CN103058652A - Preparation method of calcium-borate-glass-modified strontium titanate-lanthanum aluminate composite ceramic - Google Patents

Preparation method of calcium-borate-glass-modified strontium titanate-lanthanum aluminate composite ceramic Download PDF

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CN103058652A
CN103058652A CN2013100039098A CN201310003909A CN103058652A CN 103058652 A CN103058652 A CN 103058652A CN 2013100039098 A CN2013100039098 A CN 2013100039098A CN 201310003909 A CN201310003909 A CN 201310003909A CN 103058652 A CN103058652 A CN 103058652A
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sintering
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strontium titanate
lanthanum aluminate
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CN103058652B (en
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樊慧庆
雷慎辉
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Dongguan Meitu Baoxin Material Co.,Ltd.
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Northwestern Polytechnical University
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Abstract

The invention discloses a preparation method of calcium-borate-glass-modified strontium titanate-lanthanum aluminate composite ceramic. The method is used for solving a technical problem of high preparation temperature of an existing STO-LAO ceramic material preparation method. According to a technical scheme provided by the invention, alumina, lanthanum oxide, titanium dioxide and strontium carbonate are adopted as raw materials, and are subjected to ball milling in a nylon tank with anhydrous ethanol as a grinding medium; bake-drying and grinding are carried out, and the material is sintered in a sintering reaction furnace; calcium borate glass is added, and secondary ball milling is carried out; bake-drying and grinding are carried out, and the material is pressed and molded by using a cold isostatic pressing machine; and sintering is carried out after molding, such that the calcium-borate-glass-modified strontium titanate-lanthanum aluminate composite ceramic is obtained. In a solid-phase sintering reaction, the added calcium borate glass sintering aid system produces a proper amount of an additive liquid phase, such that atom migration diffusion rate is accelerated, mass transfer process is enhanced, reaction process is accelerated, and reaction temperature and time are reduced. The preparation temperature is reduced from 1100-1250 DEG C of a background technology to 1550-1680 DEG C.

Description

The preparation method of lime borate glass modification strontium titanate-lanthanum aluminate composite ceramics
Technical field
The present invention relates to the preparation method of a kind of strontium titanate-lanthanum aluminate composite ceramics, be specifically related to the preparation method of a kind of lime borate glass modification strontium titanate-lanthanum aluminate composite ceramics.
Background technology
Strontium titanate-lanthanum aluminate (hereinafter to be referred as STO-LAO) stupalith is important study hotspot material, and it is at super crystal lattice material, heterojunction material, and monocrystal material, substrate material and function film can direction have large quantity research.And everybody has often ignored its microwave communication material applications.Because the STO-LAO ceramic material microwave is functional, material as microwave devices such as resonator, wave filter, vibrator, clamper, polyrod antenna, medium guided wave loops, be widely used in mobile communication, high definition satellite communication and military commerical radar, the fields such as vehicle-mounted airborne wireless telecommunications system.
Document 1 " T.Shimada; K.Kura; S.Ohtsuki.Dielectric properties and far infrared reflectivity of lanthanum aluminate-strontium titanate ceramics.Journal of the European Ceramic Society; 2006; 26:2017-2021. " discloses a kind of preparation method of STO-LAO stupalith, the method employing purity is 99.9% Strontium carbonate powder, titanium dioxide, aluminum oxide, lanthanum oxide powder is raw material, raw material powder is dried accurate weighing, lanthanum trioxide is 500 ℃ of oven dry in addition, be grinding medium with deionized water after the weighing, behind the ball milling at 1400 ℃ of preburning powdered materials, after the 150MPa pressure forming, then adopt the oxide compound mixed-sintering method to send out and prepared STO-LAO system pottery, sintering temperature is 1580～1680 ℃, and concrete sintering process such as soaking time etc. does not provide detailed introduction.
Document 2 " Seo-Yong Cho, Kug Sun Hong, Kyung-Hyun Ko.Mixture-like behavior in the microwave dielectric properties of the (1-x) LaAlO 3XSrTiO 3System.Materials Research Bulletin, 3,1999,34 (4): 511～516. " disclose a kind of preparation method of STO-LAO stupalith, the method has been prepared (1-x) LaAlO with traditional solid sintering technology at 1550～1650 ° of C sintering 3XSrTiO 3(x=0.0～1.0) pottery.It has adopted purity is that 99.9% Strontium carbonate powder, titanium dioxide, aluminum oxide, lanthanum oxide powder are raw material, raw material powder is dried accurate weighing, with zirconium dioxide abrading-ball ball milling 24h in ball grinder, afterwards at 1300 ℃ of pre-burning 2h, behind the secondary ball milling 24h under air atmosphere, 1550～1650 ° of C sintering 2 hours.
The preparation method of the disclosed STO-LAO stupalith of above-mentioned document, its preparation temperature is all too high.
Summary of the invention
In order to overcome the high deficiency of preparation method's preparation temperature of existing STO-LAO stupalith, the invention provides the preparation method of a kind of lime borate glass modification strontium titanate-lanthanum aluminate composite ceramics.The method is take high-purity strontium carbonate, aluminum oxide, lanthanum trioxide, titanium dioxide and dehydrated alcohol as raw material, add sintering aid system lime borate oxide glass, get high performance strontium titanate-lanthanum aluminate stupalith by traditional solid reaction process in lower temperature and short time.Because in the solid state sintering reaction, the lime borate oxide glass sintering aid system of interpolation produces an amount of additive liquid phase, can accelerate the diffusion mobility speed of atom, and then strengthens mass transfer process, the accelerated reaction process reduces temperature of reaction and time.
The technical solution adopted for the present invention to solve the technical problems is: the preparation method of a kind of lime borate glass modification strontium titanate-lanthanum aluminate composite ceramics is characterized in may further comprise the steps:
(a) by stoichiometry mol ratio aluminum oxide: lanthanum trioxide: titanium dioxide: Strontium carbonate powder=x: x: (1-x): (1-x) [x=0～1] weighing purity is higher than 99.5% aluminum oxide, lanthanum trioxide, titanium dioxide and Strontium carbonate powder raw material powder, and be poured in the nylon tank that zirconium oxide balls is housed, be that requirement below 60% adds the analytical pure dehydrated alcohol as grinding medium by compactedness, with ball milling 5～10h under the speed of 450～500r/min, oven dry is incubated 3～10h after grinding in the sintering reaction stove of 1300～1400 ° of C;
(b) powder behind the taking-up sintering adds 1～10wt%, purity is higher than 99.5% lime borate glass, secondary ball milling 5～10h under the speed of 450～500r/min, taking-up after oven dry is ground;
(c) use cold isostatic press in 300～500Mpa compression moulding;
(d) after the moulding at 1100～1250 ° of C sintering 3～4h, obtain the strontium titanate of lime borate glass modification-lanthanum aluminate composite ceramics.
In the described step (b), the preparation method of lime borate glass is that calcium oxide and boric acid oxide compound glass are according to CaO: B 2O 3Mol ratio=2: 1～1: 2 batching, 800～900 ° of C insulations were as cold as room temperature in the deionized water middling speed after one hour, were ground to maximum particle diameter less than 30 μ m.
The invention has the beneficial effects as follows: because take high-purity strontium carbonate, aluminum oxide, lanthanum trioxide, titanium dioxide and dehydrated alcohol as raw material, add sintering aid system lime borate oxide glass, get high performance strontium titanate-lanthanum aluminate stupalith by traditional solid reaction process in lower temperature and short time.Because in the solid state sintering reaction, the lime borate oxide glass sintering aid system of interpolation produces an amount of additive liquid phase, has accelerated the diffusion mobility speed of atom, and then has strengthened mass transfer process, has accelerated reaction process, has reduced temperature of reaction and time.Preparation temperature is reduced to 1550～1680 ° of C by 1100～1250 of background technology.
Below in conjunction with drawings and Examples the present invention is elaborated.
Description of drawings
Fig. 1 is the XRD figure spectrum of the strontium titanate-lanthanum aluminate composite ceramics of the embodiment of the invention 1～4 preparation.
Fig. 2 is the stereoscan photograph of the strontium titanate-lanthanum aluminate composite ceramics of the embodiment of the invention 1～4 preparation.
Fig. 3 is the performance curve of the strontium titanate-lanthanum aluminate composite ceramics of the embodiment of the invention 1～4 preparation.
Fig. 4 is the strontium titanate-dielectric properties curve of lanthanum aluminate composite ceramics under microwave frequency band 7GHz of the embodiment of the invention 1～4 preparation.
Embodiment
With reference to Fig. 1～4.Preparation method's concrete steps of lime borate glass modification strontium titanate of the present invention-lanthanum aluminate composite ceramics are as follows:
Embodiment 1,0.3: 0.3: 0.7 in molar ratio: 0.7 weighing purity was higher than 99.5% alumina raw material powder 3.0588g, lanthanum trioxide 9.7743g, titanium dioxide 5.5906g and Strontium carbonate powder 10.3340g, and be poured in the nylon tank that zirconium oxide balls is housed, be that requirement below 60% adds the analytical pure dehydrated alcohol as grinding medium by compactedness, with the speed ball milling 10h of 450r/min, oven dry is incubated 10h after grinding in the sintering reaction stove of 1300 ° of C; High-purity (〉=99.5%) calcium oxide of powder adding 1wt% (0.2876g) behind the taking-up sintering and boric acid oxide glass (hereinafter to be referred as BC, CaO: B 2O 3Mol ratio is 2: 1, and 850 ° of C insulations are as cold as room temperature in the deionized water middling speed after one hour and make glass, are ground to maximum particle diameter less than 30 μ m) at the speed secondary ball milling 10h of 450r/min, after grinding, oven dry takes out; With cold isostatic press in 300Mpa compression moulding; At 1250 ° of C sintering 3h, obtain the strontium titanate of lime borate glass modification-lanthanum aluminate composite ceramics after the moulding.
Embodiment 2,0.3: 0.3: 0.7 in molar ratio: 0.7 weighing purity was higher than 99.5% alumina raw material powder 3.0588g, lanthanum trioxide 9.7743g, titanium dioxide 5.5906g and Strontium carbonate powder 10.3340g, and be poured in the nylon tank that the agate abrading-ball is housed, be that requirement below 60% adds deionized water as the speed ball milling 9h of grinding medium with 470r/min by compactedness, oven dry is incubated 7h after grinding in the sintering reaction stove of 1330 ° of C; High-purity (〉=99.5%) calcium oxide of powder adding 2wt% (0.5752g) behind the taking-up sintering and boric acid oxide glass (hereinafter to be referred as BC, CaO: B 2O 3Mol ratio is 1: 2, and 900 ° of C insulations are as cold as room temperature in the deionized water middling speed after one hour and make glass, are ground to maximum particle diameter less than 30 μ m) at the speed secondary ball milling 9h of 470r/min, after grinding, oven dry takes out; With cold isostatic press in 370Mpa compression moulding; At 1200 ° of C sintering 3.3h, obtain the strontium titanate of lime borate glass modification-lanthanum aluminate composite ceramics after the moulding.
Embodiment 3,0.6: 0.6: 0.4 in molar ratio: 0.4 weighing purity was higher than 99.5% alumina raw material powder 6.1177g, lanthanum trioxide 19.5485g, titanium dioxide 3.1946g and Strontium carbonate powder 5.9052g, and be poured in the nylon tank that zirconium oxide balls is housed, be that requirement below 60% adds the analytical pure dehydrated alcohol as the speed ball milling 7h of grinding medium with 490r/min by compactedness, oven dry is incubated 5h after grinding in the sintering reaction stove of 1360 ° of C; High-purity (〉=99.5%) calcium oxide of powder adding 5wt% (1.7383g) behind the taking-up sintering and boric acid oxide glass (hereinafter to be referred as BC, CaO: B 2O 3Mol ratio is 1: 1, and 800 ° of C insulations are as cold as room temperature in the deionized water middling speed after one hour and make glass, are ground to maximum particle diameter less than 30 μ m) at the speed secondary ball milling 7h of 490r/min, after grinding, oven dry takes out; With cold isostatic press in 430Mpa compression moulding; At 1150 ° of C sintering 3.7h, obtain the strontium titanate of lime borate glass modification-lanthanum aluminate composite ceramics after the moulding.
Embodiment 4,0.4: 0.4: 0.6 in molar ratio: 0.6 weighing purity was higher than 99.5% alumina raw material powder 4.0785g, lanthanum trioxide 13.0324g, titanium dioxide 4.7919g and Strontium carbonate powder 8.8577g, and be poured in the nylon tank that the agate abrading-ball is housed, be that requirement below 60% adds deionized water as the speed ball milling 5h of grinding medium with 500r/min by compactedness, oven dry is incubated 3h after grinding in the sintering reaction stove of 1400 ° of C; High-purity (〉=99.5%) calcium oxide of powder adding 10wt% (3.076g) behind the taking-up sintering and boric acid oxide glass (hereinafter to be referred as BC, CaO: B 2O 3Mol ratio is 1: 1, and 900 ° of C insulations are as cold as room temperature in the deionized water middling speed after one hour and make glass, are ground to maximum particle diameter less than 30 μ m) at the speed secondary ball milling 5h of 500r/min, after grinding, oven dry takes out; With cold isostatic press in 500Mpa compression moulding; At 1100 ° of C sintering 4h, obtain the strontium titanate of lime borate glass modification-lanthanum aluminate composite ceramics after the moulding.
Above concrete numerical value is groped out through summary of experience by great many of experiments, for example: Ball-milling Time 5～10 hours, the uniform granularity degree of powder below 5 hours is not ideal enough, and more than 10 hours, then performance is substantially unchanged, thereby cause waste.In like manner, being incubated 3～10h in the sintering reaction stove also is the optimized scope that test obtains.For example rotating speed is between 450～500r/min again, and rotating speed crosses that low then granularity is excessive, and the too high powder cohesiveness that then causes of rotating speed increases, and is unfavorable for subsequent disposal.The addition of zinc oxide and boric acid oxide compound 1～10wt% has then guaranteed the comprehensive excellent properties of strontium titanate-lanthanum aluminate composite ceramics, and performance is more excellent during few additive, and when addition strengthened, cooling-down effect was more obvious.
As can be seen from Figure 1, obtained lime borate glass modification strontium titanate-lanthanum aluminate composite ceramics crystal property is intact, and the phase homogeneous chemical composition is substantially without dephasign.
As can be seen from Figure 2, obtained lime borate glass modification strontium titanate-the lanthanum aluminate composite ceramic particle is complete, the well-crystallized, and crystal grain is evenly tiny, without separating out of second-phase and dephasign.
As can be seen from Figure 3, prepared different components and add the xSTO-1-x of the BC glass of 1～10wt%) the LAO composite ceramics is under radio frequency, ceramic loss is very low, temperature stability is good.
As can be seen from Figure 4, matrix strontium titanate-lanthanum aluminate composite ceramics excellent performance under 7GHz, specific inductivity be near 50, minimum more than 30 of up-to-date domestic and international commercial applications that surpassed.Q f mechanical quality factor reaches that wherein minimum sintered ceramic such as figure are about 42,000GHz near 50,000GHz(), and reached nearly zero temperature coefficient of resonance frequency (≤± 40 * 10 -6), applicability is very high.Prepared lime borate glass modification strontium titanate-lanthanum aluminate composite ceramics, the excellent properties that has kept the matrix pottery, and sintering temperature significantly is reduced to 1100 ° below the C by 1680 ° of C of background technology, being better than international present low-temperature sintering type microwave dielectric ceramic novel material 50%～100%(experiment gained of reporting is 10 as scheming minimum, about 000GHz, and the international literature report is commonly 5 at present, 000～8, the integrated chip type technique burning of 000GHz) being convenient to product and metal is made, and has very large commercial application prospect and excellent practical performance.

Claims (1)

1. the preparation method of lime borate glass modification strontium titanate-lanthanum aluminate composite ceramics is characterized in that may further comprise the steps:
(a) by stoichiometry mol ratio aluminum oxide: lanthanum trioxide: titanium dioxide: Strontium carbonate powder=x: x: (1-x): (1-x) [x=0～1] weighing purity is higher than 99.5% aluminum oxide, lanthanum trioxide, titanium dioxide and Strontium carbonate powder raw material powder, and be poured in the nylon tank that zirconium oxide balls is housed, be that requirement below 60% adds the analytical pure dehydrated alcohol as grinding medium by compactedness, with ball milling 5～10h under the speed of 450～500r/min, oven dry is incubated 3～10h after grinding in the sintering reaction stove of 1300～1400 ° of C;
(b) powder behind the taking-up sintering adds 1～10wt%, purity is higher than 99.5% lime borate glass, secondary ball milling 5～10h under the speed of 450～500r/min, taking-up after oven dry is ground;
(c) use cold isostatic press in 300～500Mpa compression moulding;
(d) after the moulding at 1100～1250 ° of C sintering 3～4h, obtain the strontium titanate of lime borate glass modification-lanthanum aluminate composite ceramics;
In the described step (b), the preparation method of lime borate glass is that calcium oxide and boric acid oxide compound glass are according to CaO: B 2O 3Mol ratio=2: 1～1: 2 batching, 800～900 ° of C insulations were as cold as room temperature in the deionized water middling speed after one hour, were ground to maximum particle diameter less than 30 μ m.
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Cited By (5)

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CN104072113A (en) * 2014-06-30 2014-10-01 江苏南瓷绝缘子股份有限公司 High-strength ceramic prepared from glass and production process thereof
CN114133254A (en) * 2021-12-15 2022-03-04 营口丰华耐火材料有限公司 Infrared radiation castable for cement kiln mouth and preparation method thereof
CN115304990A (en) * 2022-09-07 2022-11-08 广州市佐力新材料科技有限公司 Leather coating agent with lasting gloss and preparation method thereof
CN116497324A (en) * 2023-06-09 2023-07-28 深圳市汉嵙新材料技术有限公司 Composite perovskite target material, preparation method thereof and preparation method of perovskite solar cell
CN116751046A (en) * 2023-06-19 2023-09-15 陕西科技大学 Low-loss microwave dielectric ceramic material, preparation method and application

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104072113A (en) * 2014-06-30 2014-10-01 江苏南瓷绝缘子股份有限公司 High-strength ceramic prepared from glass and production process thereof
CN104072113B (en) * 2014-06-30 2016-06-29 江苏南瓷绝缘子股份有限公司 A kind of high-strength ceramic utilizing glass to make and production technology thereof
CN114133254A (en) * 2021-12-15 2022-03-04 营口丰华耐火材料有限公司 Infrared radiation castable for cement kiln mouth and preparation method thereof
CN114133254B (en) * 2021-12-15 2022-09-20 营口丰华耐火材料有限公司 Infrared radiation castable for cement kiln mouth and preparation method thereof
CN115304990A (en) * 2022-09-07 2022-11-08 广州市佐力新材料科技有限公司 Leather coating agent with lasting gloss and preparation method thereof
CN115304990B (en) * 2022-09-07 2023-12-08 广州市佐力新材料科技有限公司 Leather coating agent with lasting luster and preparation method thereof
CN116497324A (en) * 2023-06-09 2023-07-28 深圳市汉嵙新材料技术有限公司 Composite perovskite target material, preparation method thereof and preparation method of perovskite solar cell
CN116751046A (en) * 2023-06-19 2023-09-15 陕西科技大学 Low-loss microwave dielectric ceramic material, preparation method and application

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