CN104803412A - Method for preparing barium dititanate by hydrothermal method - Google Patents
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- CN104803412A CN104803412A CN201510226049.3A CN201510226049A CN104803412A CN 104803412 A CN104803412 A CN 104803412A CN 201510226049 A CN201510226049 A CN 201510226049A CN 104803412 A CN104803412 A CN 104803412A
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Abstract
The invention relates to a method for preparing barium dititanate by a hydrothermal method. The method comprises the following steps of firstly, mixing barium hydroxide monohydrate and sodium hydroxide in deionized water, and fully mixing to obtain a mixed solution; secondly, dropping titanium tetrachloride in the mixed solution in the first step to obtain a reacting solution in a vacuum glove box; thirdly, adding the prepared reacting solution in a polytetrafluoroethylene liner, and placing the liner in a hydrothermal reactor for reacting; fourthly, centrifugally cleaning and drying a product obtained by reacting to obtain a precursor; fifthly, performing heat treatment on the precursor in a muffle furnace to obtain the barium dititanate. The method disclosed by the invention has the beneficial effects that higher-purity barium dititanate powder can be obtained, and the higher-purity barium dititanate powder is further prepared by sintering into barium dititanate ceramics. According to the method disclosed by the invention, no high pressure is needed, the required equipment is simple, and the cost is lower.
Description
Technical field
The present invention relates to ferroelectric material technical field, particularly relate to a kind of hydrothermal preparing process at b direction of principal axis with ferroelectric material two barium titanate of larger specific inductivity.
Background technology
Ferroelectricity is nineteen twenty, ceases salt (Seignette salt, NaKC by Frenchman Valasek at sieve
4h
4o
64H
2o) find in.The crystalline structure with ferroelectric material just has spontaneous polarization phenomenon when not adding external electric field, and its direction of polarization can change along with the change in external electrical field direction.The crystalline structure of ferroelectric material can change in certain temperature, and change paraelectric phase into by ferroelectric phase, therefore can be applied in Ferroelectric Random Access Memory, dynamic RAM, the temperature that structure is undergone mutation is called Curie temperature.
Study very ripe BaTiO
3based leadless piezoelectric ceramics is BaO-TiO
2a kind of compound in system, environmentally friendly and there is higher specific inductivity, but its low Curie temperature limits its application.The ferroelectricity of two barium titanates had been found in recent years, and its spacer is the C of low-symmetry
2, be BaTiO at the axial specific inductivity of b
32 ~ 3 times, and Curie temperature is 380-470 DEG C, has a good application prospect.But two barium titanates are thermodynamically stable at 1220-1230 DEG C, be all metastable condition, therefore prepare two barium titanate pure phases and have certain difficulty at other temperature.
In the method for current known preparation two barium titanate, there are molten-salt growth method, solid reaction process, sol-gel method, laser chemical vapor deposition, discharge plasma sintering, float-zone method etc.Two one-step hydrothermals that utilize delivered for 2006 prepare the document Wang L of two barium titanates, Li G, Zhang Z.Synthesis of nanobelts [J] .Materials Research Bulletin, 2006,41 (4): 842-846 preparation-obtained materials are not two barium titanates according to the reality of X ray diffracting spectrum shown in this article.Therefore hydrothermal method is not also utilized successfully to prepare the relevant report of two barium titanate phases so far.
Summary of the invention
In view of this, the object of this invention is to provide a kind of hydrothermal method that utilizes newly and prepare the preparation method of two barium titanates.This preparation method take Hydrothermal Synthesis as key step, and equipment used is simple, and lower cost, can synthesize two barium carbonate powders, and can sinter two barium titanate ferroelectric ceramicses further into this.
The present invention solves the problems of the technologies described above adopted technical scheme: hydrothermal method prepares the method for two barium titanates, includes following steps:
1) dried barium hydroxide and sodium hydroxide are mixed in deionized water, after fully stirring, obtain mixing solutions; The mol ratio of described dried barium hydroxide and sodium hydroxide is 1:6 ~ 10;
2) in vacuum glove box, titanium tetrachloride is added drop-wise to step 1) described in mixing solutions in obtain reaction soln; The mol ratio of described dried barium hydroxide and titanium tetrachloride is 1:1.8 ~ 2.1;
3) the described reaction soln configured is joined in polytetrafluoroethyllining lining, then liner is put into hydrothermal reaction kettle react;
4) by obtain after described reaction product eccentric cleaning, drying, obtain presoma;
5) by the thermal treatment in retort furnace of described presoma, obtain that there is ferroelectric material two barium titanate compared with high-curie temperature.
By such scheme, step 2) regulate the pH value of described reaction soln to be 11-14.
By such scheme, step 3) compactedness in described polytetrafluoroethyllining lining is 70%-80%.
By such scheme, the temperature of described hydro-thermal reaction is 160 ~ 240 DEG C, and the time of described hydro-thermal reaction is 18 ~ 72 hours.
By such scheme, described heat treated temperature is 900 ~ 1200 DEG C, and the described heat treated time is 3 ~ 6 hours.
The technical process that the present invention prepares two barium titanates mainly comprises hydro-thermal reaction and thermal treatment, in hydrothermal reaction process, and titanium ion (Ti
4+), barium ion (Ba
2+) and solution in hydroxide ion (OH
-) react, generate the amorphous phase of rich titanium.Because barium/titanium mol ratio controls near 1:2, the nucleus of two barium titanates therefore can be formed.In heat treatment process subsequently, the nucleus of two barium titanates, through nucleation and growth process, crystallizes into two barium titanate crystalline phases.
The invention has the beneficial effects as follows: provide a kind of hydrothermal method that utilizes newly and prepare the preparation method of two barium titanates, two purer barium carbonate powders can be obtained, and barium dititanate can be prepared with this further by sintering.The present invention does not need very high pressure, and equipment used is simple, lower cost, can be applicable to the preparation of two barium carbonate powders and pottery.
Accompanying drawing explanation
The X-ray diffractogram of the ferroelectric material that Fig. 1 provides for the embodiment of the present invention 1;
The dielectric properties test pattern of the ferroelectric material that Fig. 2 provides for the embodiment of the present invention 1;
The scanning electron microscope (SEM) photograph of the ferroelectric material that Fig. 3 provides for the embodiment of the present invention 1;
The X-ray diffractogram of the ferroelectric material that Fig. 4 provides for the embodiment of the present invention 2;
The X-ray diffractogram of the ferroelectric material that Fig. 5 provides for the embodiment of the present invention 3;
The X-ray diffractogram of the ferroelectric material that Fig. 6 provides for the embodiment of the present invention 4.
Embodiment
In the present invention, chemical feedstocks used is streat drug, first dried barium hydroxide and sodium hydroxide mix by the present invention in deionized water, the mol ratio of described dried barium hydroxide and sodium hydroxide is 1:x, described x meets the following conditions: 6<x<10, is preferably 7≤x≤9.In above-mentioned solution, add titanium tetrachloride, obtain reaction soln.In the present invention, described titanium tetrachloride measures, drips and stirs in vacuum glove box, and then inhibits the hydrolysis of titanium tetrachloride.In the present invention, the mol ratio of described dried barium hydroxide and titanium tetrachloride is preferably 1:1.8 ~ 2.1.After obtaining reaction soln, joined in polytetrafluoroethyllining lining, compactedness is preferably 70% ~ 80%.Described reaction soln need use sodium hydroxide adjust ph, is preferably 11 ~ 14.Again described polytetrafluoroethyllining lining is put into hydrothermal reaction kettle and carry out hydro-thermal reaction, the temperature of described hydro-thermal reaction is preferably 160 ~ 240 DEG C, is more preferably 170 ~ 230 DEG C, most preferably is 180 ~ 220 DEG C, the time of described hydro-thermal reaction is preferably 18 ~ 72 hours, is more preferably 30 ~ 48 hours.After hydro-thermal reaction terminates, by product eccentric cleaning 6 ~ 8 times, then drying obtains presoma.The present invention is not particularly limited hydro-thermal reaction device, can be thermostatic drying chamber.After obtaining presoma, by its thermal treatment, can obtain that there is ferroelectric material two barium titanate compared with high-curie temperature, described heat treated temperature is preferably 900 ~ 1200 DEG C, be more preferably 920 ~ 1120 DEG C, most preferably be 940 ~ 1100 DEG C, described heat treatment time is preferably 3 ~ 6 hours.The present invention is not particularly limited thermal treatment unit, can be chamber type electric resistance furnace.
Carry out Performance Detection to ferroelectric material provided by the invention, result shows, ferroelectric material prepared by the present invention is two purer barium titanates, and has higher Curie temperature, and its Curie temperature is 389 DEG C.
In order to further illustrate the present invention, below in conjunction with example, the preparation method that hydrothermal method provided by the invention prepares two barium titanates is described in detail.
Embodiment 1
Be the dried barium hydroxide (Ba (OH) of 99% by purity
2h
2o) 0.00248mol and purity be 98% sodium hydroxide (NaOH) 0.01984mol (mol ratio 1:8) mix in deionized water, obtain mixing solutions.Be the titanium tetrachloride (TiCl of 99.5% by purity in vacuum glove box
4) 0.00496mol (barium/titanium mol ratio 1:2) is added drop-wise in described mixing solutions, obtains reaction soln after stirring.Described reaction soln is poured in polytetrafluoroethyllining lining, regulate compactedness be 80% and pH value be put into hydrothermal reaction kettle after 12 ~ 13 (regulating with sodium hydroxide).Utilize thermostatic drying chamber, described hydrothermal reaction kettle is heated to 180 DEG C of reactions 36 hours, then by reaction product eccentric cleaning 6 times, after drying, obtains presoma; By presoma 1050 DEG C of thermal treatment 4 hours in chamber type electric resistance furnace, obtain material, described material is two purer barium titanates.
Be that German Bruker company D8 type X-ray ff diffractometer carries out composition analysis to the material obtained by model, result is see Fig. 1.Fig. 1 is the X ray picture of material prepared by the embodiment of the present invention.As shown in Figure 1, material prepared by the present embodiment is two purer barium titanates, and its molecular formula is BaTi
2o
5.
Be that Britain Wayne Kerr 6500B precise impedance analyser carries out dielectric properties test to the material obtained by model, result is see Fig. 2.Fig. 2 is the dielectric properties figure of material prepared by the embodiment of the present invention.As shown in Figure 2, the Curie temperature of material that prepared by the present embodiment is 389 DEG C.
Be that Japanese JSM-5510LV scanning electronic microscope carries out pattern test to the material obtained by model, result is see Fig. 3.Fig. 3 is the scanning electron microscope (SEM) photograph of material prepared by inventive embodiments.As shown in Figure 3, material prepared by the present embodiment is elementary cell is irregular bar-shaped, micro-meter scale size.
Embodiment 2
Be the dried barium hydroxide (Ba (OH) of 99% by purity
2h
2o) 0.00248mol and purity be 98% sodium hydroxide (NaOH) 0.0248mol (mol ratio 1:10) mix in deionized water, obtain mixing solutions.Be the titanium tetrachloride (TiCl of 99.5% by purity in vacuum glove box
4) 0.005208mol (barium/titanium mol ratio 1:2.1) is added drop-wise in described mixing solutions, obtains reaction soln after stirring.Described reaction soln is poured in polytetrafluoroethyllining lining, regulate compactedness be 80% and pH value be put into hydrothermal reaction kettle after 13 ~ 14 (regulating with sodium hydroxide).Utilize thermostatic drying chamber, described hydrothermal reaction kettle is heated to 180 DEG C of reactions 50 hours, then by reaction product eccentric cleaning 6 times, after drying, obtains presoma; By presoma 1050 DEG C of thermal treatment 4 hours in chamber type electric resistance furnace, obtain material, described material principal phase is two barium titanates.
Be that German Bruker company D8 type X-ray diffractometer carries out composition analysis to the material obtained by model, result is see Fig. 4.Fig. 4 is the X ray picture of material prepared by the embodiment of the present invention.As shown in Figure 4, material prepared by the present embodiment is two barium titanates, but also simultaneously containing a small amount of rutile and a small amount of ferroelectric material barium titanate (BaTiO
3).The change of preparation technology parameter cause obtained material purity comparatively embodiment 1 decrease.
Embodiment 3
Be the dried barium hydroxide (Ba (OH) of 99% by purity
2h
2o) 0.00248mol and purity be 98% sodium hydroxide (NaOH) 0.01488mol (mol ratio 1:6) mix in deionized water, obtain mixing solutions.Be the titanium tetrachloride (TiCl of 99.5% by purity in vacuum glove box
4) 0.004464mol (barium/titanium mol ratio 1:1.8) is added drop-wise in described mixing solutions, obtains reaction soln after stirring.Described reaction soln is poured in polytetrafluoroethyllining lining, regulate compactedness be 80% and pH value be put into hydrothermal reaction kettle after 11 ~ 12.Utilize thermostatic drying chamber, described hydrothermal reaction kettle is heated to 160 DEG C of reactions 24 hours, then by reaction product eccentric cleaning 6 times, after drying, obtains presoma; By presoma 950 DEG C of thermal treatment 4 hours in chamber type electric resistance furnace.Finally obtain based on the product of two barium titanates.
Be that German Bruker company D8 type X-ray diffractometer carries out composition analysis to the material obtained by model, result is see Fig. 5.Fig. 5 is the X ray picture of material prepared by the embodiment of the present invention.As shown in Figure 5, material principal phase prepared by the present embodiment is two barium titanates, but has occurred content barium titanate (BaTiO more more than embodiment 2 simultaneously
3) and a small amount of microwave dielectric material Ba
4ti
13o
30.The change of preparation technology parameter cause obtained material purity comparatively embodiment 1 decrease.
Embodiment 4
Be the dried barium hydroxide (Ba (OH) of 99% by purity
2h
2o) 0.00248mol and purity be 98% sodium hydroxide (NaOH) 0.01984mol (mol ratio 1:8) mix in deionized water, obtain mixing solutions.Be the titanium tetrachloride (TiCl of 99.5% by purity in vacuum glove box
4) 0.00496mol (barium/titanium mol ratio 1:2) is added drop-wise in described mixing solutions, obtains reaction soln after stirring.Described reaction soln is poured in polytetrafluoroethyllining lining, regulate compactedness be 70% and pH value be put into hydrothermal reaction kettle after 12 ~ 13.Utilize thermostatic drying chamber, described hydrothermal reaction kettle is heated to 240 DEG C of reactions 72 hours, then by reaction product eccentric cleaning 6 times, after drying, obtains presoma; By presoma 1100 DEG C of thermal treatment 6 hours in chamber type electric resistance furnace.The thing finally obtained is mainly two barium titanates mutually.
Be that German Bruker company D8 type X-ray diffractometer carries out composition analysis to the material obtained by model, result is see Fig. 6.Fig. 6 is the X ray picture of material prepared by the embodiment of the present invention.As shown in Figure 6, material principal phase prepared by the present embodiment is two barium titanates, but simultaneously containing a small amount of ferroelectric material barium titanate (BaTiO
3) and Ba
6ti
17o
40.The change of preparation technology parameter cause obtained material purity comparatively embodiment 1 decrease.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
Claims (5)
1. hydrothermal method prepares the method for two barium titanates, includes following steps:
1) dried barium hydroxide and sodium hydroxide are mixed in deionized water, after fully stirring, obtain mixing solutions; The mol ratio of described dried barium hydroxide and sodium hydroxide is 1:6 ~ 10;
2) in vacuum glove box, titanium tetrachloride is added drop-wise to step 1) described in mixing solutions in obtain reaction soln; The mol ratio of described dried barium hydroxide and titanium tetrachloride is 1:1.8 ~ 2.1;
3) the described reaction soln configured is joined in polytetrafluoroethyllining lining, then liner is put into hydrothermal reaction kettle react;
4) by obtain after described reaction product eccentric cleaning, drying, obtain presoma;
5) by the thermal treatment in retort furnace of described presoma, obtain that there is ferroelectric material two barium titanate compared with high-curie temperature.
2. hydrothermal method according to claim 1 prepares the method for two barium titanates, it is characterized in that, step 2) regulate the pH value of described reaction soln to be 11-14.
3. hydrothermal method according to claim 1 prepares the method for two barium titanates, it is characterized in that, step 3) compactedness in described polytetrafluoroethyllining lining is 70%-80%.
4. hydrothermal method according to claim 1 prepares the method for two barium titanates, it is characterized in that, the temperature of described hydro-thermal reaction is 160 ~ 240 DEG C, and the time of described hydro-thermal reaction is 18 ~ 72 hours.
5. hydrothermal method according to claim 1 prepares the method for two barium titanates, it is characterized in that, described heat treated temperature is 900 ~ 1200 DEG C, and the described heat treated time is 3 ~ 6 hours.
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Cited By (5)
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| JP2017119607A (en) * | 2015-12-28 | 2017-07-06 | 株式会社サムスン日本研究所 | Dielectric body ceramic composition and method for producing the same, and ceramic electronic component |
| CN107644944A (en) * | 2017-09-12 | 2018-01-30 | 武汉华星光电半导体显示技术有限公司 | Flexible material and preparation method thereof, flexible cover plate and preparation method thereof |
| CN109704734A (en) * | 2018-09-30 | 2019-05-03 | 佛山市优特尔纺织实业有限公司 | A kind of internal combustion vehicle energy-saving coatings and preparation method thereof |
| CN110129772A (en) * | 2019-04-10 | 2019-08-16 | 广东省医疗器械研究所 | A kind of preparation method of barium titanate in-situ TEM |
| CN113788494A (en) * | 2021-10-27 | 2021-12-14 | 上海大学(浙江·嘉兴)新兴产业研究院 | Preparation method of barium dititanate |
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| JP2017119607A (en) * | 2015-12-28 | 2017-07-06 | 株式会社サムスン日本研究所 | Dielectric body ceramic composition and method for producing the same, and ceramic electronic component |
| CN107644944A (en) * | 2017-09-12 | 2018-01-30 | 武汉华星光电半导体显示技术有限公司 | Flexible material and preparation method thereof, flexible cover plate and preparation method thereof |
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| US10665824B2 (en) * | 2017-09-12 | 2020-05-26 | Wuhan China Star Optoelectronics Semiconductor Display Technology Co., Ltd. | Flexible material and preparation method thereof, flexible cover plate and preparation method thereof |
| CN109704734A (en) * | 2018-09-30 | 2019-05-03 | 佛山市优特尔纺织实业有限公司 | A kind of internal combustion vehicle energy-saving coatings and preparation method thereof |
| CN110129772A (en) * | 2019-04-10 | 2019-08-16 | 广东省医疗器械研究所 | A kind of preparation method of barium titanate in-situ TEM |
| CN110129772B (en) * | 2019-04-10 | 2021-06-22 | 广东省医疗器械研究所 | Preparation method of barium titanate in-situ coating |
| CN113788494A (en) * | 2021-10-27 | 2021-12-14 | 上海大学(浙江·嘉兴)新兴产业研究院 | Preparation method of barium dititanate |
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