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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- CN102992763B CN102992763B CN201310000183.2A CN201310000183A CN102992763B CN 102992763 B CN102992763 B CN 102992763B CN 201310000183 A CN201310000183 A CN 201310000183A CN 102992763 B CN102992763 B CN 102992763B
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Abstract
The invention discloses a potassium sodium niobate-titanium zinc bismuth-bismuth aluminate ternary lead-free high-temperature capacitor dielectric material and a preparation method thereof. A capacitance porcelain system is prepared by a matrix with a general formula of (1-y-z) K1-xNaxNbO3-yBi (Zn0.5Ti0.5)O3-zBiAlO3 and bismuth trioxide occupying 0.5-3% by weight of the matrix, wherein 0.5<=x<=0.53, 0.005<=y<=0.12, and 0.005<=z<=0.08. The preparation method includes: refining raw material powder, ball-milling, mixing, pre-burning, pelletizing, sieving, blank making, sintering, getting electric shock and the like. The lead-free niobium acid base ternary high-temperature capacitor dielectric material is small in used raw material varieties and simple in preparation process, and has the remarkable advantages of being free of harmful substances of lead, cadmium and the like and environment-friendly and having a high dielectric constant, low loss and good stability at a high-temperature area. A capacitance porcelain material can meet requirements of working environment with temperature ranging from -50 DEC G to 30 DEG C.
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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| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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