CN1683273A - Method for high temperature quick synthesizing blender or compound titanate ceramic powder - Google Patents
Method for high temperature quick synthesizing blender or compound titanate ceramic powder Download PDFInfo
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- CN1683273A CN1683273A CN 200510041837 CN200510041837A CN1683273A CN 1683273 A CN1683273 A CN 1683273A CN 200510041837 CN200510041837 CN 200510041837 CN 200510041837 A CN200510041837 A CN 200510041837A CN 1683273 A CN1683273 A CN 1683273A
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- titanate
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Abstract
The present invention provides high temperature synthesizing process of blended or compound titanate ceramic powder. The method includes fully mixing titanate synthesized in advance and blended elements, grinding and tabletting, fast reaction of the mixture in argon atmosphere inside vacuum arc furnace, and grinding the reacted solid into the blended titanate ceramic powder. The present invention has simple technological process, easy operation, short reaction period, low cost, and high quality and performance of prepared blended titanate ceramic powder.
Description
Technical field
The present invention relates to the multifunction electronic stupalith---the preparation method of doping or compound titanate ceramic powder relates in particular to a kind of method of utilizing vacuum arc melting furnace high temperature quick synthesizing blender or compound titanate ceramic powder.
Technical background
The perovskite typed titanate (is mainly: BaTiO
3, SrTiO
3, PbTiO
3, CaTiO
3) be a kind of dielectric substance, photoelectric material with high dielectric constant, have the characteristics of heavy body, high dispersion frequency, low dielectric consume, low-temperature coefficient.Single titanate material has mixed electronic and ionic conductance, makes it be widely used at aspects such as high-temperature superconducting thin film, catalysis, high temperature solid oxide fuel cell electrode materials, electrochemical sensor, multiple sull substrate material, special optical window and high-quality sputtering target materials.Doping or compound titanate stupalith have multi-functional characteristic, the product of making can have piezoelectricity, ferroelectric, conduction, semi-conductor, magnetic etc. respectively or have high-strength, high-ductility, characteristics such as high hard, wear-resisting, corrosion-resistant, high temperature resistant, high thermal conductance, thermal insulation or good biocompatibility are a class advanced person multifunctional ceramic materials.
Titanate is of many uses aspect electronic devices and components, is described as " pillar of electronic industry ".As be used to make ceramic insulating material, ceramic substrate material, the ceramic packaging material of chip and be used to make condenser ceramics, piezoelectric ceramics, ferrite magnetic material of electron device etc.Titanate is mixed and compoundly can also obtain being used to make dielectric resonator, the microwave ceramics of microwave integrated circuit substrate, element etc.Metatitanic acid alkali pottery also can be used for making the susceptibility stupalith to temperature, pressure, humidity, atmosphere, light etc.Titanate is carried out oxide-doped, can obtain temperature-sensitive, pressure-sensitive, humidity-sensitive material.The doping of lead titanate ceramics and composite modified then can the good piezoelectric ceramics of obtained performance.Difunctional doped titanate stupalith then has the quick characteristic of electric capacity and voltage simultaneously, can be used for surge and absorbs and overvoltage protection.The beginning of the eighties, company of Japanese TAIYO YUDAN and TDK company, U.S.'s Bell Laboratory and Dutch Fei Lipu company develop titanium oxide respectively, as SrTiO
3And TiO
2Capacitance-voltage sensitive resistor, its function are equivalent to the effect of an electrical condenser and a piezoresistor parallel connection.Therefore be called as the quick bifunctional material of capacitance-voltage.Be covered with one deck acceptor impurity (Ag, Na, Ca, Mn, Fe, CuO, Cu in methods such as the surface coated of titanate ceramics, evaporation, plating, electrolysis
2O, MnO
2, Bi
2O
3, Tl
2O
3Deng) form low solution altogether mutually with titanate ceramics, can prepare elements such as boundary ceramics electrical condenser, PTC thermistor, also can be used as piezoceramic material.In order to reduce the room temperature resistivity that titanate is the PTC pottery, improve thermal conductivity, the metal composite of titanate has been carried out big quantity research.Japanese Patent report is blended in titanate and metal powder in vacuum, neutrality, the reducing atmosphere and burns till, and prevents that metal powder is oxidized when high temperature sintering, carries out oxide treatment after burning till again.For preventing that metal powder from reoxidizing when the oxide treatment, the metal powder of employing is generally refractory metal.
The preparation of titanate sill have a lot of methods as, chemical coprecipitation, sol-gel method, hydrothermal method, solid reaction process, chemical coprecipitation, step-by-step precipitation method, chemical Vapor deposition process, physical vaporous deposition, sputtering method, Hydrothermal Electrochemical method, spraying thermal decomposition method, microwave process for synthesizing, laser synthesis method, radio frequency sputtering method, rf magnetron sputtering etc.No matter any method all must have the stage that sinters porcelain into.The solid phase calcination method is difficult to guarantee material homogeneity, high-temperature thermal oxidation process in the technology easily makes diffusant run off, diffusing capacity is wayward, the powder foreign matter content height that makes, chemical constitution has fluctuation, and size of particles is big, size-grade distribution is wide, but the sintering temperature height, reaction time is long, huge, the complicated operation of equipment; Though improved method report is arranged, and the gained powder still can not satisfy the requirement that the high-performance electronic element is produced.In the liquid phase method, oxalic acid coprecipitation gained powder purity height, particle diameter are little, complex process, and production cost is higher; Carbonate precipitation method still needs the high-temperature calcination process; Urea-sodium hydroxide precipitator method are easily introduced alkali metal impurity.Organic method gained powder purity height, particle diameter are little, be evenly distributed, but the production cost height.Hydrothermal method can reduce temperature of reaction, and product purity height, particle diameter are little, are evenly distributed, and cost is relatively low, and has accomplished advantages of nontoxic raw materials, harmless, and process is not polluted, and the result does not produce the characteristics of Green Chemistry such as refuse.Domestic manufacturer generally all adopts the method for the direct mixed calcining of oxide compound, and the quality product that this method is produced is stable inadequately, high-quality dielectric materials and the device of uncomfortable cooperation.Chemical gas phase reaction then is under quite high temperature, and the surface interaction of mixed gas and matrix decomposes some composition of mixed gas, and form the solid film of a kind of metal or compound on matrix.
Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing the vacuum arc melting furnace high temperature quick synthesizing blender or being combined into titanate ceramic powder, this method technology is simple, easily behaviour is convenient, reaction time is short, cost is low, and the doping that makes or compound titanate ceramic powder evenly, inclusion-free.
Purpose of the present invention can realize by following measure:
The method of a kind of high temperature synthesizing blender or compound titanate ceramic powder comprises the processing step of following order: 1. synthetic titanate and doped element thorough mixing in advance earlier, grind also compressing tablet; 2. utilize vacuum arc melting furnace to make mixture rapid reaction in argon gas atmosphere; 3. with reacted solid fragmentation, pulverize the doped titanate ceramic powder.
The chemical formula of the described titanate of synthetic in advance is: ATiO
3, wherein A is a kind of in barium, calcium, strontium, the lead ion.
Described doped element is the oxide compound that Si, La element form.
Described doped element is the metallic element monomer.
The described titanate of synthetic in advance is calcium titanate CaTiO
3, the oxide compound of described doped element is silicon-dioxide SiO
2With lanthanum sesquioxide La
2O
3
The described titanate of synthetic in advance is barium titanate BaTiO
3Described doped element is metal nickel powder Ni.
The add-on of described doped element oxide compound is 1%～25% of a titanate quality.
The add-on of described metal simple-substance is 5%～15% of a titanate quality.
Described in vacuum arc melting furnace electric current be 40-180A, the reaction times is 10-60 second.
The present invention compared with prior art has following advantage:
(1) speed of response is fast: the present invention utilizes vacuum arc melting furnace to prepare the titanate ceramics material, the temperature of reaction height reaches as high as 5000 ℃, can various reactants be reacted under molten state in moment, speed is exceedingly fast, and can finish the synthetic and phase transformation of sample in the several seconds; Condensing rate is fast, reduces to room temperature in several minutes, and the acquisition of sample approximately only prepares to finish from raw material needs one hour.
(2) quality product height: the present invention utilizes the vacuum arc melting furnace preparation to mix or the compound titanate stupalith, making reactant reach the ion level level mixes, reactant is even, rapid reaction under ionic condition, the titanate base ceramic material quality height of acquisition, and performance is good.
(3) constant product quality and favorable reproducibility, impurity is few: owing to can obtain high temperature, without any need for fusing assistant, additive, catalyzer, reduced the introducing of impurity, constant product quality and favorable reproducibility.
(4) reaction of the present invention is to finish in the inert atmosphere argon gas, and it is complete to promote titanate ceramic powder crystal grain to grow; Help forming the intercrystalline grain boundary layer of titanate ceramic powder simultaneously, improved the good semiconductor transformation degree of titanate base ceramic material.
(5) technology of the present invention is simple, and is easy to operate, and cost is low, and entire reaction course is nontoxic, harmless, pollution-free.
Embodiment
Embodiment one: a kind of calcium titanate pottery (100%CaTiO for preparing doped silicon oxide, lanthanum sesquioxide
3-10%SiO
2-5%La
2O
3) method; Earlier with 2.719g (0.02mol) synthetic calcium titanate (CaTiO in advance
3), 0.272g (4.53 * 10
-3Mol) silicon-dioxide (SiO
2) and 0.136g (4.17 * 10
-4Mol) lanthanum sesquioxide (La
2O
3), thorough mixing grinds, and is pressed into simple geometric bodies such as sheet or column, said mixture is put into the copper crucible of vacuum arc melting furnace again, leads to water coolant, is evacuated to 10
-3Normal atmosphere, applying argon gas also keep an a little higher than atmospheric pressure, regulate electric current, light electric arc sample is heated, and electric current is 80A, about 20 seconds in reaction times; After reaction was finished, powered-down, adjusting pressure, taking-up sample were pulverized.Products obtained therefrom is the calcium titanate pottery (100%CaTiO of doped silicon oxide, lanthanum sesquioxide
3-10%SiO
2-5%La
2O
3).
Embodiment two: a kind of preparation barium titanate-metallic nickel composite material (100%BaTiO
3-10%Ni) method; Be earlier with 4.664g (0.02mol) synthetic barium titanate (BaTiO in advance
3) and 0.466g (9.02 * 10
-3Mol) metal nickel powder (Ni), thorough mixing grinds, and is pressed into simple geometric bodies such as sheet or column, said mixture is put into the copper crucible of vacuum arc melting furnace again, leads to water coolant, is evacuated to 10
-3Normal atmosphere, applying argon gas also keep an a little higher than atmospheric pressure, regulate electric current, light electric arc sample is heated, and electric current is 160A, about 30 seconds in reaction times; After question response was finished, powered-down, adjusting pressure, taking-up sample were pulverized.Products obtained therefrom is barium titanate-metallic nickel composite material (100%BaTiO
3-10%Ni).
Claims (9)
1, the method for a kind of high temperature synthesizing blender or compound titanate ceramic powder comprises the processing step of following order: 1. synthetic titanate and doped element thorough mixing in advance earlier, grind also compressing tablet; 2. utilize vacuum arc melting furnace to make mixture rapid reaction in argon gas atmosphere; 3. with reacted solid fragmentation, pulverize the doped titanate ceramic powder.
2, the method for high temperature synthesizing blender as claimed in claim 1 or compound titanate ceramic powder is characterized in that: the chemical formula of the described titanate of synthetic in advance is: ATiO
3, wherein A is a kind of in barium, calcium, strontium, the lead ion.
3, the method for high temperature synthesizing blender as claimed in claim 2 or compound titanate ceramic powder is characterized in that: described doped element is the oxide compound that silicon Si, lanthanum La element form.
4, the method for high temperature synthesizing blender as claimed in claim 2 or compound titanate ceramic powder is characterized in that: described doped element is the metallic element monomer.
5, the method for high temperature synthesizing blender as claimed in claim 2 or compound titanate ceramic powder is characterized in that: the described titanate of synthetic in advance is calcium titanate CaTiO
3, the oxide compound of described doped element is silicon-dioxide SiO
2With lanthanum sesquioxide La
2O
3
6, the method for high temperature synthesizing blender as claimed in claim 2 or compound titanate ceramic powder is characterized in that: the described titanate of synthetic in advance is barium titanate BaTiO
3Described doped element is metal nickel powder Ni.
7, as the method for claim 1,2,3,4,5,6 described arbitrary high temperature synthesizing blenders or compound titanate ceramic powder, it is characterized in that: the add-on of described doped element oxide compound is 1%～25% of a titanate quality.
8, as the method for claim 1,2,3,4,5,6 described arbitrary high temperature synthesizing blenders or compound titanate ceramic powder, it is characterized in that: the add-on of described metal simple-substance is 5%～15% of a titanate quality.
9, the method for high temperature synthesizing blender as claimed in claim 1 or 2 or compound titanate ceramic powder is characterized in that: described in vacuum arc melting furnace electric current be 40-180A, the reaction times is 10-60 second.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100418371A CN100358835C (en) | 2005-03-10 | 2005-03-10 | Method for high temperature quick synthesizing blender or compound titanate ceramic powder |
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|---|---|---|---|
| CNB2005100418371A CN100358835C (en) | 2005-03-10 | 2005-03-10 | Method for high temperature quick synthesizing blender or compound titanate ceramic powder |
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| Publication Number | Publication Date |
|---|---|
| CN1683273A true CN1683273A (en) | 2005-10-19 |
| CN100358835C CN100358835C (en) | 2008-01-02 |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951418A (en) * | 2014-04-16 | 2014-07-30 | 中国科学院青海盐湖研究所 | Method for preparing doped or composite barium strontium titanate ceramic powder |
| CN106077584A (en) * | 2016-06-23 | 2016-11-09 | 奇男子五金制品（浙江）有限公司 | The preparation method of superhard wear composite blade |
| CN109133914A (en) * | 2018-11-23 | 2019-01-04 | 陕西师范大学 | A kind of titanium dioxide base ceramic material of high thermal stability and preparation method thereof |
| CN110317485A (en) * | 2019-08-05 | 2019-10-11 | 西南大学 | A kind of more barium titanate yellow solar heat reflection pigment of nickel doping |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3606079B2 (en) * | 1998-12-25 | 2005-01-05 | 株式会社村田製作所 | Nonlinear dielectric porcelain, capacitor for pulse generation, high pressure steam discharge lamp circuit and high pressure steam discharge lamp |
| CN1532166A (en) * | 2003-03-21 | 2004-09-29 | 广东风华高新科技集团有限公司 | Method for producing high dielectric constant ceramic powder and ceramic capacitor |
| JP4547945B2 (en) * | 2004-03-11 | 2010-09-22 | Ｔｄｋ株式会社 | Electronic component, dielectric ceramic composition and method for producing the same |
-
2005
- 2005-03-10 CN CNB2005100418371A patent/CN100358835C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951418A (en) * | 2014-04-16 | 2014-07-30 | 中国科学院青海盐湖研究所 | Method for preparing doped or composite barium strontium titanate ceramic powder |
| CN106077584A (en) * | 2016-06-23 | 2016-11-09 | 奇男子五金制品（浙江）有限公司 | The preparation method of superhard wear composite blade |
| CN106077584B (en) * | 2016-06-23 | 2018-10-09 | 奇男子五金制品（浙江）有限公司 | The preparation method of superhard wear composite blade |
| CN109133914A (en) * | 2018-11-23 | 2019-01-04 | 陕西师范大学 | A kind of titanium dioxide base ceramic material of high thermal stability and preparation method thereof |
| CN109133914B (en) * | 2018-11-23 | 2021-07-06 | 陕西师范大学 | Titanium dioxide-based ceramic material with high thermal stability and preparation method thereof |
| CN110317485A (en) * | 2019-08-05 | 2019-10-11 | 西南大学 | A kind of more barium titanate yellow solar heat reflection pigment of nickel doping |
| CN110317485B (en) * | 2019-08-05 | 2021-07-09 | 西南大学 | Nickel-doped barium polytitanate yellow solar heat reflection pigment |
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| Publication number | Publication date |
|---|---|
| CN100358835C (en) | 2008-01-02 |
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Granted publication date: 20080102 Termination date: 20110310 |