CN102992763B - Potassium sodium niobate-titanium zinc bismuth-bismuth aluminate ternary lead-free high-temperature capacitor dielectric material and preparation method thereof - Google Patents
Potassium sodium niobate-titanium zinc bismuth-bismuth aluminate ternary lead-free high-temperature capacitor dielectric material and preparation method thereof Download PDFInfo
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- 239000003989 dielectric material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000003990 capacitor Substances 0.000 title claims abstract description 11
- 229940104825 bismuth aluminate Drugs 0.000 title claims abstract description 7
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 44
- 238000000498 ball milling Methods 0.000 claims abstract description 36
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000919 ceramic Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 238000005469 granulation Methods 0.000 claims abstract description 8
- 230000003179 granulation Effects 0.000 claims abstract description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 42
- 239000000463 material Substances 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 21
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 20
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 20
- 239000011230 binding agent Substances 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 229910052758 niobium Inorganic materials 0.000 claims description 10
- 239000010955 niobium Substances 0.000 claims description 10
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 10
- 235000015320 potassium carbonate Nutrition 0.000 claims description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 10
- 239000004408 titanium dioxide Substances 0.000 claims description 10
- 239000011787 zinc oxide Substances 0.000 claims description 10
- 239000011701 zinc Substances 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 238000000748 compression moulding Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 5
- IYNWNKYVHCVUCJ-UHFFFAOYSA-N bismuth Chemical compound [Bi].[Bi] IYNWNKYVHCVUCJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 238000001354 calcination Methods 0.000 abstract description 6
- 229910052793 cadmium Inorganic materials 0.000 abstract description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract description 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract 2
- 229910002115 bismuth titanate Inorganic materials 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 239000011734 sodium Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 6
- 239000003985 ceramic capacitor Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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Abstract
本发明公开一种铌酸钠钾-钛锌酸铋-铝酸铋三元系无铅高温电容介质材料及其制备方法。电容瓷料体系通式为(1-y-z)K1-xNaxNbO3-yBi(Zn0.5Ti0.5)O3-zBiAlO3的基体和占基体0.5-3wt%的三氧化二铋制备而得，其中0.5≤x≤0.53，0.005≤y≤0.12，0.005≤z≤0.08。其制备方法包括细化原料粉体、球磨混料、预烧、造粒、过筛、制坯，烧结、被电极等。本发明提供一种无铅铌酸盐基三元系高温电容介质材料，所用的原料种类少，制备工艺简单。其显著优点在于：不含铅、镉等有害物质，对环境友好；具有较高的介电常数，较低的损耗，在高温区域具有良好的温度稳定性；本发明提供的电容陶瓷材料可满足温度范围为-50～300℃的工作环境需要。
The invention discloses a sodium potassium niobate-bismuth titanate zincate-bismuth aluminate ternary system lead-free high-temperature capacitor dielectric material and a preparation method thereof. The general formula of the capacitor ceramic system is (1-yz)K 1-x Na x NbO 3 -yBi(Zn 0.5 Ti 0.5 )O 3 -zBiAlO 3 matrix and prepared from bismuth trioxide accounting for 0.5-3wt% of the matrix , where 0.5≤x≤0.53, 0.005≤y≤0.12, 0.005≤z≤0.08. Its preparation method includes fine raw material powder, ball milling, pre-calcination, granulation, sieving, billet making, sintering, electrode and the like. The invention provides a lead-free niobate-based ternary system high-temperature capacitor dielectric material, which uses few types of raw materials and has a simple preparation process. Its remarkable advantages are: it does not contain harmful substances such as lead and cadmium, and is environmentally friendly; it has high dielectric constant, low loss, and good temperature stability in high temperature areas; the capacitor ceramic material provided by the invention can meet It is required for the working environment with temperature range of -50～300℃.
Description
Technical field
The present invention relates to a kind of polynary system niobate pyroceramic dielectric material combination thing, particularly a kind of potassium-sodium niobate-titanium zincic acid bismuth-Bismuth Aluminate three component system lead-free high-temperature electric capacity porcelain and preparation method thereof.
Background technology
Along with fast development and the update in the fields such as mobile phone, computer, automotive electronics and stereo set, growing with each passing day in the status of laminated ceramic capacitor (being called for short MLCC), in electrical condenser market, has accounted for leading.Meanwhile, along with the continuous expansion of the market requirement, the innovation of ceramic condenser technology is also constantly being carried out.Thin layer heavy body, lowpriced metallization, high temperature resistant, environmental protection etc. are the Main Trends of The Developments of current laminated ceramic capacitor.
In current laminated ceramic capacitor product, due to X7R type MLCC have high-k and good temperature stability (55 ℃～125 ℃, C/C
25 ℃≤ ± 15%), thereby be most widely used.And engine electronic control unit, fuel injection program controling module, ABS (Anti-lock Braking System) etc. are because working conditions is special, require the working temperature upper limit of its electric capacity to bring up to 150 ℃.X7R type MLCC obviously can not meet the demands, and in order to adapt to exploitation and the application of electronic vehicle product, X8R type porcelain arises at the historic moment, and its maximum operating temperature is 150 ℃, has obtained in actual applications significant progress.Yet the harsher field of a few thing condition is as enngine control system, aerospace detection, drilling well etc., it is high temperature resistant, and electronics requires the upper temperature limit of its ceramic condenser to be increased to 200 ℃.Therefore, urgently develop the pyroceramic capacitor dielectric material with good temperature stability.The MLCC that China produces at present is mainly divided into two kinds, BaTiO
3base and Pb base.As everyone knows, BaTiO
3the firing temperature of base MLCC is conventionally more than 1300 ℃, must be with precious metal palladium or platinum as interior electrode, to realize and BaTiO
3the common burning of base ceramic dielectric material.If reduction sintering temperature, on the one hand can energy efficient, be expected on the other hand realize and palladium, the common burning of silver or its alloy, reduces production costs.Therefore the ceramic capacitor dielectric material of exploitation low temperature sintering has important practical significance.In addition, in the dielectric material of Pb base MLCC, contain a large amount of lead, the objectionable impuritiess such as cadmium, the MLCC dielectric material that these contain heavy metal in manufacture and after scrapping pollution on the environment day by day serious, developing unleaded, eco-friendly ceramic medium material has become global trend.
Summary of the invention
The object of the present invention is to provide a kind of good temperature stability that has in wide temperature range, can be at the unleaded multi-layer ceramic capacitance dielectric material of sintering below 1100 ℃ and preparation method thereof.This material has higher specific inductivity, lower loss and good repeatability.Adopt traditional electronic ceramic technology, be applicable to mass production.
The chemical constitution general formula of potassium-sodium niobate-titanium zincic acid bismuth-Bismuth Aluminate three component system lead-free high-temperature capacitor dielectric material involved in the present invention is: (1-y-z) K
1-xna
xnbO
3-yBi (Zn
0.5ti
0.5) O
3-zBiAlO
3, wherein: 0.5≤x≤0.53,0.005≤y≤0.12,0.005≤z≤0.08; X, y, z is molar weight.In order to compensate the volatilization of A bit element under high temperature, when batching, add the bismuthous oxide bismuth trioxide of total quality of material 0.5 ~ 3%.
The preparation process of above-mentioned potassium-sodium niobate-titanium zincic acid bismuth-Bismuth Aluminate three component system lead-free high-temperature capacitor dielectric material is:
(1), by the raw material ball milling of sodium carbonate, salt of wormwood, Niobium Pentxoxide, bismuthous oxide bismuth trioxide, zinc oxide, titanium dioxide and aluminium sesquioxide, guarantee that the specific surface area of each initial feed powder is not less than 15m
2/ g.
(2) step (1) gained material is pressed to (1-y-z) K
1-xna
xnbO
3-yBi (Zn
0.5ti
0.5) O
3-zBiAlO
3stoichiometric ratio batching, wherein: 0.5≤x≤0.53,0.005≤y≤0.12,0.005≤z≤0.08; X, y, z is molar weight; And add the bismuthous oxide bismuth trioxide of the total mass 0.5 ~ 3% of preparing burden.
(3) step (2) gained material is put into ball grinder and carried out wet ball-milling mixing 4 ~ 24 hours, ball-milling medium is zirconia ball and dehydrated alcohol, added zirconia ball quality is 5 ~ 10 times of batching quality, and added dehydrated alcohol quality is 0.8 ~ 2 times of batching total mass; The slurry that ball milling is crossed is pressed into cylinder after drying, and in 800 ~ 900 ℃ of air atmosphere, pre-burning is 2 ~ 8 hours; Cylinder after pre-burning is ground again to ball milling and within 4 ~ 12 hours, obtains preburning powder, added zirconia ball quality by 4 ~ 8 times of mill powder quality, added dehydrated alcohol quality by 0.8 ~ 1.5 times of mill powder quality; Then in preburning powder, add binding agent, granulation, sieves, then compression moulding; Last sintering 2 ~ 8 hours in the air atmosphere of 900 ~ 1100 ℃, described binding agent adopts the polyvinyl alcohol water solution that mass concentration is 5%, and add-on accounts for 4% ~ 10% of preburning powder gross weight.
Above-mentioned sodium carbonate, salt of wormwood, Niobium Pentxoxide, bismuthous oxide bismuth trioxide, zinc oxide, titanium dioxide, aluminium sesquioxide are analytical pure.
The invention provides a kind of unleaded niobate three component system high temperature capacitor dielectric material, raw material type used is few, and preparation technology is simple.Its remarkable advantage is: the objectionable impurities such as not leaded, cadmium, and environmentally friendly; Have higher specific inductivity, lower loss, has good temperature stability at high-temperature area; Capacitance ceramic material provided by the invention can satisfied temperature scope be the Working environment needs of-50 ~ 300 ℃.
Accompanying drawing explanation
Fig. 1 is the curve that the dielectric constant with temperature of sample in the embodiment of the present invention 4 changes.
Embodiment
Below will to the present invention, be described in detail by embodiment, the object that these embodiment just illustrate for exemplary, and be not intended to limit the present invention.Following sodium carbonate, salt of wormwood, Niobium Pentxoxide, bismuthous oxide bismuth trioxide, zinc oxide, titanium dioxide, aluminium sesquioxide are analytical pure.The specific surface area of powder is tested with BET specific surface area method of testing.
Embodiment 1:
(1), by the raw material ball milling of sodium carbonate, salt of wormwood, Niobium Pentxoxide, bismuthous oxide bismuth trioxide, zinc oxide, titanium dioxide and aluminium sesquioxide, make the specific surface area of each material powder reach 15m
2/ g.
(2) by step (1) gained material according to 0.99K
0.47na
0.53nbO
3-0.005Bi (Zn
0.5ti
0.5) O
3)-0.005BiAlO
3stoichiometric ratio is prepared burden, and adds the bismuthous oxide bismuth trioxide of total quality of material 0.5%.
(3) step (2) gained material is put into ball grinder and carried out wet ball-milling mixing 4 hours, ball-milling medium is zirconia ball and dehydrated alcohol, added zirconia ball quality is 10 times of batching total mass, and added dehydrated alcohol quality is 2 times of batching total mass; The slurry that ball milling is crossed is pressed into cylinder after drying, and in 900 ℃ of air atmosphere, pre-burning is 2 hours; Cylinder after calcining is ground again to ball milling and within 4 hours, obtains preburning powder, added zirconia ball quality is powder quality 8 times, added dehydrated alcohol quality is powder quality 2 times; Then in preburning powder, add binding agent, granulation, sieves, then compression moulding; Last in the air atmosphere of 1100 ℃ sintering 2 hours, described binding agent adopts the polyvinyl alcohol water solution that mass concentration is 5%, add-on accounts for 4% of preburning powder gross weight.
Embodiment 2:
(1), by the raw material ball milling of sodium carbonate, salt of wormwood, Niobium Pentxoxide, bismuthous oxide bismuth trioxide, zinc oxide, titanium dioxide and aluminium sesquioxide, make the specific surface area of each material powder reach 15m
2/ g.
(2) by step (1) gained material according to 0.98K
0.485na
0.515nbO
3-0.01Bi (Zn
0.5ti
0.5) O
3)-0.01BiAlO
3stoichiometric ratio is prepared burden, and adds the bismuthous oxide bismuth trioxide of total quality of material 1%.
(3) step (2) gained material is put into ball grinder and carried out wet ball-milling mixing 8 hours, ball-milling medium is zirconia ball and dehydrated alcohol, added zirconia ball quality is 9 times of batching total mass, and added dehydrated alcohol quality is 1.6 times of batching total mass; The slurry that ball milling is crossed is pressed into cylinder after drying, and in 880 ℃ of air atmosphere, pre-burning is 4 hours; Cylinder after calcining is ground again to ball milling and within 6 hours, obtains preburning powder, added zirconia ball quality is powder quality 7 times, added dehydrated alcohol quality is powder quality 1.2 times; Then in preburning powder, add binding agent, granulation, sieves, then compression moulding; Last in the air atmosphere of 1050 ℃ sintering 4 hours, described binding agent adopts the polyvinyl alcohol water solution that mass concentration is 5%, add-on accounts for 6% of preburning powder gross weight.
Embodiment 3:
(1), by the raw material ball milling of sodium carbonate, salt of wormwood, Niobium Pentxoxide, bismuthous oxide bismuth trioxide, zinc oxide, titanium dioxide and aluminium sesquioxide, make the specific surface area of each material powder reach 15m
2/ g.
(2) by step (1) gained material 0.94K
0.48na
0.52nbO
3-0.03Bi (Zn
0.5ti
0.5) O
3)-0.03BiAlO
3stoichiometric ratio is prepared burden, and adds the bismuthous oxide bismuth trioxide of total quality of material 1.5%.
(3) step (2) gained material is put into ball grinder and carried out wet ball-milling mixing 12 hours, ball-milling medium is zirconia ball and dehydrated alcohol, added zirconia ball quality is 8 times of batching total mass, and added dehydrated alcohol quality is 1.2 times of batching total mass; The slurry that ball milling is crossed is pressed into cylinder after drying, and in 860 ℃ of air atmosphere, pre-burning is 6 hours; Cylinder after calcining is ground again to ball milling and within 8 hours, obtains preburning powder, added zirconia ball quality is powder quality 6 times, added dehydrated alcohol quality is powder quality 1 times; Then in preburning powder, add binding agent, granulation, sieves, then compression moulding; Last in the air atmosphere of 1000 ℃ sintering 8 hours, described binding agent adopts the polyvinyl alcohol water solution that mass concentration is 5%, add-on accounts for 8% of preburning powder gross weight.
Embodiment 4:
(1), by the raw material ball milling of sodium carbonate, salt of wormwood, Niobium Pentxoxide, bismuthous oxide bismuth trioxide, zinc oxide, titanium dioxide and aluminium sesquioxide, make the specific surface area of each material powder reach 15m
2/ g.
(2) by step (1) gained material according to 0.83K
0.475na
0.525nbO
3-0.1Bi (Zn
0.5ti
0.5) O
3)-0.07BiAlO
3stoichiometric ratio is prepared burden, and adds the bismuthous oxide bismuth trioxide of total quality of material 2.0%.
(3) step (2) gained material is put into ball grinder and carried out wet ball-milling mixing 16 hours, ball-milling medium is zirconia ball and dehydrated alcohol, added zirconia ball quality is 7 times of batching total mass, and added dehydrated alcohol quality is 1 times of batching total mass; The slurry that ball milling is crossed is pressed into cylinder after drying, and in 840 ℃ of air atmosphere, pre-burning is 8 hours; Cylinder after calcining is ground again to ball milling and within 10 hours, obtains preburning powder, added zirconia ball quality is powder quality 5 times, added dehydrated alcohol quality is powder quality 0.9 times; Then in preburning powder, add binding agent, granulation, sieves, then compression moulding; Last in the air atmosphere of 850 ℃ sintering 4 hours, described binding agent adopts the polyvinyl alcohol water solution that mass concentration is 5%, add-on accounts for 10% of preburning powder gross weight.
Embodiment 5:
(1), by the raw material ball milling of sodium carbonate, salt of wormwood, Niobium Pentxoxide, bismuthous oxide bismuth trioxide, zinc oxide, titanium dioxide and aluminium sesquioxide, make the specific surface area of each material powder reach 15m
2/ g.
(2) by step (1) gained material according to 0.80K
0.47na
0.53nbO
3-0.12Bi (Zn
0.5ti
0.5) O
3)-0.08BiAlO
3stoichiometric ratio is prepared burden, and adds the bismuthous oxide bismuth trioxide of total quality of material 3%.
(3) step (2) gained material is put into ball grinder and carried out wet ball-milling mixing 24 hours, ball-milling medium is zirconia ball and dehydrated alcohol, added zirconia ball quality is 5 times of batching total mass, and added dehydrated alcohol quality is 0.8 times of batching total mass; The slurry that ball milling is crossed is pressed into cylinder after drying, and in 800 ℃ of air atmosphere, pre-burning is 6 hours; Cylinder after calcining is ground again to ball milling and within 12 hours, obtains preburning powder, added zirconia ball quality is powder quality 4 times, added dehydrated alcohol quality is powder quality 0.8 times; Then in preburning powder, add binding agent, granulation, sieves, then compression moulding; Last in the air atmosphere of 900 ℃ sintering 2 hours, described binding agent adopts the polyvinyl alcohol water solution that mass concentration is 5%, add-on accounts for 5% of preburning powder gross weight.
The dielectric properties of specific embodiment, the dielectric properties evaluation while carrying out 100kHz with electric impedance analyzer.
Pyroceramic capacitance ceramic prepared by the present invention has following characteristics: under 100kHz, there is higher specific inductivity, and lower dielectric loss, electric capacity varies with temperature little, and temperature range is wide, and preparation technology is simple.Utilize capacitance ceramic material provided by the invention can make the use temperature of ceramic condenser bring up to 300 ℃, so the present invention have great value in high-temperature ceramic capacitor field.
The sample of preparing in above 5 embodiment is under 100kHz, and when 25 ℃ and 300 ℃, specific inductivity and loss are as shown in the table:
Claims (2)
1. potassium-sodium niobate-titanium zincic acid bismuth-Bismuth Aluminate three component system lead-free high-temperature capacitance ceramic dielectric material, is characterised in that it forms general formula and is: (1-y-z) K
1-xna
xnbO
3-yBi (Zn
0.5ti
0.5) O
3-zBiAlO
3, wherein: 0.5≤x≤0.53,0.005≤y≤0.12,0.005≤z≤0.08; X, y, z is molar weight.
2. the preparation method of three component system lead-free high-temperature capacitor dielectric material according to claim 1, is characterized in that concrete preparation method is:
(1), by raw material sodium carbonate, salt of wormwood, Niobium Pentxoxide, bismuthous oxide bismuth trioxide, zinc oxide, titanium dioxide and aluminium sesquioxide ball milling, guarantee that the specific surface area of each initial feed powder reaches 15m
2/ g;
(2) step (1) gained material is pressed to (1-y-z) K
1-xna
xnbO
3-yBi (Zn
0.5ti
0.5) O
3-zBiAlO
3stoichiometric ratio batching, wherein: 0.5≤x≤0.53,0.005≤y≤0.12,0.005≤z≤0.08; X, y, z is molar weight; And add the bismuthous oxide bismuth trioxide of total quality of material 0.5 ~ 3%;
(3) step (2) gained material is put into ball grinder and carried out wet ball-milling mixing 4 ~ 24 hours, ball-milling medium is zirconia ball and dehydrated alcohol, added zirconia ball quality is 5 ~ 10 times of batching total mass, and added dehydrated alcohol quality is 0.8 ~ 2 times of batching total mass; The slurry that ball milling is crossed is pressed into cylinder after drying, and in 800 ~ 900 ℃ of air atmosphere, pre-burning is 2 ~ 8 hours; Cylinder after pre-burning is ground again to ball milling and within 4 ~ 12 hours, obtains preburning powder, added zirconia ball quality is powder quality 4 ~ 8 times, added dehydrated alcohol quality is powder quality 0.8 ~ 1.5 times; Then in preburning powder, add binding agent, granulation, sieves, then compression moulding; Last sintering 2 ~ 8 hours in the air atmosphere of 900 ~ 1100 ℃, described binding agent adopts the polyvinyl alcohol water solution that mass concentration is 5%, and add-on accounts for 4% ~ 10% of preburning powder gross weight;
Described sodium carbonate, salt of wormwood, Niobium Pentxoxide, bismuthous oxide bismuth trioxide, zinc oxide, titanium dioxide, aluminium sesquioxide are analytical pure.
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| CN102070337B (en) * | 2010-10-29 | 2012-12-05 | 景德镇陶瓷学院 | Low-temperature sintered potassium sodium niobate lead-free piezoelectric ceramic and preparation method thereof |
| CN102531597A (en) * | 2011-12-16 | 2012-07-04 | 桂林理工大学 | Potassium sodium niobate-strontium manganate ceramic and preparation method |
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| EP1422209A2 (en) * | 2002-11-22 | 2004-05-26 | Paratek Microwave, Inc. | Method for producing low-loss tunable ceramic composites with improved breakdown strengths |
| US20050263807A1 (en) * | 2004-04-13 | 2005-12-01 | Tai-Bor Wu | Semiconductor device and method for forming a ferroelectric capacitor of the semiconductor device |
| CN101798227A (en) * | 2010-03-24 | 2010-08-11 | 桂林理工大学 | Solid phase synthetic method of niobate-titanate nano-powder |
| CN101823876A (en) * | 2010-04-20 | 2010-09-08 | 武汉理工大学 | Ceramic material for temperature stabilization type multilayer ceramic capacitor and preparation method thereof |
| CN102199035A (en) * | 2011-03-22 | 2011-09-28 | 清华大学 | X9r ceramic capacitor dielectric material and preparation method thereof |
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