CN102992763A - 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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- CN102992763A CN102992763A CN2013100001832A CN201310000183A CN102992763A CN 102992763 A CN102992763 A CN 102992763A CN 2013100001832 A CN2013100001832 A CN 2013100001832A CN 201310000183 A CN201310000183 A CN 201310000183A CN 102992763 A CN102992763 A CN 102992763A
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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), has accounted for leading in electrical condenser market.Simultaneously, 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 the present laminated ceramic capacitor product and since 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. require the working temperature upper limit of its electric capacity to bring up to 150 ℃ because working conditions is special.X7R type MLCC obviously can not meet the demands, and for exploitation and the application that adapts to the 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 field that a few thing condition is relatively harsher such as enngine control system, aerospace detection, drilling well etc., its high temperature resistant electronics requires the upper temperature limit of its ceramic condenser to be increased to 200 ℃.Therefore, demand developing the pyroceramic capacitor dielectric material with good temperature stability urgently.The MLCC of at present China's production mainly is divided into two kinds, BaTiO
3Base and Pb base.As everyone knows, BaTiO
3The firing temperature of base MLCC must be with precious metal palladium or platinum as interior electrode, to realize and BaTiO usually more than 1300 ℃
3The common burning of base ceramic dielectric material.If the reduction sintering temperature on the one hand can energy efficient, be expected on the other hand realize and palladium that the common burning of silver or its alloy reduces production costs.So the ceramic capacitor dielectric material of exploitation low temperature sintering has important practical significance.In addition, contain a large amount of lead in the dielectric material of Pb base MLCC, the objectionable impuritiess such as cadmium, these MLCC dielectric materials that 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 in wide temperature range, has, 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 fit to mass production.
The chemical constitution general formula of potassium-sodium niobate involved in the present invention-titanium zincic acid bismuth-Bismuth Aluminate three component system lead-free high-temperature capacitor dielectric material 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 are molar weight.In order to compensate the volatilization of A bit element under the high temperature, when batching, add the bismuthous oxide bismuth trioxide of total quality of material 0.5 ~ 3%.
Above-mentioned potassium-sodium niobate-titanium zincic acid bismuth-Bismuth Aluminate three component system lead-free high-temperature capacitor dielectric material preparation step is:
(1) with the raw material ball milling of yellow soda ash, salt of wormwood, Niobium Pentxoxide, bismuthous oxide bismuth trioxide, zinc oxide, titanium dioxide and aluminium sesquioxide, guarantees that the specific surface area of each initial feed powder is not less than 15m
2/ g.
(2) step (1) gained material is pressed (1-y-z) K
1-xNa
xNbO
3-yBi (Zn
0.5Ti
0.5) O
3-zBiAlO
3The stoichiometric ratio batching, wherein: 0.5≤x≤0.53,0.005≤y≤0.12,0.005≤z≤0.08; X, y, z are molar weight; And the bismuthous oxide bismuth trioxide of adding batching total mass 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 the batching quality, and added dehydrated alcohol quality is 0.8 ~ 2 times of the batching total mass; Be pressed into cylinder after the slurry oven dry that ball milling is crossed, pre-burning is 2 ~ 8 hours in 800 ~ 900 ℃ of air atmosphere; Cylinder after the pre-burning was ground again ball milling 4 ~ 12 hours, and added zirconia ball quality is 4 ~ 8 times of institute's abrasive dust material quality, and added dehydrated alcohol quality is 0.8 ~ 1.5 times of institute's abrasive dust material quality; Then add binding agent in preburning powder, granulation is sieved, again compression moulding; It is 5% polyvinyl alcohol water solution that last sintering 2 ~ 8 hours in 900 ~ 1100 ℃ air atmosphere, described binding agent adopt mass concentration, and add-on accounts for 4% ~ 10% of preburning powder gross weight.
Above-mentioned yellow soda ash, 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, used raw material type 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; But capacitance ceramic material satisfied temperature scope provided by the invention is-50 ~ 300 ℃ Working environment needs.
Description of drawings
Fig. 1 is the curve that the dielectric constant with temperature of sample in the embodiment of the invention 4 changes.
Embodiment
Below will be described in detail the present invention by embodiment, the purpose that these embodiment just illustrate for exemplary, and be not for limiting the present invention.Following yellow soda ash, 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) with the raw material ball milling of yellow soda ash, 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) with 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 the batching total mass, and added dehydrated alcohol quality is 2 times of the batching total mass; Be pressed into cylinder after the slurry oven dry that ball milling is crossed, pre-burning is 2 hours in 900 ℃ of air atmosphere; Cylinder after the calcining was ground again ball milling 4 hours, and added zirconia ball quality is 8 times of powder quality, and added dehydrated alcohol quality is 2 times of powder quality; Then add binding agent in preburning powder, granulation is sieved, again compression moulding; Last in 1100 ℃ air atmosphere sintering 2 hours, it is 5% polyvinyl alcohol water solution that described binding agent adopts mass concentration, add-on accounts for 4% of preburning powder gross weight.
Embodiment 2:
(1) with the raw material ball milling of yellow soda ash, 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) with 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 the batching total mass, and added dehydrated alcohol quality is 1.6 times of the batching total mass; Be pressed into cylinder after the slurry oven dry that ball milling is crossed, pre-burning is 4 hours in 880 ℃ of air atmosphere; Cylinder after the calcining was ground again ball milling 6 hours, and added zirconia ball quality is 7 times of powder quality, and added dehydrated alcohol quality is 1.2 times of powder quality; Then add binding agent in preburning powder, granulation is sieved, again compression moulding; Last in 1050 ℃ air atmosphere sintering 4 hours, it is 5% polyvinyl alcohol water solution that described binding agent adopts mass concentration, add-on accounts for 6% of preburning powder gross weight.
Embodiment 3:
(1) with the raw material ball milling of yellow soda ash, 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) with 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 the batching total mass, and added dehydrated alcohol quality is 1.2 times of the batching total mass; Be pressed into cylinder after the slurry oven dry that ball milling is crossed, pre-burning is 6 hours in 860 ℃ of air atmosphere; Cylinder after the calcining was ground again ball milling 8 hours, and added zirconia ball quality is 6 times of powder quality, and added dehydrated alcohol quality is 1 times of powder quality; Then add binding agent in preburning powder, granulation is sieved, again compression moulding; Last in 1000 ℃ air atmosphere sintering 8 hours, it is 5% polyvinyl alcohol water solution that described binding agent adopts mass concentration, add-on accounts for 8% of preburning powder gross weight.
Embodiment 4:
(1) with the raw material ball milling of yellow soda ash, 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) with 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 the batching total mass, and added dehydrated alcohol quality is 1 times of the batching total mass; Be pressed into cylinder after the slurry oven dry that ball milling is crossed, pre-burning is 8 hours in 840 ℃ of air atmosphere; Cylinder after the calcining was ground again ball milling 10 hours, and added zirconia ball quality is 5 times of powder quality, and added dehydrated alcohol quality is 0.9 times of powder quality; Then add binding agent in preburning powder, granulation is sieved, again compression moulding; Last in 850 ℃ air atmosphere sintering 4 hours, it is 5% polyvinyl alcohol water solution that described binding agent adopts mass concentration, add-on accounts for 10% of preburning powder gross weight.
Embodiment 5:
(1) with the raw material ball milling of yellow soda ash, 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) with 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 the batching total mass, and added dehydrated alcohol quality is 0.8 times of the batching total mass; Be pressed into cylinder after the slurry oven dry that ball milling is crossed, pre-burning is 6 hours in 800 ℃ of air atmosphere; Cylinder after the calcining was ground again ball milling 12 hours, and added zirconia ball quality is 4 times of powder quality, and added dehydrated alcohol quality is 0.8 times of powder quality; Then add binding agent in preburning powder, granulation is sieved, again compression moulding; Last in 900 ℃ air atmosphere sintering 2 hours, it is 5% polyvinyl alcohol water solution that described binding agent adopts mass concentration, add-on accounts for 5% of preburning powder gross weight.
The dielectric properties of specific embodiment, the dielectric properties evaluation when carrying out 100kHz with electric impedance analyzer.
The pyroceramic capacitance ceramic of the present invention's preparation has following characteristics: under 100kHz, have 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 the high-temperature ceramic capacitor field.
More than the sample for preparing among 5 embodiment under 100kHz, specific inductivity and loss are as shown in the table when 25 ℃ and 300 ℃:
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 are molar weight.
2. three component system lead-free high-temperature capacitor dielectric material preparation method according to claim 1 is characterized in that concrete preparation method is:
(1) with raw material yellow soda ash, salt of wormwood, Niobium Pentxoxide, bismuthous oxide bismuth trioxide, zinc oxide, titanium dioxide and aluminium sesquioxide ball milling, guarantees that the specific surface area of each initial feed powder reaches 15m
2/ g;
(2) step (1) gained material is pressed (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 are 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 the batching total mass, and added dehydrated alcohol quality is 0.8 ~ 2 times of the batching total mass; Be pressed into cylinder after the slurry oven dry that ball milling is crossed, pre-burning is 2 ~ 8 hours in 800 ~ 900 ℃ of air atmosphere; Cylinder after the pre-burning was ground again ball milling 4 ~ 12 hours, and added zirconia ball quality is 4 ~ 8 times of powder quality, and added dehydrated alcohol quality is 0.8 ~ 1.5 times of powder quality; Then add binding agent in preburning powder, granulation is sieved, again compression moulding; It is 5% polyvinyl alcohol water solution that last sintering 2 ~ 8 hours in 900 ~ 1100 ℃ air atmosphere, described binding agent adopt mass concentration, and add-on accounts for 4% ~ 10% of preburning powder gross weight;
Described yellow soda ash, 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 |
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| 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 |
| CN102070337A (en) * | 2010-10-29 | 2011-05-25 | 景德镇陶瓷学院 | Low-temperature sintered potassium sodium niobate lead-free piezoelectric ceramic 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 |
| CN102531597A (en) * | 2011-12-16 | 2012-07-04 | 桂林理工大学 | Potassium sodium niobate-strontium manganate ceramic and preparation method |
-
2013
- 2013-01-02 CN CN201310000183.2A patent/CN102992763B/en active Active
Patent Citations (7)
| 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 |
| CN102070337A (en) * | 2010-10-29 | 2011-05-25 | 景德镇陶瓷学院 | Low-temperature sintered potassium sodium niobate lead-free piezoelectric ceramic and preparation method thereof |
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| 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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