CN104557038B - A kind of compound system pyroelectric ceramic material and preparation method thereof - Google Patents
A kind of compound system pyroelectric ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of compound system pyroelectric ceramic material and preparation method thereof, the chemical general formula of the material is:Pb{[(Me1/3Nb2/3)x(W1/3Fe2/3)1‑x]y(Zr0.9Ti0.1)1‑y}O3‑nMe’;Wherein, Me is the one kind in Mg or Zn;X, y represent molar fraction, 0.125≤x≤0.875,0.08≤y≤0.11 respectively;Me ' is modifying element, is one or more in Li, La or Sb, and its molar ratio range is 0mol%≤n≤5mol%.The compound system pyroelectric ceramic material that the present invention is provided, with pyroelectric coefficient and adjustable dielectric properties higher, thus has preferable application prospect in various pyroelectric detectors.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of new four-element complex system pyroelectric ceramic material and its
Preparation method.
Background technology
Pyroelectricity material can be used for Infrared Detectors, infrared radiation thermometer and video camera etc., and these equipment are in flame detecting, ring
The fields such as border pollution monitoring, non-contact type temperature measurement, medical diagnosis, industrial process are monitored automatically, Security alert obtain extensively
General application.
The use of more extensive pyroelectric ceramics is at present rich zirconium type lead zirconate titanate (PZT).But the material at low temperature ferroelectricity
Rhombohedral phase (FRL) arrive high temperature ferroelectricity rhombohedral phase (FRH) first order phase change temperature range it is narrow (2~3 DEG C), this is unfavorable for it infrared
Application in terms of detection.The ceramic material with different phase transition temperatures is added to be made compound system, expansible this F in PZTRL-
FRHTransition temperature range, is a kind of effective way for improving its pyroelectricity material performance.Lead iron tungstate Pb (W1/3Fe2/3)O3
(PFW) be a kind of ferroelectric material of complex perovskite structure, with typical Relaxation Ferroelectrics characteristic, its dielectric constant compared with
Greatly, phase transition temperature range is wide, and with relatively low sintering temperature (Current Applied Physics 2011, Vol 11,
S154-S156).Similar with this effect also has Pb (Mg1/3Nb2/3)O3And Pb (Zn (PMN)1/3Nb2/3)O3(PZN), these systems
Continuous solid solution can be all formed with PZT.Therefore being combined with rich zirconium type binary PZT using a small amount of the graduates of three governmental examinations quaternary system can
Modified polynary system pyroelectricity material is prepared, and these materials can obtain adjustable in certain limit by the adjustment of different component
The comprehensive electrical performance of control, so as to different composite requests of the different pyroelectric electric devices to performance can be met.In addition, composition is appropriate
Multivariate solid solution system can also obtain the ceramics of densification in sintering range wider.
However, releasing electrostrictive coefficient and the adjustable new quaternary composite construction pyroelectric ceramics body of electrical property with higher thermal at present
System is but very limited.
The content of the invention
The embodiment of the invention provides a kind of compound system pyroelectric ceramic material and preparation method thereof.What the present invention was provided
Compound system pyroelectric ceramic material, with pyroelectric coefficient and adjustable dielectric properties higher, thus in various pyroelectricities
There is preferable application prospect in detector.
In a first aspect, the embodiment of the invention provides a kind of compound system pyroelectric ceramic material and preparation method thereof, institute
The chemical general formula for stating material is:
Pb{[(Me1/3Nb2/3)x(W1/3Fe2/3)1-x]y(Zr0.9Ti0.1)1-y}O3-nMe’;
Wherein, Me is the one kind in Mg or Zn;X, y represent molar fraction respectively, 0.125≤x≤0.875, and 0.08≤y≤
0.11;Me ' is modifying element, is one or more in Li, La or Sb, and its molar ratio range is 0mol%≤n≤5mol%.
Second aspect, the embodiment of the invention provides a kind of system of the pyroelectric ceramic material as described in above-mentioned first aspect
Preparation Method, the preparation method includes:
By Fe2O3And WO3By 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made FeWO4Precursor
Material, and by MgO and Nb2O5Or ZnO and Nb2O5One of which press 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying
Mill, is made MgNb2O6Or ZnNb2O6Presoma powder;
By Pb3O4、ZrO2、TiO2、FeWO4Presoma powder, MnNb2O6Or ZnNb2O6Presoma powder, modifying element Me '
Oxide or salt according to the chemical general formula described in the claims 1 molar ratio weighing, then mixing and ball milling, is starched
Material;
Pre-burning will be carried out after slurry drying, sieving, and the block that the pre-burning is obtained ball milling again;
The slurry drying that will be obtained after ball milling again obtains powder, adds polyvinyl alcohol (PVA) to bond in the powder
Agent is ground granulation, and ageing is sieved after placing, and obtains powder;
By the powder pressing into ceramic body;
To be placed in close crucible after the ceramic blank-body exhaust glue, sinter ceramic body into;
After the ceramic body being polished, is polished, applying silver electrode, it is put into oil bath and heats up, applied voltage is polarized,
The pyroelectric ceramic material is obtained after cooling.
Preferably, the calcined temperature is 750 DEG C~900 DEG C, and the time is 1.5~5 hours.
Preferably, the PVA bonding agents are specially:The PVA aqueous solution of 1wt%~6wt%.
Preferably, the time of the ageing was no more than 12 hours.
Preferably, the temperature of the sintering is 1000 DEG C~1200 DEG C, and the time is 2~5 hours.
Preferably, the temperature of the polarization is 80 DEG C~120 DEG C, and the electric-field intensity of polarization is 3kV/mm~5kV/mm, pole
The time of change is 10~20 minutes.
New four-element complex system pyroelectric ceramic material Pb { [(Me provided in an embodiment of the present invention1/3Nb2/3)x(W1/ 3Fe2/3)1-x]y(Zr0.9Ti0.1)1-y}O3- nMe ' has pyroelectric coefficient (λ=5 × 10 higher-8C·cm-2·K-1~20 ×
10-8C·cm-2·K-1), suitable permittivity εr(100~800) and relatively low dielectric loss tan δ (0.008~0.030),
And these performances are adjustable in relative broad range, and the ceramic body of dense uniform can be at a relatively low sintering temperature obtained, thus be somebody's turn to do
Material and its preparation method can be applied to different pyroelectric detector parts.
Brief description of the drawings
Below by drawings and Examples, the technical scheme to the embodiment of the present invention is described in further detail.
Fig. 1 is the preparation method flow chart of the compound system pyroelectric ceramic material that the embodiment of the present invention 2 is provided;
Fig. 2 is the preparation method that provides of the embodiment of the present invention 3 gained quaternary after sintering, insulation 2.5 hours at 1100 DEG C
Compound system pyroelectric ceramic material Pb { [(Mg1/3Nb2/3)0.25(W1/3Fe2/3)0.75]0.08(Zr0.9Ti0.1)0.92}O3Scanning electricity
Mirror (SEM) image;
Fig. 3 is the preparation method that provides of the embodiment of the present invention 3 gained quaternary after sintering, insulation 2.5 hours at 1100 DEG C
Compound system pyroelectric ceramic material Pb { [(Mg1/3Nb2/3)0.25(W1/3Fe2/3)0.75]0.08(Zr0.9Ti0.1)0.92}O3Pyroelectricity
Curve;
Gained quaternary is multiple after Fig. 4 is sintered at 1120 DEG C, is incubated 3 hours for the preparation method of the offer of the embodiment of the present invention 5
Zoarium system pyroelectric ceramic material Pb { [(Zn1/3Nb2/3)0.25(W1/3Fe2/3)0.75]0.08(Zr0.9Ti0.1)0.92}O3ESEM
(SEM) image;
Fig. 5 is the preparation method that provides of the embodiment of the present invention 5 gained complex after sintering, insulation 3 hours at 1120 DEG C
It is pyroelectric ceramic material Pb { [(Zn1/3Nb2/3)0.25(W1/3Fe2/3)0.75]0.08(Zr0.9Ti0.1)0.92}O3Pyroelectricity curve.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but is not intended to limit guarantor of the invention
Shield scope.
Embodiment 1
The embodiment of the present invention 1 provides a kind of new four-element complex system pyroelectric ceramic material, and its chemical general formula is:
Pb{[(Me1/3Nb2/3)x(W1/3Fe2/3)1-x]y(Zr0.9Ti0.1)1-y}O3-nMe’;
Wherein, Me is the one kind in Mg or Zn;X, y represent molar fraction respectively, 0.125≤x≤0.875, and 0.08≤y≤
0.11;Me ' is the conventional modifying element for mixing, and can be one or more in Li, La or Sb, and its molar ratio range is
0mol%≤n≤5mol%.
New four-element complex system pyroelectric ceramic material Pb { [(Me provided in an embodiment of the present invention1/3Nb2/3)x(W1/ 3Fe2/3)1-x]y(Zr0.9Ti0.1)1-y}O3- nMe ' has pyroelectric coefficient (λ=5 × 10 higher-8C·cm-2·K-1~20 ×
10-8C·cm-2·K-1), suitable dielectric constant (100~800) and relatively low dielectric loss (0.008~0.030), and these
Performance is adjustable in relative broad range, and can at a relatively low sintering temperature obtain the ceramic body of dense uniform, thus the material can
It is applied to different pyroelectric detector parts.
Embodiment 2
The preparation method of the pyroelectric ceramic material in above-described embodiment 1 is present embodiments provided, as shown in figure 1, including:
Step 201, by Fe2O3And WO3By 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made FeWO4Before
Body powder is driven, and by MgO and Nb2O5Or ZnO and Nb2O5One of which press 1:1 mixed in molar ratio ball milling, forges again after drying
Burn and grind, be made MgNb2O6Or ZnNb2O6Presoma powder;
Step 202, by Pb3O4、ZrO2、TiO2、FeWO4Presoma powder, MnNb2O6Or ZnNb2O6Presoma powder, change
The oxide or salt of property element M e ' are according to chemical general formula Pb { [(Me1/3Nb2/3)x(W1/3Fe2/3)1-x]y(Zr0.9Ti0.1)1-y}O3-
The molar ratio weighing of nMe ', then mixing and ball milling, obtains slurry;
Wherein, Me is the one kind in Mg or Zn;X, y represent molar fraction respectively, 0.125≤x≤0.875, and 0.08≤y≤
0.11;Me ' is modifying element, is one or more in Li, La or Sb, and its molar ratio range is 0mol%≤n≤5mol%.
Step 203, will carry out pre-burning after slurry drying, sieving, and the block that the pre-burning is obtained ball milling again;
Specifically, the calcined temperature is 750 DEG C~900 DEG C, the time is 1.5~5 hours.
Step 204, the slurry drying that will be obtained after ball milling again obtains powder, and polyvinyl alcohol is added in the powder
(PVA) binding agent is ground granulation, and ageing is sieved after placing, and obtains powder;
Specifically, the PVA bonding agents are specially:The PVA aqueous solution of 1wt%~6wt%, and the ageing time
No more than 12 hours.
Step 205, by the powder pressing into ceramic body;
Step 206, will be placed in close crucible after the ceramic blank-body exhaust glue, sinter ceramic body into;
Specifically, sintering temperature can be preferably 1000 DEG C~1200 DEG C, the time of sintering is preferably 2~5 hours.
Step 207, after being polished the ceramic body, polished, applying silver electrode, is put into oil bath and heats up, applied voltage
Polarized, the pyroelectric ceramic material is obtained after cooling.
Specifically, polarization process includes:
In 80 DEG C~120 DEG C of silicone oil, by the ceramic body under the polarized electric field intensity of 3kV/mm~5kV/mm pole
Change 10~20 minutes.
The preparation method of the new four-element complex system pyroelectric ceramic material that the present embodiment is provided, can be used in preparing
State the compound system pyroelectric ceramic material described in embodiment 1.The material for preparing has pyroelectric coefficient (λ higher
=5 × 10-8C·cm-2·K-1~20 × 10-8C·cm-2·K-1), suitable dielectric constant (100~800) and relatively low dielectric
Loss (0.008~0.030), and these performances are adjustable in relative broad range, and can at a relatively low sintering temperature obtain densification
Uniform ceramic body, thus the material and its preparation method can be applied to different pyroelectric detector parts.
The technical scheme for providing for a better understanding of the present invention, it is following to be described separately using the present invention with multiple instantiations
The preparation method that above-described embodiment is provided prepares the detailed process of compound system pyroelectric ceramic material, and its performance.
Embodiment 3
By MgO and Nb2O5By 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made MgNb2O6Precursor
Material;By Fe2O3And WO3By 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made FeWO4Presoma powder.Will
Pb3O4、ZrO2、TiO2、MgNb2O6Presoma powder and FeWO4Presoma powder presses Pb { [(Mg1/3Nb2/3)0.25(W1/ 3Fe2/3)0.75]0.08(Zr0.9Ti0.1)0.92}O3Molar ratio weighing, add anhydrous ethanol medium mixing and ball milling, drying sieving after
750 DEG C of pre-burnings 2 hours.The block that will be obtained after pre-burning carries out ball milling, drying again, and adds 5%PVA to granulate, and is aged 6 hours,
A diameter of 15mm is pressed into after sieving, thickness is the base substrate of 1.5mm or so, and dumping is obtained after being sintered 2.5 hours at 1100 DEG C
Ceramic body.By gained ceramic body by polishing, polishing, by silver after, with 4kV/mm electric field polarizations 20 minutes in 120 DEG C of silicone oil,
Compound system pyroelectric ceramic material Pb { [(Mg needed for being obtained after cooling1/3Nb2/3)0.25(W1/3Fe2/3)0.75]0.08
(Zr0.9Ti0.1)0.92}O3Ceramics sample.
Testing gained comprehensive electrochemical properties is:λ is 5 × 10-8C·cm-2·K-1~14 × 10-8C·cm-2·K-1, εr=
561, tan δ=0.008.ESEM (SEM) image is shown in Fig. 2, and pyroelectricity curve is shown in Fig. 3.
Embodiment 4
By MgO and Nb2O5By 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made MgNb2O6Precursor
Material;By Fe2O3And WO3By 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made FeWO4Presoma powder.Will
Pb3O4、ZrO2、TiO2、MgNb2O6Presoma powder and FeWO4Presoma powder presses Pb { [(Mg1/3Nb2/3)0.875(W1/ 3Fe2/3)0.125]0.09(Zr0.9Ti0.1)0.91}O3Molar ratio weighing, add anhydrous ethanol medium mixing and ball milling, drying sieving after
750 DEG C of pre-burnings 2 hours.The block that will be obtained after pre-burning carries out ball milling, drying again, and adds 6%PVA to granulate, and is aged 6 hours,
A diameter of 15mm is pressed into after sieving, thickness is the base substrate of 1.5mm or so, and dumping is made pottery after being sintered 3 hours at 1100 DEG C
Porcelain body.By gained ceramic body by polishing, polishing, by silver after, with 4kV/mm electric field polarizations 10 minutes in 110 DEG C of silicone oil, drop
Compound system pyroelectric ceramic material Pb { [(Mg needed for being obtained after temperature1/3Nb2/3)0.875(W1/3Fe2/3)0.125]0.09
(Zr0.9Ti0.1)0.91}O3Ceramics sample.
Testing gained comprehensive electrochemical properties is:λ is 8 × 10-8C·cm-2·K-1~11 × 10-8C·cm-2·K-1, εr=
313, tan δ=0.017.
Embodiment 5
By ZnO and Nb2O5By 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made ZnNb2O6Precursor
Material;By Fe2O3And WO3By 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made FeWO4Presoma powder.Will
Pb3O4、ZrO2、TiO2、ZnNb2O6Presoma powder and FeWO4Presoma powder presses Pb { [(Zn1/3Nb2/3)0.25(W1/ 3Fe2/3)0.75]0.08(Zr0.9Ti0.1)0.92}O3Molar ratio weighing, add anhydrous ethanol medium mixing and ball milling, drying sieving after
800 DEG C of pre-burnings 2 hours.The block that will be obtained after pre-burning carries out ball milling, drying again, and adds 5%PVA to granulate, and is aged 6 hours,
A diameter of 15mm is pressed into after sieving, thickness is the base substrate of 1.5mm or so, and dumping is made pottery after being sintered 3 hours at 1120 DEG C
Porcelain body.By gained ceramic body by polishing, polishing, by silver after, with 4kV/mm electric field polarizations 10 minutes in 120 DEG C of silicone oil, drop
Compound system pyroelectric ceramic material Pb { [(Zn needed for being obtained after temperature1/3Nb2/3)0.25(W1/3Fe2/3)0.75]0.08
(Zr0.9Ti0.1)0.92}O3Ceramics sample.
Testing gained comprehensive electrochemical properties is:λ is 6 × 10-8C·cm-2·K-1~17 × 10-8C·cm-2·K-1, εr=
407, tan δ=0.025.ESEM (SEM) image is shown in Fig. 4, and pyroelectricity curve is shown in Fig. 5.
Embodiment 6
By ZnO and Nb2O5By 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made ZnNb2O6Precursor
Material;By Fe2O3And WO3By 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made FeWO4Presoma powder.Will
Pb3O4、ZrO2、TiO2、ZnNb2O6Presoma powder and FeWO4Presoma powder presses Pb { [(Zn1/3Nb2/3)0.75(W1/ 3Fe2/3)0.25]0.09(Zr0.9Ti0.1)0.91}O3Molar ratio weighing, add anhydrous ethanol medium mixing and ball milling, drying sieving after
800 DEG C of pre-burnings 2 hours.The block that will be obtained after pre-burning carries out ball milling, drying again, and adds 5%PVA to granulate, and is aged 10 hours,
A diameter of 12mm is pressed into after sieving, thickness is the base substrate of 1.2mm or so, and dumping is obtained after being sintered 2.5 hours at 1150 DEG C
Ceramic body.By gained ceramic body by polishing, polishing, by silver after, with 4kV/mm electric field polarizations 20 minutes in 120 DEG C of silicone oil,
Compound system pyroelectric ceramic material Pb { [(Zn needed for being obtained after cooling1/3Nb2/3)0.75(W1/3Fe2/3)0.25]0.09
(Zr0.9Ti0.1)0.91}O3Ceramics sample.
Testing gained comprehensive electrochemical properties is:λ is 5 × 10-8C·cm-2·K-1~14 × 10-8C·cm-2·K-1, εr=
204, tan δ=0.029.
Embodiment 7
By MgO and Nb2O5By 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made MgNb2O6Precursor
Material;By Fe2O3And WO3By 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made FeWO4Presoma powder.Will
Pb3O4、ZrO2、TiO2、La2O3And FeWO4Presoma powder presses Pb { [(Mg1/3Nb2/3)0.5(W1/3Fe2/3)0.5]0.11
(Zr0.9Ti0.1)0.89}O3- 0.5mol%La molar ratio weighings, add anhydrous ethanol medium mixing and ball milling, and drying sieving is after 750
DEG C pre-burning 2 hours.The block that will be obtained after pre-burning carries out ball milling, drying again, and adds 5%PVA to granulate, and is aged 6 hours, sieving
After be pressed into a diameter of 15mm, thickness is the base substrate of 1.5mm or so, and dumping obtains ceramics after being sintered 3 hours at 1050 DEG C
Body.By gained ceramic body by polishing, polishing, by silver after, with 4kV/mm electric field polarizations 20 minutes in 90 DEG C of silicone oil, after cooling
Compound system pyroelectric ceramic material Pb { [(Mg needed for being obtained1/3Nb2/3)0.5(W1/3Fe2/3)0.5]0.11(Zr0.9Ti0.1)0.89}O3-
The ceramics sample of 0.5mol%La.
Testing gained comprehensive electrochemical properties is:λ is 10 × 10-8C·cm-2·K-1~20 × 10-8C·cm-2·K-1, εr=
755, tan δ=0.009.
Above example be premised on technical solution of the present invention under, the detailed implementation material component that is given and specific preparation
Technical process, but protection scope of the present invention is not limited to above-described embodiment.
New four-element complex system pyroelectric ceramic material Pb { [(Me provided in an embodiment of the present invention1/3Nb2/3)x(W1/ 3Fe2/3)1-x]y(Zr0.9Ti0.1)1-y}O3- nMe ' has pyroelectric coefficient (λ=5 × 10 higher-8C·cm-2·K-1~20 ×
10-8C·cm-2·K-1), suitable permittivity εr(100~800) and relatively low dielectric loss tan δ (0.008~0.030),
And these performances are adjustable in relative broad range, and the ceramic body of dense uniform can be at a relatively low sintering temperature obtained, thus be somebody's turn to do
Material and its preparation method can be applied to different pyroelectric detector parts.
Above-described specific embodiment, has been carried out further to the purpose of the present invention, technical scheme and beneficial effect
Describe in detail, should be understood that and the foregoing is only specific embodiment of the invention, be not intended to limit the present invention
Protection domain, all any modification, equivalent substitution and improvements within the spirit and principles in the present invention, done etc. all should include
Within protection scope of the present invention.
Claims (7)
1. a kind of compound system pyroelectric ceramic material, it is characterised in that the chemical general formula of the material is:Pb{[(Me1/ 3Nb2/3)x(W1/3Fe2/3)1-x]y(Zr0.9Ti0.1)1-y}O3-nMe’;
Wherein, Me is the one kind in Mg or Zn;X, y represent molar fraction respectively, 0.125≤x≤0.875, and 0.08≤y≤
0.11;Me ' is modifying element, is one or more in Li, La or Sb, and its molar ratio range is 0 < n≤5mol%;
Wherein, the preparation method of the compound system pyroelectric ceramic material includes:
By Fe2O3And WO3By 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made FeWO4Presoma powder, and will
MgO and Nb2O5Or ZnO and Nb2O5One of which press 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made
MgNb2O6Or ZnNb2O6Presoma powder;
By Pb3O4、ZrO2、TiO2、FeWO4Presoma powder, MgNb2O6Or ZnNb2O6The oxygen of presoma powder, modifying element Me '
Compound or salt according to above-mentioned chemical general formula molar ratio weighing, then mixing and ball milling, obtains slurry;
Pre-burning will be carried out after slurry drying, sieving, and the block that the pre-burning is obtained ball milling again;
The slurry drying that will be obtained after ball milling again obtains powder, adds polyvinyl alcohol adhesive to be ground in the powder
Granulation, ageing is sieved after placing, and obtains powder;
By the powder pressing into ceramic body;
To be placed in close crucible after the ceramic blank-body exhaust glue, sinter ceramic body into;
After the ceramic body being polished, is polished, applying silver electrode, it is put into oil bath and heats up, applied voltage is polarized, and is lowered the temperature
Obtain the pyroelectric ceramic material afterwards.
2. a kind of preparation method of pyroelectric ceramic material as described in above-mentioned claim 1, it is characterised in that the preparation side
Method includes:
By Fe2O3And WO3By 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made FeWO4Presoma powder, and will
MgO and Nb2O5Or ZnO and Nb2O5One of which press 1:1 mixed in molar ratio ball milling, calcines and grinds again after drying, and is made
MgNb2O6Or ZnNb2O6Presoma powder;
By Pb3O4、ZrO2、TiO2、FeWO4Presoma powder, MgNb2O6Or ZnNb2O6The oxygen of presoma powder, modifying element Me '
Compound or salt according to above-mentioned chemical general formula molar ratio weighing, then mixing and ball milling, obtains slurry;
Pre-burning will be carried out after slurry drying, sieving, and the block that pre-burning is obtained ball milling again;
The slurry drying that will be obtained after ball milling again obtains powder, adds polyvinyl alcohol adhesive to be ground in the powder
Granulation, ageing is sieved after placing, and obtains powder;
By the powder pressing into ceramic body;
To be placed in close crucible after the ceramic blank-body exhaust glue, sinter ceramic body into;
After the ceramic body being polished, is polished, applying silver electrode, it is put into oil bath and heats up, applied voltage is polarized, and is lowered the temperature
Obtain the pyroelectric ceramic material afterwards.
3. preparation method according to claim 2, it is characterised in that the temperature of the pre-burning is 750 DEG C~900 DEG C, when
Between be 1.5~5 hours.
4. preparation method according to claim 2, it is characterised in that the polyvinyl alcohol adhesive is specially:1wt%~
The PVA aqueous solution of 6wt%.
5. preparation method according to claim 2, it is characterised in that the time of the ageing is no more than 12 hours.
6. preparation method according to claim 2, it is characterised in that the temperature of the sintering is 1000 DEG C~1200 DEG C,
Time is 2~5 hours.
7. preparation method according to claim 2, it is characterised in that the temperature of the polarization is 80 DEG C~120 DEG C, polarization
Electric-field intensity be 3kV/mm~5kV/mm, time of polarization is 10~20 minutes.
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JPS57168405A (en) * | 1981-04-09 | 1982-10-16 | Matsushita Electric Ind Co Ltd | High dielectric porcelain composition |
CN100344576C (en) * | 2005-09-09 | 2007-10-24 | 中国科学院上海硅酸盐研究所 | Lanthanum-doped lead niobate zincate zirconate titanate piezo-electric ceramic material and its preparation method |
JP5063606B2 (en) * | 2005-11-04 | 2012-10-31 | セラコンプ カンパニー, リミテッド | Piezoelectric single crystal and method for manufacturing the same, and piezoelectric applied parts and dielectric applied parts using the piezoelectric single crystal |
US8470211B2 (en) * | 2006-04-13 | 2013-06-25 | Agency For Science, Technology And Research | Ferroelectric ceramic material with a low sintering temperature |
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---|
La掺杂PZST反铁电陶瓷电场诱导热释电现象;杨同青等;《压电与声光》;19981031;第20卷(第5期);第350页至第353页 * |
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