CN103951418A - Method for preparing doped or composite barium strontium titanate ceramic powder - Google Patents
Method for preparing doped or composite barium strontium titanate ceramic powder Download PDFInfo
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- CN103951418A CN103951418A CN201410153715.0A CN201410153715A CN103951418A CN 103951418 A CN103951418 A CN 103951418A CN 201410153715 A CN201410153715 A CN 201410153715A CN 103951418 A CN103951418 A CN 103951418A
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- strontium
- mgo
- doping
- strontium titanate
- oxide
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Abstract
The invention discloses a method for preparing doped or composite barium strontium titanate ceramic powder. The method comprises the following steps: (1) doping a barium strontium titanate Ba[x]Sr[1-x]TiO3 (x is more than 0 and less than 1) precursor with doping oxide, wherein the doping oxide is MgO, Al2O3 or a mixture of MgO and Al2O3; (2) adding a bonder, grinding, and tabletting; and (3) putting a pressed blank into a reaction chamber, filling inert gas, igniting electric arc for reacting a sample, and grinding a product into powder. According to the preparation method and the doping material, the dielectric properties of barium strontium titanate can be improved, the dielectric constant and the dielectric loss rate of the material can be reduced, the wide-range coordinability of the material can be kept, and the material can be well applied to phased-array antenna materials.
Description
Technical field
The present invention relates to the preparation method of a kind of doping or composite barium strontium titanate ceramics powder, relate in particular to a kind of method of utilizing direct current arc method to prepare fast doping or composite barium strontium titanate ceramics powder.
Background technology
Strontium-barium titanate (BST) is the ferroelectric material of perovskite typed, because it has good dielectric properties and ferroelectric property, and be widely used in field of electronic ceramic materials, especially strontium-barium titanate is can hamony scope large, can regulate within a large range specific inductivity and Curie temperature, there is specific purposes, as phased array antenna.But the specific inductivity of barium strontium titanate material and dielectric loss rate are higher, be difficult to reach the theoretical requirement of phased array antenna application, limit the application of its material.In recent years the improvement of this material is mainly concentrated on the dielectric properties of strontium-barium titanate, to reduce specific inductivity and the dielectric loss rate of material, keeping simultaneously in a big way can hamony, thereby make it be applied to better phased array antenna.
Magnesium oxide (MgO) and aluminium sesquioxide (Al
2o
3) etc. dielectric material there is lower specific inductivity and dielectric loss, can be used as the properties-correcting agent of barium strontium titanate material.For example, U.S. Patent application file US531290, US5635434 and US5427988 disclose by doping magnesium oxide (MgO) or aluminium sesquioxide (Al
2o
3) modification, make its material have low-k, low dielectric loss, high can hamony, Curie-point temperature is low and stability is high advantageous property, can meet the theoretical requirement of phased array antenna completely.
Direct current arc plasma is that the quick synthetic technology of high temperature has temperature of reaction high, and temperature of reaction reaches as high as 5000 DEG C.Many countries such as the U.S., Japan utilize preparation, structure, mechanism and the phasor etc. of the exotic materialss such as direct current arc method research inorganic metal, nonmetal, high-meltiing alloy in recent years.Can within the several seconds, complete because direct current arc method itself heats up and lowers the temperature, can under molten state, make reactant with the evenly reaction rapidly of atom level state, therefore can make material moment synthetic, obtain the material that quality is high, performance is good.Especially synthetic for doping or composite inorganic material, because doping oxide is diffusion and solid solution rapidly at matrix crystal boundary, makes on the boundary of matrix grain, to form insulation grain boundary layer, can make being not insulated of whole crystal grain, and have semi-conductive character.
Strontium-barium titanate electron ceramic material is at present generally by solid phase method and Liquid preparation methods.The powder foreign matter content that solid phase method makes is high, broad particle distribution, and the method exists that sintering temperature is high, reaction time long and the defect such as complicated operation.Also there are some shortcomings that are difficult to overcome and greatly limited its practical application in liquid phase method, for example: coprecipitation method raw materials cost is higher, complex process, the powder reuniting of preparation is comparatively serious, and is difficult to remove foreign ion; That crystal grain that hydrothermal method obtains is grown is good, even particle size distribution, reunion are less, without calcining, but synthetic BST material property is not necessarily good, its reaction also lacks enough thermodynamic datas, and conventionally under High Temperature High Pressure, carry out, equipment requirements is high, cost is larger, and this brings certain difficulty to the suitability for industrialized production of the method.The powder purity of general sol-gel method products obtained therefrom is higher, but because the powder that its expensive cost of material, high-temperature heat treatment cause is reunited fast, and reaction time is long and reaction conditions is wayward, and output is less, therefore will realize its suitability for industrialized production, difficulty is higher.
Arc process is generally used for the preparation of the property materials such as inorganic metal, nonmetal, high-meltiing alloy, Chinese patent application file CN1683274A and CN1683273A all disclose the method for high temperature quick synthesizing blender or compound titanate ceramic powder, synthesizing of the ceramic powder that the method can be adulterated for list, but for complicated system, the raw material that need to use many oxide and different in kind, prior art rarely has and relates to.
Summary of the invention
The preparation method who the invention provides a kind of doping or composite barium strontium titanate ceramics powder, comprising:
1) by doping oxide or doping oxide presoma and strontium-barium titanate Ba
xsr
1-xtiO
3(0<x<1) presoma mixes; Described doping oxide is MgO or Al
2o
3, or MgO and Al
2o
3mixture.Described doping oxide presoma can obtain described doping oxide after burning and losing.
Described doping oxide presoma can use oxyhydroxide or carbonic acid thing, because it at high temperature can resolve into oxide compound, as magnesiumcarbonate can be decomposed into magnesium oxide and titanium dioxide at 800 DEG C, it can be also corresponding organic metal salt.Described Ba
xsr
1-xtiO
3(0<x<1) presoma is that after roasting, component is Ba
xsr
1-xtiO
3mixture, the source of each element can be oxide compound or corresponding carbonic acid or other inorganic/organic salt, such as barium source in described mixture can be BaO or barium carbonate, Sr source can be strontium oxide or Strontium carbonate powder.
Preferably, the quality of described strontium-barium titanate presoma is pressed Ba
xsr
1-xtiO
3(0<x<1), while calculating, the add-on of described doping oxide is 1～60% of strontium-barium titanate presoma.
2) add tackiness agent, grind compressing tablet;
Preferably, described binding agent is macrogol, and add-on is 5-10wt%.
3) then pressed compact is put into reaction chamber, be filled with rare gas element, light electric arc sample is reacted, product abrasive dust.
Preferably, when reaction, electric current is 50-200A, and the reaction times is about 15-60 second.
The present invention has advantages of as follows:
(1) speed of response is fast: the present invention utilizes plasma body direct-current discharge, preparation doping or composite barium strontium titanate ceramics material, top temperature can reach 5000 DEG C, and heat-up rate is exceedingly fast, can various reactants be reacted under molten state in moment, can within the several seconds, complete the synthetic and phase transformation of sample; Speed of cooling is fast, near room temperature in several minutes, and the acquisition of sample has been prepared about needs one hour from raw material.
(2) product purity is high, performance good: plasma body is the gaseous substance in highly ionized state, this condition is undoubtedly favourable to there is chemical reaction, the present invention utilizes vacuum melting furnace direct-current discharge, preparation doping or composite barium strontium titanate ceramics material, making reactant reach ion level level mixes, reactant is even, rapid reaction under ionic condition, and the material purity of acquisition is high, and performance is good.
(3) constant product quality and favorable reproducibility, impurity is few: plasma body is that pure ionization produces, and can not introduce any impurity, because its temperature is high, without any need for solubility promoter, additive, catalyzer, constant product quality and favorable reproducibility.
(4) reaction of the present invention is to complete in inert atmosphere argon gas, can promote composite barium strontium titanate ceramics powder crystal grain to grow complete; Be conducive to form intercrystalline grain boundary layer simultaneously, improved the good semiconductor transformation degree of barium-strontium titanate ceramic material.
(5) technique of the present invention is simple, easy to operate, and cost is low, and whole reaction process is nontoxic, harmless, pollution-free.
Preparation method of the present invention and dopant material can improve the dielectric properties of strontium-barium titanate, reduce specific inductivity and the dielectric loss rate of material, material can keep in a big way can hamony, thereby make it be applied to better phased array antenna material.
Embodiment
Be below two preferred embodiments of the present invention, it is only as explanation of the invention instead of restriction.
Following examples all adopt following step to be prepared:
By oxide M gO, Al
2o
3, MgO and Al
2o
3be doped to respectively strontium-barium titanate Ba
xsr
1-xtiO
3(0<x<1) in.Raw material is mixed, add 5-10wt% macrogol (PVA) as tackiness agent, grind compressing tablet, then pressed compact is put into the copper crucible of reaction chamber, pass into water coolant, vacuumize, be filled with argon gas, regulate electric current, light electric arc sample is reacted, electric current is 50-200A, and the reaction times is about 15-60 second.And the sample obtaining after reaction is worn into powder.
Embodiment mono-: one is prepared aluminium sesquioxide (Al
2o
3) barium strontium titanate doped stupalith (80wt%Ba
0.6sr
0.4tiO
3+ 20wt%Al
2o
3) method:
Take respectively 1.8399g(0.012mol) barium oxide (BaO), 0.8289g(0.008mol) strontium oxide (SrO), 1.5976g(0.02mol) titanium dioxide (TiO
2) and 1.0666g(0.01046mol) aluminium sesquioxide (Al
2o
3).Proportioning raw materials is mixed, add 5wt% macrogol (PVA) as tackiness agent, grind 15 minutes, be then pressed into the pressed compact that diameter is 15mm, then pressed compact put into the copper crucible of the reaction chamber of direct current arc electric discharge device, pass into water coolant, be evacuated to 10
-3normal atmosphere, be filled with argon gas and keep an a little higher than atmospheric pressure, regulate electric current, light electric arc sample is reacted, electric current is 100A, and the reaction times is about 20 seconds; After having reacted, powered-down, adjusting pressure, taking-up sample are worn into powder.It is aluminium sesquioxide (Al that the analysis of process XRD diffractogram can obtain product
2o
3) doping strontium-barium titanate ceramic powder.
Embodiment bis-: one is prepared the barium strontium titanate doped stupalith (80wt%Ba of magnesium oxide (MgO)
0.6sr
0.4tiO
3+ 20wt%MgO) method:
Take respectively 1.8399g(0.012mol) barium oxide (BaO), 0.8289g(0.008mol) strontium oxide (SrO), 1.5976g(0.02mol) titanium dioxide (TiO
2) and 1.0666g(0.02646mol) magnesium oxide (MgO).Raw material is mixed, add 5wt% macrogol (PVA) as tackiness agent, grind 15 minutes, be then pressed into the pressed compact that diameter is 15mm, then pressed compact put into the copper crucible of the reaction chamber of direct current arc electric discharge device, pass into water coolant, be evacuated to 10
-3normal atmosphere, be filled with argon gas and keep an a little higher than atmospheric pressure, regulate electric current, light electric arc sample is reacted, electric current is 100A, and the reaction times is about 20 seconds; After having reacted, powered-down, adjusting pressure, taking-up sample are worn into powder.Through XRD diffractogram, analysis can obtain the strontium-barium titanate ceramic powder that product is magnesium oxide (MgO) doping.
Embodiment tri-: one is prepared aluminium sesquioxide (Al
2o
3) barium strontium titanate doped stupalith (99wt%Ba
0.5sr
0.5tiO
3+ 1wt%Al
2o
3) method:
Take respectively 1.5333g(0.01mol) barium oxide (BaO), 1.0362g(0.01mol) strontium oxide (SrO), 1.5976g(0.02mol) titanium dioxide (TiO
2) and 0.0421g(0.0004mol) aluminium sesquioxide (Al
2o
3).Raw material is mixed, add 5wt% macrogol (PVA) as tackiness agent, grind 15 minutes, be then pressed into the pressed compact that diameter is 15mm, then pressed compact put into the copper crucible of the reaction chamber of direct current arc electric discharge device, pass into water coolant, be evacuated to 10
-3normal atmosphere, be filled with argon gas and keep an a little higher than atmospheric pressure, regulate electric current, light electric arc sample is reacted, electric current is 100A, and the reaction times is about 20 seconds; After having reacted, powered-down, adjusting pressure, taking-up sample are worn into powder.It is aluminium sesquioxide (Al that the analysis of process XRD diffractogram can obtain product
2o
3) doping strontium-barium titanate ceramic powder.
Embodiment tetra-: one is prepared the barium strontium titanate doped stupalith (99wt%Ba of magnesium oxide (MgO)
0.2sr
0.8tiO
3+ 1wt%MgO) method:
Take respectively 0.6133g(0.004mol) barium oxide (BaO), 1.6579g(0.016mol) strontium oxide (SrO), 1.5976g(0.02mol) titanium dioxide (TiO
2) and 0.0391g(0.001mol) magnesium oxide (MgO).Raw material is mixed, add 5wt% macrogol (PVA) as tackiness agent, grind 15 minutes, be then pressed into the pressed compact that diameter is 15mm, then pressed compact put into the copper crucible of the reaction chamber of direct current arc electric discharge device, pass into water coolant, be evacuated to 10
-3normal atmosphere, be filled with argon gas and keep an a little higher than atmospheric pressure, regulate electric current, light electric arc sample is reacted, electric current is 100A, and the reaction times is about 20 seconds; After having reacted, powered-down, adjusting pressure, taking-up sample are worn into powder.Through XRD diffractogram, analysis can obtain the strontium-barium titanate ceramic powder that product is magnesium oxide (MgO) doping.
Embodiment five: one is prepared aluminium sesquioxide (Al
2o
3) barium strontium titanate doped stupalith (40wt%Ba
0.6sr
0.4tiO
3+ 60wt%Al
2o
3) method:
Take respectively 2.3680g(0.012mol) barium carbonate (BaCO
3), 1.1810g(0.008mol) Strontium carbonate powder (SrCO
3), 1.5976g(0.02mol) titanium dioxide (TiO
2) and 7.7199g(0.0751mol) aluminium sesquioxide (Al
2o
3).Proportioning raw materials is mixed, add 5wt% macrogol (PVA) as tackiness agent, grind 15 minutes, be then pressed into the pressed compact that diameter is 15mm, then pressed compact put into the copper crucible of the reaction chamber of direct current arc electric discharge device, pass into water coolant, be evacuated to 10
-3normal atmosphere, be filled with argon gas and keep an a little higher than atmospheric pressure, regulate electric current, light electric arc sample is reacted, electric current is 100A, and the reaction times is about 20 seconds; After having reacted, powered-down, adjusting pressure, taking-up sample are worn into powder.Obtain aluminium sesquioxide (Al
2o
3) doping strontium-barium titanate ceramic powder.
Embodiment six: one is prepared the barium strontium titanate doped stupalith (40wt%Ba of magnesium oxide (MgO)
0.6sr
0.4tiO
3+ 60wt%MgO) method:
Take respectively 2.3680g(0.012mol) barium carbonate (BaCO
3), 1.1810g(0.008mol) Strontium carbonate powder (SrCO
3), 1.5976g(0.02mol) titanium dioxide (TiO
2) and 7.7199g(0.1915mol) magnesium oxide (MgO).Raw material is mixed, add 5wt% macrogol (PVA) as tackiness agent, grind 15 minutes, be then pressed into the pressed compact that diameter is 15mm, then pressed compact put into the copper crucible of the reaction chamber of direct current arc electric discharge device, pass into water coolant, be evacuated to 10
-3normal atmosphere, be filled with argon gas and keep an a little higher than atmospheric pressure, regulate electric current, light electric arc sample is reacted, electric current is 100A, and the reaction times is about 20 seconds; After having reacted, powered-down, adjusting pressure, taking-up sample are worn into powder.Obtain the strontium-barium titanate ceramic powder of magnesium oxide (MgO) doping.
Embodiment seven: one is prepared aluminium sesquioxide (Al
2o
3) and the barium strontium titanate doped stupalith (40wt%Ba of magnesium oxide (MgO)
0.6sr
0.4tiO
3+ 30wt%Al
2o
3+ 30wt%MgO) method:
Take respectively 1.8399g(0.012mol) barium oxide (BaO), 0.8289g(0.008mol) strontium oxide (SrO), 1.5976g(0.02mol) titanium dioxide (TiO
2), 3.1998g(0.03138mol) aluminium sesquioxide (Al
2o
3) and 3.1988g(0.0723mol) magnesium oxide (MgO).Proportioning raw materials is mixed, add 5wt% macrogol (PVA) as tackiness agent, grind 15 minutes, be then pressed into the pressed compact that diameter is 15mm, then pressed compact put into the copper crucible of the reaction chamber of direct current arc electric discharge device, pass into water coolant, be evacuated to 10
-3normal atmosphere, be filled with argon gas and keep an a little higher than atmospheric pressure, regulate electric current, light electric arc sample is reacted, electric current is 100A, and the reaction times is about 20 seconds; After having reacted, powered-down, adjusting pressure, taking-up sample are worn into powder.Can obtain product is aluminium sesquioxide (Al
2o
3) and the strontium-barium titanate ceramic powder of magnesium oxide (MgO) doping.
Claims (4)
1. prepare the method for doped and compounded strontium-barium titanate ceramic powder for one kind
1) by doping oxide or doping oxide presoma and strontium-barium titanate Ba
xsr
1-xtiO
3(0<x<1) presoma mixes; Described doping oxide MgO or Al
2o
3, or MgO and Al
2o
3mixture; Described doping oxide presoma can obtain described doping oxide after burning and losing;
2) add tackiness agent, grind compressing tablet;
3) then pressed compact is put into reaction chamber, be filled with rare gas element, light electric arc sample is reacted, product abrasive dust.
2. method according to claim 1, is characterized in that, the quality of described strontium-barium titanate presoma is pressed Ba
xsr
1-xtiO
3(0<x<1), while calculating, the add-on of described doping oxide is 1～60% of strontium-barium titanate presoma.
3. method according to claim 1, is characterized in that, described binding agent is macrogol, and add-on is 5-10wt%.
4. method according to claim 1, is characterized in that step 3) when reaction electric current be 50-200A, the reaction times is about 15-60 second.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105272217A (en) * | 2015-10-21 | 2016-01-27 | 浙江大学 | Barium strontium titanate based aluminum oxide composite ceramic with high energy storage density and preparation method of barium strontium titanate based aluminum oxide composite ceramic |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5312790A (en) * | 1993-06-09 | 1994-05-17 | The United States Of America As Represented By The Secretary Of The Army | Ceramic ferroelectric material |
| CN1683273A (en) * | 2005-03-10 | 2005-10-19 | 中国科学院青海盐湖研究所 | Method for high temperature quick synthesizing blender or compound titanate ceramic powder |
| CN103214238A (en) * | 2013-04-03 | 2013-07-24 | 湖北大学 | Preparation method of barium strontium titanate dielectric temperature stable ceramic capacitor material |
-
2014
- 2014-04-16 CN CN201410153715.0A patent/CN103951418A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5312790A (en) * | 1993-06-09 | 1994-05-17 | The United States Of America As Represented By The Secretary Of The Army | Ceramic ferroelectric material |
| US5427988A (en) * | 1993-06-09 | 1995-06-27 | The United States Of America As Represented By The Secretary Of The Army | Ceramic ferroelectric composite material - BSTO-MgO |
| CN1683273A (en) * | 2005-03-10 | 2005-10-19 | 中国科学院青海盐湖研究所 | Method for high temperature quick synthesizing blender or compound titanate ceramic powder |
| CN103214238A (en) * | 2013-04-03 | 2013-07-24 | 湖北大学 | Preparation method of barium strontium titanate dielectric temperature stable ceramic capacitor material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105272217A (en) * | 2015-10-21 | 2016-01-27 | 浙江大学 | Barium strontium titanate based aluminum oxide composite ceramic with high energy storage density and preparation method of barium strontium titanate based aluminum oxide composite ceramic |
| CN105272217B (en) * | 2015-10-21 | 2017-06-23 | 浙江大学 | A kind of barium-strontium titanate-based Toughened Alumina Ceramics of high energy storage density and preparation method thereof |
| 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 |
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Application publication date: 20140730 |