CN107056294A - A kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility - Google Patents
A kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility, with Pb (Zr0.52Ti0.48)O3For intermediate layer, xPb (Zr0.52Ti0.48)O3‑(1‑x)Sr(K0.25Nb0.75)O3（x=0.95~0.98）For surface layer up and down, the shaping of row sandwich structure is molded into by multilayer, it is sintered at 1150~1225 DEG C, it is prepared for the laminated piezoelectric ceramic that lead volatility is less than 2.5wt%, the composition and processing step of the present invention is simple, easily operated, reproducible, present invention is mainly used for environment-friendly type piezoelectric transformer and transducer etc..
Description
Technical field
The present invention relates to piezoelectric ceramics field, the PZT based sandwich structure piezoelectric ceramics of especially a kind of low lead volatility
Preparation method.
Background technology
Piezoelectric ceramics is a kind of ceramic material that can mutually convert electric energy and mechanical energy, belongs to inorganic non-metallic
One kind of material, piezoelectric ceramics has stable chemical characteristic, excellent physical property, is easy to system due to its piezo-electric effect
It is standby thus to be widely used in transformer, wave filter, sensor into variously-shaped and arbitrary polarisation direction material characteristic,
Various sonic transducers etc., not only have in daily life and industrial production and widely apply, while being also that military field is closed closely
One class material of note.
Lead zirconate titanate（PZT）Base piezoelectric ceramic contains a large amount of lead, the PbO's (or Pb3O4) originated in production as lead
Usage amount is up to more than 70wt%, and lead is different from other metals, it is easy to melt, when temperature be 327oC when, that is, start liquefaction, when up to
During to 400oC, just start a large amount of evaporations, the volatilization of lead can cause the pollution of environment, endanger the health of the mankind.In recent years, environment
Problem is increasingly serious, and in order to reduce the volatilization of lead in PZT base piezoelectric ceramic sintering processes, researcher is also constantly being explored.
The content of the invention
In order to solve the deficiencies in the prior art, it is an object of the invention to provide one kind have multi-layer compound structure, can
Effectively reduce the volatile quantity of lead in sintering, the PZT during reduction PZT Production of Ceramics to the low lead volatility of the pollution level of environment
The preparation method of based sandwich structure piezoelectric ceramics.
In order to realize above-mentioned technical purpose, the technical scheme is that：
A kind of PZT based sandwich structure piezoelectric ceramics of low lead volatility, it sequentially includes upper layer, intermediate layer and cutting optimal, its
The chemical composition formula of upper layer and following layer material is：xPb(Zr0.52Ti0.48)O3-(1-x)Sr(K0.25Nb0.75)O3, wherein x
=0.95~0.98；The chemical general formula of intermediate layer material is：Pb(Zr0.52Ti0.48)O3。
Further, the thickness of the upper layer and cutting optimal is 0.2~0.5mm, the thickness in intermediate layer for 0.5~
0.8mm。
Further, described sandwich structure piezoelectric ceramics for upper layer, intermediate layer and cutting optimal powder material sequentially
The heap poststack that tiles is compressing.
A kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility, it comprises the following steps：
（1）Dispensing：By chemical composition formula xPb (Zr0.52Ti0.48)O3-(1-x)Sr(K0.25Nb0.75)O3, wherein x=0.95~
0.98 stoichiometric proportion weighs raw material PbO, ZrO2、TiO2、SrCO3、K2CO3And Nb2O5Progress is mixed to get compound A；Press
Chemical composition formula Pb (Zr0.52Ti0.48)O3Stoichiometric proportion weigh raw material PbO, ZrO2、TiO2Progress is mixed to get compound
B；
（2）Ball milling：Respectively toward adding ball-milling medium in compound A and compound B, then compound A and compound B are respectively charged into
In different ball grinders carry out 2~12h of ball milling, after ball milling terminates, then respectively by compound A and compound B be placed in baking oven with
80~85 DEG C of temperature is dried, and then compound A and compound B are put into different mortars again and are ground；
（3）Pre-burning：Compound A and compound B after above-mentioned grinding is added separately in different crucibles, after compacting, capping,
It is placed in Muffle furnace, is incubated under 500~800 DEG C of temperature conditionss after 0.5~2h and is warming up to 800~1000 DEG C of progress constant temperature again
1~6h of pre-burning, then naturally cools to after room temperature and to take out crucible again；
（4）Secondary ball milling：After ball-milling medium being separately added into the above-mentioned compound A by pre-burning and compound B, then by its point
It is not fitted into different ball grinders, carries out 2~12h of ball milling, after ball milling terminates, compound A and compound B are being placed in baking respectively
Dried in case with 80~85 DEG C of temperature, then again after the screen cloth sieving through 90~100 mesh, you can powder A is made respectively
With powder B, wherein powder A chemical composition formula is xPb (Zr0.52Ti0.48)O3-(1-x)Sr(K0.25Nb0.75)O3, wherein x=
0.95~0.98, powder B chemical composition formula are Pb (Zr0.52Ti0.48)O3；
（5）Granulation：The PVA solution that 0.5~5wt% is separately added into powder A obtained above and powder B is well mixed,
Then it is placed in baking oven and is dried with 90~130 DEG C of temperature again, then is sieved by the screen cloth of 90~100 mesh；
（6）Step will be passed through（5）Powder A and powder B after processing sequentially add progress tiling stacking, wherein upper layer in mould
Be powder A with cutting optimal, intermediate layer is powder B, after the completion of tiling, with 150~250Mpa pressure carry out pressurize compacting 3~
5min, you can molded tablet is made；
（7）Dumping：Molded tablet made from above-mentioned molding is placed in pallet and is capped, is then placed in Muffle furnace, 400~
30~180min is incubated at a temperature of 650 DEG C and carries out dumping, it is then naturally cooled into room temperature with stove again；
（8）Sintering：Step will be passed through（7）Molded tablet after dumping processing is placed in Muffle furnace, in 1150~1225 DEG C of temperature
Under the conditions of degree, 30~240min is sintered, the molded tablet after then re-sintering naturally cools to room temperature, you can be made
PZT based sandwich structure piezoelectric ceramics.
Further, described step（1）Also include compound A and compound B is carried out into solid phase legal system powder respectively.
Further, step（2）And step（4）The rotational speed of ball-mill of middle ball milling is 150~280r/min.
Further, step（2）And step（4）Described in ball-milling medium constituted for alcohol and zirconia ball, described ball
Grinding media by zirconia ball, alcohol, treat ball-milled mixtures mass ratio be 2：0.5：1 mass ratio is added to the mixing for treating ball milling
Expect in A or compound B.
Further, the step（2）And step（4）Ball grinder be nylon ball grinder, step（7）Described in pallet
For oxidation aluminium material.
Further, described PbO, ZrO2、TiO2、SrCO3、K2CO3And Nb2O5It is that analysis is pure.
Further, the lead volatility amount of PZT based sandwich structure piezoelectric ceramics made from the sintering is less than 2.5wt%.
Using above-mentioned technical scheme, compared with prior art, beneficial effects of the present invention are：It is compound by using three layers
Structure prepare piezoelectric ceramics, can effectively reduce a large amount of lead that PZT base piezoelectric ceramics produce in high-temperature sintering process and wave
Question is inscribed, and is reduced problem of environmental pollution, is environmentally friendly piezoceramic material while can also ensure that the piezoelectric property of piezoelectric ceramics
Industrialized production establish theory and practice basis.
Brief description of the drawings
The present invention is further elaborated with reference to the accompanying drawings and detailed description：
Fig. 1 is the simplified diagram of piezoelectric ceramics sintering processing of the embodiment of the present invention, wherein with 0.98PZT-0.02SKN/PZT's
Exemplified by structure.
Embodiment
A kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility, it comprises the following steps：
（1）Dispensing：By chemical composition formula xPb (Zr0.52Ti0.48)O3-(1-x)Sr(K0.25Nb0.75)O3, wherein x=0.95~
0.98 stoichiometric proportion weighs raw material PbO, ZrO2、TiO2、SrCO3、K2CO3And Nb2O5Progress is mixed to get compound A；Press
Chemical composition formula Pb (Zr0.52Ti0.48)O3Stoichiometric proportion weigh raw material PbO, ZrO2、TiO2Progress is mixed to get compound
B；
（2）Ball milling：Respectively toward adding ball-milling medium in compound A and compound B, then compound A and compound B are respectively charged into
In different ball grinders carry out 2~12h of ball milling, after ball milling terminates, then respectively by compound A and compound B be placed in baking oven with
80~85 DEG C of temperature is dried, and then compound A and compound B are put into different mortars again and are ground；
（3）Pre-burning：Compound A and compound B after above-mentioned grinding is added separately in different crucibles, after compacting, capping,
It is placed in Muffle furnace, is incubated under 500~800 DEG C of temperature conditionss after 0.5~2h and is warming up to 800~1000 DEG C of progress constant temperature again
1~6h of pre-burning, then naturally cools to after room temperature and to take out crucible again；
（4）Secondary ball milling：After ball-milling medium being separately added into the above-mentioned compound A by pre-burning and compound B, then by its point
It is not fitted into different ball grinders, carries out 2~12h of ball milling, after ball milling terminates, compound A and compound B are being placed in baking respectively
Dried in case with 80~85 DEG C of temperature, then again after the screen cloth sieving through 90~100 mesh, you can powder A is made respectively
With powder B, wherein powder A chemical composition formula is xPb (Zr0.52Ti0.48)O3-(1-x)Sr(K0.25Nb0.75)O3, wherein x=
0.95~0.98, powder B chemical composition formula are Pb (Zr0.52Ti0.48)O3；
（5）Granulation：The PVA solution that 0.5~5wt% is separately added into powder A obtained above and powder B is well mixed,
Then it is placed in baking oven and is dried with 90~130 DEG C of temperature again, then is sieved by the screen cloth of 90~100 mesh；
（6）Step will be passed through（5）Powder A and powder B after processing sequentially add progress tiling stacking, wherein upper layer in mould
Be powder A with cutting optimal, intermediate layer is powder B, after the completion of tiling, with 150~250Mpa pressure carry out pressurize compacting 3~
5min, you can molded tablet is made；
（7）Dumping：Molded tablet made from above-mentioned molding is placed in pallet and is capped, is then placed in Muffle furnace, 400~
30~180min is incubated at a temperature of 650 DEG C and carries out dumping, it is then naturally cooled into room temperature with stove again；
（8）Sintering：Step will be passed through（7）Molded tablet after dumping processing is placed in Muffle furnace, in 1150~1225 DEG C of temperature
Under the conditions of degree, 30~240min is sintered, the molded tablet after then re-sintering naturally cools to room temperature, you can be made
PZT based sandwich structure piezoelectric ceramics.
Further, described step（1）Also include compound A and compound B is carried out into solid phase legal system powder respectively.
Further, step（2）And step（4）The rotational speed of ball-mill of middle ball milling is 150~280r/min.
Further, step（2）And step（4）Described in ball-milling medium constituted for alcohol and zirconia ball, described ball
Grinding media by zirconia ball, alcohol, treat ball-milled mixtures mass ratio be 2：0.5：1 mass ratio is added to the mixing for treating ball milling
Expect in A or compound B.
Further, the step（2）And step（4）Ball grinder be nylon ball grinder, step（7）Described in pallet
For oxidation aluminium material.
Further, described PbO, ZrO2、TiO2、SrCO3、K2CO3And Nb2O5It is that analysis is pure.
Further, the lead volatility amount of PZT based sandwich structure piezoelectric ceramics made from the sintering is less than 2.5wt%.
Embodiment 1
A kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility, it comprises the following steps：
（1）Dispensing：By chemical composition formula 0.95Pb (Zr0.52Ti0.48)O3-0.05Sr(K0.25Nb0.75)O3Stoichiometric proportion
Weigh raw material PbO, ZrO2、TiO2、SrCO3、K2CO3And Nb2O5Progress is mixed to get compound A；By chemical composition formula Pb
(Zr0.52Ti0.48)O3Stoichiometric proportion weigh raw material PbO, ZrO2、TiO2Progress is mixed to get compound B；
（2）Ball milling：Respectively toward adding ball-milling medium in compound A and compound B, then compound A and compound B are respectively charged into
Ball milling 2h is carried out in different nylon ball grinders, rotational speed of ball-mill is 260r/min, after ball milling terminates, then respectively by compound A and
Compound B is placed in baking oven is dried with 80 DEG C of temperature, and compound A and compound B then are put into different mortars again
Inside be ground, wherein, described ball-milling medium is that alcohol and zirconia ball are constituted, described ball-milling medium by zirconia ball,
Alcohol, treat ball-milled mixtures mass ratio be 2：0.5：1 mass ratio is added in the compound A or compound B for treating ball milling；
（3）Pre-burning：Compound A and compound B after above-mentioned grinding is added separately in different crucibles, after compacting, capping,
It is placed in Muffle furnace, is incubated under 650 DEG C of temperature conditionss after 1.5h and is warming up to 850 DEG C of progress constant temperature pre-burnings 2h, Ran Houzai again
Naturally cool to after room temperature and to take out crucible；
（4）Secondary ball milling：Ball-milling medium is separately added into the compound A and compound B of above-mentioned process pre-burning, wherein, it is described
Ball-milling medium constituted for alcohol and zirconia ball, described ball-milling medium by zirconia ball, alcohol, treat the matter of ball-milled mixtures
Amount is than being 2：0.5：1 mass ratio is added in the compound A or compound B for treating ball milling, then the mixing that will add ball-milling medium
Material A and compound B is respectively charged into different nylon ball grinders, carries out ball milling 2h, rotational speed of ball-mill is 260r/min, and ball milling terminates
Afterwards, dried with 80 DEG C of temperature compound A and compound B are placed in baking oven respectively, then the screen cloth again through 100 mesh
After sieving, you can powder A and powder B is made respectively, wherein powder A chemical composition formula is 0.95Pb (Zr0.52Ti0.48)O3-
0.05Sr(K0.25Nb0.75)O3, powder B chemical composition formula is Pb (Zr0.52Ti0.48)O3；
（5）Granulation：The PVA solution that 5wt% is separately added into powder A obtained above and powder B is well mixed, then
It is placed in baking oven and is dried with 120 DEG C of temperature again, then is sieved by the screen cloth of 100 mesh；
（6）Step will be passed through（5）Powder A and powder B after processing sequentially add progress tiling stacking, wherein upper layer in mould
It is powder A with cutting optimal, intermediate layer is powder B, and the thickness of upper layer and cutting optimal is respectively 0.5mm, and intermediate layer thickness is
0.5mm, after the completion of tiling, carries out pressurize compacting 3min, you can molded tablet is made with 250Mpa pressure；
（7）Dumping：Molded tablet made from above-mentioned molding is placed in pallet and is capped, is then placed in Muffle furnace, at 650 DEG C
At a temperature of be incubated 60min carry out dumping, it is then naturally cooled into room temperature with stove again；
（8）Sintering：Step will be passed through（7）Molded tablet after dumping processing is placed in Muffle furnace, in 1175 DEG C of temperature conditionss
Under, 120min is sintered, the molded tablet after then re-sintering naturally cools to room temperature, you can PZT bases Sanming City is made
Control structure piezoelectric ceramics.
Performance test
The surface for sintering obtained PZT based sandwich structure piezoelectric ceramics is coated into silver paste, then is placed in Muffle furnace with 650
DEG C carry out silver ink firing processing 15min, then will test d after sample polarization again33Value, takes and PZT based sandwich made from the present embodiment
The pure PZT base piezoelectric ceramics of structure piezoelectric ceramics same thickness are carried out after same treatment, survey its d33Value, d33Test result shows,
The d of PZT based sandwich structure piezoelectric ceramics made from the present embodiment33For 155, and the pure PZT base piezoelectric ceramics of same thickness
d33For 107；Again by PZT based sandwich structure piezoelectric ceramics made from the present embodiment and the pure PZT bases piezoelectricity of same thickness
Ceramics carry out weightless test, and through weightless test, the lead volatility amount of PZT based sandwich structure piezoelectric ceramics is made from the present embodiment
1.44wt%, and the lead volatility amount of the pure PZT base piezoelectric ceramics of same thickness is 3.15wt%.
Embodiment 2
A kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility, it comprises the following steps：
（1）Dispensing：By chemical composition formula 0.96Pb (Zr0.52Ti0.48)O3-0.04Sr(K0.25Nb0.75)O3Stoichiometric proportion
Weigh raw material PbO, ZrO2、TiO2、SrCO3、K2CO3And Nb2O5Progress is mixed to get compound A；By chemical composition formula Pb
(Zr0.52Ti0.48)O3Stoichiometric proportion weigh raw material PbO, ZrO2、TiO2Progress is mixed to get compound B；
（2）Ball milling：Respectively toward adding ball-milling medium in compound A and compound B, then compound A and compound B are respectively charged into
Ball milling 12h is carried out in different nylon ball grinders, rotational speed of ball-mill is 260r/min, after ball milling terminates, then respectively by compound A and
Compound B is placed in baking oven is dried with 85 DEG C of temperature, and compound A and compound B then are put into different mortars again
Inside be ground, wherein, described ball-milling medium is that alcohol and zirconia ball are constituted, described ball-milling medium by zirconia ball,
Alcohol, treat ball-milled mixtures mass ratio be 2：0.5：1 mass ratio is added in the compound A or compound B for treating ball milling；
（3）Pre-burning：Compound A and compound B after above-mentioned grinding is added separately in different crucibles, after compacting, capping,
It is placed in Muffle furnace, is incubated under 650 DEG C of temperature conditionss after 1.5h and is warming up to 850 DEG C of progress constant temperature pre-burnings 2h, Ran Houzai again
Naturally cool to after room temperature and to take out crucible；
（4）Secondary ball milling：Ball-milling medium is separately added into the compound A and compound B of above-mentioned process pre-burning, wherein, it is described
Ball-milling medium constituted for alcohol and zirconia ball, described ball-milling medium by zirconia ball, alcohol, treat the matter of ball-milled mixtures
Amount is than being 2：0.5：1 mass ratio is added in the compound A or compound B for treating ball milling, then the mixing that will add ball-milling medium
Material A and compound B is respectively charged into different nylon ball grinders, carries out ball milling 12h, rotational speed of ball-mill is 260r/min, ball milling knot
Shu Hou, is dried compound A and compound B are placed in baking oven respectively with 85 DEG C of temperature, then the sieve again through 100 mesh
After net sieving, you can powder A and powder B is made respectively, wherein powder A chemical composition formula is 0.96Pb (Zr0.52Ti0.48)
O3-0.04Sr(K0.25Nb0.75)O3, powder B chemical composition formula is Pb (Zr0.52Ti0.48)O3；
（5）Granulation：The PVA solution that 3wt% is separately added into powder A obtained above and powder B is well mixed, then
It is placed in baking oven and is dried with 120 DEG C of temperature again, then is sieved by the screen cloth of 100 mesh；
（6）Step will be passed through（5）Powder A and powder B after processing sequentially add progress tiling stacking, wherein upper layer in mould
It is powder A with cutting optimal, intermediate layer is powder B, and the thickness of upper layer and cutting optimal is respectively 0.5mm, and intermediate layer thickness is
0.5mm, after the completion of tiling, carries out pressurize compacting 3min, you can molded tablet is made with 250Mpa pressure；
（7）Dumping：Molded tablet made from above-mentioned molding is placed in pallet and is capped, is then placed in Muffle furnace, at 650 DEG C
At a temperature of be incubated 60min carry out dumping, it is then naturally cooled into room temperature with stove again；
（8）Sintering：Step will be passed through（7）Molded tablet after dumping processing is placed in Muffle furnace, in 1200 DEG C of temperature conditionss
Under, 120min is sintered, the molded tablet after then re-sintering naturally cools to room temperature, you can PZT bases Sanming City is made
Control structure piezoelectric ceramics.
Performance test
The surface for sintering obtained PZT based sandwich structure piezoelectric ceramics is coated into silver paste, then is placed in Muffle furnace with 650
DEG C carry out silver ink firing processing 15min, then will test d after sample polarization again33Value, takes and PZT based sandwich made from the present embodiment
The pure PZT base piezoelectric ceramics of structure piezoelectric ceramics same thickness are carried out after same treatment, survey its d33Value, d33Test result shows,
The d of PZT based sandwich structure piezoelectric ceramics made from the present embodiment33For 194, and the pure PZT base piezoelectric ceramics of same thickness
d33For 156；Again by PZT based sandwich structure piezoelectric ceramics made from the present embodiment and the pure PZT bases piezoelectricity of same thickness
Ceramics carry out weightless test, and through weightless test, the lead volatility amount of PZT based sandwich structure piezoelectric ceramics is made from the present embodiment
1.74wt%, and the lead volatility amount of the pure PZT base piezoelectric ceramics of same thickness is 3.25wt%.
Embodiment 3
A kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility, it comprises the following steps：
（1）Dispensing：By chemical composition formula 0.98Pb (Zr0.52Ti0.48)O3-0.02Sr(K0.25Nb0.75)O3Stoichiometric proportion
Weigh raw material PbO, ZrO2、TiO2、SrCO3、K2CO3And Nb2O5Progress is mixed to get compound A；By chemical composition formula Pb
(Zr0.52Ti0.48)O3Stoichiometric proportion weigh raw material PbO, ZrO2、TiO2Progress is mixed to get compound B；
（2）Ball milling：Respectively toward adding ball-milling medium in compound A and compound B, then compound A and compound B are respectively charged into
Ball milling 8h is carried out in different nylon ball grinders, rotational speed of ball-mill is 260r/min, after ball milling terminates, then respectively by compound A and
Compound B is placed in baking oven is dried with 85 DEG C of temperature, and compound A and compound B then are put into different mortars again
Inside be ground, wherein, described ball-milling medium is that alcohol and zirconia ball are constituted, described ball-milling medium by zirconia ball,
Alcohol, treat ball-milled mixtures mass ratio be 2：0.5：1 mass ratio is added in the compound A or compound B for treating ball milling；
（3）Pre-burning：Compound A and compound B after above-mentioned grinding is added separately in different crucibles, after compacting, capping,
It is placed in Muffle furnace, is incubated under 650 DEG C of temperature conditionss after 1.5h and is warming up to 850 DEG C of progress constant temperature pre-burnings 1h, Ran Houzai again
Naturally cool to after room temperature and to take out crucible；
（4）Secondary ball milling：Ball-milling medium is separately added into the compound A and compound B of above-mentioned process pre-burning, wherein, it is described
Ball-milling medium constituted for alcohol and zirconia ball, described ball-milling medium by zirconia ball, alcohol, treat the matter of ball-milled mixtures
Amount is than being 2：0.5：1 mass ratio is added in the compound A or compound B for treating ball milling, then the mixing that will add ball-milling medium
Material A and compound B is respectively charged into different nylon ball grinders, carries out ball milling 8h, rotational speed of ball-mill is 260r/min, and ball milling terminates
Afterwards, dried with 85 DEG C of temperature compound A and compound B are placed in baking oven respectively, then the screen cloth again through 100 mesh
After sieving, you can powder A and powder B is made respectively, wherein powder A chemical composition formula is 0.98Pb (Zr0.52Ti0.48)O3-
0.02Sr(K0.25Nb0.75)O3, powder B chemical composition formula is Pb (Zr0.52Ti0.48)O3；
（5）Granulation：The PVA solution that 0.5wt% is separately added into powder A obtained above and powder B is well mixed, so
It is placed in baking oven and is dried with 130 DEG C of temperature again afterwards, then is sieved by the screen cloth of 100 mesh；
（6）Step will be passed through（5）Powder A and powder B after processing sequentially add progress tiling stacking, wherein upper layer in mould
It is powder A with cutting optimal, intermediate layer is powder B, and the thickness of upper layer and cutting optimal is respectively 0.5mm, and intermediate layer thickness is
0.5mm, after the completion of tiling, carries out pressurize compacting 5min, you can molded tablet is made with 150Mpa pressure；
（7）Dumping：Molded tablet made from above-mentioned molding is placed in pallet and is capped, is then placed in Muffle furnace, at 650 DEG C
At a temperature of be incubated 60min carry out dumping, it is then naturally cooled into room temperature with stove again；
（8）Sintering：Step will be passed through（7）Molded tablet after dumping processing is placed in Muffle furnace, in 1225 DEG C of temperature conditionss
Under, 120min is sintered, the molded tablet after then re-sintering naturally cools to room temperature, you can PZT bases Sanming City is made
Control structure piezoelectric ceramics.
Performance test
The surface for sintering obtained PZT based sandwich structure piezoelectric ceramics is coated into silver paste, then is placed in Muffle furnace with 650
DEG C carry out silver ink firing processing 15min, then will test d after sample polarization again33Value, takes and PZT based sandwich made from the present embodiment
The pure PZT base piezoelectric ceramics of structure piezoelectric ceramics same thickness are carried out after same treatment, survey its d33Value, d33Test result shows,
The d of PZT based sandwich structure piezoelectric ceramics made from the present embodiment33For 236, and the pure PZT base piezoelectric ceramics of same thickness
d33For 178；Again by PZT based sandwich structure piezoelectric ceramics made from the present embodiment and the pure PZT bases piezoelectricity of same thickness
Ceramics carry out weightless test, and through weightless test, the lead volatility amount of PZT based sandwich structure piezoelectric ceramics is made from the present embodiment
2.05wt%, and the lead volatility amount of the pure PZT base piezoelectric ceramics of same thickness is 4.75wt%.
Embodiment 4
A kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility, it comprises the following steps：
（1）Dispensing：By chemical composition formula 0.98Pb (Zr0.52Ti0.48)O3-0.02Sr(K0.25Nb0.75)O3Stoichiometric proportion
Weigh raw material PbO, ZrO2、TiO2、SrCO3、K2CO3And Nb2O5Progress is mixed to get compound A；By chemical composition formula Pb
(Zr0.52Ti0.48)O3Stoichiometric proportion weigh raw material PbO, ZrO2、TiO2Progress is mixed to get compound B；
（2）Ball milling：Respectively toward adding ball-milling medium in compound A and compound B, then compound A and compound B are respectively charged into
Ball milling 12h is carried out in different nylon ball grinders, rotational speed of ball-mill is 280r/min, after ball milling terminates, then respectively by compound A and
Compound B is placed in baking oven is dried with 80 DEG C of temperature, and compound A and compound B then are put into different mortars again
Inside be ground, wherein, described ball-milling medium is that alcohol and zirconia ball are constituted, described ball-milling medium by zirconia ball,
Alcohol, treat ball-milled mixtures mass ratio be 2：0.5：1 mass ratio is added in the compound A or compound B for treating ball milling；
（3）Pre-burning：Compound A and compound B after above-mentioned grinding is added separately in different crucibles, after compacting, capping,
It is placed in Muffle furnace, is incubated under 800 DEG C of temperature conditionss after 0.5h and is warming up to 1000 DEG C of progress constant temperature pre-burnings 6h, Ran Houzai again
Naturally cool to after room temperature and to take out crucible；
（4）Secondary ball milling：Ball-milling medium is separately added into the compound A and compound B of above-mentioned process pre-burning, wherein, it is described
Ball-milling medium constituted for alcohol and zirconia ball, described ball-milling medium by zirconia ball, alcohol, treat the matter of ball-milled mixtures
Amount is than being 2：0.5：1 mass ratio is added in the compound A or compound B for treating ball milling, then the mixing that will add ball-milling medium
Material A and compound B is respectively charged into different nylon ball grinders, carries out ball milling 8h, rotational speed of ball-mill is 260r/min, and ball milling terminates
Afterwards, dried with 80 DEG C of temperature compound A and compound B are placed in baking oven respectively, then the screen cloth again through 100 mesh
After sieving, you can powder A and powder B is made respectively, wherein powder A chemical composition formula is 0.98Pb (Zr0.52Ti0.48)O3-
0.02Sr(K0.25Nb0.75)O3, powder B chemical composition formula is Pb (Zr0.52Ti0.48)O3；
（5）Granulation：The PVA solution that 0.5wt% is separately added into powder A obtained above and powder B is well mixed, so
It is placed in baking oven and is dried with 90 DEG C of temperature again afterwards, then is sieved by the screen cloth of 100 mesh；
（6）Step will be passed through（5）Powder A and powder B after processing sequentially add progress tiling stacking, wherein upper layer in mould
It is powder A with cutting optimal, intermediate layer is powder B, and the thickness of upper layer and cutting optimal is respectively 0.5mm, and intermediate layer thickness is
0.5mm, after the completion of tiling, carries out pressurize compacting 5min, you can molded tablet is made with 150Mpa pressure；
（7）Dumping：Molded tablet made from above-mentioned molding is placed in pallet and is capped, is then placed in Muffle furnace, at 400 DEG C
At a temperature of be incubated 180min carry out dumping, it is then naturally cooled into room temperature with stove again；
（8）Sintering：Step will be passed through（7）Molded tablet after dumping processing is placed in Muffle furnace, in 1150 DEG C of temperature conditionss
Under, 240min is sintered, the molded tablet after then re-sintering naturally cools to room temperature, you can PZT bases Sanming City is made
Control structure piezoelectric ceramics.
Performance test
The surface for sintering obtained PZT based sandwich structure piezoelectric ceramics is coated into silver paste, then is placed in Muffle furnace with 650
DEG C carry out silver ink firing processing 15min, then will test d after sample polarization again33Value, takes and PZT based sandwich made from the present embodiment
The pure PZT base piezoelectric ceramics of structure piezoelectric ceramics same thickness are carried out after same treatment, survey its d33Value, d33Test result shows,
The d of PZT based sandwich structure piezoelectric ceramics made from the present embodiment33For 226, and the pure PZT base piezoelectric ceramics of same thickness
d33For 170；Again by PZT based sandwich structure piezoelectric ceramics made from the present embodiment and the pure PZT bases piezoelectricity of same thickness
Ceramics carry out weightless test, and through weightless test, the lead volatility amount of PZT based sandwich structure piezoelectric ceramics is made from the present embodiment
2.5wt%, and the lead volatility amount of the pure PZT base piezoelectric ceramics of same thickness is 4.45wt%.
Embodiment 5
A kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility, it comprises the following steps：
（1）Dispensing：By chemical composition formula 0.96Pb (Zr0.52Ti0.48)O3-0.04Sr(K0.25Nb0.75)O3Stoichiometric proportion
Weigh raw material PbO, ZrO2、TiO2、SrCO3、K2CO3And Nb2O5Progress is mixed to get compound A；By chemical composition formula Pb
(Zr0.52Ti0.48)O3Stoichiometric proportion weigh raw material PbO, ZrO2、TiO2Progress is mixed to get compound B；
（2）Ball milling：Respectively toward adding ball-milling medium in compound A and compound B, then compound A and compound B are respectively charged into
Ball milling 12h is carried out in different nylon ball grinders, rotational speed of ball-mill is 150r/min, after ball milling terminates, then respectively by compound A and
Compound B is placed in baking oven is dried with 80 DEG C of temperature, and compound A and compound B then are put into different mortars again
Inside be ground, wherein, described ball-milling medium is that alcohol and zirconia ball are constituted, described ball-milling medium by zirconia ball,
Alcohol, treat ball-milled mixtures mass ratio be 2：0.5：1 mass ratio is added in the compound A or compound B for treating ball milling；
（3）Pre-burning：Compound A and compound B after above-mentioned grinding is added separately in different crucibles, after compacting, capping,
It is placed in Muffle furnace, is incubated under 500 DEG C of temperature conditionss after 0.5h and is warming up to 800 DEG C of progress constant temperature pre-burnings 1h, Ran Houzai again
Naturally cool to after room temperature and to take out crucible；
（4）Secondary ball milling：Ball-milling medium is separately added into the compound A and compound B of above-mentioned process pre-burning, wherein, it is described
Ball-milling medium constituted for alcohol and zirconia ball, described ball-milling medium by zirconia ball, alcohol, treat the matter of ball-milled mixtures
Amount is than being 2：0.5：1 mass ratio is added in the compound A or compound B for treating ball milling, then the mixing that will add ball-milling medium
Material A and compound B is respectively charged into different nylon ball grinders, carries out ball milling 8h, rotational speed of ball-mill is 150r/min, and ball milling terminates
Afterwards, dried with 80 DEG C of temperature compound A and compound B are placed in baking oven respectively, then the screen cloth again through 90 mesh
After sieving, you can powder A and powder B is made respectively, wherein powder A chemical composition formula is 0.96Pb (Zr0.52Ti0.48)O3-
0.04Sr(K0.25Nb0.75)O3, powder B chemical composition formula is Pb (Zr0.52Ti0.48)O3；
（5）Granulation：The PVA solution that 0.5wt% is separately added into powder A obtained above and powder B is well mixed, so
It is placed in baking oven and is dried with 130 DEG C of temperature again afterwards, then is sieved by the screen cloth of 90 mesh；
（6）Step will be passed through（5）Powder A and powder B after processing sequentially add progress tiling stacking, wherein upper layer in mould
It is powder A with cutting optimal, intermediate layer is powder B, and the thickness of upper layer and cutting optimal is respectively 0.5mm, and intermediate layer thickness is
0.5mm, after the completion of tiling, carries out pressurize compacting 4min, you can molded tablet is made with 200Mpa pressure；
（7）Dumping：Molded tablet made from above-mentioned molding is placed in pallet and is capped, is then placed in Muffle furnace, at 500 DEG C
At a temperature of be incubated 30min carry out dumping, it is then naturally cooled into room temperature with stove again；
（8）Sintering：Step will be passed through（7）Molded tablet after dumping processing is placed in Muffle furnace, in 1150 DEG C of temperature conditionss
Under, 30min is sintered, the molded tablet after then re-sintering naturally cools to room temperature, you can PZT based sandwich is made
Structure piezoelectric ceramics.
Performance test
The surface for sintering obtained PZT based sandwich structure piezoelectric ceramics is coated into silver paste, then is placed in Muffle furnace with 650
DEG C carry out silver ink firing processing 15min, then will test d after sample polarization again33Value, takes and PZT based sandwich made from the present embodiment
The pure PZT base piezoelectric ceramics of structure piezoelectric ceramics same thickness are carried out after same treatment, survey its d33Value, d33Test result shows,
The d of PZT based sandwich structure piezoelectric ceramics made from the present embodiment33For 216, and the pure PZT base piezoelectric ceramics of same thickness
d33For 162；Again by PZT based sandwich structure piezoelectric ceramics made from the present embodiment and the pure PZT bases piezoelectricity of same thickness
Ceramics carry out weightless test, and through weightless test, the lead volatility amount of PZT based sandwich structure piezoelectric ceramics is made from the present embodiment
2.25wt%, and the lead volatility amount of the pure PZT base piezoelectric ceramics of same thickness is 4.25wt%.
Described above is embodiments of the invention, for the ordinary skill in the art, according to the religion of the present invention
Lead, without departing from the principles and spirit of the present invention all equivalent changes done according to scope of the present invention patent, repair
Change, replace and modification, should all belong to the covering scope of the present invention.
Claims (10)
1. a kind of PZT based sandwich structure piezoelectric ceramics of low lead volatility, it is characterised in that：It sequentially includes upper layer, centre
Layer and cutting optimal, the chemical composition formula of its upper layer and following layer material is：xPb(Zr0.52Ti0.48)O3-(1-x)Sr
(K0.25Nb0.75)O3, wherein x=0.95~0.98；The chemical general formula of intermediate layer material is：Pb(Zr0.52Ti0.48)O3。
2. a kind of PZT based sandwich structure piezoelectric ceramics of low lead volatility according to claim 1, it is characterised in that：Institute
The thickness for stating upper layer and cutting optimal is 0.2~0.5mm, and the thickness in intermediate layer is 0.5~0.8mm.
3. a kind of PZT based sandwich structure piezoelectric ceramics of low lead volatility according to claim 1, it is characterised in that：Institute
The sandwich structure piezoelectric ceramics stated is pressed into for the powder material heap poststack that sequentially tiles of upper layer, intermediate layer and cutting optimal
Type.
4. a kind of preparation side of the PZT based sandwich structure piezoelectric ceramics of low lead volatility according to any of the above-described claim
Method, it is characterised in that：It comprises the following steps：
（1）Dispensing：By chemical composition formula xPb (Zr0.52Ti0.48)O3-(1-x)Sr(K0.25Nb0.75)O3, wherein x=0.95~
0.98 stoichiometric proportion weighs raw material PbO, ZrO2、TiO2、SrCO3、K2CO3And Nb2O5Progress is mixed to get compound A；Press
Chemical composition formula Pb (Zr0.52Ti0.48)O3Stoichiometric proportion weigh raw material PbO, ZrO2、TiO2Progress is mixed to get compound
B；
（2）Ball milling：Respectively toward adding ball-milling medium in compound A and compound B, then compound A and compound B are respectively charged into
In different ball grinders carry out 2~12h of ball milling, after ball milling terminates, then respectively by compound A and compound B be placed in baking oven with
80~85 DEG C of temperature is dried, and then compound A and compound B are put into different mortars again and are ground；
（3）Pre-burning：Compound A and compound B after above-mentioned grinding is added separately in different crucibles, after compacting, capping,
It is placed in Muffle furnace, is incubated under 500~800 DEG C of temperature conditionss after 0.5~2h and is warming up to 800~1000 DEG C of progress constant temperature again
1~6h of pre-burning, then naturally cools to after room temperature and to take out crucible again；
（4）Secondary ball milling：After ball-milling medium being separately added into the above-mentioned compound A by pre-burning and compound B, then by its point
It is not fitted into different ball grinders, carries out 2~12h of ball milling, after ball milling terminates, compound A and compound B are being placed in baking respectively
Dried in case with 80~85 DEG C of temperature, then again after the screen cloth sieving through 90~100 mesh, you can powder A is made respectively
With powder B, wherein powder A chemical composition formula is xPb (Zr0.52Ti0.48)O3-(1-x)Sr(K0.25Nb0.75)O3, wherein x=
0.95~0.98, powder B chemical composition formula are Pb (Zr0.52Ti0.48)O3；
（5）Granulation：The PVA solution that 0.5~5wt% is separately added into powder A obtained above and powder B is well mixed,
Then it is placed in baking oven and is dried with 90~130 DEG C of temperature again, then is sieved by the screen cloth of 90~100 mesh；
（6）Step will be passed through（5）Powder A and powder B after processing sequentially add progress tiling stacking, wherein upper layer in mould
Be powder A with cutting optimal, intermediate layer is powder B, after the completion of tiling, with 150~250Mpa pressure carry out pressurize compacting 3~
5min, you can molded tablet is made；
（7）Dumping：Molded tablet made from above-mentioned molding is placed in pallet and is capped, is then placed in Muffle furnace, 400~
30~180min is incubated at a temperature of 650 DEG C and carries out dumping, it is then naturally cooled into room temperature with stove again；
（8）Sintering：Step will be passed through（7）Molded tablet after dumping processing is placed in Muffle furnace, in 1150~1225 DEG C of temperature
Under the conditions of degree, 30~240min is sintered, the molded tablet after then re-sintering naturally cools to room temperature, you can be made
PZT based sandwich structure piezoelectric ceramics.
5. a kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility according to claim 4, it is special
Levy and be：Described step（1）Also include compound A and compound B is carried out into solid phase legal system powder respectively.
6. a kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility according to claim 4, it is special
Levy and be：Step（2）And step（4）The rotational speed of ball-mill of middle ball milling is 150~280r/min.
7. a kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility according to claim 4, it is special
Levy and be：Step（2）And step（4）Described in ball-milling medium constituted for alcohol and zirconia ball, described ball-milling medium is pressed
Zirconia ball, alcohol, treat ball-milled mixtures mass ratio be 2：0.5：1 mass ratio is added to the compound A or mixed for treating ball milling
Close in material B.
8. a kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility according to claim 4, it is special
Levy and be：The step（2）And step（4）Ball grinder be nylon ball grinder, step（7）Described in pallet be aluminum oxide
Material.
9. a kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility according to claim 4, it is special
Levy and be：Described PbO, ZrO2、TiO2、SrCO3、K2CO3And Nb2O5It is that analysis is pure.
10. a kind of preparation method of the PZT based sandwich structure piezoelectric ceramics of low lead volatility according to claim 4, its
It is characterised by：The lead volatility amount of PZT based sandwich structure piezoelectric ceramics made from the sintering is less than 2.5wt%.
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|---|---|---|---|---|
| JP3156383B2 (en) * | 1992-08-20 | 2001-04-16 | トヨタ自動車株式会社 | Method for producing bismuth layered compound sintered body |
| CN103641475A (en) * | 2013-11-29 | 2014-03-19 | 苏州衡业新材料科技有限公司 | Low-temperature cofiring multilayer piezoelectric ceramic and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3156383B2 (en) * | 1992-08-20 | 2001-04-16 | トヨタ自動車株式会社 | Method for producing bismuth layered compound sintered body |
| CN103641475A (en) * | 2013-11-29 | 2014-03-19 | 苏州衡业新材料科技有限公司 | Low-temperature cofiring multilayer piezoelectric ceramic and preparation method thereof |
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| CN116813336A (en) * | 2023-06-30 | 2023-09-29 | 北京邮电大学 | Method for optimizing PZT-based piezoelectric ceramic solid-phase sintering process |
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