CN1850719A - Strontium titanate pressure-sensitive resistor medium and preparing method - Google Patents
Strontium titanate pressure-sensitive resistor medium and preparing method Download PDFInfo
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- CN1850719A CN1850719A CN 200610042810 CN200610042810A CN1850719A CN 1850719 A CN1850719 A CN 1850719A CN 200610042810 CN200610042810 CN 200610042810 CN 200610042810 A CN200610042810 A CN 200610042810A CN 1850719 A CN1850719 A CN 1850719A
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Abstract
This invention discloses strontium titanate piezo resistor medium and its preparation method. It is consisted by following parts, the first part is main material SrxTiyO3, the second part is giver additive, the third part is acceptor additive, the fourth is sintering auxiliary agent. Their mol ratio is 100:0.1-1.0: 0.1-1.0:0.5-1.0. Main material SrxTiyO3 is synthesized by SrCO3 and Ti02, x/y is 0.8-2.0. Giver additive is at least one of W03, rare earth oxide Nb2O5, La2O3, Ta2O5, CeO2, Nd2O3, Y2O3, Sm2O3, Pr6O11, and Dy2O3. Acceptor additive is Na20. Sintering auxiliary agent is SiO2 and Al2O3. Good electrical specification piezo resistor medium can be got through main materials synthesis, giver and acceptor additive adding, spray and graining, compression molding, batch dropping, liquid ammonia decomposition reduction burning and heat treatment. This invention can be used to make annular and round piece shape piezo resistor, it is widely used in spark noise-eliminating and pulse protection in direct current micro motor fields.
Description
Technical field
The present invention relates to pressure-sensitive resistor medium and preparation method thereof, particularly a kind of strontium titanate pressure-sensitive resistor medium and preparation method thereof.
Background technology
The strontium titanate voltage-sensitive ceramic has pressure-sensitive character and big electrical capacity simultaneously owing to it, and has bigger nonlinear factor and anti-preferably surge capacity, nonpolarity, therefore obtains using very widely in suppressing the wider frequency range noise.Can effectively absorb the sparking voltage that commutator produces in the micromotor by its strontium titanate annular voltage-sensitive resistor for preparing, and then electronicss such as stereo set, vision facilities are played effective protective effect.Traditional strontium titanate pressure-sensitive ceramic dielectric is by the synthetic major ingredient SrTiO of pre-burning
3And isomer, introduce Ba, Ca ion as position at Sr, mix micro-alms giver's additive then or be subjected to the master additive agent modified, alms giver's additive generally comprises rare earth oxide Nb
2O
5, Ta
2O
5, La
2O
3, CeO
2, Nd
2O
3, Y
2O
3, Sm
2O
3, Pr
6O
11, Dy
2O
3A kind of or several; Be subjected to main additive that Na is generally arranged
2O, CuO, MnCO
3Deng, obtain the strontium titanate pressure-sensitive ceramic dielectric through high-temperature heat treatment in reducing atmosphere sintering and the air.Major ingredient SrTiO wherein
3Synthetic method mainly contain following several:
1) adopts pure SrTiO
3As major ingredient, in the European patent EP 70540 and EP0101824 as the application of company of TAIYO YUDAN, as the SrTiO of main ingredient
3Adopt following method to obtain: to be 99.8% SrCO with purity
3And TiO
2With 1: 1 mixed, ball milling 10 hours, dry, pulverize, 1200 ℃ of sintering 2 hours, it was standby to be ground into powder again.
2) adopt Sr
(1-x)Ca
xTiO
3As major ingredient, open the method for mentioning among the clear 59-218702 as the Japanese Patent spy: be 99.0% SrCO with purity
3, CaCO
3And TiO
2Respectively weighing, mixing and ball milling 10 hours, dry, pulverize, 1200 ℃ of sintering 2 hours, it was standby to be ground into powder again.
3) adopt Sr
(1-x-y)Ba
xCa
yTiO
3As major ingredient, the method for mentioning among the patent CN1 353097 as the application of Japanese TDK company: as raw material, carry out weighing with the compound of Ba and Ca, Sr respectively, synthetic after the mixing and ball milling at 1080～1250 ℃ of sintering that carry out 2～4 hours.
Above-mentioned major ingredient SrTiO
3Synthetic method, difference is the SrTiO that obtains
3Structure body difference, these strontium titanate major ingredients all adopt 95%N when being used to prepare voltage-sensitive ceramic
2+ 5%H
2Weakly reducing atmosphere carry out sintering, sintering temperature is usually above 1400 ℃.Because sintering atmosphere need adopt the mixing of two kinds of gases, so blending ratio is wayward; Adulterated in addition binder component and addition are also relatively poor to ceramic dielectic voltage-dependent characteristic controllability.
Summary of the invention
The purpose of this invention is to provide a kind of even microstructure that has, the strontium titanate pressure-sensitive resistor medium good to the unit for electrical property parameters controllability; Another object of the present invention is to improve existing strontium titanate pressure-sensitive ceramic dielectric mixing reducing atmosphere agglomerating defective, and the pressure-sensitive resistor medium that a kind of sintering process is easy, the sintering cost is low preparation method is provided.
For reaching above purpose, the present invention takes following technical scheme to be achieved:
A kind of strontium titanate pressure-sensitive resistor medium is made of following component: first component is major ingredient Sr
xTi
yO
3, second component is alms giver's additive, and the 3rd component is for being subjected to main additive, and the 4th component is a sintering aid; The mol ratio of described four kinds of components is 100: 0.1～1.0: 0.1～1.0: 0.5～1.0 in order, described major ingredient Sr
xTi
yO
3By SrCO
3With TiO
2Synthetic, wherein x/y is 0.8～2.0; Described sintering aid is SiO
2And Al
2O
3
Above-mentioned strontium titanate pressure-sensitive resistor medium, major ingredient Sr
xTi
yO
3The ratio of x/y be preferably 1.01～1.05.Described alms giver's additive, be subjected to the median size of main additive and sintering aid less than 20um.Alms giver's additive can be WO
3, rare earth oxide Nb
2O
5, La
2O
3, Ta
2O
5, CeO
2, Nd
2O
3, Y
2O
3, Sm
2O
3, Pr
6O
11, Dy
2O
3At least a, be preferably Nb
2O
5Be subjected to the main Na that is added to
2O.
A kind of preparation method of strontium titanate pressure-sensitive resistor medium is characterized in that, comprises the steps:
A. at first synthetic major ingredient is with the SrCO of x mole
3With y mole TiO
2Weighing mixes, and wherein the ratio of x and y is 0.8～2.0, is preferably 1.01～1.05.Above-mentioned compound added behind the dispersion agent grind more than 10 hours, sieve after drying, obtain mixed powder;
B. mixed powder is put into saggar and made between the powder contact closely, saggar is put into sintering oven be heated to 1100 ℃ with 600 ℃/hour heat-up rate, be incubated 2～5 hours, cooling promptly makes the major ingredient of strontium titanate voltage-sensitive ceramic afterwards after sieve.
C. with 100 moles of above-mentioned major ingredients, with alms giver's additive of 0.5～1.0 mole, 0.2～0.8 mole the sintering aid SiO that is subjected to main additive and 0.5～1.0 mole
2And Al
2O
3Mix, add dispersion agent, tackiness agent, in ball grinder, grind more than 10 hours, carry out mist projection granulating afterwards, obtain the marumerizer material;
D. the granulation material is packed in the mould, adopt pressure molding to obtain molding, above-mentioned molding is warming up to 1000 ℃ of binder removals obtained base substrate in 2 hours, base substrate is put into atmosphere furnace, heat-up rate with 600 ℃/hour in nitrogen that is decomposed generation by liquefied ammonia and hydrogen mixed gas atmosphere is heated to 1350～1400 ℃, is incubated and obtains sintered compact after 2～5 hours.
E. with 800～1000 ℃ of thermal treatment 3 hours in air of above-mentioned sintered compact, promptly obtain strontium titanate pressure-sensitive resistor medium.
In the aforesaid method, SrCO among the step a
3With TiO
2Preferred molar ratio value x/y be 1.01～1.05; SrCO
3And TiO
2Quality purity be not less than 99%.Alms giver's additive among the step c, be subjected to the median size of main additive and sintering aid less than 20um.Alms giver's additive adopts WO
3, rare earth oxide Nb
2O
5, La
2O
3, Ta
2O
5, CeO
2, Nd
2O
3, Y
2O
3, Sm
2O
3, Pr
6O
11, Dy
2O
3At least a, be preferably Nb
2O
5Be subjected to main additive to adopt Na
2O.The nitrogen that is obtained by the liquefied ammonia decomposition in the steps d and the volume ratio of hydrogen are 3: 1.
The formula adjustment of traditional strontium titanate voltage-sensitive ceramic is to introduce Ba, Ca ion by the position of Sr in major ingredient, perhaps by adjusting other micro-alms givers or being subjected to main additive to improve performance.The strontium titanate pressure-sensitive resistor medium of the present invention's preparation, its major ingredient is to utilize the variation of different Sr/Ti ratios to come the processing parameter and the performance perameter of product are regulated and control.Its advantage is: the cost of material of (1) preparation major ingredient is cheap, does not introduce other elements; (2) need not only regulate the Sr/Ti ratio of major ingredient by adjusting the content of trace mineral supplement, just can in very large range regulate and control the unit for electrical property parameters of piezoresistor; (3) suitable Sr/Ti is than the sintering temperature of voltage-sensitive ceramic being spent from being reduced to 1350 more than 1400 degree.Adopt liquefied ammonia to decompose the mixed gas sintering process in addition, can produce strongly reducing atmosphere, promote ceramic dielectic densification process, reduce sintering energy consumption.Therefore; the present invention compared with prior art; have the superior economy and the reliability of product performance; the strontium titanate annular voltage-sensitive resistor of manufacturing and disc piezoresistor, but widespread use and the protecting component that the spark in direct current micromotor and other Low-voltage Electronic devices and noise are absorbed.
Description of drawings
Fig. 1 for Sr/Ti than the SEM photo that is 0.98 o'clock strontium titanate voltage-sensitive ceramic sample.
Fig. 2 for Sr/Ti than the SEM photo that is 1.01 o'clock strontium titanate voltage-sensitive ceramic sample.
Fig. 3 for Sr/Ti than the SEM photo that is 1.05 o'clock strontium titanate voltage-sensitive ceramic sample.
Embodiment
The present invention is described in further detail below in conjunction with specific embodiment;
A kind of strontium titanate pressure-sensitive resistor medium is made of following component: first component is by SrCO
3With TiO
2Synthetic major ingredient Sr
xTi
yO
3Second component is alms giver's additive, and the 3rd component is for being subjected to main additive Na
2O; The 4th component is sintering aid SiO
2, Al
2O
3The mole of described four kinds of components (mol) is 100: 0.1～1.0: 0.1～1.0: 0.5～1.0 than in order; Described major ingredient Sr
xTi
yO
3X/y be 0.8～2.0; Described alms giver's additive, be subjected to main additive and sintering aid median size less than 20um (um represents micron); Alms giver's additive can be WO
3, rare earth oxide Nb
2O
5, La
2O
3, Ta
2O
5, CeO
2, Nd
2O
3, Y
2O
3, Sm
2O
3, Pr
6O
11, Dy
2O
3In at least a; Concrete composition is as shown in table 1.
A kind of preparation method of strontium titanate pressure-sensitive resistor medium comprises the steps:
A. at first synthetic major ingredient is according to the mol ratio, with the SrCO of x part
3TiO with y part
2Weighing mixes, and wherein the ratio of x and y is 0.8～2.0, and concrete ratio sees Table 1.SrCO wherein
3And TiO
2Purity be 99%, SrCO
3Median size be 0.5-20um, TiO
2Median size less than 10um.Above-mentioned different SrCO
3/ TiO
2The compound of ratio grinds respectively more than 10 hours after adding dispersion agent, after drying, sieves with 120 order sub-sieves, obtains the mixed powder of 12 examples.
B. above-mentioned mixed powder is put into different saggars respectively, apply certain pressure and make its surfacing, contact closely between the powder.Saggar is put into sintering oven, in air with 600 the degree/hour heat-up rate be heated to 1100 ℃, the saggar insulation of the saggar insulation 2 hours of example 1～2, the saggar insulation 3 hours of example 3～9, example 10～12 5 hours, separated pulverizing becomes powder more after cooling, cross 120 mesh sieves, obtain 12 different SrCO
3/ TiO
2The major ingredient of ratio is standby.
C. with the major ingredient of above-mentioned 100mol, with the sintering aid that is subjected to main additive and 0.5～1.0mol of alms giver's additive of 0.5～1.0mol, 0.2～0.8mol by the composition of table 1 respectively weighing mix, the adhesive polyethylene alcohol that adds dispersion agent, pure water and 2% weight, put into different ball grinders and numbering respectively, each jar (is no more than 20 hours) at ball milling on the agitator mill more than 10 hours, send into the mist projection granulating tower afterwards respectively and carry out granulation, obtaining particle is 12 granulation material of forming example of spheric.
In the embodiment shown in the table 1 1～12, each additive adopts chemically pure reagent, alms giver's additive, be subjected to the median size of main additive and sintering aid less than 20um, wherein the average particulate diameter of silicon-dioxide generally is controlled at 0.1-20um, if during less than 0.1um, powder condenses easily, and operation is difficulty relatively; Then can cause the pore part in the voltage-sensitive ceramic to become excessive during greater than 20um.Therefore the average particulate diameter of silicon-dioxide preferably is controlled between the 0.5-20um.
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D. the granulation material of each being formed example is packed in the mould, with 1500kg/cm
2Pressure forming, make diameter 15mm, thickness is that 12 of 1mm forms bodies, every composition body is 3.Above-mentioned molding was handled 2 hours at 1000 ℃, and the venting tackiness agent obtains having 36 of 12 groups of different strontium titanate voltage-sensitive ceramic base substrates of forming of certain physical strength.Each assembly body is put into atmosphere furnace, decomposing the N that obtains by liquefied ammonia
2: H
2In the strong reducing property mixed gas of=3: 1 (volume ratio), with 600 degree/hour heat-up rate be heated to 1350～1400 ℃, be incubated and obtains sintered compact after 2～5 hours, specifically the sintering parameter sees Table 1.
E. above-mentioned sintered compact 600 is spent to 1000 and heat-treated 3 hours in air, obtain 12 groups of strontium titanate pressure-sensitive resistor medium samples.
The sample of method for preparing, the about 10mm of diameter, thickness is about 0.8mm.Use commercially available silver electrode paste at the electrode coated layer of two end faces of these ceramics at last, after 800 ℃ of burning infiltrations, measure electric property, as shown in table 2.20 ℃ of room temperatures, the 1mA electric current is measured pressure sensitive voltage E down
1, the 10mA electric current is measured pressure sensitive voltage E down
10And by formula:
α=1/log (E
10/ E
1) calculating the nonlinear factor of voltage: electrical capacity C is the observed value under the 1kHz condition.The free content of strontium of synthetic major ingredient is measured with the EDTA method.
The different performance perameters of forming example of table 2 strontium titanate pressure-sensitive resistor medium of the present invention
| The Sr/Ti ratio | Free content of strontium in the major ingredient. | E 10(V) | α | C(nF) | |
| Example 1 | 0.80 | 0.12％ | 11.30 | 2.5 | 53.2 |
| Example 2 | 0.90 | 0.11％ | 9.41 | 3.6 | 47.5 |
| Example 3 | 0.95 | 0.14％ | 7.10 | 6.1 | 40.2 |
| Example 4 | 0.98 | 0.16％ | 6.84 | 5.7 | 41.9 |
| Example 5 | 1.00 | 0.24％ | 6.12 | 5.8 | 45.4 |
| Example 6 | 1.01 | 0.26％ | 5.96 | 5.6 | 48.1 |
| Example 7 | 1.02 | 0.3％ | 5.52 | 5.2 | 52.0 |
| Example 8 | 1.03 | 1.2％ | 5.21 | 5.0 | 54.8 |
| Example 9 | 1.05 | 1.5％ | 4.50 | 4.8 | 63.6 |
| Example 10 | 1.10 | 1.8％ | 5.12 | 3.8 | 53.2 |
| Example 11 | 1.50 | 2.1％ | 5.82 | 3.4 | 48.3 |
| Example 12 | 2.00 | 2.5％ | 7.25 | 2.8 | 41.6 |
Can find out from table 1 and table 2 example 3～9, suitably adjust the Sr/Ti value (0.95～1.05) of major ingredient, add under the constant condition of component concentration in preparation technology and other, not only can effectively reduce sintering temperature, can also stablize the unit for electrical property parameters of adjusting sample within the specific limits, adapt to the requirement of variant production.Fig. 1, Fig. 2 and shown in Figure 3 be respectively Sr/Ti than being 0.98,1.01 and the electron scanning micrograph of 1.05 o'clock samples, that bigger Sr/Ti ratio helps obtaining is fine and close, microstructure uniformly, Sr/Ti increases, crystal grain is grown.As can be seen, in 1.01～1.05 scope, with the increase of Sr/Ti ratio, near sintering temperature can be reduced to 1350 degree from 1400 degree, this was significant for cutting down the consumption of energy as the Sr/Ti of example 6～9.
Claims (9)
1. a strontium titanate pressure-sensitive resistor medium is characterized in that, is made of following component: first component is major ingredient Sr
xTi
yO
3, second component is alms giver's additive, and the 3rd component is for being subjected to main additive, and the 4th component is a sintering aid; The mol ratio of described four kinds of components is 100: 0.1～1.0: 0.1～1.0: 0.5～1.0 in order; Described major ingredient Sr
xTi
yO
3By SrCO
3With TiO
2Synthetic, wherein x/y is 0.8～2.0; Described alms giver's additive is WO
3, rare earth oxide Nb
2O
5, La
2O
3, Ta
2O
5, CeO
2, Nd
2O
3, Y
2O
3, Sm
2O
3, Pr
6O
11, Dy
2O
3At least a; It is described that to be subjected to main additive be Na
2O; Described sintering aid is SiO
2And Al
2O
3
2. strontium titanate pressure-sensitive resistor medium according to claim 1 is characterized in that, described major ingredient Sr
xTi
yO
3The ratio of x/y be 1.01～1.05.
3. strontium titanate pressure-sensitive resistor medium according to claim 1 is characterized in that, described alms giver's additive, is subjected to the median size of main additive and sintering aid less than 20um.
4. according to the strontium titanate pressure-sensitive resistor medium of one of claim 1～3, it is characterized in that described alms giver's additive is Nb
2O
5
5. the preparation method of a strontium titanate pressure-sensitive resistor medium is characterized in that, comprises the steps:
A. at first synthetic major ingredient is with the SrCO of x mole
3With y mole TiO
2Weighing mixes, and wherein the ratio of x and y is 0.8～2.0, and above-mentioned compound grinds more than 10 hours after adding dispersion agent, sieves after drying, obtains mixed powder;
B. mixed powder is put into saggar and compressed, saggar is put into sintering oven be heated to 1100 ℃ with 600 ℃/hour heat-up rate, be incubated 2～5 hours, crushing screening again after the cooling promptly makes the major ingredient of strontium titanate voltage-sensitive ceramic;
C. with 100 moles of above-mentioned major ingredients, with alms giver's additive of 0.5～1.0 mole, 0.2～0.8 mole be subjected to main additive Na
2The sintering aid SiO of O and 0.5～1.0 mole
2And Al
2O
3Weighing mixes, and adds dispersion agent, tackiness agent, grinds more than 10 hours in ball grinder, carries out mist projection granulating afterwards, obtains the marumerizer material; Described alms giver's additive adopts WO
3, rare earth oxide Nb
2O
5, La
2O
3, Ta
2O
5, CeO
2, Nd
2O
3, Y
2O
3, Sm
2O
3, Pr
6O
11, Dy
2O
3At least a;
D. the granulation material is packed in the mould, adopt pressure molding to obtain molding, above-mentioned molding is warming up to 1000 ℃ of binder removals obtained base substrate in 2 hours, base substrate is put into atmosphere furnace, heat-up rate with 600 ℃/hour in nitrogen that is decomposed generation by liquefied ammonia and hydrogen mixed gas atmosphere is heated to 1350～1400 ℃, is incubated and obtains sintered compact after 2～5 hours;
E promptly obtains strontium titanate pressure-sensitive resistor medium with 800～1000 ℃ of thermal treatment 3 hours in air of above-mentioned sintered compact.
6. the preparation method of strontium titanate pressure-sensitive resistor medium according to claim 5 is characterized in that, SrCO among the described step a
3With TiO
2Molar ratio x/y be 1.01～1.05; SrCO
3And TiO
2Quality purity be not less than 99%.
7. the preparation method of strontium titanate pressure-sensitive resistor medium according to claim 5 is characterized in that, the alms giver's additive among the described step c, is subjected to the median size of main additive and sintering aid less than 20um.
8. according to the preparation method of the strontium titanate pressure-sensitive resistor medium of one of claim 5～7, it is characterized in that the alms giver's additive among the described step c adopts Nb
2O
5
9. the preparation method of strontium titanate pressure-sensitive resistor medium according to claim 5 is characterized in that, the nitrogen that is obtained by the liquefied ammonia decomposition in the described steps d and the volume ratio of hydrogen are 3: 1.
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|---|---|---|---|
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