CN103508736A - Barium titanate coated nanometer nickel powder for inner electrode of MLCC (Multilayer Ceramic Capacitor) and preparation method thereof - Google Patents
Barium titanate coated nanometer nickel powder for inner electrode of MLCC (Multilayer Ceramic Capacitor) and preparation method thereof Download PDFInfo
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- CN103508736A CN103508736A CN201210213403.5A CN201210213403A CN103508736A CN 103508736 A CN103508736 A CN 103508736A CN 201210213403 A CN201210213403 A CN 201210213403A CN 103508736 A CN103508736 A CN 103508736A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910002113 barium titanate Inorganic materials 0.000 title abstract description 12
- 239000003985 ceramic capacitor Substances 0.000 title abstract description 11
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title abstract description 10
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 47
- 239000011258 core-shell material Substances 0.000 claims abstract description 38
- 238000002425 crystallisation Methods 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 29
- 230000008025 crystallization Effects 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 8
- 239000011858 nanopowder Substances 0.000 claims description 30
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 20
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 16
- 239000008187 granular material Substances 0.000 claims description 15
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- -1 polyoxyethylene Polymers 0.000 claims description 11
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 8
- 235000011187 glycerol Nutrition 0.000 claims description 8
- 229960004418 trolamine Drugs 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- MTZOKGSUOABQEO-UHFFFAOYSA-L barium(2+);phthalate Chemical compound [Ba+2].[O-]C(=O)C1=CC=CC=C1C([O-])=O MTZOKGSUOABQEO-UHFFFAOYSA-L 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 5
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 5
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 229910001864 baryta Inorganic materials 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 3
- 230000003252 repetitive effect Effects 0.000 claims description 2
- 238000005201 scrubbing Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000005216 hydrothermal crystallization Methods 0.000 abstract description 2
- 239000007772 electrode material Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 11
- 230000000694 effects Effects 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 239000010953 base metal Substances 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 2
- 229910001863 barium hydroxide Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 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
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses barium titanate coated nanometer nickel powder for the inner electrode of an MLCC (Multilayer Ceramic Capacitor) and a preparation method thereof. The Ni-BaTiO3 composite powder comprises the following components in percentage by weight: 85%-96% of nickel powder and 4%-15% of nanometer barium titanate layers coated on the nickel powder. By using the method disclosed by the invention, the surface of the nickel powder is modified by coating the barium titanate layers on the surfaces of nickel powder particles by adopting normal pressure coating hydrothermal crystallization and normal pressure coating crystallization and can be used for preparing the Ni-BaTiO3 core-shell structural composite powder which is suitable for the inner electrode material of the multilayer ceramic capacitor and has good inoxidizability and sintering property.
Description
Technical field
The present invention relates to electrode barium titanate clad nano nickel powder and preparation method thereof in a kind of laminated ceramic capacitor.
Background technology
Along with the develop rapidly of electronic industry, new function ceramic components is constantly to miniaturization, high capacity, high reliability and cost degradation future development.The laminated ceramic capacitor (MLCC) that the barium titanate of take is matrix is a wherein important class.The laminated ceramic capacitor (MLCC) that the barium titanate of take is matrix is in order to adapt to people to MLCC low cost, miniaturization, jumbo requirement, must reduce the sintering temperature of dielectric materials, improve its specific inductivity and the warm stability that is situated between, for this reason, vast researcher has been done a large amount of research work, be devoted to research and using cheap Ni and replace the electrodes in base metal laminated ceramic capacitor that the precious metals such as platinum, palladium are end electrode as inner electrode, the copper of take, reduce the cost of MLCC.
But in base metal inner electrode multilayer ceramic capacitor sintering procedure, exist inner electrode nickel powder oxidized and cause conduction bad, interior electrode nickel slurry and the Shrinkage behavior of ceramic dielectric layer in sintering process do not mate and make MLCC easily produce two problems of layered structure defect.
Summary of the invention
The object of this invention is to provide the Ni-BaTiO that a kind of laminated ceramic capacitor base metal (nickel) inner electrode has core-shell structure
3composite granule and preparation method thereof.
Ni-BaTiO provided by the present invention
3composite granule is comprised of the nano barium phthalate layer of nickel powder and coated described nickel powder; Wherein, the massfraction of nickel powder is 85～96%, and the massfraction of nano barium phthalate layer is 4～15%.
The size of described nickel powder specifically can be 50～200nm, and the thickness of nano barium phthalate layer is 2.5～25nm.
Described Ni-BaTiO
3the oxidation onset temperature of composite granule can reach more than 370 ℃; Shrinking starting temperature can reach more than 730 ℃.
Above-mentioned Ni-BaTiO
3composite granule is, by Chemical coating method, barium titanate is evenly coated on to nickel particle surface, the Ni-BaTiO with good oxidation-resistance and sintering character preparing
3core-shell structure composite granule.
Specifically can be divided into following two kinds of methods:
(1) scheme (preparation flow is shown in Fig. 1) of the coated hydrothermal crystallizing of normal pressure:
Nickel powder, tetrabutyl titanate and trolamine, glycerine, polyoxyethylene glycol are joined in solvent, obtain mixing solutions; Described mixing solutions is carried out to supersound process nickel powder is uniformly dispersed, then drip wherein baryta water, after dropwising, be heated to 25～100 ℃ of reaction 4～8h, obtain BaTiO
3non-crystallized Ni-BaTiO
3core-shell structured composite nano powder; Adopt again hydrothermal method to make Ni-BaTiO
3core-shell structured composite nano powder carries out crystallization, obtains the good Ni-BaTiO of crystallization
3core-shell structured composite nano powder.
Wherein, described solvent be selected from following at least one: DEG (glycol ether), Virahol, n-propyl alcohol and propyl carbinol.
In described supersound process, ultrasonic power can be 50～400W, and ultrasonic time can be 10～60 minutes.
BaTiO
3after coated Ni powder, BaTiO
3crystallization effect is not clearly, and this programme adopts hydrothermal method to carry out in water heating kettle, BaTiO
3obtained fine crystallization.The temperature of described crystallization is 140～240 ℃, and the time is 4～12 hours.
(2) scheme (preparation flow is shown in Fig. 7) of the coated crystallization of normal pressure:
Nickel powder, tetrabutyl titanate and trolamine, glycerine, polyoxyethylene glycol are joined in solvent, obtain mixing solutions; Described mixing solutions is carried out to supersound process nickel powder is uniformly dispersed, then drip wherein deionized water, stirring reaction 4～8h, obtains coated TiO
2nickel powder; Again by described coated TiO
2nickel powder join in deionized water, and add baryta water wherein, be heated to 60～100 ℃ of reaction 4～12h, obtain Ni-BaTiO
3core-shell structured composite nano powder.
Wherein, described solvent be selected from following at least one: DEG (glycol ether), Virahol, n-propyl alcohol and propyl carbinol.
In above-mentioned two kinds of methods, the size of described nickel powder can be 50-200nm.
The add-on of described trolamine is the 0.4-10% of nickel powder quality.
The volume ratio of the add-on of described solvent and glycerine add-on is 100: 2-10.
The weight-average molecular weight of described polyoxyethylene glycol (PEG) specifically can be 6000-20000.
The add-on of described polyoxyethylene glycol (PEG) is the 0.5-8% of nickel powder quality.
The mol ratio of described nickel powder and tetrabutyl titanate is 22.5-95: 1.
In the preparation method of the coated hydrothermal crystallizing of normal pressure, hydrated barta and tetrabutyl titanate are according to Ba/Ti mol ratio 1.0-2.0: 1 ratio adds.
In the preparation method of the coated crystallization of normal pressure, hydrated barta and tetrabutyl titanate are according to Ba/Ti mol ratio 1.0-8.0: 1 ratio adds.
Described two kinds of methods all also comprise the Ni-BaTiO to obtaining
3the step that core-shell structured composite nano powder cleans and dries.
Concrete purging method is as follows: by described Ni-BaTiO
3ethanol and acetic acid repetitive scrubbing for core-shell structured composite nano powder; The method of described oven dry is as follows: under 70～90 ℃ of temperature condition, carry out vacuum-drying.
The present invention has following beneficial effect: adopt the two schemes of the coated hydrothermal crystallizing of normal pressure and the coated crystallization of normal pressure in the coated barium titanate layer of nickel powder particle surface, nickel powder is carried out to surface modification, the Ni-BaTiO preparing
3core-shell structured composite nano powder, coating layer is homogeneously crystallized good, has good oxidation-resistance and sintering character.Oxidation onset temperature can reach more than 370 ℃, before coated, has not improved 100～150 ℃; Shrink starting temperature and can reach more than 730 ℃, before coated, do not improved 300 ℃～600 ℃.The Ni-BaTiO preparing
3core-shell structured composite nano powder is applicable to the inner electrode of laminated ceramic capacitor.Compare two schemes, normal pressure is coated hydrothermal crystallizing option b aTiO
3the covered effect of coated Ni powder is more satisfactory, BaTiO
3crystallization effect is fine, but need under this high-pressure situations of water heating kettle, realize; Normal pressure is coated crystallization scheme, BaTiO
3the covered effect of coated Ni powder is more satisfactory, and has good anti-oxidant and sintering character, especially crystallization environment and only need under normal pressure, just can realize, and is very beneficial for the large production of industrialization.
Accompanying drawing explanation
Fig. 1 is that the coated hydrothermal crystallizing scheme of normal pressure is prepared Ni-BaTiO
3the schema of core-shell structured composite nano powder;
Fig. 2 is the Ni-BaTiO that the coated hydrothermal crystallizing scheme of normal pressure prepares
3the XRD figure of core-shell structured composite nano powder;
Fig. 3 is the Ni-BaTiO that the coated hydrothermal crystallizing scheme of normal pressure prepares
3the TEM figure of core-shell structured composite nano powder;
Fig. 4 is the Ni-BaTiO that the coated hydrothermal crystallizing scheme of normal pressure prepares
3core-shell structured composite nano powder through after water heating kettle crystallization TEM figure;
Fig. 5 is the Ni-BaTiO that the coated hydrothermal crystallizing scheme of normal pressure prepares
3the thermal expansion graphic representation of core-shell structured composite nano powder;
Fig. 6,7 is respectively the Ni-BaTiO that the coated hydrothermal crystallizing scheme of normal pressure prepares
3the TG figure of core-shell structured composite nano powder and DTA figure;
Fig. 8 is that the scheme of the coated crystallization of normal pressure is prepared Ni-BaTiO
3the schema of core-shell structured composite nano powder;
Fig. 9 is the Ni-BaTiO that the scheme of the coated crystallization of normal pressure prepares
3the XRD figure of core-shell structured composite nano powder;
Figure 10 is the Ni-BaTiO that the scheme of the coated crystallization of normal pressure prepares
3the TEM figure of core-shell structured composite nano powder;
Figure 11 is the Ni-BaTiO that the scheme of the coated crystallization of normal pressure prepares
3the thermal expansion graphic representation of core-shell structured composite nano powder.
Embodiment
Below by specific embodiment, method of the present invention is described, but the present invention is not limited thereto.
Experimental technique described in following embodiment, if no special instructions, is ordinary method; Described reagent and material, if no special instructions, all can obtain from commercial channels.
Embodiment 1, the coated hydrothermal crystallization method of normal pressure are prepared Ni-BaTiO
3core-shell structure composite granule
The solvent that the present embodiment adopts is Virahol (100ml), Ni/BaTiO
3mass ratio is 96/4, to add in Virahol needed particle diameter be 100nm nickel powder (5g) and tetrabutyl titanate (0.0009mol) and trolamine (0.05g), glycerine (2ml), the weight-average molecular weight polyoxyethylene glycol (0.05g) that is 6000 afterwards, by ultrasonic wave (250W), mixing solutions is carried out ultrasonicly, the time is 40 minutes; Meanwhile, barium hydroxide is joined in deionized water and dissolved, then the aqueous solution of barium hydroxide (containing hydrated barta 0.0009mol) is slowly added drop-wise in above-mentioned mixing solutions, after dropwising, solution is heated to 80 ℃, after reaction 4-8h, pour out solution and dry, obtaining Ni-BaTiO
3core-shell structured composite nano powder.
Fig. 3 is the Ni-BaTiO preparing
3the TEM figure of core-shell structured composite nano powder.
As seen from the figure, BaTiO
3the coating thickness of coated Ni powder is 3.8nm, the homogeneity of coating layer is fine, after coated, antioxidant property has obtained good raising, anti-Shrinkage behavior in sintering process improves obvious, there is no the coated contraction starting temperature of Ni powder is before 417 ℃, and oxidation onset temperature is 251 ℃, after being coated, shrink starting temperature and increase to 631 ℃, oxidation onset temperature is 310 ℃.
From the XRD spectral line of Fig. 2, can find out, not occur BaTiO
3peak crystallization, illustrates BaTiO
3after coated Ni powder, BaTiO
3crystallization effect is not clearly.This programme adopts hydrothermal method to carry out in water heating kettle, through after 200 ℃, the reaction of 8h, and BaTiO
3peak crystallization is very obvious, BaTiO
3obtained fine crystallization.
Fig. 4 is Ni-BaTiO
3core-shell structured composite nano powder is through the TEM figure after water heating kettle crystallization.Fig. 5 is Ni-BaTiO before and after crystallization
3the thermal expansion graphic representation of core-shell structured composite nano powder.As shown in Figure 5, shrinking starting temperature has obtained further raising and has reached 730 ℃.Fig. 6,7 is respectively the Ni-BaTiO that the coated hydrothermal crystallizing scheme of normal pressure prepares
3the TG-DTA figure of core-shell structured composite nano powder.From Fig. 6,7, it is 374 ℃ that oxidation onset temperature is also further brought up to.
Embodiment 2, the coated crystallization legal system of normal pressure are for Ni-BaTiO
3core-shell structure composite granule
Coated process adopts normal pressure coated, after being coated, adopts normal pressure to carry out crystallization.
The solvent that the present embodiment adopts is propyl carbinol (100ml), Ni/BaTiO
3mass ratio is that 85/15, Ba/Ti mol ratio is 6.To add in solvent needed particle diameter be 150nm nickel powder (5g) and tetrabutyl titanate (0.0038mol) and trolamine (0.1g), glycerine (2ml), the weight-average molecular weight polyoxyethylene glycol (0.04g) that is 10000 afterwards, by ultrasonic wave (250W), to mixing solutions, carry out ultrasonic, time is 15 minutes, after complete, in solution, drip 2ml deionized water and stir always, reacting after 8 hours centrifugal the obtaining of reaction solution is coated to TiO
2nickel powder.By the coated TiO obtaining
2nickel powder join in deionized water, and to add 50ml concentration be the Ba (OH) of 0.1mol/L
28H
2the aqueous solution of O, is then heated to 100 ℃ (crystallization temperature) reaction 6-8h (crystallization time), obtains Ni-BaTiO
3core-shell structure composite granule, particle diameter is 172nm left and right.
Figure 10 is the Ni-BaTiO preparing
3the TEM figure of core-shell structured composite nano powder.Result shows BaTiO
3the homogeneity of the coating layer of coated Ni powder is better.From the XRD figure spectrum of Fig. 9, can find out BaTiO
3peak crystallization is very obvious, BaTiO
3crystallization effect is more satisfactory.Figure 11 is the Ni-BaTiO preparing
3the thermal expansion graphic representation of core-shell structured composite nano powder.As shown in Figure 11, it shrinks starting temperature and has reached 997 ℃, illustrates that its anti-Shrinkage behavior is very good.
Claims (10)
1. a Ni-BaTiO with core shell structure
3composite granule, is comprised of nickel powder and the nano barium phthalate layer of coated described nickel powder; Wherein, the massfraction of nickel powder is 85～96%, and the massfraction of nano barium phthalate layer is 4～15%.
2. Ni-BaTiO according to claim 1
3composite granule, is characterized in that: the particle diameter of described nickel powder is 50～200nm; The thickness of described nano barium phthalate layer is 2.5～25nm.
3. Ni-BaTiO according to claim 1 and 2
3composite granule, is characterized in that: described Ni-BaTiO
3the oxidation onset temperature of composite granule is more than 370 ℃; It is more than 730 ℃ shrinking starting temperature.
4. prepare the Ni-BaTiO with core shell structure described in any one in claim 1-3
3the method of composite granule, comprises the steps: nickel powder, tetrabutyl titanate and trolamine, glycerine, polyoxyethylene glycol to join in solvent, obtains mixing solutions; Described mixing solutions is carried out to supersound process nickel powder is uniformly dispersed, then drip wherein baryta water, after dropwising, be heated to 25～100 ℃ of reactions 4～8 hours, obtain BaTiO
3non-crystallized Ni-BaTiO
3composite granule; Adopt again hydrothermal method to make Ni-BaTiO
3composite nano powder carries out crystallization, obtains having the Ni-BaTiO of core shell structure
3composite nano powder.
5. method according to claim 4, is characterized in that: the temperature of described crystallization is 140～240 ℃, and the time is 4～12 hours;
Described hydrated barta and tetrabutyl titanate are according to Ba/Ti mol ratio 1.0-2.0: 1 ratio adds.
6. prepare the Ni-BaTiO with core shell structure described in any one in claim 1-3
3the method of composite granule, comprises the steps: nickel powder, tetrabutyl titanate and trolamine, glycerine, polyoxyethylene glycol to join in solvent, obtains mixing solutions; Described mixing solutions is carried out to supersound process nickel powder is uniformly dispersed, then drip wherein deionized water, stirring reaction 4～8h, obtains coated TiO
2nickel powder; Again by described coated TiO
2nickel powder join in deionized water, and add baryta water wherein, be heated to 60～100 ℃ of reaction 4～12h, described in obtaining, there is the Ni-BaTiO of core shell structure
3composite nano powder.
7. method according to claim 6, is characterized in that: described hydrated barta and tetrabutyl titanate are according to Ba/Ti mol ratio 1.0-8.0: 1 ratio adds.
8. according to the method described in any one in claim 4-7, it is characterized in that: the particle diameter of described nickel powder is 50-200nm; Described solvent be selected from following at least one: glycol ether, Virahol, n-propyl alcohol and propyl carbinol; In described supersound process, ultrasonic power is 50～400W, and ultrasonic time is 10～60 minutes.
9. according to the method described in any one in claim 4-8, it is characterized in that: the add-on of described trolamine is the 0.4-10% of described nickel powder quality; The volume ratio of the add-on of described solvent and described glycerine add-on is 100: 2-10;
The weight-average molecular weight of described polyoxyethylene glycol is 6000-20000, and the add-on of described polyoxyethylene glycol is the 0.5-8% of described nickel powder quality;
Described nickel powder and and the mol ratio of tetrabutyl titanate be 22.5-95: 1.
10. according to the method described in any one in claim 4-9, it is characterized in that: described method also comprises the Ni-BaTiO with core shell structure to obtaining
3the step that composite nano powder cleans and dries;
The method of described cleaning is as follows: by described Ni-BaTiO
3ethanol and acetic acid repetitive scrubbing for core-shell structured composite nano powder; The method of described oven dry is as follows: under 70～90 ℃ of temperature condition, carry out vacuum-drying.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108358355A (en) * | 2018-02-05 | 2018-08-03 | 平阳铮盛建设有限公司 | A kind of device for municipal sewage plant integration deodorization and sewage disposal |
| CN112151268A (en) * | 2019-06-28 | 2020-12-29 | 株式会社村田制作所 | Laminated electronic component |
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| CN108358355A (en) * | 2018-02-05 | 2018-08-03 | 平阳铮盛建设有限公司 | A kind of device for municipal sewage plant integration deodorization and sewage disposal |
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| CN103508736B (en) | 2015-08-05 |
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