CN108178616A - A kind of method for preparing the ceramics containing bismuth oxide-based layered perovskite - Google Patents
A kind of method for preparing the ceramics containing bismuth oxide-based layered perovskite Download PDFInfo
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Abstract
The invention discloses a kind of method for preparing the ceramics containing bismuth oxide-based layered perovskite, the present invention mixes reaction oxide with fused salt in certain proportion, and heating after mixing melts salt therein, and reactant is reacted in salt, you can obtains reaction product.Fused salt therein, which is cleaned, after cooling obtains powder.This method can reduce the required temperature of reaction, it is only necessary to reach the fusing point of fused salt therein, while can also reduce the reaction required time, along with easy to operate.The sample with high c-axis preferred orientation has been obtained on this basis.
Description
Technical field
Present invention relates particularly to a kind of methods for preparing the ceramics containing bismuth oxide-based layered perovskite.
Background technology
Multi-iron material because at least while have ferroelectric order, ferromagnetic ordering and iron bullet it is orderly in two kinds orderly, and passing
There is great basic physics meaning in the practical applications such as sensor, brake, multistate memory.
Bismuth system lamellar structure compound (BLSFs) is a kind of potential single phase multi-iron material family.The general formula of BLSFs structures
It can be expressed as (Bi2O2)(Am-1BmO3m+1), wherein, A is usually the larger monovalence of ionic radius, divalent or trivalent ion, such as：
Ba2+, Pb2+, Sr2+, Ca2+, Bi3+Deng generally taking up the position between titanyl octahedral body；The smaller tetravalence of B expression ionic radius,
Pentavalent or sexavalence ion, such as：Fe3+, Mn3+, Ti4+, V5+, Nb5+, Ta5+, W6+Deng generally taking up titanyl octahedral body inside center position
It puts；M is generally the integer between 1~5, represents adjacent two layers bismuth oxygen layer (Bi in a structure cell2O2)2+Between folded along c-axis direction
The number of plies of the oxygen octahedra added.Bismuth oxygen layer (Bi2O2)2+Structure is stablized relatively, is not easy to be doped element substitution.Total is by class
Calcium titanium ore bed (Am-1BmO3m+1)2-With bismuth oxygen layer (Bi2O2)2+It alternates and stacks along c-axis direction as sandwich.
For ceramic material, using certain micro-structure control measures, make in ceramic material microstructure it is each to
Different in nature crystal grain is realized to carry out regularly arranged or occurs orientation probability increase in those directions along certain specific directions, in this way
The ceramics prepared are exactly the textured ceramic for having preferred orientation.Preparation about BLSFs textured ceramics at present, substantially have with
Lower several method：(1) hot-working process, such as be hot-forged, hot pressing or superplastic deformation；(2) by silk-screen printing be aligned crystal seed or
Being cast or suppress under high pressure makes flaky crystalline grain deflection alignment, then carries out pressureless sintering；(3) apply when being sintered greatly outer
Add magnetic field.Above method is used, although textured ceramic can be prepared, texture microstructure is nearly all the side in external drive
Help it is lower could be formed, this results in complicated, of high cost, to equipment the requirement of preparation process also higher, in many cases, prepares
The ceramic degree of orientation actual demand is also not achieved.Therefore, it how with simple method, with relatively low cost, prepares with height
The BLFs textured ceramics (BNdT, BTF) of preferred orientation, are a problem to be solved.
Forged method refers to that applying uniaxial tension in sintering process makes nonequiaxial crystal grain deflect to have ceramics
A certain particular orientation.In sintering process, due to the sintering aid often containing some low melting points, these substances occur at high temperature
Melting.Under the action of ambient pressure, ceramic body is extending on pressure direction, is received on pressure direction is parallel to
Contracting.Along with this deformation, under the current lubrication collective effect of external force and liquid phase, crystal grain is deflected and is slid so that
Crystal grain has obtained oriented alignment.Simultaneously because crystal grain can also grow up in sintering process so that some small crystalline substances irregularly arranged
Grain depends on big crystal grain and grows up, so as to which global orientation arranges.Fig. 1 (a) and (b) are Takenaka T[5]Et al. use forged
Method, preparing has c-axis preferred orientation Bi4Ti3O12The equipment schematic diagram of ceramics, each alphabetical meaning is A in Fig. 1 (a)：Resistance furnace,
B：Sample, C, C'：Platinum sheet, D, D'：Aluminum pan, E, E'：Aoxidize aluminum piston, F：Thermocouple, G：Heater, H：Unidirectional pressure lotus；
Each numerology is 1 in Fig. 1 (b)：Resistance furnace, 2：Guider, 3：Control-rod, 4：Counterweight, 5：Jack, 6：Dial, 7：
Plug.Fig. 1 (c) is forged sintering process curve, wherein sintering temperature Tm, soaking time tp, sintering time taWith pressure PhIt is all right
The orientation of final sample has a major impact.Fig. 1 is it is found that complicated, with high costs, to the sample degree of orientation the shadow of forged method Preparation equipment
Ring that factor is various and low production efficiency.Molten-salt growth method used in this patent can solve problem above.First, molten-salt growth method institute
The equipment used is needed to include balance, planetary ball mill, tube furnace, drying box, tablet press machine.These equipment are all common set
It is standby, use also fairly simple convenience.Secondly, experimentation to reaction condition there is no particular/special requirement, than such as whether vacuum
Atmosphere sintering needs impressed pressure etc..
Suzuki etc. is prepared for the BTF that there is a to be orientated ceramics, sample preparation procedure with the electrophoretic deposition that high-intensity magnetic field assists
Schematic diagram is shown in Figure 2.The BTF powder sintered is dispersed in stable colloidal suspension liquid first, by additional
12T high-intensity magnetic fields make powder particle unanimously be arranged along ab planes, then deposit to the powder particle in colloid by applying electric field
On the electrode of colloid bottom, after disposing colloid, crystal grain is in face of together, being calcined powder along ab in the powder base deposited on electrode
Base is ceramic with regard to that can obtain having the BTF of a axle preferrel orientations.According to this method experiment flow it is found that experimentation is complex, if
Standby investment is higher, and Master Cost is not also cheap, needs high-intensity magnetic field and electric field-assisted, more demanding to experiment condition.
Invention content
For above-mentioned background technology there are the problem of, the present invention is intended to provide it is a kind of prepare containing bismuth oxide-based layered perovskite ceramics
Method.
For this purpose, the present invention uses following technical scheme：A kind of method for preparing the ceramics containing bismuth oxide-based layered perovskite, feature
It is,
Step 1：Reaction oxide is mixed to pour into fused salt with certain mass ratio, ball milling, salt are carried out in ball grinder
Mainly play a part of reaction medium either solvent, the contact that can be effectively promoted between reactant, and then be conducive to
The progress of reaction, then dries slurry；
Step 2：Mixed raw material after drying is calcined, the blocky powder after calcining is carried out with hot deionized water
Cleaning
Heating melts salt therein after mixing, and reactant is reacted in salt, obtains reaction product；Cool down it
After clean fused salt therein and obtain powder；
Step 3：By the mold compression moulding of the powder after drying, then the powder base sample suppressed is placed in stove and is burnt
Knot, and 500 DEG C are risen to 100 DEG C/h of speed, it is kept for 1 hour in the temperature, finger is risen to 5 DEG C/min of speed later
Determine sintering temperature, kept for 4 hours in predetermined sintering temperature, program determination after heat preservation, sample cools to room temperature with the furnace, completes
It prepares.
As the supplement to above-mentioned technical proposal and perfect, the invention also includes following technical characteristics.
The fused salt is divided into two classes：One kind is metal or alloy melt (being usually Ga, In and Sn etc.)；Another kind of being
Species are closed, including oxide and salt (such as PbO, NaCI and K2SO4Deng).
The ball grinder of step 1 is agate jar.
The step 1 raw material adds in absolute ethyl alcohol to ball grinder, is then first carried out with glass bar before upper ball mill
Stirring, the quantity of ball are paved with two layers, and 2nd/1 to three/3rds of the volume of jar is accounted for after the mixing of ball material.
Ball milling is carried out using planetary ball mill in the step 1, parameters are set as：Unidirectional timing operates, the time
It it is 12 hours, operating frequency is 20 hertz.
The mixed raw material after drying first in mortar is ground 5 to 10 minutes in the step 2, is subsequently poured into aluminium oxide
It in crucible, is put into batch-type furnace and carries out pre-burning, calcined temperature is 650 DEG C, and sintering atmosphere is air.Temperature-rise period is every according to 5 DEG C
Minute setting reaches stove program determination after predetermined temperature keeps the temperature 4 hours, sample furnace cooling to room temperature.
The deionized water of the blocky powder heat after pre-burning is cleaned in the step 2, on the one hand can dissolve powder
On the other hand material can also play the role of cleaning fused salt, after being completely dissolved block, by slurry pour into ball grinder ball milling with
The higher powder of activity is obtained, Ball-milling Time is 4 hours, and the slurry after ball milling further cleans fused salt with deionized water, is used
AgNO3Solution is titrated, and whether detection fused salt detaches completely, and then drying obtains powder.
It needs to grind before molding in the step 3, PVA is instilled in pre-burning powder, in order to which PVA is made to be mixed with pre-burning powder
It obtains evenly, needs to add in 10ml alcohol, after mixing dry tabletting again.
By the stainless steel mould compression moulding of the powder after drying, under the pressure of 240 megapascal, compacting in the step 3
Into diameter 1cm, thickness is in the slice, thin piece of 0.1cm or so.
It by the powder base sample to suppressing in the step 3, is placed on corundum plate, while one layer is padded on corundum plate
The identical powder of ingredient runs program, 500 is risen to from room temperature with 100 DEG C/h of speed to avoid pollution, setting tube furnace
DEG C, it is kept for 1 hour in the temperature, this process is for dumping；Specified sintering temperature is risen to 5 DEG C/min of speed later,
BTF sintering temperatures are 850 DEG C, and the sintering temperature of BNdT is 1100 DEG C, is kept for 4 hours, kept the temperature in predetermined sintering temperature respectively
Program determination after finishing, sample cool to room temperature with the furnace.
The present invention can reach following advantageous effect：Molten-salt growth method of the present invention is easy to operate, and experimental period is short, goes out sample efficiency
It is high, it is often more important that the sample with high c-axis preferred orientation can be prepared.The equipment that the molten-salt growth method of the present invention is used all is common
Equipment, including balance, planetary ball mill, tube furnace, drying box, tablet press machine, these equipment operations are simple and convenient.Secondly, it melts
The experimentation of salt method does not need to increase other subsidiary conditions, than such as whether needing to add magnetic field electric field etc..The method energy of the present invention
Enough reduce reacts required temperature, it is only necessary to reach the fusing point of fused salt therein, while can also reduce needed for reaction
The time wanted prepares the powder with given activity.
Description of the drawings
Fig. 1 is the schematic diagram of existing forged method.
Fig. 2 is the schematic diagram of existing high-intensity magnetic field auxiliary law.
Fig. 3 is the flow diagram of the present invention.
Fig. 4 is the XRD diagram of the BNdT and BTF of the present invention
Specific embodiment
The specific embodiment of the present invention is described in detail below in conjunction with the accompanying drawings.
As shown in figure 3, specific embodiments of the present invention are as follows：
(1) selection of raw material
Shown in table 1.
1 experimental raw of table and place of production information
(2) ball grinder is cleaned
Ball grinder is agate jar used in experimentation, after tap water simply cleans, is poured into ball grinder
Suitable deionized water using planetary ball mill ball milling 4 hours, is taken out to be rinsed with deionized water again and is dried up.
(3) dispensing
It is expected that obtaining 10g powder samples, oxide is prepared according to stoichiometric ratio：In view of long-time high-temperature burning process
Middle Bi2O3It is volatile, therefore increase Bi2O315% (mass percent) of stoichiometric ratio is compensated, fused salt choose KCl and
NaCl, according to molar ratio KCl:NaCl=1:1 prepares.
(4) it mixes
The oxide weighed and fused salt are poured into ball grinder, then add in 10g absolute ethyl alcohols in ball grinder, the number of ball
Amount is desirable to be paved with two layers, and ball material mixed volume accounts for 2nd/1 to three/3rds of ball grinder, and egg one is beaten with glass bar picture
After sample is stirred solution, ball milling is carried out using planetary ball mill, parameters are set as, unidirectional periodically to operate, and the time is
12 hours, operating frequency was 20 hertz, and separation slurry, which is put into drying box, after treating dries.
(5) pre-burning
Mixed raw material after drying first in mortar is ground 5 to 10 minutes, is subsequently poured into alumina crucible, is put into case
Pre-burning is carried out in formula stove, calcined temperature is 650 DEG C, and sintering atmosphere is air.Temperature-rise period is reached according to 5 DEG C of settings per minute
Stove program determination after predetermined temperature keeps the temperature 4 hours, sample furnace cooling to room temperature.
(6) separation fused salt is with crushing
The deionized water of blocky powder heat after pre-burning is cleaned, on the one hand can dissolve powder, on the other hand
Also it can play the role of cleaning fused salt, after being completely dissolved block, slurry is poured into ball grinder ball milling to obtain activity more
High powder, Ball-milling Time are 4 hours, and the slurry after ball milling further cleans fused salt with deionized water, uses AgNO3Solution carries out
Whether titration, detection fused salt detach completely, and then drying obtains powder.
(7) it is molded
It needs to grind before molding, instills PVA in pre-burning powder, in order to which PVA is made to mix evenly with pre-burning powder, need
10ml alcohol is added in, after mixing dry tabletting again.By the stainless steel mould compression moulding of the powder after drying, 240,000,000
Under the pressure of pa, it is pressed into diameter 1cm, for thickness in the slice, thin piece of 0.1cm or so, some are difficult to the powder of compression moulding in film-making
A small amount of binder PVA can be added in the process.
(8) it is sintered
It to the powder base sample suppressed, is placed on corundum plate, while the identical powder of a composition of layer is padded on corundum plate
To avoid pollution, setting tube furnace runs program, and 500 DEG C are risen to from room temperature with 100 DEG C/h of speed, and 1 is kept in the temperature
Hour, this process is for dumping；Specified sintering temperature is risen to 5 DEG C/min of speed later, BTF sintering temperatures are 850
DEG C, the sintering temperature of BNdT is 1100 DEG C, is kept for 4 hours in predetermined sintering temperature respectively, program determination after heat preservation, sample
Cool to room temperature with the furnace.
Here is that we are used to calculate the formula of the degree of orientation：
Pc=[∑ I (00k)]/[∑ I (hlk)] × 100%
∑ I (00k) represents the sum of the relative peak intensities in all (00k) directions in formula, and ∑ I (hlk) represents all (hlk) side
To the sum of relative peak intensities.
Compared with the relative intensity of standard card, the highest peak of BNdT is no longer (117), and the highest peak of BTF is no longer
(119), the relative intensity at (00l) peak is remarkably reinforced, this shows that the ceramic powders have c-axis preferred orientation, by calculating BNdT
The degree of orientation LF=0.988, BTF degree of orientation LF=0.926.
For the crystal grain of powder sample into discoid, the crystal grain of cross-sectional sample is strip.Bismuth system Aurivillius stratiform chemical combination
The crystal structure of object is by very strong anisotropy, and lattice constant c is than a, and b will be grown very much, and the growth rate along each axis direction is not
With, which results in the generation of nonequiaxial crystal grain, finally formed crystal grain is generally sheet or plate-like, along die thickness direction
For c-axis direction.Having been reacted in Fig. 4 with sample prepared by molten-salt growth method there is high c to be orientated.
Brief summary：Molten-salt growth method is that a kind of oxide that will react mixes in certain proportion with fused salt, and heating after mixing makes
Salt fusing therein, reactant are reacted in salt, you can obtain reaction product.Fused salt therein is cleaned after cooling to obtain
Powder.This method can reduce the required temperature of reaction, it is only necessary to reach the fusing point of fused salt therein, while also can
The required time is reacted in enough reductions, along with easy to operate.The sample with high c-axis preferred orientation has been obtained on this basis
Product.
The basic principles, main features and the advantages of the invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
1. a kind of method for preparing the ceramics containing bismuth oxide-based layered perovskite, it is characterized in that,
Step 1：Reaction oxide is mixed to pour into fused salt with certain mass ratio, ball milling is carried out in ball grinder, then will
Slurry is dried；
Step 2：Mixed raw material after drying is calcined, the blocky powder after calcining is cleaned with hot deionized water,
Heating melts salt therein after mixing, and reactant is reacted in salt, obtains reaction product, it is cleaned after cooling
In fused salt dry to obtain powder；
Step 3：By the mold compression moulding of the powder after drying, then the powder base sample suppressed is placed in stove and is sintered, and
500 DEG C are risen to 100 DEG C/h of speed, is kept for 1 hour in the temperature, specified burning is risen to 5 DEG C/min of speed later
Junction temperature is kept for 4 hours, program determination after heat preservation in predetermined sintering temperature, and sample cools to room temperature with the furnace, completes system
It is standby.
2. a kind of method for preparing the ceramics containing bismuth oxide-based layered perovskite according to claim 1, it is characterized in that, the fused salt
It is divided into two classes：One kind is metal or alloy melt；Another kind of is compounds, including oxide and salt.
3. a kind of method for preparing the ceramics containing bismuth oxide-based layered perovskite according to claim 1, it is characterized in that, the ball of step 1
Grinding jar is agate jar.
4. a kind of method for preparing the ceramics containing bismuth oxide-based layered perovskite according to claim 1, it is characterized in that, the step 1
Raw material adds in absolute ethyl alcohol to ball grinder, is then first stirred with glass bar, the quantity of ball is paved with two before upper ball mill
Layer accounts for 2nd/1 to three/3rds of the volume of jar after the mixing of ball material.
5. a kind of method for preparing the ceramics containing bismuth oxide-based layered perovskite according to claim 4, it is characterized in that, the step 1
Middle to carry out ball milling using planetary ball mill, parameters are set as：Unidirectional timing operates, and the time is 12 hours, operating frequency
It is 20 hertz.
6. a kind of method for preparing the ceramics containing bismuth oxide-based layered perovskite according to claim 1 or 5, it is characterized in that, the step
The mixed raw material after drying first in mortar is ground 5 to 10 minutes in rapid two, is subsequently poured into alumina crucible, is put into box
Pre-burning is carried out in stove, calcined temperature is 650 DEG C, and sintering atmosphere is air；Temperature-rise period reaches pre- according to 5 DEG C of settings per minute
Determine stove program determination after 4 hours of temperature, sample furnace cooling to room temperature.
7. a kind of method for preparing the ceramics containing bismuth oxide-based layered perovskite according to claim 6, it is characterized in that, the step 2
The deionized water of the middle blocky powder heat by after pre-burning is cleaned, and after being completely dissolved block, slurry is poured into ball milling
Ball milling is to obtain the higher powder of activity in tank, and Ball-milling Time is 4 hours, and the slurry after ball milling is further cleaned with deionized water
Fused salt uses AgNO3Solution is titrated, and whether detection fused salt detaches completely, and then drying obtains powder.
8. a kind of method for preparing the ceramics containing bismuth oxide-based layered perovskite according to claim 1 or 7, it is characterized in that, the step
It needs to grind before molding in rapid three, instills PVA in pre-burning powder, in order to which PVA is made to mix evenly with pre-burning powder, need to add
Enter 10ml alcohol, after mixing dry tabletting again.
9. a kind of method for preparing the ceramics containing bismuth oxide-based layered perovskite according to claim 8, it is characterized in that, the step 3
The stainless steel mould compression moulding of the middle powder by after drying, under the pressure of 240 megapascal, is pressed into diameter 1cm, thickness exists
The slice, thin piece of 0.1cm.
10. a kind of method for preparing the ceramics containing bismuth oxide-based layered perovskite according to claim 9, it is characterized in that, the step
By the powder base sample to suppressing in three, be placed on corundum plate, at the same pad on corundum plate the identical powder of a composition of layer with
It avoids polluting, setting tube furnace runs program, and 500 DEG C are risen to from room temperature with 100 DEG C/h of speed, small in temperature holding 1
When；Specified sintering temperature is risen to 5 DEG C/min of speed later, is kept for 4 hours in predetermined sintering temperature respectively, heat preservation finishes
Program determination afterwards, sample cool to room temperature with the furnace.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109444464A (en) * | 2018-12-21 | 2019-03-08 | 中国电子科技集团公司第四十九研究所 | A kind of high-temperature piezoelectric ceramic sensor element |
| CN109678503A (en) * | 2019-01-07 | 2019-04-26 | 陕西科技大学 | It is a kind of it is difficult to understand in the single-phase multiferroic powder body material of viral this structure, textured ceramics and preparation method thereof |
| WO2020125483A1 (en) * | 2018-12-17 | 2020-06-25 | 深圳先进技术研究院 | Preparation method for metal oxide or composite material thereof, metal oxide or composite material and application thereof, and battery |
| CN113797932A (en) * | 2021-10-13 | 2021-12-17 | 陕西科技大学 | Doped bismuth niobate titanate nanosheet and preparation method thereof |
| CN113797919A (en) * | 2021-10-13 | 2021-12-17 | 陕西科技大学 | High-exposure {001} crystal face bismuth niobate titanate nanosheet piezoelectric catalyst and preparation method and application thereof |
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2018
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020125483A1 (en) * | 2018-12-17 | 2020-06-25 | 深圳先进技术研究院 | Preparation method for metal oxide or composite material thereof, metal oxide or composite material and application thereof, and battery |
| CN109444464A (en) * | 2018-12-21 | 2019-03-08 | 中国电子科技集团公司第四十九研究所 | A kind of high-temperature piezoelectric ceramic sensor element |
| CN109678503A (en) * | 2019-01-07 | 2019-04-26 | 陕西科技大学 | It is a kind of it is difficult to understand in the single-phase multiferroic powder body material of viral this structure, textured ceramics and preparation method thereof |
| CN113797932A (en) * | 2021-10-13 | 2021-12-17 | 陕西科技大学 | Doped bismuth niobate titanate nanosheet and preparation method thereof |
| CN113797919A (en) * | 2021-10-13 | 2021-12-17 | 陕西科技大学 | High-exposure {001} crystal face bismuth niobate titanate nanosheet piezoelectric catalyst and preparation method and application thereof |
| CN113797919B (en) * | 2021-10-13 | 2024-03-08 | 陕西科技大学 | High-exposure {001} crystal face bismuth titanate niobate nanosheet piezoelectric catalyst and preparation method and application thereof |
| CN113797932B (en) * | 2021-10-13 | 2024-03-08 | 陕西科技大学 | Doped bismuth titanate niobate nanosheets and preparation method thereof |
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Application publication date: 20180619 |