CN103951416B - A kind of composite Nano ZnO voltage-sensitive ceramic raw powder's production technology - Google Patents
A kind of composite Nano ZnO voltage-sensitive ceramic raw powder's production technology Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 46
- 239000000919 ceramic Substances 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000002131 composite material Substances 0.000 title claims abstract description 11
- 238000005516 engineering process Methods 0.000 title claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000243 solution Substances 0.000 claims abstract description 16
- 238000010992 reflux Methods 0.000 claims abstract description 15
- 238000000967 suction filtration Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000001291 vacuum drying Methods 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 150000001621 bismuth Chemical class 0.000 claims abstract 4
- 150000002696 manganese Chemical class 0.000 claims abstract 4
- 150000003751 zinc Chemical class 0.000 claims abstract 4
- 150000001868 cobalt Chemical class 0.000 claims abstract 3
- 238000002360 preparation method Methods 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 12
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000015895 biscuits Nutrition 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 2
- 239000012266 salt solution Substances 0.000 claims 2
- 238000007873 sieving Methods 0.000 claims 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims 1
- 239000012267 brine Substances 0.000 claims 1
- 239000010941 cobalt Substances 0.000 claims 1
- 229910017052 cobalt Inorganic materials 0.000 claims 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 107
- 239000011787 zinc oxide Substances 0.000 description 54
- 238000000034 method Methods 0.000 description 25
- 239000000463 material Substances 0.000 description 9
- 238000005265 energy consumption Methods 0.000 description 4
- 239000012716 precipitator Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 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
- 238000000748 compression moulding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- CNFDGXZLMLFIJV-UHFFFAOYSA-L manganese(II) chloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Mn+2] CNFDGXZLMLFIJV-UHFFFAOYSA-L 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention relates to ZnO pressure-sensitive ceramic material, refer in particular to a kind of composite Nano ZnO voltage-sensitive ceramic raw powder's production technology.With soluble zinc salt, bismuth salt, cobalt salt, manganese salt is raw material, is configured to the aqueous solution respectively, calculates with molar content, according to the ZnO of 95%, the Bi of 3%
2o
3, the proportioning mixing of the CoO of 1%, the MnO of 1%, stirs; Ammoniacal liquor is slowly added in the mixing solutions that step (1) obtains, regulate pH 8 ~ 8.5, obtain mixing solutions, continue to be stirred to and mix; The precipitation suction filtration of step (2) gained, and fully wash removal impurity with deionized water and ethanol, the presoma obtained is placed in water or ethanol medium the 2 ~ 8h that refluxes, reflux temperature controls at 70 ~ 80 DEG C; Finally by the powder suction filtration obtained that refluxes, and fully wash removal impurity with deionized water and ethanol, finally dry in vacuum drying oven, obtain nano combined ZnO powder after grinding.
Description
Technical field
The present invention relates to ZnO pressure-sensitive ceramic material, refer in particular to a kind of composite Nano ZnO voltage-sensitive ceramic raw powder's production technology, belong to electronic ceramic preparation and applied technical field.
Background technology
ZnO pressure-sensitive ceramic material is based on ZnO powder, add the multifunctional composite ceramic material of a small amount of Multimetal oxide modification, there is surface effects, small-size effect, the nano effects such as quantum size effect, and the nonlinear wind vibration of excellence and huge pulse energy receptivity, nano-ZnO is widely used in power system and electronic circuit.
ZnO voltage-sensitive ceramic mainly adopts traditional high temperature solid-phase sintering method preparation, and this method is generally by a certain percentage by ZnO, Bi
2o
3with the metal oxide mixing and ball milling such as CoO, compression moulding, then carry out high temperature solid state reaction, finally by polishing, the operations such as polishing obtain product.But the problem of this method is that the powder granularity that ball milling obtains is large, it is serious to reunite and pattern uneven being difficult to prepares high-quality nano-powder material; Modern material science requirements is while development novel material, explore a kind of method technique simple, with low cost, less energy-consumption, eco-friendly synthetic route is carried out synthesis of nano ceramic powder and is had extremely important science and realistic meaning, so explore the focus that new preparation technology has become research and development.
Current making ZnO pressure-sensitive ceramic material is except solid phase method, and mainly adopt liquid phase method, liquid phase method mainly comprises the precipitator method, hydrothermal method, sol-gel method, microemulsion method etc.; Precipitator method application is the most general in these methods, because the precipitator method have convenient operation, technique is simple, is applicable to the advantages such as large scale industry production; But adopt during precipitator method synthesis of nano ZnO powder and usually need the presoma obtained to be converted into ZnO, this process generally adopts high temperature sintering to obtain stable nano ZnO powder, the nano ZnO powder dispersiveness that the method obtains is poor, products collection efficiency is lower, granular size is uneven, and this reaction process needs higher temperature, energy consumption is higher, adds production cost.
Therefore, the emphasis of at present research inquires into a kind of new method traditional to obtain stable nano combined ZnO powder by high temperature sintering to replace; The present invention mainly adopts heating reflux method direct synthesis of nano compound ZnO powder, thus obtained high performance ZnO pressure-sensitive ceramic material.The method energy consumption in implementation process is lower, and products collection efficiency is higher, thing is uniformly dispersed mutually, can avoid the agglomeration traits produced because of high temperature sintering.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of ZnO pressure-sensitive ceramic material, overcoming conventional solid-state method take oxide compound as the shortcoming that the existence of nano combined ZnO powder prepared by raw material, mostly ZnO powder need be generated by powder sintering with the current ZnO pressure-sensitive ceramic material preparation of solution, complex process, production cost is high, and the zinc oxide pattern obtained is uneven, the problem that granular size differs, improve ZnO powder microtexture according to heating reflux method, improve the electrical property of ZnO pressure-sensitive ceramic material.
The method applied in the present invention relates to many factors, as the proportioning of reactant, temperature of reaction, reaction times and pH value etc.It comprises the following steps:
1, the preparation of nano combined ZnO powder
(1) with analytically pure Zn (NO
3)
26H
2o, Bi (NO
3)
25H
2o, Co (NO
3)
26H
2o, MnCl
24H
2o is raw material, configures Zn (NO respectively
3)
2, Bi (NO
3)
2, Co (NO
3)
2, MnCl
2the aqueous solution, calculates with molar content, according to the ZnO of 95%, and the Bi of 3%
2o
3, the proportioning mixing of the CoO of 1%, the MnO of 1%, stirs.
(2) slowly added by ammoniacal liquor in the mixing solutions that step (1) obtains, adjust ph is 8 ~ 8.5, obtains mixing solutions, continues to be stirred to mix.
(3) the precipitation suction filtration of step (2) gained, and fully wash removal impurity with deionized water and ethanol, the presoma obtained is placed in water or ethanol medium the 2 ~ 8h that refluxes, reflux temperature controls at 70 ~ 80 DEG C.
(4) finally by the powder suction filtration obtained that refluxes, and fully wash removal impurity with deionized water and ethanol, finally dry in vacuum drying oven, after taking-up, in agate mortar, grinding obtains nano combined ZnO powder..
Zn (the NO of configuration in described step 1
3)
2, Bi (NO
3)
2, Co (NO
3)
2and MnCl
2concentration of aqueous solution is 0.1mol/L.
Ammonia concn in described step 2 is 10wt%.
Drying in described step 4 refers to dry 4h at 70 DEG C.
2, the preparation of ZnO voltage-sensitive ceramic
(1) in nano combined ZnO powder, add the polyvinyl alcohol (PVA) that massfraction is 5%, grind in mortar, with 200 object sieve granulations, under 30 ~ 80MPa, be pressed into sheet.
(2) sintered at 1050 ~ 1200 DEG C by the sheet biscuit that step (1) is obtained, under air atmosphere, be incubated 2h, temperature rate 5 DEG C/min, obtains ZnO voltage-sensitive ceramic.
(3) by the ZnO voltage-sensitive ceramic surface finish that step (2) is obtained, polishing, silver-colored, make electrode.
Material prescription provided by the invention and the nano combined ZnO powder obtained by preparation method are brown, and ZnO voltage-sensitive ceramic sheet is dark gray solid, shrinking percentage 5% ~ 13%, pressure sensitive voltage V
1mAbe 500 ~ 600V/mm, leakage current J
leakbe 2 ~ 8 μ A(0.78V
1mA), nonlinear factor α is 27.7 ~ 34.5; Because potential gradient is relatively high, may be used for the overvoltage protection product etc. manufacturing high pressure, extra-high voltage Force system.
The present invention adopts the advantage of technique scheme to be:
liquid-phase reflux directly can obtain nano combined ZnO powder, does not need high temperature sintering process, and products collection efficiency is high, purity is high, and favorable dispersity, thing are even mutually, and energy consumption is lower;
adopt the ZnO voltage-sensitive ceramic prepared of the present invention, potential gradient is higher, and nonlinear factor is comparatively large, and leakage current is little, meets the requirement of overvoltage protection product of high pressure, extra-high voltage Force system.
Accompanying drawing explanation
Fig. 1 is the XRD figure of nano combined ZnO powder obtained by the present invention, and in figure, the characteristic peak of 1 and the characteristic peak of ZnO powder diffractogram are consistent, and illustrate that this circumfluence method can obtain stable ZnO powder.
Fig. 2 is the TEM figure of nano combined ZnO powder obtained by the present invention, and as can be seen from the figure nano ZnO powder granular size is homogeneous, better dispersed.
Fig. 3 is the SEM figure of the ZnO voltage-sensitive ceramic obtained by the present invention, and the ZnO pressure-sensitive ceramic material compactness in figure is good, and pattern is homogeneous, and granular size is 7 ~ 9 μm.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be further described, but never limit the scope of the invention:
Embodiment 1
1, the preparation of nano combined ZnO powder
(1) zinc nitrate of 11.4349g is configured to the solution of 0.1mol/L; Bismuth trinitrate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, Manganous chloride tetrahydrate are dissolved into the aqueous solution respectively, are added in 0.1mol/L zinc nitrate solution under whipped state, it is 95:3:1:1 that the add-on of various material meets mol ratio, with ammoniacal liquor regulator solution pH to 8, continues to stir 2h.
(2) the precipitation suction filtration of gained, and fully wash removal impurity with deionized water and ethanol, the presoma obtained is placed in ethanol medium the 2h that refluxes, and reflux temperature controls at 80 DEG C.
(3) finally by the powder suction filtration that obtains of refluxing, and fully wash removal impurity with deionized water and ethanol, finally in vacuum drying oven at 70 DEG C dry 4h, grind in agate mortar after taking-up and obtain nano combined ZnO powder.
2, the preparation of ZnO voltage-sensitive ceramic
(1) in nano combined ZnO powder, add the polyvinyl alcohol (PVA) that massfraction is 5%, grind in mortar, with 200 object sieve granulations, tabletted under 50MPa.
(2) sintered at 1100 DEG C by the sheet biscuit that step (1) is obtained, under air atmosphere, be incubated 2h, temperature rate 5 DEG C/min, obtains ZnO voltage-sensitive ceramic.
Embodiment 2
In the present embodiment, when preparing nano combined ZnO powder, each composition weight in the same manner as in Example 1, is 8.5 by ammoniacal liquor regulator solution pH value, continues to stir 2h; The precipitation suction filtration of gained, washing, 78 DEG C of backflow 3h in ethanol medium; Above-mentioned materials adopts the processing step identical with embodiment 1, and be prepared into ZnO voltage-sensitive ceramic, its difference is that ceramic sintering temperature is 1150 DEG C.
Embodiment 3
In the present embodiment, when preparing nano combined ZnO powder, each component weight in the same manner as in Example 1, is 8 by ammoniacal liquor regulator solution pH value, continues to stir 2h; The precipitation suction filtration of gained, washing, 75 DEG C of backflow backflow 4h in ethanol medium; Above-mentioned materials adopts the processing step identical with embodiment 1, and be prepared into ZnO voltage-sensitive ceramic, its difference is that ceramic sintering temperature is 1050 DEG C.
Embodiment 4
In the present embodiment, when preparing nano combined ZnO powder, each component weight in the same manner as in Example 1, is 8 by ammoniacal liquor regulator solution pH value, continues to stir 2h; The precipitation suction filtration of gained, washing, 72 DEG C of backflow backflow 6h in ethanol medium; Above-mentioned materials adopts the processing step identical with embodiment 1, and be prepared into ZnO voltage-sensitive ceramic, its difference is that ceramic sintering temperature is 1200 DEG C.
Embodiment 5
In the present embodiment, when preparing nano combined ZnO powder, each component weight in the same manner as in Example 1, is 8.5 by ammoniacal liquor regulator solution pH value, continues to stir 2h; The precipitation suction filtration of gained, washing, 70 DEG C of backflow 8h in ethanol medium; Above-mentioned materials adopts the processing step identical with embodiment 1, and be prepared into ZnO voltage-sensitive ceramic, its difference is that ceramic sintering temperature is 1150 DEG C.
Claims (9)
1. a composite Nano ZnO voltage-sensitive ceramic raw powder's production technology, is characterized in that carrying out according to step:
(1) with soluble zinc salt, bismuth salt, cobalt salt, manganese salt is raw material, configures zinc salt solution, bismuth salt brine solution, cobalt saline solution, manganese salt solution respectively, calculates with molar content, according to the ZnO of 95%, the Bi of 3%
2o
3, the proportioning mixing of the CoO of 1%, the MnO of 1%, stirs;
(2) ammoniacal liquor is slowly added in the mixing solutions that step (1) obtains, regulate pH 8 ~ 8.5, obtain mixing solutions, continue to be stirred to and mix;
(3) the precipitation suction filtration of step (2) gained, and fully wash removal impurity with deionized water and ethanol, the presoma obtained is placed in water or ethanol medium the 2 ~ 8h that refluxes, reflux temperature controls at 70 ~ 80 DEG C;
(4) finally by the powder suction filtration obtained that refluxes, and fully wash removal impurity with deionized water and ethanol, finally dry in vacuum drying oven, after taking-up, in agate mortar, grinding obtains nano combined ZnO powder.
2. a kind of composite Nano ZnO voltage-sensitive ceramic raw powder's production technology as claimed in claim 1, is characterized in that: described zinc salt refers to Zn (NO
3)
26H
2o; Described bismuth salt refers to Bi (NO
3)
25H
2o, described cobalt salt refers to Co (NO
3)
26H
2o, described manganese salt refers to MnCl
24H
2o is raw material, configures Zn (NO respectively
3)
2the aqueous solution, Bi (NO
3)
2the aqueous solution, Co (NO
3)
2the aqueous solution and MnCl
2the aqueous solution.
3. a kind of composite Nano ZnO voltage-sensitive ceramic raw powder's production technology as claimed in claim 2, is characterized in that: in described step (1), the strength of solution of configuration is 0.1mol/L.
4. a kind of composite Nano ZnO voltage-sensitive ceramic raw powder's production technology as claimed in claim 1, is characterized in that: the ammonia concn in described step (2) is 10wt%.
5. a kind of composite Nano ZnO voltage-sensitive ceramic raw powder's production technology as claimed in claim 1, is characterized in that: the drying in described step (4) refers to dry 4h at 70 DEG C.
6. ZnO voltage-sensitive ceramic prepared by the composite Nano ZnO voltage-sensitive ceramic powder using preparation method as claimed in claim 1 to prepare, is characterized in that: the shrinking percentage 5% ~ 13% of described ZnO voltage-sensitive ceramic, pressure sensitive voltage V
1mAbe 500 ~ 600V/mm; At 0.78V
1mAunder, leakage current J
leakbe 2 ~ 8 μ A; Nonlinear factor α is 27.7 ~ 34.5.
7. the preparation method of ZnO voltage-sensitive ceramic as claimed in claim 6, is characterized in that carrying out in accordance with the following steps:
(1) in nano combined ZnO powder, add caking agent, grind, granulation of sieving, be pressed into sheet;
(2) ZnO voltage-sensitive ceramic is obtained by after sheet biscuit sintering obtained for step (1).
8. the preparation method of ZnO voltage-sensitive ceramic as claimed in claim 7, is characterized in that: described caking agent to be massfraction be 5% polyvinyl alcohol, described in granulation of sieving refer to 200 object sieve granulations; The described sheet that is pressed into refers to be pressed into sheet under 30 ~ 80MPa.
9. the preparation method of ZnO voltage-sensitive ceramic as claimed in claim 7, is characterized in that: described sintering refers to sinter at 1050 ~ 1200 DEG C, is incubated 2h, temperature rate 5 DEG C/min under air atmosphere.
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| CN104291790B (en) * | 2014-09-22 | 2016-04-13 | 常州大学 | A kind of ZnO/Bi 2o 3the preparation method of composite granule |
| CN104402038A (en) * | 2014-10-28 | 2015-03-11 | 常州市创捷防雷电子有限公司 | Preparation method for monodisperse nanometer ZnO pressure-sensitive ceramic powder |
| CN108863344B (en) * | 2018-10-10 | 2024-02-23 | 贵州大学 | Preparation process of high-performance ZnO pressure-sensitive ceramic |
| CN109867519B (en) * | 2019-04-25 | 2022-04-15 | 重庆大学 | High potential gradient ZnO voltage-sensitive ceramic and preparation method thereof |
| CN111484338A (en) * | 2020-04-16 | 2020-08-04 | 刘建恒 | Production process of composite nano ceramic powder |
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