of the resistance chip, and coating insulating glaze on the side surfaces to obtain the zinc oxide-based nano composite powder resistance chip.
Preferably, the mole percentages of the components of the mixture of metal salts are as follows: zinc salt: 80-90%, bismuth salt: 4% -5%, antimony salt: 4% -5%, magnesium salt: 1% -2%, aluminum salt: 1% -2%, cobalt salt: 1% -2%, chromium salt: 0% -1%, manganese salt: 0% -1%, titanium salt: 0% -1%, yttrium salt: 0 to 0.1 percent.
Preferably, the metal salt is one of nitrate and acetate.
Preferably, the concentration of the metal salt solution is 0.6-0.8 mol/L.
Preferably, the surface modifier is one or more of sodium dodecyl sulfate, triammonium citrate and tween 80, and the dosage of the surface modifier is 2 to 3 percent of the weight of the metal salt.
Preferably, the complexing agent is one or more of oxalic acid, citric acid and triammonium citrate.
Preferably, the concentration of the absolute ethyl alcohol solution of the complexing agent is 0.6-0.8 mol/L.
Preferably, in the step (2), the stirring temperature is 80-90 ℃, and the stirring time is 1-2 hours; the heat preservation temperature is 80-90 ℃, and the heat preservation time is 0.5-1 h.
Preferably, in the step (3), the drying temperature of the white gel is 80-90 ℃, and the drying time is 1-2 hours.
Preferably, in the step (3), the calcination temperature of the gel is 300-400 ℃, and the heat preservation time is 2-3 h.
Preferably, in the step (4), 1 to 1.5 mass percent of distilled water is added into the zinc oxide-based nano composite powder.
Preferably, in the step (6), the calcining temperature is 1100-1200 ℃, and the heat preservation time is 90-100 h.
The invention also provides the zinc oxide-based nano composite powder resistor disc prepared by the preparation method of the zinc oxide-based nano composite powder resistor disc.
The principle of the invention is as follows: the invention adopts a chemical sol-gel method to prepare the nano-scale composite powder, and all components are uniformly mixed from the molecular level, so that ball milling is not needed, and the gel adopts incomplete calcination (300-400 ℃ C.) during calcination, and the heat preservation is carried outThe time is 2-3 h), so that partial hydroxyl groups are reserved in the prepared composite powder, the interaction between the powder can be enhanced due to the hydrogen bonds between the hydroxyl groups, a binding agent polyvinyl alcohol is not required to be added, granulation is not required, the blank prepared by directly carrying out water-containing and tabletting on the zinc oxide-based nano composite powder can also keep good strength, cracks can not appear during calcination, and CO can not be generated during sintering due to the fact that polyvinyl alcohol is not required to be added2、H2And the porosity of the zinc oxide resistance card is reduced by the O and the carbon black, and the distribution uniformity of each component of the resistance card is improved, so that the potential gradient, the through-current capacity and the large-current impact resistance capacity of the zinc oxide resistance card are improved.
Compared with the prior art, the invention has the following beneficial technical effects:
(1) the various metal oxides including zinc oxide prepared by the chemical sol-gel method are nano-level powder, all the components are uniformly mixed, and the particle size distribution of the particles is small, so that the potential gradient, the through-current capacity and the large-current impact resistance of the zinc oxide resistance chip are improved.
(2) The preparation of the zinc oxide resistance card does not need ball milling and granulation processes, so that the cost can be saved, the production efficiency is improved, and the batch production is facilitated.
(3) According to the invention, polyvinyl alcohol as an adhesive is not added, the rough blank prepared by tabletting can keep good strength, cracks can not occur during calcination, the production cost is reduced, and the method is environment-friendly.
Drawings
Fig. 1 is an SEM image of the microstructure of the zinc oxide resistor sheet obtained in example 1 of the present invention.
Fig. 2 is an SEM image of the microstructure of the zinc oxide resistor sheet obtained in example 2 of the present invention.
Fig. 3 is an SEM image of the microstructure of the zinc oxide resistor sheet obtained in example 3 of the present invention.
Fig. 4 is an SEM image of the microstructure of the zinc oxide resistor sheet prepared in comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by those skilled in the art without any creative work based on the embodiments of the present invention belong to the protection scope of the present invention.
The experimental procedures described in the following examples are conventional unless otherwise specified, and the reagents and materials described therein are commercially available without further specification.
Example 1
The raw materials of this example were prepared according to the following mole percentages, and the specific formulation was as follows:
zinc salt: 85%, bismuth salt: 4%, antimony salt: 4%, magnesium salt: 2%, aluminum salt: 2%, cobalt salt: 1.5%, chromium salt: 0.5%, manganese salt: 0.5%, titanium salt: 0.4%, yttrium salt: 0.1 percent.
The invention relates to a preparation method of a zinc oxide-based nano composite powder resistor disc, which comprises the following steps:
(1) accurately weighing 101.108g of zinc acetate, 10.036g of bismuth acetate, 7.774g of antimony acetate, 1.846g of magnesium acetate, 2.652g of aluminum acetate, 1.726g of cobalt acetate, 0.744g of chromium acetate, 0.562g of manganese acetate, 0.738g of titanium acetate and 0.173g of yttrium acetate, dissolving in 1L of distilled water to form a metal salt water solution, adding 2.547g of sodium dodecyl sulfate, and stirring vigorously to dissolve the metal salt water solution fully to obtain a metal salt mixed solution;
(2) accurately weighing 162g of oxalic acid, dissolving in 3L of absolute ethyl alcohol to prepare an oxalic acid absolute ethyl alcohol solution, slowly dripping the prepared metal salt mixed solution into the oxalic acid absolute ethyl alcohol solution, placing the solution in a water bath at 85 ℃ to stir for 1 hour to fully dissolve the solution, then preserving heat to react for 0.5 hour, and filtering to obtain white gel;
(3) washing the white gel twice with distilled water and absolute ethyl alcohol respectively, placing the white gel in a vacuum drying oven at 80 ℃ for drying for 2h, placing the dried gel in a tubular furnace at 300 ℃ for calcining for 3h, washing the obtained product twice with distilled water and absolute ethyl alcohol respectively, and drying to obtain zinc oxide-based nano composite powder;
(4) water content: adding 1% of distilled water by mass fraction into the zinc oxide-based nano composite powder, and fully and uniformly stirring;
(5) tabletting: putting the powder containing water into a tablet press to press into a sheet rough blank;
(6) and (3) sintering: calcining the rough blank at 1100 ℃ for 100 h;
(7) grinding and cleaning: grinding two ends of the resistance card, and cleaning the resistance card by using distilled water;
(8) spraying aluminum and coating insulating glaze on the side surfaces: and spraying aluminum electrodes at two ends of the resistance chip, and coating insulating glaze on the side surface to obtain the zinc oxide-based nano composite powder resistance chip.
The obtained zinc oxide-based nano composite powder is prepared into a resistor disc for a lightning arrester with the specification of phi 70 (the diameter of an outer ring is 72mm, the diameter of an inner ring is 26mm, and the height is 22.5mm), the microstructure of the zinc oxide resistor disc is analyzed by adopting a scanning electron microscope SEM (scanning electron microscope), as shown in figure 1, the grain size is 7.6 mu m, and the voltage gradient, the current capacity and the large-current impact resistance capacity of the resistor disc are tested, as shown in Table 1.
Example 2
The raw materials of this example were prepared according to the following mole percentages, and the specific formulation was as follows:
zinc salt: 85%, bismuth salt: 4.5%, antimony salt: 4.5%, magnesium salt: 1%, aluminum salt: 2%, cobalt salt: 1.8%, chromium salt: 0.6%, manganese salt: 0.5%, yttrium salt: 0.1 percent.
The invention relates to a preparation method of a zinc oxide-based nano composite powder resistor disc, which comprises the following steps:
(1) accurately weighing 108.885g of zinc acetate, 12.159g of bismuth acetate, 9.419g of antimony acetate, 0.994g of magnesium acetate, 2.856g of aluminum acetate, 2.23g of cobalt acetate, 0.962g of chromium acetate, 0.606g of manganese acetate and 0.186g of yttrium acetate, dissolving in 1L of distilled water to form a metal salt water solution, adding 2.766g of tween 80, and vigorously stirring to fully dissolve the metal salt water solution to obtain a metal salt mixed solution;
(2) accurately weighing 346g of citric acid, dissolving in 3L of absolute ethyl alcohol to prepare an absolute ethyl alcohol solution of the citric acid, slowly dripping the prepared metal salt mixed solution into the absolute ethyl alcohol solution of the citric acid, placing the solution in a water bath at 80 ℃ and stirring for 2 hours to fully dissolve the solution, preserving heat and reacting for 1 hour, and filtering to obtain white gel;
(3) washing the white gel twice with distilled water and absolute ethyl alcohol respectively, drying in a vacuum drying oven at 90 ℃ for 1h, calcining the dried gel in a tubular furnace at 400 ℃ for 3h, washing the obtained product twice with distilled water and absolute ethyl alcohol respectively, and drying to obtain zinc oxide-based nano composite powder;
(4) water content: adding 1.5 percent of distilled water by mass fraction into the zinc oxide-based nano composite powder, and fully and uniformly stirring;
(5) tabletting: putting the powder containing water into a tablet press to press into a sheet rough blank;
(6) and (3) sintering: calcining the rough blank at 1150 ℃ for 96 h;
(7) grinding and cleaning: grinding two ends of the resistance card, and cleaning the resistance card by using distilled water;
(8) spraying aluminum and coating insulating glaze on the side surfaces: and spraying aluminum electrodes at two ends of the resistance chip, and coating insulating glaze on the side surface to obtain the zinc oxide-based nano composite powder resistance chip.
The obtained zinc oxide-based nano composite powder is prepared into a resistor disc for a lightning arrester with the specification of phi 70 (the diameter of an outer ring is 72mm, the diameter of an inner ring is 26mm, and the height is 22.5mm), the microstructure of the zinc oxide resistor disc is analyzed by adopting a scanning electron microscope SEM (scanning electron microscope), as shown in figure 2, the grain size is 8.1 mu m, and the voltage gradient, the current capacity and the large-current impact resistance capacity of the resistor disc are tested, as shown in Table 1.
Example 3
The raw materials of this example were prepared according to the following mole percentages, and the specific formulation was as follows:
zinc salt: 85%, bismuth salt: 5%, antimony salt: 5%, magnesium salt: 1%, aluminum salt: 1%, cobalt salt: 1.4%, chromium salt: 0.5%, manganese salt: 0.5%, titanium salt: 0.5%, yttrium salt: 0.1 percent.
The invention relates to a preparation method of a zinc oxide-based nano composite powder resistor disc, which comprises the following steps:
(1) accurately weighing 128.52g of zinc nitrate, 15.8g of bismuth nitrate, 12.32g of antimony nitrate, 1.184g of magnesium nitrate, 1.704g of aluminum nitrate, 2.05g of cobalt nitrate, 0.952g of chromium nitrate, 0.716g of manganese nitrate, 1.184g of titanium nitrate and 0.22g of yttrium nitrate, dissolving in 1L of distilled water to form a metal salt aqueous solution, adding 3.293g of triammonium citrate, and vigorously stirring to fully dissolve the metal salt aqueous solution to obtain a metal salt mixed solution;
(2) accurately weighing 162g of oxalic acid, dissolving in 3L of absolute ethyl alcohol to prepare an absolute ethyl alcohol solution of oxalic acid, slowly dripping the prepared metal salt mixed solution into the absolute ethyl alcohol solution of oxalic acid, stirring in a water bath at 90 ℃ for 1h to fully dissolve the metal salt mixed solution, preserving heat for 0.5h, and filtering to obtain white gel;
(3) washing the white gel twice with distilled water and absolute ethyl alcohol respectively, placing the white gel in a vacuum drying oven at 85 ℃ for drying for 2h, placing the dried gel in a tubular furnace at 350 ℃ for calcining for 2.5h, washing the obtained product twice with distilled water and absolute ethyl alcohol respectively, and drying to obtain zinc oxide-based nano composite powder;
(4) water content: adding 1.2 mass percent of distilled water into the zinc oxide-based nano composite powder, and fully and uniformly stirring;
(5) tabletting: putting the powder containing water into a tablet press to press into a sheet rough blank;
(6) and (3) sintering: calcining the rough blank at 1200 ℃ for 90 hours;
(7) grinding and cleaning: grinding two ends of the resistance card, and cleaning the resistance card by using distilled water;
(8) spraying aluminum and coating insulating glaze on the side surfaces: and spraying aluminum electrodes at two ends of the resistance chip, and coating insulating glaze on the side surface to obtain the zinc oxide-based nano composite powder resistance chip.
The obtained zinc oxide-based nano composite powder is prepared into a resistor disc for a lightning arrester with the specification of phi 70 (the diameter of an outer ring is 72mm, the diameter of an inner ring is 26mm, and the height is 22.5mm), the microstructure of the zinc oxide resistor disc is analyzed by adopting a scanning electron microscope SEM (scanning electron microscope), as shown in figure 3, the grain size is 8.0 mu m, and the voltage gradient, the current capacity and the large-current impact resistance capacity of the resistor disc are tested.
Comparative example 1
The preparation method of the zinc oxide-based composite powder resistor disc obtained by adopting a common ball milling method comprises the following steps:
(1) preparing raw materials:
weighing 44.007g of zinc oxide, 3.471g of bismuth oxide, 2.952g of antimony oxide, 0.324g of magnesium oxide, 0.288g of aluminum oxide, 0.486g of cobalt oxide and 0.192g of chromium oxide, mixing, and then putting into a ball mill for grinding for 12 hours to obtain zinc oxide-based composite powder;
(2) grinding: adding the weighed raw materials into distilled water with the mass fraction of 300%, uniformly stirring, and then putting into a sand mill for grinding for 2 hours;
(3) and (3) granulation: adding 5% of polyvinyl alcohol by mass fraction into the ground slurry, and then putting the slurry into a granulator for spray granulation;
(4) water content: adding 1.5 percent of distilled water by mass fraction into the granulated powder, and fully and uniformly stirring;
(5) tabletting: putting the powder containing water into a tablet press to press into a sheet rough blank;
(6) and (3) sintering: calcining the rough blank at 1150 ℃ for 96 h;
(7) grinding and cleaning: grinding two ends of the resistance card, and cleaning the resistance card by using distilled water;
(8) spraying aluminum and coating insulating glaze on the side surfaces: and spraying aluminum electrodes on two ends of the resistor disc, and coating insulating glaze on the side surface to obtain the zinc oxide resistor disc for the lightning arrester.
The obtained zinc oxide-based nano composite powder is prepared into a resistor disc for a lightning arrester with the specification of phi 70 (the diameter of an outer ring is 72mm, the diameter of an inner ring is 26mm, and the height is 22.5mm), the microstructure of the zinc oxide-based composite powder resistor disc obtained by a ball milling method is analyzed by adopting a scanning electron microscope SEM (scanning electron microscope), as shown in figure 4, the grain size is 13.2 mu m, and the voltage gradient, the current capacity and the large-current impact resistance capacity of the resistor disc are tested, as shown in Table 1.
TABLE 1 comparison of parameters of zinc oxide-based composite powder resistance card
It can be seen from examples 1-3 and comparative example 1 that the size of the particle size of the zinc oxide resistance card synthesized by the method provided by the present invention is much smaller than that of the zinc oxide resistance card obtained by the conventional ball milling method, and the potential gradient and the current capacity of the zinc oxide resistance card prepared by using the zinc oxide-based nano composite powder synthesized by the method provided by the present invention are significantly improved compared with those of the zinc oxide resistance card prepared by the conventional method, which indicates that the zinc oxide-based nano composite powder synthesized by the method provided by the present invention has more uniform components and particle size distribution compared with the zinc oxide-based composite powder obtained by the conventional ball milling method. The process of preparing the zinc oxide resistance card by the method provided by the invention does not need ball milling and granulation processes, and does not need adding adhesive polyvinyl alcohol, so that the prepared zinc oxide resistance card still has good performance, the production cost is reduced, and the production efficiency is improved.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-described embodiments. Modifications and variations that may occur to those skilled in the art without departing from the spirit and scope of the invention are to be considered as within the scope of the invention.
Claims (9)
1. A preparation method of a zinc oxide based nano composite powder resistance card comprises the following steps:
(1) preparing a mixture of a plurality of metal salts including zinc salt into an aqueous solution, dripping a surface modifier into the aqueous solution, and uniformly stirring to obtain a metal salt mixed solution;
(2) dissolving a complexing agent in absolute ethyl alcohol to prepare absolute ethyl alcohol solution of the complexing agent, dripping the metal salt mixed solution into the absolute ethyl alcohol solution of the complexing agent, stirring at a set temperature to fully dissolve the metal salt mixed solution, then preserving heat, and filtering to obtain white gel;
(3) washing the white gel, drying, putting the white gel into a tubular furnace, calcining at a set temperature, washing the obtained product, and drying to obtain zinc oxide-based nano composite powder;
(4) water content: adding a predetermined amount of distilled water into the zinc oxide-based nano composite powder, and fully and uniformly stirring;
(5) tabletting: putting the powder containing water into a tablet press to press into a sheet rough blank;
(6) and (3) sintering: calcining the rough blank in a muffle furnace;
(7) grinding and cleaning;
(8) spraying aluminum and coating insulating glaze on the side surface;
in the step (3), the calcination temperature of the gel is 300-400 ℃, and the heat preservation time is 2-3 h.
2. The method for preparing the zinc oxide-based nano composite powder resistance card according to claim 1, wherein the mixture of the plurality of metal salts comprises the following components in percentage by mole: zinc salt: 80-90%, bismuth salt: 4% -5%, antimony salt: 4% -5%, magnesium salt: 1% -2%, aluminum salt: 1% -2%, cobalt salt: 1% -2%, chromium salt: 0% -1%, manganese salt: 0% -1%, titanium salt: 0% -1%, yttrium salt: 0 to 0.1 percent, and the sum of all the components is 100 percent.
3. The method for preparing the zinc oxide-based nano composite powder resistance card according to claim 1 or 2, wherein the metal salt is one of acetate and nitrate; the concentration of the metal salt solution is 0.6-0.8 mol/L.
4. The method for preparing the zinc oxide-based nano composite powder resistance card according to claim 1 or 2, wherein the surface modifier is one or more of sodium dodecyl sulfate, triammonium citrate and tween 80, and the dosage of the surface modifier is 2 to 3 percent of the weight of the metal salt.
5. The method for preparing the zinc oxide-based nano composite powder resistance card according to claim 1 or 2, wherein the complexing agent is one or more of oxalic acid, citric acid and triammonium citrate; the concentration of the absolute ethyl alcohol solution of the complexing agent is 0.6-0.8 mol/L.
6. The preparation method of the zinc oxide-based nano composite powder resistor disc as claimed in claim 1 or 2, wherein in the step (2), the stirring temperature is 80-90 ℃, and the stirring time is 1-2 h; the heat preservation temperature is 80-90 ℃, and the heat preservation time is 0.5-1 h.
7. The method for preparing the zinc oxide-based nano composite powder resistor disc as claimed in claim 1 or 2, wherein in the step (4), 1-1.5% of distilled water by mass fraction is added into the zinc oxide-based nano composite powder.
8. The preparation method of the zinc oxide-based nano composite powder resistance card according to claim 1 or 2, wherein in the step (6), the calcining temperature is 1100-1200 ℃, and the heat preservation time is 90-100 h.
9. The zinc oxide-based nano composite powder resistor disc prepared by the preparation method of the zinc oxide-based nano composite powder resistor disc according to claim 1.
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| JP2007280910A (en) * | 2006-04-03 | 2007-10-25 | Ind Technol Res Inst | Aluminum-added zinc oxide transparent conductive film and its manufacturing method containing metallic nano particles |
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| JP2007280910A (en) * | 2006-04-03 | 2007-10-25 | Ind Technol Res Inst | Aluminum-added zinc oxide transparent conductive film and its manufacturing method containing metallic nano particles |
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