CN106478089B - A kind of preferred orientation BaTiO3/SrTiO3The preparation method of nano composite ceramic - Google Patents
A kind of preferred orientation BaTiO3/SrTiO3The preparation method of nano composite ceramic Download PDFInfo
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Abstract
The invention discloses a kind of preferred orientation BaTiO3/SrTiO3The preparation method of nano composite ceramic, this method is using metatitanic acid, barium hydroxide and strontium hydroxide as raw material, using hydro-thermal method Optimizing Process Parameters, BT and ST ceramic powder is synthesized, through powder obtained by scanning electron microscope test interpretation of result all in nanoscale, green structure is laminated by curtain coating with template grain growth, and it is sintered to obtain composite ceramics by special process, it calculates and finds that the ceramics have certain orientation, the ceramics after polarization, piezoelectric constant (d33) larger, it can be used as a kind of lead-free piezoceramic material.
Description
Technical field
The invention belongs to nano ceramic material technical fields, in particular to a kind of preferred orientation BaTiO3/
SrTiO3The preparation method of nano composite ceramic.
Background technique
Nano material is the hot spot of present material research, due to the variation of its material structure in itself, scientists
It wishes to using this variation to obtain the novel of image height intensity metal or alloy and certain composite properties
Material.Nano ceramics is one kind of nano material, and people, which study it, starts from the eighties mid-term.So-called nano ceramics refers to
In the microstructure of ceramic material, crystal grain, crystal boundary and combination its size at least one dimension between them are in nanometer water
It is flat.This not only significantly improves the intensity, toughness and superplasticity of material, also overcomes many deficiencies of general ceramics, such as: crisp
Property big, processing difficulties etc..With the maturation of nanotechnology, researchers wish to using this technology come overcome ceramic material this
A little disadvantages.
What the excellent performance of ceramic material was mainly realized by its special chemical composition and microstructure.And this with
Each processing link of ceramics, such as: powder preparation solidifies and forms, is sintered and has important association；It can be said that any one
A processing link can all influence the final performance of ceramics.Powder preparation is used as the first step, is the preparation stage of raw material, powder characteristic
Quality (such as: partial size, purity) can directly affect ceramics structure and composition.The preparation method of nano-ceramic powder is according to synthesis
The reaction condition of powder is different, can be divided into vapor phase method, liquid phase method and solid phase method (Tian Mingyuan, Shi Er fear, Zhong Weizhuo, Pang Wenqin,
Guo Jingkun nano ceramics and nano ceramic powder [J] Journal of Inorganic Materials, 1998,13 (2): 131-137.).Molding is to burn
A process before knot, it is easy to reunite and lead to particle packing in biscuit since the partial size of nano-ceramic powder is small, therefore select proper
When forming method to preparation, to meet the biscuit of production requirement be vital.
Piezoelectric ceramics has very extensive purposes in modern functions ceramics.Currently, commercial piezoelectric ceramics is still with Pb
(Zr,Ti)O3(Hou Yudong, Cui Lei, Wang Sai, Wang Chao, Zhu Mankang, Yan Hui based on (lead zirconate titanate is abbreviated as PZT) sill
.BiAlO3Progress [J] Journal of Inorganic Materials of base high-temperature leadless piezoelectric ceramics, 2010,25 (3): 225-229.).But
Its raw material is based on PbO and has biggish toxicity, during production and recovery processing can health to the mankind and environment make
At very big injury.With the sustainable development of society, the leadless piezoelectric ceramics that has excellent performance is studied to replace lead base piezoelectricity to make pottery
Porcelain has great importance.Barium titanate is a kind of strong dielectric compound material, has ferroelectricity and piezoelectricity, but BaTiO3(BT)
Belong to the piezoelectric property material of medium rank, for the service performance for improving BT, researchers generally use two kinds of improved method (Lee
Electrical current research [J] the material Leader with texturing leadless piezoelectric ceramics of Hua Ping, Zhu Demei, Zhang Dongjie high pressure, 2010,
24:313-316.): it is 1. to mix oxide or with SrTiO3(ST) etc. it is added as the second constituent element.Wherein, strontium titanates exists
Manufacture ceramic capacitor, piezoceramic material, Ceramic sensible devices, microwave ceramics element are commonly used in ceramic field.And BT and
ST structure is close, and the position difference where the diffraction maximum of their X-ray diffractions (XRD) is little.2. being selection preferably preparation skill
Art, the technology that there is now include: traditional solid sintering technology, template grain growth (TGG) and reaction template grain growth method
(RTGG) etc..Wherein solid sintering technology is one of most common method, at low cost, manufacturing process is simple, but the period is long, and is made
Standby ceramic anisotropic degree out is low, therefore piezoelectric constant (d33) lower.
Summary of the invention
The present inventor has been devoted to the research of piezoelectric ceramics, and finds piezoelectric ceramics performance not only by crystal under study for action
Structure and chemical composition determine, are also influenced by ceramic internal microstructure, and if crystallographic axis is orientated in crystal grain, crystal grain crystallographic axis is by certain side
It is known as preferred orientation to arrangement, to enhance the piezoelectric property of ceramics.Therefore, the purpose of the present invention is to provide one kind preferentially to take
Tropism BaTiO3/SrTiO3The preparation method of nano composite ceramic.
In order to achieve the object of the present invention, inventor is with titanium dioxide (TiO2), barium hydroxide (Ba (OH)2·8H2O) and
Strontium hydroxide (Sr (OH)2·8H2O) it is raw material, using hydro-thermal method Optimizing Process Parameters, BT and ST ceramic powder is synthesized, through scanning
Powder obtained by electron microscope (SEM) test result analysis passes through curtain coating with template grain growth all in nanoscale
It is laminated into green structure, and is sintered to obtain composite ceramics by special process, calculates and finds that the ceramics have certain orientation, pole
Ceramics after change, piezoelectric constant (d33) larger.
Specifically, the object of the present invention is achieved like this: a kind of novel orientation BaTiO3/SrTiO3Nano combined pottery
The preparation method of porcelain, this method comprises the following steps:
(1) 1:(0.5-1 in mass ratio): (0.08-0.10) weighs nano-titanium dioxide, potassium hydroxide, hydroxide respectively
Lithium is added distilled water, reacts 18-24h in homogeneous reactor at 240-260 DEG C, product is washed with distilled water, is filtered,
It is dry, obtain KTLO crystal；
(2) KTLO crystal acid solution stir process 20-25h, uses H+Exchange K+And Li+, then it is washed with distilled water, acid
The metatitanic acid H of stratiform protonation has just been obtained after change processing1.07T1.73□0.27O4·H2O crystal (vacancy that is balancing charge), will
Obtained crystal uses distilled water and ethanol washing and drying respectively, obtains HT crystal；
(3) 1:(4.8-6.0 in mass ratio) HT crystal, barium hydroxide are weighed, distilled water is added, after mixing evenly,
10-16h is reacted at 190-210 DEG C in homogeneous reactor, filters, is washed with HAc solution to remove excessive hydrogen-oxygen after cooling
Change barium, is successively washed with distilled water and dehydrated alcohol, it is dry, barium titanate powder is obtained, it is spare；
(4) 1:(5.5-6.3 in mass ratio) HT crystal, strontium hydroxide are weighed, distilled water is added, after mixing evenly,
10-16h is reacted at 190-210 DEG C in homogeneous reactor, filters, is washed with HAc solution to remove excessive hydrogen-oxygen after cooling
Change strontium, is successively washed with distilled water and dehydrated alcohol, it is dry, strontium titanates powder is obtained, it is spare；
(5) 1:(0.9-1.1 in molar ratio) barium titanate powder, strontium titanates powder are weighed, with solvent, adhesive and plasticizing
Ball-milling reaction 18-30h is dried, tabletting, is sintered then by the slurry curtain coating of synthesis together for agent, and polarization obtains orientation
BaTiO3/SrTiO3Nano composite ceramic.
Preferably, novel orientation BaTiO as described above3/SrTiO3The preparation method of nano composite ceramic, wherein step
(1) nano-titanium dioxide in, potassium hydroxide, lithium hydroxide mass ratio be 1:(0.7-0.8): (0.08-0.09).
Preferably, novel orientation BaTiO as described above3/SrTiO3The preparation method of nano composite ceramic, wherein step
(2) HNO that the acid solution described in is 0.1-0.3mol/L3。
Preferably, novel orientation BaTiO as described above3/SrTiO3The preparation method of nano composite ceramic, wherein step
(3) HT crystal in, barium hydroxide mass ratio be 1:(4.8-5.0).
Preferably, novel orientation BaTiO as described above3/SrTiO3The preparation method of nano composite ceramic, wherein step
(4) HT crystal in, strontium hydroxide mass ratio be 1:(5.5-5.8).
In specific test example of the invention, novel orientation BaTiO as described above3/SrTiO3The system of nano composite ceramic
Preparation Method, the molar ratio of barium titanate powder and strontium titanates powder is preferably 1:1 in step (5).
In specific test example of the invention, novel orientation BaTiO as described above3/SrTiO3The system of nano composite ceramic
Preparation Method, solvent described in step (5) is preferably toluene: dehydrated alcohol volume ratio=6:4 mixed solution.
Preferably, novel orientation BaTiO as described above3/SrTiO3The preparation method of nano composite ceramic, wherein step
(5) adhesive described in is in polyvinyl acetate, polyvinyl butyral resin, polyacrylate, urea-formaldehyde resin adhesive
It is at least one.The plasticiser in dibutyl phthalate, polyvinyl alcohol, terpinol, carboxymethyl cellulose at least
It is a kind of.
In specific test example of the invention, novel orientation BaTiO as described above3/SrTiO3The system of nano composite ceramic
Preparation Method, sintering step technological parameter described in step (5) are preferred are as follows: first 500 DEG C are raised to from room temperature, constant temperature 3 hours,
Then 900 DEG C, constant temperature 3 hours are warming up to；Continue to be warming up to 1100 DEG C, constant temperature 3 hours；Finally, naturally cooling to room temperature.
It should be noted that novel orientation BaTiO of the present invention3/SrTiO3In nano composite ceramic preparation method,
Barium titanate (BaTiO3) and strontium titanates (SrTiO3) reaction principle during the preparation process are as follows:
TiO2+KOH+LiOH+H2O→K0.80Li0.27Ti1.73O4·xH2O(KTLO)
Above-mentioned character is the vacancy of balancing charge.
H1.08Ti1.73O4·H2O+Ba(OH)2·8H2O→BaTiO3+H2O
H1.08Ti1.73O4·H2O+Sr(OH)2·8H2O→SrTiO3+H2O
BaTiO3+SrTiO3→BaTiO3/SrTiO3
The technical effects of the invention are that: ceramic preferred orientation is to make the pottery of script disordered orientation by manufacture craft
Porcelain grain orientation reaches with the performance close to monocrystalline.The present invention makes matrix according to single crystalline templates particle by heat treatment
It is nucleated and is grown the microstructure oriented so as to cause one, piezoelectric constant is larger after polarization, can be used as a kind of unleaded pressure
Electroceramics material has great economy meaning.
Detailed description of the invention
Fig. 1: at 200 DEG C, HT and Ba (OH)2·8H2The XRD spectrum of the BT sample obtained after O reaction 12h.
Fig. 2: at 200 DEG C, HT and Ba (OH)2·8H2SEM of the BT obtained after O reaction 12h under different amplification
Figure, wherein (a) amplifies 50000 times, (b) 10000 times of amplification before sintering.
Fig. 3: at 200 DEG C, HT and Sr (OH)2·8H2The XRD spectrum of the ST sample obtained after O reaction 12h.
Fig. 4: at 200 DEG C, HT and Sr (OH)2·8H2SEM of the ST obtained after O reaction 12h under different amplification
Figure, wherein (a) amplifies 50000 times, (b) 6000 times of amplification before sintering.
Gained produces after Fig. 5: BT and ST mixes with 1:1 ratio and react respectively under 500-900-1100 DEG C of temperature hierarchy 3h
Product XRD diffraction pattern, wherein after (a) sintering, before (b) being sintered.
Fig. 6: BT and ST is blended under 500-900-1100 DEG C of temperature hierarchy with 1:1 ratio react 3h respectively after gained ceramics
With the XRD diffraction pattern of non-preferred orientation BT/ST composite ceramics.
Specific embodiment
Below by specific embodiment, invention is further described in detail.It will be apparent, however, to one skilled in the art, that
The following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.In addition, being not specified in embodiment specific
Technical operation step or condition person, described technology or conditions or according to product description according to the literature in the art
It carries out.Reagents or instruments used without specified manufacturer, being can be with conventional products that are commercially available.
The preparation of embodiment 1:HT crystal
Nano-titanium dioxide 6.9g, potassium hydroxide 5.1g, lithium hydroxide 0.6g are accurately weighed with electronic balance, measures distillation
Water 25mL reacts for 24 hours in homogeneous reactor at 250 DEG C in 50mL reaction kettle.After hydro-thermal process, by sample distilled water
Washing, filtering, drying, obtain K0.80Ti1.73Li0.27O4·xH2O (KTLO) crystal.The KTLO crystal is with 500mL concentration
The HNO of 0.2mol/L3Stir process for 24 hours, uses H+Exchange K+And Li+.Then it is washed with distilled water sample, acidification two is taken second place
The metatitanic acid H of stratiform protonation has just been obtained afterwards1.07T1.73□0.27O4·H2O crystal.Obtained crystal is used into distilled water and second respectively
Alcohol washing and the dry 12h in 60 DEG C of drying box, can obtain HT crystal.
Embodiment 2: the preparation of barium carbonate powder
0.1g metatitanic acid and 0.4927g barium hydroxide (excessive 50%) are accurately weighed, it is anti-that measurement 30mL distilled water is placed in 50mL
It answers in kettle, after mixing evenly, reacts 12h in homogeneous reactor at 200 DEG C.It is filtered after cooling, is with 10mL concentration
The HAc solution of 0.1mol/L is washed to remove excessive barium hydroxide, is successively washed with distilled water and dehydrated alcohol, and drying is standby
With.
The composition of barium carbonate powder, granularity, microstructure etc. are characterized using XRD, SEM, wherein use
The XRD of Ultima IV model carries out structure and crystal phase analysis, CuK α target, and the nm of λ=0.15418 scans tube voltage and tube current
Respectively 40kV, 40mA, scanning range are 3 °~60 °, and scanning speed is 5 °/min, and the resolution ratio of the SEM of sample pattern is
3.5nm, maximum amplification 300000, maximum acceleration voltage be 30kV, sample stage having a size ofAs a result as schemed
1, shown in Fig. 2.
Fig. 1 shows at 200 DEG C, HT and Ba (OH)2·8H2The XRD diagram of the BT sample obtained after O reaction 12h
Spectrum, all diffraction maximums of sample are all consistent with the standard diffraction card of cubic phase BT.Sample is all made of BT crystal phase, has no other
Crystal phase diffraction maximum, diffracted primary peak is stronger, and crystal property is good.Fig. 2 is that the SEM of made sample schemes, and as seen from the figure, sample is that have rule
Blocky geometrical body then, appearance are in short strip shape, average grain diameter 85nm.The above result of study shows at 200 DEG C, HT and Ba
(OH)2·8H2O reaction 12h can prepare partial size in nanoscale BT powder.
Embodiment 3: the preparation of Sr titanate powder
When producing strontium titanates, 0.1g metatitanic acid and 0.5534g strontium hydroxide (excessive 100%) are weighed, 30mL distilled water is measured
It is placed in 50mL reaction kettle, after mixing evenly, reacts 12h at 200 DEG C in homogeneous reactor, filtered after cooling, it is dense with 10mL
The HAc solution that degree is 0.1mol/L is washed to remove excessive strontium hydroxide, is successively washed with distilled water and dehydrated alcohol, dry
It is spare.
(the same embodiment of method is characterized to the composition of Sr titanate powder, granularity, microstructure etc. using XRD, SEM
2), as a result as shown in Figure 3, Figure 4.Fig. 3 shows at 200 DEG C, HT and Sr (OH)2·8H2It is obtained after O reaction 12h
The XRD spectrum of ST sample, all diffraction maximums of sample are all consistent with the standard diffraction card of cubic phase ST.Sample is all by ST crystal phase
Composition, has no other crystal phase diffraction maximums, main peak is stronger, and crystal property is good.Fig. 4 is that the SEM of made sample schemes, as seen from the figure, sample
Product are well-regulated blocky geometrical bodies, and appearance is in coccoid, average grain diameter 45nm.The above result of study shows at 200 DEG C
Under, HT and Sr (OH)2·8H2O reaction 12h can prepare partial size in nanoscale ST powder.Compared with BT, ST partial size ratio BT
Small nearly half.
Embodiment 4:BaTiO3/SrTiO3The preparation of nano composite ceramic
Barium titanate 0.78g and strontium titanates 0.62g are taken, with 3g solvent (toluene: dehydrated alcohol=6:4, volume ratio), 0.20g
3/4ths bottle volumes are added in the ball milling bottle of 20mL in polyvinyl acetate and 100 μ L dibutyl phthalates
Diameter is the Zirconia beads of 5mm, and ball milling is for 24 hours.Then the slurry of synthesis is layered in PET film with casting machine.After to be dried,
It is 15mm or so that film, which is taken off, and builds up long and width all, and 0.3MPa constant pressure lower sheeting 3min is set in tablet press machine, uses scissors
Surrounding is cut off, and its shape is trimmed to square or rectangle diaphragm.
Above-mentioned resulting diaphragm is placed on backing plate, is sintered in cabinet-type electric furnace, in sintering process, is first raised to from room temperature
500 DEG C, constant temperature 3 hours, then it is warming up to 900 DEG C, constant temperature 3-9 hours；Continue to be warming up to 1100-1300 DEG C, constant temperature 3 hours.
Finally, naturally cooling to room temperature with furnace.
(the same embodiment of method is characterized to the composition of Sr titanate powder, granularity, microstructure etc. using XRD, SEM
2), as a result as shown in Figure 5, Figure 6.Curve (a) and (b) respectively represent the XRD diagram picture after sintering and before sintering in Fig. 5；In Fig. 6 just
The diffraction peak of the non-preferred orientation BT/ST composite ceramics of representative of rectangular and triangle respectively, curve indicate ceramics after sintering
XRD diagram picture.It can be obtained by Fig. 5, the diffraction peak intensity in [110] direction is basically unchanged after sintering, other direction weakeneds.Sintering
Afterwards compared with standard diffraction peak, the diffraction peak intensity in [110] direction is remarkably reinforced.Other direction approximations are unchanged.According to reference
Document and Fig. 6 XRD diffraction patterns calculate the orientation of ceramics,
The orientation in this research calculating [110] direction.Wherein, ∑ I and ∑ I0Orientation and non orientation are respectively indicated
The sum of peak value of diffraction maximum of sample, taking the standard sample of BT and ST is respectively standard specimen JCPDS 31-0174 and standard specimen JCPDS
35—0734.It is computed, the degree of orientation of BT is 15-60% in ceramics, and the degree of orientation of ST is 25-80%.
Embodiment 5:BaTiO3/SrTiO3The polarization of nano composite ceramic
(1) Tu Yin.Silver paste is stirred evenly before coating, causes smooth surface, uniformity, and reserved insulation side, prevents
Only spill over.Then silver paste is dried in 60 DEG C of baking oven, partial solvent is made to volatilize, in order to avoid make silver layer peeling when silver ink firing.
Every face applies three times.
(2) silver ink firing.Degree burns half an hour more than 500, divides following several stages in detail: the first stage, main by room temperature to 350 DEG C
If the adhesive in silver ink firing slurry.There is a bulk gas generation in this stage, heating rate per hour preferably not more than 150~
200 DEG C, in order to avoid silver layer bubble or split.Second stage, 500 DEG C are raised to from 350 DEG C can be slightly fast, then constant temperature 30min.
(3) it polarizes.Safety system inspection is carried out first.It is boiled in silicone oil to bubble-free, then in the silicon of polarization
It polarizes in oil, poling temperature is exactly the temperature of silicone oil.It is then added to desired voltage and is kept for a period of time.Polarization knot
Shu Houyong wood tweezers take out sample toluene cleaning ceramic chip from polarization room, are wiped completely with cotton wool.It is placed after polarization
24h.Obtained ceramics with a thickness of 0.25-0.50mm, E is obtained by formulab=2.72d0.39, institute's making alive is 1.6-3.5kV.
Polarization time is 15-30 minutes.
The polarization of ceramics refer to ceramics under the action of strong dc electric field, the original polairzed area of disorientation, along electric field side
To ordered arrangement, the electricdomain after electric field removes in ceramic body still retains certain preferred orientation along direction of an electric field.In this way
It is originally that isotropic polycrystal (there is no the offsets of electric center of gravity, do not show piezoelectricity) becomes anisotropic polycrystal, from
And just ceramics is made to be provided with piezoelectric property.
Embodiment 6:BaTiO3/SrTiO3The measurement of nano composite ceramic piezoelectric property
Piezoelectric constant (d is tested using quasi-static method33).Test philosophy is applied on piezoelectric vibrator according to direct piezoelectric effect
Add a frequency to be far below the low-frequency alternating power of oscillator resonance frequency, generates alternation charge.When oscillator is in no External Electrical Field,
Meet electrical short condition, only along when being parallel to polarization direction stress, piezoelectric equations can be reduced to
D3=d33T33That is d33=D3/T3=Q/F
In formula: D3Dielectric displacement component, pC/m2；
T3Longitudinal stress, N/m2；
d33Longitudinal piezoelectric strain constant, pC/N or pm/V；
The piezoelectric charge of Q- oscillator release, C；
The longitudinal direction F- low-frequency alternating power, N.
Through detecting, for composite ceramics prepared by embodiment 4 after polarizing, measuring piezoelectric constant is 178pC/N.
Claims (9)
1. a kind of orientation BaTiO3/SrTiO3The preparation method of nano composite ceramic, which is characterized in that this method includes as follows
Step:
(1) 1:(0.5-1 in mass ratio): (0.08-0.10) weighs nano-titanium dioxide, potassium hydroxide, lithium hydroxide respectively, adds
Enter distilled water, react 18-24h in homogeneous reactor at 240-260 DEG C, product is washed with distilled water, filter, is dried,
Obtain KTLO crystal；
(2) KTLO crystal acid solution stir process 20-25h, uses H+Exchange K+And Li+, then it is washed with distilled water, at acidification
The metatitanic acid H of stratiform protonation has just been obtained after reason1.07T1.73□0.27O4·H2O crystal, by obtained crystal use respectively distilled water and
Ethanol washing and drying obtain HT crystal；
(3) 1:(4.8-6.0 in mass ratio) HT crystal, barium hydroxide are weighed, distilled water is added, after mixing evenly, in 190-210
It reacts 10-16h at DEG C in homogeneous reactor, is filtered after cooling, washed with HAc solution to remove excessive barium hydroxide, according to
It is secondary to be washed with distilled water and dehydrated alcohol, it is dry, barium titanate powder is obtained, it is spare；
(4) 1:(5.5-6.3 in mass ratio) HT crystal, strontium hydroxide are weighed, distilled water is added, after mixing evenly, in 190-210
It reacts 10-16h at DEG C in homogeneous reactor, is filtered after cooling, washed with HAc solution to remove excessive strontium hydroxide, according to
It is secondary to be washed with distilled water and dehydrated alcohol, it is dry, strontium titanates powder is obtained, it is spare；
(5) 1:(0.9-1.1 in molar ratio) barium titanate powder, strontium titanates powder are weighed, with solvent, adhesive and plasticiser one
Ball-milling reaction 18-30h is played, is then cast the slurry of synthesis, dry, tabletting is sintered, and polarization obtains orientation BaTiO3/
SrTiO3Nano composite ceramic；
Sintering step technological parameter described in step (5) are as follows: be first raised to 500 DEG C from room temperature, constant temperature 3 hours, be then warming up to
900 DEG C, constant temperature 3-9 hours；Continue to be warming up to 110-1300 DEG C, constant temperature 3 hours；Finally, naturally cooling to room temperature.
2. orientation BaTiO according to claim 13/SrTiO3The preparation method of nano composite ceramic, which is characterized in that step
Suddenly nano-titanium dioxide in (1), potassium hydroxide, lithium hydroxide mass ratio be 1:(0.7-0.8): (0.08-0.09).
3. orientation BaTiO according to claim 13/SrTiO3The preparation method of nano composite ceramic, which is characterized in that step
Suddenly acid solution described in (2) is the HNO of 0.1-0.3mol/L3。
4. orientation BaTiO according to claim 13/SrTiO3The preparation method of nano composite ceramic, which is characterized in that step
Suddenly HT crystal in (3), barium hydroxide mass ratio be 1:(4.8-5.0).
5. orientation BaTiO according to claim 13/SrTiO3The preparation method of nano composite ceramic, which is characterized in that step
Suddenly HT crystal in (4), strontium hydroxide mass ratio be 1:(5.5-5.8).
6. orientation BaTiO according to claim 13/SrTiO3The preparation method of nano composite ceramic, which is characterized in that step
Suddenly the molar ratio of barium titanate powder and strontium titanates powder is 1:1 in (5).
7. orientation BaTiO according to claim 13/SrTiO3The preparation method of nano composite ceramic, which is characterized in that step
Suddenly solvent described in (5) is toluene: dehydrated alcohol volume ratio=6:4 mixed solution.
8. orientation BaTiO according to claim 13/SrTiO3The preparation method of nano composite ceramic, which is characterized in that step
Suddenly adhesive described in (5) is in polyvinyl acetate, polyvinyl butyral resin, polyacrylate, urea-formaldehyde resin adhesive
At least one.
9. orientation BaTiO according to claim 13/SrTiO3The preparation method of nano composite ceramic, which is characterized in that step
Suddenly plasticiser described in (5) in dibutyl phthalate, polyvinyl alcohol, terpinol, carboxymethyl cellulose at least one
Kind.
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| CN101921106A (en) * | 2010-06-29 | 2010-12-22 | 上海大学 | Preparation method of (Ba, Sr)TiO3 nanometer/micrometer/nanometer laminated structure ceramics |
| CN104609856A (en) * | 2015-01-30 | 2015-05-13 | 同济大学 | Preparation method of highly preferred oriented sodium bismuth titanate-barium titanate lead-free piezoelectric thin film |
| CN105948735A (en) * | 2016-04-28 | 2016-09-21 | 山东大学 | Synthesis method of SrTiO3 heterogeneously coated BaTiO3 ultrafine nano-powder |
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| CN104609856A (en) * | 2015-01-30 | 2015-05-13 | 同济大学 | Preparation method of highly preferred oriented sodium bismuth titanate-barium titanate lead-free piezoelectric thin film |
| CN105948735A (en) * | 2016-04-28 | 2016-09-21 | 山东大学 | Synthesis method of SrTiO3 heterogeneously coated BaTiO3 ultrafine nano-powder |
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