CN101104562B - Constant pressure hydro-thermal preparation method for barium zirconate titanate powder - Google Patents
Constant pressure hydro-thermal preparation method for barium zirconate titanate powder Download PDFInfo
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- CN101104562B CN101104562B CN2007100523771A CN200710052377A CN101104562B CN 101104562 B CN101104562 B CN 101104562B CN 2007100523771 A CN2007100523771 A CN 2007100523771A CN 200710052377 A CN200710052377 A CN 200710052377A CN 101104562 B CN101104562 B CN 101104562B
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- zirconate titanate
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- 239000000843 powder Substances 0.000 title claims abstract description 33
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910021523 barium zirconate Inorganic materials 0.000 title claims abstract description 23
- DQBAOWPVHRWLJC-UHFFFAOYSA-N barium(2+);dioxido(oxo)zirconium Chemical compound [Ba+2].[O-][Zr]([O-])=O DQBAOWPVHRWLJC-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 16
- 239000010936 titanium Substances 0.000 claims abstract description 12
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229910001626 barium chloride Inorganic materials 0.000 claims abstract description 9
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 9
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 229910002113 barium titanate Inorganic materials 0.000 claims description 11
- YIMPFANPVKETMG-UHFFFAOYSA-N barium zirconium Chemical compound [Zr].[Ba] YIMPFANPVKETMG-UHFFFAOYSA-N 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 9
- 229940045511 barium chloride Drugs 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 6
- 230000036571 hydration Effects 0.000 claims description 5
- 238000006703 hydration reaction Methods 0.000 claims description 5
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- NZSLBYVEIXCMBT-UHFFFAOYSA-N chloro hypochlorite;zirconium Chemical class [Zr].ClOCl NZSLBYVEIXCMBT-UHFFFAOYSA-N 0.000 claims description 3
- 238000002955 isolation Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 9
- 238000009826 distribution Methods 0.000 abstract description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract description 4
- 229910052788 barium Inorganic materials 0.000 abstract description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000011780 sodium chloride Substances 0.000 abstract description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract 2
- PWKQBKSENWCEOJ-UHFFFAOYSA-N O(Cl)Cl.[O] Chemical compound O(Cl)Cl.[O] PWKQBKSENWCEOJ-UHFFFAOYSA-N 0.000 abstract 1
- 230000036632 reaction speed Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 19
- 239000002245 particle Substances 0.000 description 7
- 238000001035 drying Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000010532 solid phase synthesis reaction Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- ZWGDULLGQACGJD-UHFFFAOYSA-H barium(2+) zirconium(4+) tricarbonate Chemical compound [Zr+4].[Ba++].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O ZWGDULLGQACGJD-UHFFFAOYSA-H 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- -1 organo-metallic alkoxide Chemical class 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011172 small scale experimental method Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Disclosed is a normal-pressure hydrothermal preparation method for barium zirconate titanate powder. Pure titanium tetrachloride is used as the source of titanium; zirconia oxygen dichlorohydrate is used as the source for zirconium; barium chloride is used as the barium source; sodium hydroxide is taken as the reaction agent; in conjunction with technology, the reaction conditions are timely and strictly controlled, thus the reaction speed is greatly accelerated and the sodium chloride and other remnants left after the reaction are easy to be washed to cause less pollution on environment. The reaction of the invention is carried through in normal-pressure and low-temperature environment, thus the various parameters in the reaction process can be easily adjusted and controlled. The barium zirconate titanate powder prepared through the invention has the advantages of integral grains, even granularity distribution, non-reunion, high activity and low cost, which can fully meet the requirements on the high-performance of barium zirconate titanate in the electronic industry.
Description
Technical field
The present invention relates to a kind of preparation method of barium zirconate titanate powder, especially relate to a kind of constant pressure hydro-thermal preparation method of barium zirconate titanate powder.
Background technology
The electronic ceramics that utilizes barium zirconate titanate powder to make, have good dielectric, piezoelectricity, ferroelectric, pyroelectric effect, can be used to make large value capacitor, non-volatility ferroelectric storer, piezoelectric actuator etc., therefore have great application prospect at microelectronic.The preparation method of existing barium zirconate titanate powder mainly contains solid phase method and sol-gel method.Solid phase method is to adopt BaCO
3, TiO
2, ZrO
2Be mixed in proportion, make through high temperature (1280 ℃-1300 ℃) calcining, this method requires high to synthesis device, and the uniformity coefficient to raw material during production is difficult to grasp; And the powder purity that makes is low, particle diameter is big and size-grade distribution is inhomogeneous, and reactive behavior is poor, so the electronic element products quality can not get guaranteeing.And gel method, general employing organo-metallic alkoxide or stearate are raw material, by hydrolysis, polymerization, obtain the mixture gel after the cooling, again drying and high-temperature calcination and make this method starting material costliness, gelation process is slower, production cycle is longer, is difficult to realize industrialization, therefore can only rest on the small scale experiments stage.
Advance in the past few years, the someone proposes with high pressure Hydrothermal Preparation barium zirconate titanate powder, and is big and size-grade distribution is inhomogeneous, technical problems such as reactive behavior difference with the powder granule that overcome the solid phase method preparation.Provide a kind of " technology of preparation nano level high purity zirconium barium carbonate powder " as Chinese patent CN1472170, this technology autoclave, and under the condition of 220 ℃-250 ℃ of temperature, pressure 6-9Mpa, carry out building-up reactions, through making the zirconium barium titanate suspension liquid in 8-15 hours, washing, drying are made barium zirconate titanate powder then.Though this process portion has solved the inherent defect of solid phase method or gel method, whole technology is rather complicated, and to conversion unit performance requriements height, facility investment is big, and reaction process energy consumption height, time are long, so that production cost is higher.
Summary of the invention
The present invention solves the existing complex process of prior art barium zirconate titanate powder production method, and to conversion unit performance requriements height, reaction process energy consumption height, time are long, cost high-technology problem.
It is low that the present invention has also solved the existing powder purity of existing production barium zirconate titanate powder technology simultaneously, technical problem such as the big and size-grade distribution of particle is inhomogeneous.
The present invention is mainly solved the problems of the technologies described above by following technical proposals: it may further comprise the steps:
A. obtain solution: pure titanium tetrachloride, eight hydration zirconium oxychlorides and bariumchloride are mixed with certain density solution with deionized water respectively, must not be lower than 1.05 ratio according to the mol ratio of Ba/ (Ti+Zr) then and measure; Solution after the above-mentioned metering is mixed in the same container, and adds proper amount of deionized water, it is standby to make mixing solutions after stirring;
B. building-up reactions: mixing solutions is poured in the normal-pressure reaction kettle, open and stir, in mixing solutions, add sodium hydrate solid then, and in the assurance normal-pressure reaction kettle pH value of solution greater than 14, temperature of reaction is controlled between 80 ℃-100 ℃, just makes the zirconium barium titanate throw out like this after isothermal reaction 2-6 hour;
C. washing: will react zirconium metatitanic acid suspension liquid after synthetic and put into airtight container and cool off, cooling is then used deionized water rinsing, and with flush awaies such as sodium ion in the solution and chlorions, washing process carries out in the condition of air-isolation, to prevent airborne CO
2With the Ba (OH) that residues in the suspension liquid
2React and generation BaCO
3, influence the product electrical property.Wash to specific conductivity less than 50us/cm after, detect with x-ray fluorescence analyzer (XRF), it is qualified that its Ba/ (Ti+Zr) element is than between 0.995-1.005.
D. dry: zirconium barium titanate is filtered, and oven dry is also pulverized, and can obtain barium zirconate titanate powder.
As preferably, in the obtain solution step, the concentration of described titanium tetrachloride solution is 2.5-5.0mol/L, and the concentration of described eight hydration zirconium oxychloride solution is 1.0-3.0mol/L, and the concentration of described barium chloride solution is 0.8-1.2mol/L.
As preferably, in the building-up reactions step, described temperature of reaction is 100 ℃.
As preferably, in the described mixing solutions, the volumetric molar concentration of its titanium, zirconium and be 0.2-0.6mol/L, the optimum molar concentration of its titanium, zirconium and be 0.5mol/L.
The present invention is reflected under the normal pressure and carries out, and temperature of reaction is no more than 100 ℃, has therefore reduced the equipment input in the synthesis process, and has significantly reduced the loss to the energy; Thereby overcome in the high pressure-temperature hydrothermal synthesis method, equipment performance requires high, reaction process energy consumption high-technology defective.And because reaction is to carry out in normal pressure, low temperature environment, all than being easier to, therefore the quality of every batch products is all very stable to the adjustment of the various parameters in the process in the reaction and control.
The present invention adopts pure titanium tetrachloride to do the titanium source, eight hydration zirconium oxychlorides are done the zirconium source, bariumchloride is done the barium source, sodium hydroxide is as the reaction precipitation agent, and in the combined process,, speed of response is accelerated greatly to real-time, the strict control of reaction conditions, and residues such as reacted sodium chloride are convenient to washing, and environmental pollution is little.
Therefore, adopt the barium zirconate titanate powder of the inventive method preparation to have crystal grain and grow complete, even particle size distribution, do not reunite, active high, characteristics such as cost is low can satisfy electronic industry fully to the high performance requirement of zirconium barium titanate.
Description of drawings
Fig. 1 is BaTi
0.8Zr
0.2O
3Crystallogram;
Fig. 2 is BaTi
0.82Zr
0.18O
3Crystallogram;
Fig. 3 is BaTi
0.8Zr
0.2O
3Electron micrograph;
Fig. 4 is BaTi
0.82Zr
0.18O
3Electron micrograph.
Embodiment
Below by embodiment, and in conjunction with the accompanying drawings, technical scheme of the present invention is described in further detail.
Embodiment 1: preparation BaTi
0.8Zr
0.2O
3Measure 0.2 liter of 4.0mol/L titanium tetrachloride solution, 0.2 liter of 1.0mol/L zirconium oxychloride and 1 liter of 1.2mol/L barium chloride solution with graduated cylinder and place container, and add 0.6 liter of deionized water and stirring to mixing; Then above-mentioned mixed solution is poured in the normal-pressure reaction kettle, open to be stirred, and to wherein adding the 312g sodium hydrate solid, after 6 hours, be cooled to room temperature, wash with deionized water again with electric mantle heat temperature raising to 80 ℃ and constant temperature; Above-mentioned washing process carries out under full closeding state, wash to specific conductivity less than 50us/cm after, detect through XRF, be qualified than between 0.995-1.005 when reaching Ba/ (Ti+Zr) element, carry out drying, pulverizing after qualified, obtain barium zirconate titanate powder.
Embodiment 2: preparation BaTi
0.82Zr
0.18O
3Measure 0.328 liter of 2.5mol/L titanium tetrachloride solution, 0.06 liter of 3.0mol/L zirconium oxychloride and 1.5 liters of 0.8mol/L barium chloride solutions with graduated cylinder and place container, and add 3.11 liters of deionized water and stirring to mixing; Then above-mentioned mixed solution is poured in the normal-pressure reaction kettle, open to stir, and to wherein adding the 460g sodium hydrate solid, with electric mantle heat temperature raising to 100 ℃ and constant temperature after 2 hours, be cooled to room temperature, wash with deionized water, above-mentioned washing process carries out under full closeding state again, wash to specific conductivity less than 50us/cm after, censorship XRF, be qualified than between 0.995-1.005 when reaching Ba/ (Ti+Zr) element, carry out drying, pulverizing after qualified, obtain barium zirconate titanate powder.
Embodiment 3: preparation BaTi
0.82Zr
0.18O
3Measure 0.16 liter of 5.0mol/L titanium tetrachloride solution, 0.1 liter of 2.0mol/L zirconium oxychloride and 1 liter of 1.1mol/L barium chloride solution with graduated cylinder and place container, and add 0.41 liter of deionized water and stirring to mixing; Then above-mentioned mixed solution is poured in the normal-pressure reaction kettle, open to stir, and to wherein adding the 325g sodium hydrate solid, with electric mantle heat temperature raising to 90 ℃ and constant temperature after 4 hours, be cooled to room temperature, wash with deionized water, above-mentioned washing process carries out under full closeding state again, wash to specific conductivity less than 50us/cm after, censorship XRF, be qualified than between 0.995-1.005 when reaching Ba/ (Ti+Zr) element, carry out drying, pulverizing after qualified, obtain barium zirconate titanate powder.
Respectively to the dry powder analysis revealed of the zirconium barium titanate of the foregoing description 1,2, its thing is a cube phase zirconium barium titanate mutually with X-ray diffraction analysis equipment (XRD).
Respectively the dry powder of the zirconium barium titanate of embodiment 1 and embodiment 2 is analyzed with scanning electronic microscope (SEM).
As shown in Figure 3, the BaTi among the embodiment 1
0.8Zr
0.2O
3Electromicroscopic photograph show the pattern almost spherical of this powder particle, and good dispersity, diameter of particle on average is about 150 nanometers in the 100-200 nanometer.
As shown in Figure 4, the BaTi among the embodiment 2
0.82Zr
0.18O
3Electromicroscopic photograph show the pattern almost spherical of this powder particle, and good dispersity, diameter of particle is the 100-200 nanometer, on average is about 150 nanometers.
The dry powder of zirconium barium titanate with specific surface area absorption instrument difference practical measuring examples 1,2.Example 1BaTi
0.8Zr
0.2O
3The specific surface area of powder is 30 meters squared per gram.Example 2 BaTi
0.82Zr
0.18O
3The specific surface area of powder is 29 meters squared per gram.
Claims (4)
1. the constant pressure hydro-thermal preparation method of a barium zirconate titanate powder is characterized in that said method comprising the steps of:
A. obtain solution: A. obtain solution: pure titanium tetrachloride, eight hydration zirconium oxychlorides and bariumchloride are mixed with solution with deionized water respectively, wherein the concentration of titanium tetrachloride solution is 2.5-5.0mol/L, and the concentration of eight hydration zirconium oxychloride solution is that the concentration of 1.0-3.0mol/L barium chloride solution is 0.-1.2mol/L; Must not be lower than 1.05 ratio according to the mol ratio of Ba/ (Ti+Zr) then measures; Solution after the above-mentioned metering is mixed in the same container, and adds proper amount of deionized water, it is standby to make mixing solutions after stirring;
B. building-up reactions: mixing solutions is poured in the normal-pressure reaction kettle, open and stir, in mixing solutions, add sodium hydrate solid then, and in the assurance normal-pressure reaction kettle pH value of solution greater than 14, temperature of reaction is controlled between 80 ℃-100 ℃, just makes the zirconium barium titanate throw out after isothermal reaction 2-6 hour;
C. washing: will react and under the condition of air-isolation, use deionized water rinsing after zirconium barium titanate throw out after synthetic is put into airtight container cooling cooling;
D. dry: will wash back zirconium barium titanate feed liquid and filter, oven dry is also pulverized, and can obtain barium zirconate titanate powder.
2. the constant pressure hydro-thermal preparation method of barium zirconate titanate powder according to claim 1 is characterized in that in the building-up reactions step, and described temperature of reaction is 100 ℃.
3. the constant pressure hydro-thermal preparation method of barium zirconate titanate powder according to claim 1 is characterized in that in described mixing solutions, the volumetric molar concentration of its titanium, zirconium and be 0.2-0.6mol/L.
4. the constant pressure hydro-thermal preparation method of barium zirconate titanate powder according to claim 1 is characterized in that in described mixing solutions, the volumetric molar concentration of its titanium, zirconium and be 0.5mol/L.
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| CN101928038B (en) * | 2009-06-26 | 2013-11-13 | 中国科学院福建物质结构研究所 | Preparation method of barium titanate hollow nanospheres |
| KR102190834B1 (en) * | 2013-11-19 | 2020-12-14 | 사까이가가꾸고오교가부시끼가이샤 | Method for producing barium titanate powder |
| CN104496466A (en) * | 2014-12-15 | 2015-04-08 | 陕西科技大学 | High-solid-solubility relaxation-type nano leadless piezoelectric ceramic and preparation method thereof |
| CN104557033B (en) * | 2014-12-19 | 2017-01-04 | 广东风华高新科技股份有限公司 | The preparation method of barium zirconate titanate powder |
| CN105036740B (en) * | 2015-06-26 | 2017-04-26 | 天津大学 | Preparation method of BZT (barium titanate zirconate) target material for magnetron sputtering |
| CN109721100A (en) * | 2019-03-21 | 2019-05-07 | 成都工业学院 | A kind of method of hydro-thermal method preparation nanometer barium zirconium phthalate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1472170A (en) * | 2003-06-30 | 2004-02-04 | 山东省国腾功能陶瓷材料有限公司 | Manufacture of high purity nano grade powders of barium zirconate titanate |
| CN1583667A (en) * | 2004-06-09 | 2005-02-23 | 哈尔滨工业大学 | Preparation of zirconium barium titanate with inorganic zirconium as source |
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| CN1472170A (en) * | 2003-06-30 | 2004-02-04 | 山东省国腾功能陶瓷材料有限公司 | Manufacture of high purity nano grade powders of barium zirconate titanate |
| CN1583667A (en) * | 2004-06-09 | 2005-02-23 | 哈尔滨工业大学 | Preparation of zirconium barium titanate with inorganic zirconium as source |
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