CN102060523B - Composite material with high dielectric constant and preparation method thereof - Google Patents
Composite material with high dielectric constant and preparation method thereof Download PDFInfo
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- CN102060523B CN102060523B CN 201010545442 CN201010545442A CN102060523B CN 102060523 B CN102060523 B CN 102060523B CN 201010545442 CN201010545442 CN 201010545442 CN 201010545442 A CN201010545442 A CN 201010545442A CN 102060523 B CN102060523 B CN 102060523B
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- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 44
- 239000002994 raw material Substances 0.000 claims abstract description 34
- 238000005245 sintering Methods 0.000 claims abstract description 19
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000000758 substrate Substances 0.000 claims description 23
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 9
- 229910000831 Steel Inorganic materials 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 8
- 239000012467 final product Substances 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 8
- 230000003179 granulation Effects 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 239000010959 steel Substances 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 239000010949 copper Substances 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 8
- 229910002113 barium titanate Inorganic materials 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 3
- 230000032683 aging Effects 0.000 abstract 1
- 229910052454 barium strontium titanate Inorganic materials 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 description 12
- 238000005452 bending Methods 0.000 description 8
- 235000013339 cereals Nutrition 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000005325 percolation Methods 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
- Inorganic Insulating Materials (AREA)
Abstract
The invention provides a composite material with a high dielectric constant. The composition of the composite material is expressed as BaTiO3/xCu, wherein x is 0 to 30 weight percent. The invention also provides a preparation method of the material, which comprises: mixing barium strontium titanate powder and copper powder, which serve as raw materials, according to a BaTiO3 to Cu ratio of 1:x, wherein the x is 0 to 30 weight percent; mixing the mixture with a ball milling medium and ballstone; and ball milling, drying granulating, aging, pressing to form a film, sintering and cooling to obtain BaTiO3/xCu. In the invention, the preparation process is simple and has the characteristics of low cost and no pollution.
Description
Technical field
The invention belongs to Material Field, relate to a kind of electronic material and preparation method thereof, relate in particular to a kind of composite material with high dielectric constant and preparation method thereof.
Background technology
It is increasingly difficult that the preparation single-material makes it satisfy current development in Hi-Tech requirement, more and more adopts at present the Material cladding technology to prepare high performance composite.Ceramic-metal composite is widely used in the various technical fields with heat-resisting, wear-resisting, erosion resistance and the special excellent properties such as electrical property of its height.
As a kind of good electronic ceramics matrix, pure BaTiO
3The perovskite-type material of ferroelectric material and base is widely used in thermistor, electrical condenser, door dielectric substance and the information storage medium.Can realize BaTiO by mixing
3Charge balance, defective control, grain-size adjustment and crystal property improvement etc. in the base ceramic material, at present a lot of scholars are at BaTiO
3Adding metallographic phase in the base ceramic base is studied.Result of study shows, the introducing of metal can effectively improve the mechanical property of pottery, and metallographic phase can serve as the effect of a bridge and improve fracture toughness property and the intensity of body when the crack propagation of body.And the introducing of certain content metal can effectively improve BaTiO in the time of particularly near percolation threshold
3The specific inductivity of base ceramic material, and seepage theory thinks that in conductor-isolator compound system, along with the continuous increase of conductive phase content, material can experience the transition process of insulation phase-conductor.
Yet present existing ceramic matric composite is selected expensive raw material (such as Ag, Pt) and complicated process of preparation mostly, and how reducing manufacturing cost and carrying out the cost-effectively design is to enlarge the major subjects that ceramic matric composite is used.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of composite material with high dielectric constant and preparation method thereof, this matrix material is take BaTiO3 powder and Cu powder as starting material, and preparation technology is simple, and it is low to have a cost, free of contamination characteristics.
To achieve these goals, the technical solution used in the present invention is:
A kind of composite material with high dielectric constant, it forms expression formula and is BaTiO
3/ xCu, wherein x=0～30wt.%.
The invention allows for a kind of described composite material with high dielectric constant method for preparing, may further comprise the steps,
The first step, adopting barium carbonate powder and copper powder is raw material, according to BaTiO
3/ xCu, x=0～30wt.% prepares burden;
Second step, with raw material, ball-milling medium and ballstone mix, then in the resin balls grinding jar on planetary ball mill ball milling 4h, wherein, the mass ratio of raw material, ball-milling medium and ballstone is: raw material: ball-milling medium: ballstone=1～1.5: 1～1.5: 1.5～2;
In the 3rd step, the slurry that ball milling is good is not higher than in vacuum drying oven under 50 ℃ the condition dries, and is that 3%～5% PVA carries out granulation, grain mistake 150 mesh sieves of making, old 24h with concentration then;
In the 4th step, with old good grain, put into steel die and depress to cylindrical base substrate in the pressure of 5MPa, pressurize 30s;
The 5th step, base substrate is put into crucible, again crucible to be put into tube-type atmosphere furnace and carried out sintering, the temperature of sintering is 1300 ± 50 ℃, constant temperature 2 hours;
The 6th step, be down to room temperature, get final product to get BaTiO
3/ xCu.
Ball-milling medium in the described second step is dehydrated alcohol.
The temperature-fall period in the sintering in described the 5th step and the 6th step all carries out in nitrogen atmosphere.
The described room temperature of being down to, at 1300 ℃～1000 ℃ when interval, rate of temperature fall is 2 ℃/min.
In described the 3rd step, the slurry after per 100 gram oven dry, the volume that adds PVA is 10～20ml.
The base substrate thickness of cylindrical base substrate is 2mm in described the 4th step, and diameter is 10mm.
The present invention compared with prior art has the following advantages:
1) cost is low, and metal ingredient is selected the comparatively cheap Cu of price, has reduced cost.
2) bending strength is high, reaches as high as 130MPa.
3) fracture toughness property is strong, reaches as high as 1.55MPam
1/2
4) specific inductivity is large, can reach～9000.
5) the dielectric temperature coefficient is little, in 25 ℃～115 ℃ scopes＜5%.
Description of drawings
Fig. 1 is BaTiO of the present invention
3/ xCu, when x=5,10,15,20,25,30wt.%, the XRD figure of matrix material; Wherein X-coordinate represents the diffraction angle number of degrees, and ordinate zou represents the intensity of diffraction peak, and the solid black dice represents BaTiO among the figure
3, open circles represents Cu.
Fig. 2 is BaTiO of the present invention
3/ xCu, when x=5,10,15,20,25,30wt.%, the mechanical property of matrix material is with the change curve of copper content; Wherein X-coordinate represents Cu content, and left side ordinate zou represents bending strength, and the right ordinate zou represents fracture toughness property, and curve A is the fracture toughness property curve, and curve B is the bending strength curve.
Fig. 3 is BaTiO of the present invention
3/ xCu, when x=5,10,15,20,25,30wt.%, the resistivity of matrix material is with copper content graphic representation; Wherein X-coordinate represents the content of Cu, and ordinate zou represents resistivity.
Fig. 4 is BaTiO of the present invention
3/ xCu matrix material dielectric properties are with frequency variation curve figure; Wherein, X-coordinate represents test frequency, and ordinate zou represents specific inductivity.
Fig. 5 is BaTiO of the present invention
3The two-phase microstructure composition model of/xCu matrix material copper content below percolation threshold; Wherein, white circle expression expression BaTiO
3, the solid black circle represents Cu.
Fig. 6 is BaTiO of the present invention
3The two-phase microstructure composition model of/xCu matrix material copper content more than percolation threshold; Wherein, white circle expression expression BaTiO
3, the solid black circle represents Cu.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further details.
Embodiment one
A kind of method for preparing composite material with high dielectric constant is characterized in that, may further comprise the steps,
The first step, adopting barium carbonate powder and copper powder is raw material, according to BaTiO
3/ xCu, x=30wt.% prepares burden;
Second step, with raw material, ball-milling medium and ballstone mix, then in the resin balls grinding jar on planetary ball mill ball milling 4h, wherein, the mass ratio of raw material, ball-milling medium and ballstone is: raw material: ball-milling medium: ballstone=1: 1: 1.5;
In the 3rd step, the slurry that ball milling is good is not higher than in vacuum drying oven under 50 ℃ the condition dries, and is that 3% PVA carries out granulation, grain mistake 150 mesh sieves of making, old 24h with concentration then;
The 4th step, with old good grain, put into steel die and depress to cylindrical base substrate in the pressure of 5MPa, pressurize 30s, base substrate thickness are 2mm, diameter is 10mm;
The 5th step, base substrate is put into crucible, again crucible to be put into tube-type atmosphere furnace and carried out sintering, the temperature of sintering is 1300 ℃, constant temperature 2 hours;
The 6th step, be down to room temperature, get final product to get BaTiO
3/ xCu.
After tested, BaTiO
3/ xCu, during x=30wt.%, the bending strength of matrix material of the present invention is 130MPa, fracture toughness property is 1.16MPam
1/2, resistivity is 0.112 * 10
3Europe rice, specific inductivity are 8090, dielectric temperature coefficient＜5%.
Embodiment two
A kind of method for preparing composite material with high dielectric constant is characterized in that, may further comprise the steps,
The first step, adopting barium carbonate powder and copper powder is raw material, according to BaTiO
3/ xCu, x=10wt.% prepares burden;
Second step, with raw material, ball-milling medium and ballstone mix, then in the resin balls grinding jar on planetary ball mill ball milling 4h, wherein, the mass ratio of raw material, ball-milling medium and ballstone is: raw material: ball-milling medium: ballstone=1: 1.2: 2;
In the 3rd step, the slurry that ball milling is good is not higher than in vacuum drying oven under 50 ℃ the condition dries, and is that 4% PVA carries out granulation, grain mistake 150 mesh sieves of making, old 24h with concentration then;
The 4th step, with old good grain, put into steel die and depress to cylindrical base substrate in the pressure of 5MPa, pressurize 30s, base substrate thickness are 2mm, diameter is 10mm;
The 5th step, base substrate is put into crucible, again crucible to be put into tube-type atmosphere furnace and carried out sintering, the temperature of sintering is 1250 ℃, constant temperature 2 hours;
The 6th step, be down to room temperature, get final product to get BaTiO
3/ xCu.
After tested, BaTiO
3/ xCu, during x=10wt.%, the bending strength of matrix material of the present invention is 55MPa, fracture toughness property is 1.55MPam
1/2, resistivity is 1.3 * 10
3Europe rice, specific inductivity are 3190, dielectric temperature coefficient＜5%.
Embodiment three
A kind of method for preparing composite material with high dielectric constant is characterized in that, may further comprise the steps,
The first step, adopting barium carbonate powder and copper powder is raw material, according to BaTiO
3/ xCu, x=1wt.% prepares burden;
Second step, with raw material, ball-milling medium and ballstone mix, then in the resin balls grinding jar on planetary ball mill ball milling 4h, wherein, the mass ratio of raw material, ball-milling medium and ballstone is: raw material: ball-milling medium: ballstone=1.5: 1.5: 2;
In the 3rd step, the slurry that ball milling is good is not higher than in vacuum drying oven under 50 ℃ the condition dries, and is that 5% PVA carries out granulation, grain mistake 150 mesh sieves of making, old 24h with concentration then;
The 4th step, with old good grain, put into steel die and depress to cylindrical base substrate in the pressure of 5MPa, pressurize 30s, base substrate thickness are 2mm, diameter is 10mm;
The 5th step, base substrate is put into crucible, again crucible to be put into tube-type atmosphere furnace and carried out sintering, the temperature of sintering is 1350 ℃, constant temperature 2 hours;
The 6th step, be down to room temperature, get final product to get BaTiO
3/ xCu.
After tested, BaTiO
3/ xCu, during x=1wt.%, the bending strength of matrix material of the present invention is 68.8MPa, fracture toughness property is 1.5MPam
1/2, resistivity is 1.39 * 10
3Europe rice, specific inductivity are 2780, dielectric temperature coefficient＜5%.
By reference to the accompanying drawings 2 to 4 and embodiment, can find, the bending strength of matrix material of the present invention roughly is directly proportional with the content of Cu, fracture toughness property roughly is inversely proportional to the content of Cu, resistivity roughly is inversely proportional to the content of Cu, the specific inductivity maximum can reach～and 9000, the dielectric temperature coefficient in 25 ℃～115 ℃ scopes＜5%, compare with existing dielectric materials, have on the whole the bending strength height, fracture toughness property is strong, specific inductivity is large, the characteristics that the dielectric temperature coefficient is low, simultaneously starting material wide material sources, cheap, the present invention provides a kind of thinking for dielectric materials and preparation thereof.
Claims (9)
1. method for preparing composite material with high dielectric constant, the composition expression formula of described composite material with high dielectric constant is BaTiO
3/ xCu, wherein x=0～30wt.% is characterized in that, may further comprise the steps,
The first step, adopting barium carbonate powder and copper powder is raw material, according to BaTiO
3/ xCu, x=0～30wt.% prepares burden;
Second step, with raw material, ball-milling medium and ballstone mix, then in the resin balls grinding jar on planetary ball mill ball milling 4h, wherein, the mass ratio of raw material, ball-milling medium and ballstone is: raw material: ball-milling medium: ballstone=1～1.5:1～1.5:1.5～2;
In the 3rd step, the slurry that ball milling is good is not higher than in vacuum drying oven under 50 ℃ the condition dries, and is that 3%～5% PVA carries out granulation, grain mistake 150 mesh sieves of making, old 24h with concentration then;
In the 4th step, old good grain is put into steel die depress to cylindrical base substrate in the pressure of 5MPa, pressurize 30s;
The 5th step, base substrate is put into crucible, again crucible to be put into tube-type atmosphere furnace and carried out sintering, the temperature of sintering is 1300 ± 50 ℃, constant temperature 2 hours;
The 6th step, be down to room temperature, get final product to get BaTiO
3/ xCu.
2. a kind of method for preparing composite material with high dielectric constant according to claim 1 is characterized in that, may further comprise the steps,
The first step, adopting barium carbonate powder and copper powder is raw material, according to BaTiO
3/ xCu, x=30wt.% prepares burden;
Second step, with raw material, ball-milling medium and ballstone mix, then in the resin balls grinding jar on planetary ball mill ball milling 4h, wherein, the mass ratio of raw material, ball-milling medium and ballstone is: raw material: ball-milling medium: ballstone=1:1:1.5;
In the 3rd step, the slurry that ball milling is good is not higher than in vacuum drying oven under 50 ℃ the condition dries, and is that 3% PVA carries out granulation, grain mistake 150 mesh sieves of making, old 24h with concentration then;
In the 4th step, with old good grain, put into steel die and depress to cylindrical base substrate in the pressure of 5MPa, pressurize 30s;
The 5th step, base substrate is put into crucible, again crucible to be put into tube-type atmosphere furnace and carried out sintering, the temperature of sintering is 1300 ℃, constant temperature 2 hours;
The 6th step, be down to room temperature, get final product to get BaTiO
3/ xCu.
3. a kind of method for preparing composite material with high dielectric constant according to claim 1 is characterized in that, may further comprise the steps,
The first step, adopting barium carbonate powder and copper powder is raw material, according to BaTiO
3/ xCu, x=10wt.% prepares burden;
Second step, with raw material, ball-milling medium and ballstone mix, then in the resin balls grinding jar on planetary ball mill ball milling 4h, wherein, the mass ratio of raw material, ball-milling medium and ballstone is: raw material: ball-milling medium: ballstone=1:1.2:2;
In the 3rd step, the slurry that ball milling is good is not higher than in vacuum drying oven under 50 ℃ the condition dries, and is that 4% PVA carries out granulation, grain mistake 150 mesh sieves of making, old 24h with concentration then;
In the 4th step, with old good grain, put into steel die and depress to cylindrical base substrate in the pressure of 5MPa, pressurize 30s;
The 5th step, base substrate is put into crucible, again crucible to be put into tube-type atmosphere furnace and carried out sintering, the temperature of sintering is 1250 ℃, constant temperature 2 hours;
The 6th step, be down to room temperature, get final product to get BaTiO
3/ xCu.
4. a kind of method for preparing composite material with high dielectric constant according to claim 1 is characterized in that, may further comprise the steps,
The first step, adopting barium carbonate powder and copper powder is raw material, according to BaTiO
3/ xCu, x=1wt.% prepares burden;
Second step, with raw material, ball-milling medium and ballstone mix, then in the resin balls grinding jar on planetary ball mill ball milling 4h, wherein, the mass ratio of raw material, ball-milling medium and ballstone is: raw material: ball-milling medium: ballstone=1.5:1.5:2;
In the 3rd step, the slurry that ball milling is good is not higher than in vacuum drying oven under 50 ℃ the condition dries, and is that 5% PVA carries out granulation, grain mistake 150 mesh sieves of making, old 24h with concentration then;
In the 4th step, with old good grain, put into steel die and depress to cylindrical base substrate in the pressure of 5MPa, pressurize 30s;
The 5th step, base substrate is put into crucible, again crucible to be put into tube-type atmosphere furnace and carried out sintering, the temperature of sintering is 1350 ℃, constant temperature 2 hours;
The 6th step, be down to room temperature, get final product to get BaTiO
3/ xCu.
5. according to claim 1 to the described a kind of method for preparing composite material with high dielectric constant of 4 arbitrary claims, it is characterized in that the ball-milling medium in the described second step is dehydrated alcohol.
6. according to claim 1 to the described a kind of method for preparing composite material with high dielectric constant of 4 arbitrary claims, it is characterized in that the sintering in described the 5th step and the temperature-fall period in the 6th step all carry out in nitrogen atmosphere.
7. according to claim 1 and 2 or the described a kind of method for preparing composite material with high dielectric constant of 4 arbitrary claims, it is characterized in that, the described room temperature of being down to, at 1300 ℃～1000 ℃ when interval, rate of temperature fall is 2 ℃/min.
8. according to claim 1 to the described a kind of method for preparing composite material with high dielectric constant of 4 arbitrary claims, it is characterized in that the base substrate thickness of cylindrical base substrate is 2mm in described the 4th step, diameter is 10mm.
9. a kind of method for preparing composite material with high dielectric constant according to claim 3 is characterized in that, the described room temperature of being down to, and at 1250 ℃～1000 ℃ when interval, rate of temperature fall is 2 ℃/min.
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| CN103864421A (en) * | 2014-01-25 | 2014-06-18 | 陕西科技大学 | Method for preparing BCTZ-xCu giant dielectric ceramic |
| KR102523255B1 (en) * | 2019-06-28 | 2023-04-19 | 가부시키가이샤 무라타 세이사쿠쇼 | Multilayer Electronic Component |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4283753A (en) * | 1979-09-28 | 1981-08-11 | Sprague Electric Company | Low firing monolithic ceramic capacitor with high dielectric constant |
| 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 |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4283753A (en) * | 1979-09-28 | 1981-08-11 | Sprague Electric Company | Low firing monolithic ceramic capacitor with high dielectric constant |
| 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 |
Non-Patent Citations (3)
| Title |
|---|
| Archana Shukla et al..Structural,microstructural and electrical studies of La and Cu doped BaTiO3 ceramics.《Physica B》.2009,第405卷第99-106页. * |
| ArchanaShuklaetal..Structural microstructural and electrical studies of La and Cu doped BaTiO3 ceramics.《Physica B》.2009 |
| Nobuhiro Kumada et al..Rising Tc in Bi and Cu co-doped BaTiO3.《Materials Letters》.2009,第64卷第383-385页. * |
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