CN107216130A - A kind of preparation method of PHT PNN piezoceramic materials - Google Patents
A kind of preparation method of PHT PNN piezoceramic materials Download PDFInfo
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Abstract
A kind of preparation method of PHT PNN piezoceramic materials disclosed by the invention：Ball milling drying and calcining again after basic nickel carbonate powder and niobium oxide powder are mixed, obtains niobic acid nickel presoma powder；Lead oxide powder, titanium dioxide powder, hafnium oxide powder and niobic acid nickel powder body are weighed respectively, ball-milling treatment is carried out after all materials are mixed, matrix mixed powder is obtained, matrix mixed powder is dried, calcined and cooled down successively, hafnium lead titanates lead nickle niobate powder is obtained；Ball milling is carried out after hafnium lead titanates lead nickle niobate powder is mixed with fluorination powder for lithium, then drying obtains pre-synthesis dry mash；PVA solution is added into pre-synthesis dry mash to be granulated, idiosome is made in obtained granule；Dumping, furnace cooling and high temperature sintering are carried out to idiosome and obtain PHT PNN piezoceramic materials.The preparation method of the present invention can obtain high tension performance fluorination lithium doping hafnium lead titanates lead nickle niobate piezoceramic material.
Description
Technical field
The invention belongs to ceramic material preparation method technical field, and in particular to a kind of PHT-PNN piezoelectric ceramics material
The preparation method of material.
Background technology
Piezoelectric ceramics is a kind of functional material that can mutually change mechanical energy and electric energy, by its preferable mechanical property
Can be with stable piezoelectric property the advantages of, the high-tech areas such as aviation, medical treatment, communication and detection have been widely used in it.
According to operation principle, the application of piezoelectric ceramics is broadly divided into two aspects of piezoelectric vibrator and transducer.In piezoelectric vibrator
The application of aspect mainly has oscillator, resonator, wave filter, piezoelectric transformer and deferred mount etc.；In terms of transducer
Driven using mainly having underwater acoustic transducer, high power altrasonic transducer, medical transducer, ultrasonic, piezo-electric motor and piezoelectricity
Dynamic device etc..The different application of piezoelectric ceramics has different requirements to its performance, such as：As piezoelectric vibrator in use, needing pressure
Electroceramics possesses preferable frequency stability and higher mechanical quality factor；As transducer, then require that piezoelectric ceramics has
There is larger piezoelectric modulus and electromechanical coupling factor.But, for new big displacement driver, the underwater acoustic transducer of efficient transmission
And medical sonac, the piezoelectric ceramics piezoelectric modulus value developed at present is still relatively low, it is impossible to meet next-generation drive
Or transducer is to the demand of material, the further application of piezoelectric ceramics is constrained, therefore obtain the piezoelectric ceramics of high tension performance
It is most important.
In order to obtain high performance piezoceramic material, various countries researchers change in recipe ingredient, preparation technology and doping
Substantial amounts of work has been done in terms of property, the Pb (B that a more class material is complex perovskite structure are studied at present1B2)O3System；
Wherein B1For low price cation, such as：Mg2+、Zn2+、Fe3+、Ni2+And Sc3+Deng；B2For high-valence cationic, such as：Nb5+、Ta5+、Ti4+
And W6+Deng.Representational material has ternary system PMN-PZT, PZN-PZT, PZN-PNN and PNN-PST and quaternary system PSN-PZN-
PZT and PZN-PNN-PZT etc.；But their preparation technology is complicated, sintering condition requires higher, and piezoelectric constant d33It is difficult to prominent
Broken 850pC/N.
Recent studies indicate that：Pb(TiHf)O3-Pb(NiNb)O3(PHT-PNN) piezoelectric ceramics has excellent piezoelectricity
Performance, by suitable doping vario-property approach, and combines specific preparation technology, it can obtain piezoelectric constant d33More than 850pC/
N high-performance.
The content of the invention
It is an object of the invention to provide a kind of preparation method of PHT-PNN piezoceramic materials, the preparation method is utilized
High tension performance fluorination lithium doping hafnium lead titanates-lead nickle niobate piezoceramic material, and its piezoelectric constant d can be obtained33Highest can
Up to 957pC/N.
The technical solution adopted in the present invention, a kind of preparation method of PHT-PNN piezoceramic materials, specifically according to following
Step is implemented：
Step 1, by basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5Ball is carried out after mixing
Mill processing, forms mixed powder, is calcined after mixed powder is dried, obtain niobic acid nickel presoma powder NiNb2O6；
Step 2, elder generation are according to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric proportion weigh respectively
Lead oxide powder Pb3O4, titanium dioxide powder TiO2, hafnium oxide powder HfO2And the niobic acid nickel powder body obtained in step 1
NiNb2O6, then ball-milling treatment will be carried out after all materials weighed mixing, matrix mixed powder is obtained, finally by matrix mixed powder
Material is dried, calcined and cooling treatment successively, obtains hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O3-Pb(NiNb)O3；
Step 3, weigh fluorination powder for lithium LiF, will be through hafnium lead titanates made from step 2-lead nickle niobate powder Pb (TiHf)
O3-Pb(NiNb)O3Carried out after being mixed with fluorination powder for lithium LiF after ball-milling treatment, then drying processing, obtain pre-synthesis dry powder
Material；
Step 4, preparation PVA solution, PVA solution are added to the pre-synthesis dry mash obtained through step 3 and granulated, then
By the processing selection granule that sieves, idiosome is made after dry-pressing formed processing in obtained granule afterwards；
Step 5, dumping processing first is carried out to obtaining idiosome through step 4, then carry out furnace cooling processing, then at high temperature
It is sintered, finally gives PHT-PNN piezoceramic materials.
The features of the present invention is also resided in：
Step 1 is specifically implemented according to following steps：
Step 1.1, according to mol ratio be 1：2.5~3.5 weigh basic nickel carbonate powder NiCO respectively3-2Ni(OH)2-
4H2O and niobium oxide powder Nb2O5；
Step 1.2, by the basic nickel carbonate powder NiCO weighed in step 1.13-2Ni(OH)2-4H2O and niobium oxide powder
Nb2O5Mix, be subsequently poured into planetary ball mill, then absolute ethyl alcohol and abrading-ball are added into planetary ball mill, pass through
After ball-milling treatment, well mixed mixed powder is obtained；
Step 1.3, the mixed powder obtained through step 1.2 is placed in baking oven carries out drying and processing, obtain mixed powder
Material；
Step 1.4, the mixed powder material obtained through step 1.3 poured into crucible, and by mixed powder material in crucible
Compacting, then lid is capped on crucible, make to form confined space in crucible, the crucible be positioned in chamber type electric resistance furnace afterwards,
In the mixed powder material under air atmosphere and 1050 DEG C~1150 DEG C temperature conditionss in calcining at constant temperature crucible, heating rate control exists
3 DEG C/min~5 DEG C/min, calcination time control is 1.5h~2.5h；
Step 1.5, treat calcining in step 1.4 after the completion of, crucible is taken out from chamber type electric resistance furnace, treats that crucible is naturally cold
But room temperature is arrived, niobic acid nickel presoma powder NiNb is formed in crucible2O6。
In step 1.2：The consumption of ball-milling medium absolute ethyl alcohol treats that ball milling powder will add 0.6ml~1.2ml for every gram
Absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is (1.5~3)：1；During ball milling
Between be 10h~14h；
In step 1.3：The temperature control of drying is 80 DEG C~100 DEG C.
Step 2 is specifically implemented according to following steps：
Step 2.1, according to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric proportion weighs oxygen respectively
Change lead powder body Pb3O4, titanium oxide powder TiO2, hafnium oxide powder HfO2And the niobic acid nickel powder body NiNb obtained in step 12O6,
Form matrix mixed powder；
Step 2.2, the matrix mixed powder and abrading-ball that are obtained through step 2.1 be added in ball grinder together, then to ball
Absolute ethyl alcohol is added in grinding jar, after ball-milling treatment, matrix mixed powder is obtained；
Step 2.3, the matrix mixed powder obtained through step 2.2 is placed in baking oven carries out drying and processing, obtain matrix
Mixed powder material；
Step 2.4, the matrix mixed powder material obtained through step 2.3 poured into crucible, and by matrix mixed powder material
Lid is capped in crucible and compacting, then on crucible, makes to form confined space in crucible, the crucible is positioned over chamber type electric resistance furnace
In, in the matrix mixed powder material under air atmosphere and 750 DEG C~900 DEG C temperature conditionss in calcining at constant temperature crucible, heating rate
Control is 1.5h~2.5h in 3 DEG C/min~5 DEG C/min, calcination time control；
Step 2.5, treat calcining in step 2.4 after the completion of, crucible is taken out from chamber type electric resistance furnace, makes crucible naturally cold
But room temperature is arrived, hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O is formed in crucible3-Pb(NiNb)O3。
In step 2.2：During ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol treats that ball milling powder will for every gram
Add 0.6ml~1.2ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is：
(1.5~3)：1；Ball-milling Time is 10h~14h；
In step 2.3：The temperature control of drying is 80 DEG C~100 DEG C.
Step 3 is specifically implemented according to following steps：
Step 3.1, fluorination powder for lithium LiF is weighed, fluorination powder for lithium LiF mole is hafnium lead titanates-lead nickle niobate powder
Body Pb (TiHf) O3-Pb(NiNb)O3The 1.0%~5.0% of mole；
Step 3.2, by fluorination powder for lithium LiF and the hafnium lead titanates weighed in step 3.1-lead nickle niobate powder Pb (TiHf)
O3-Pb(NiNb)O3It is added to after mixing in ball grinder, then abrading-ball and absolute ethyl alcohol is added into ball grinder, after ball-milling treatment,
Obtain pre-synthesis powder；
Step 3.3, the pre-synthesis powder obtained through step 3.2 is placed in baking oven carries out drying and processing, obtain pre-synthesis
Dry mash.
In step 3.2：During ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol treats that ball milling powder will for every gram
Add 0.6ml~1.2ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is
(1.5~3)：1；Ball-milling Time is 10h~14h；
In step 3.3：The temperature control of drying is 80 DEG C~100 DEG C.
Step 4 is specifically implemented according to following steps：
Step 4.1, weigh PVA and be dissolved in the water, make the PVA solution that mass percent concentration is 4%~7%；
Step 4.2, the PVA solution made through step 4.1 is added in the pre-synthesis dry mash obtained through step 3
Row granulation is handled, and obtains granule；
0.1ml~0.2ml PVA solution is added in every gram of pre-synthesis dry mash；
Step 4.3, through after step 4.2, the granule of shaping is crossed into the sieve that aperture is 80 mesh, wherein particle diameter is rejected larger
Granule；
Step 4.4, will be sieved through step 4.3 after obtained granule in dry-pressing formed system under 90Mpa~110Mpa pressure
Into idiosome.
Step 5 is specifically implemented according to following steps：
Step 5.1, under the conditions of 600 DEG C~700 DEG C, to through step 4 obtain idiosome carry out dumping processing, it is then cold with stove
But to room temperature；
Step 5.2, the idiosome after being handled through step 5.1 is put into chamber type electric resistance furnace, under air atmosphere, with 2.5 DEG C/
Chamber type electric resistance furnace is warming up to 1100 DEG C~1250 DEG C by min~3.5 DEG C/min speed, and Isothermal sinter 1.5h~2.5h is produced
To PHT-PNN piezoceramic materials.
The process of dumping is specially in step 5.1：
In under air atmosphere, chamber type electric resistance furnace is warming up to by 120 DEG C, constant temperature with 2.5 DEG C/min~3.5 DEG C/min speed
0.5h, is continuously heating to 600 DEG C~700 DEG C, constant temperature 2h completes idiosome with 2.5 DEG C/min~3.5 DEG C/min speed afterwards
Dumping.
The beneficial effects of the present invention are：
(1) in the preparation process in accordance with the present invention, using traditional solid reaction process, technique that is simple, being easily achieved is passed through
Fluorination lithium doping hafnium lead titanates-lead nickle niobate piezoceramic material of high tension performance, and its piezoelectric constant d can be prepared33
Reach as high as 957pC/N；
(2) piezoceramic material prepared using the preparation method of the present invention, available for piezoelectric constant d33Have higher
It is required that device, such as：New big displacement driver, the underwater acoustic transducer of efficient transmission, medical sonac etc., with very
Big economic and social benefit.
Embodiment
With reference to embodiment, the present invention is described in detail.
A kind of preparation method of PHT-PNN piezoceramic materials of the present invention, specifically implements according to following steps：
Step 1, by basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5Ball is carried out after mixing
Mill processing, forms mixed powder；Calcined after mixed powder is dried, obtain niobic acid nickel presoma powder NiNb2O6, specifically
Implement according to following steps：
Step 1.1, according to mol ratio be 1：2.5~3.5 weigh basic nickel carbonate powder NiCO respectively3-2Ni(OH)2-
4H2O and niobium oxide powder Nb2O5；
Wherein, basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2O purity is 99.9%, niobium oxide powder Nb2O5's
Purity is 99.9%；
Step 1.2, by the basic nickel carbonate powder NiCO weighed in step 1.13-2Ni(OH)2-4H2O and niobium oxide powder
Nb2O5Mix, be subsequently poured into planetary ball mill, then absolute ethyl alcohol and abrading-ball are added into planetary ball mill, pass through
After ball-milling treatment, well mixed mixed powder is obtained；
During ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol treats that ball milling powder will add 0.6ml for every gram
~1.2ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is：(1.5~3)：
1；Ball-milling Time is 10h~14h；
Step 1.3, the mixed powder obtained through step 1.2 is placed in baking oven carries out drying and processing, obtain mixed powder
Material；
Wherein, the temperature control of drying is 80 DEG C~100 DEG C；
Step 1.4, the mixed powder material obtained through step 1.3 poured into crucible, and by mixed powder material in crucible
Compacting, then lid is capped on crucible, make to form confined space in crucible, the crucible be positioned in chamber type electric resistance furnace afterwards,
In the mixed powder material under air atmosphere and 1050 DEG C~1150 DEG C temperature conditionss in calcining at constant temperature crucible, heating rate control exists
3 DEG C/min~5 DEG C/min, calcination time control is 1.5h~2.5h；
Step 1.5, treat calcining in step 1.4 after the completion of, crucible is taken out from chamber type electric resistance furnace, treats that crucible is naturally cold
But room temperature is arrived, niobic acid nickel presoma powder NiNb is formed in crucible2O6。
Step 2, elder generation are according to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric proportion weigh respectively
Lead oxide powder Pb3O4, titanium dioxide powder TiO2, hafnium oxide powder HfO2And the niobic acid nickel powder body obtained in step 1
NiNb2O6, then ball-milling treatment will be carried out after all materials weighed mixing, matrix mixed powder is obtained, finally by matrix mixed powder
Material is dried, calcined and cooling treatment successively, obtains hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O3-Pb(NiNb)O3,
Specifically implement according to following steps：
Step 2.1, according to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric proportion weighs oxygen respectively
Change lead powder body Pb3O4, titanium oxide powder TiO2, hafnium oxide powder HfO2And the niobic acid nickel powder body NiNb obtained in step 12O6,
Form matrix mixed powder；
Wherein, Pb3O4The purity of powder is 99.9%, TiO2The purity of powder is 99.9%, HfO2The purity of powder is
99.9%；
Step 2.2, the matrix mixed powder and abrading-ball that are obtained through step 2.1 be added in ball grinder together, then to ball
Absolute ethyl alcohol is added in grinding jar, after ball-milling treatment, well mixed matrix mixed powder is obtained；
During ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol is：Every gram is treated that ball milling powder will add 0.6ml
~1.2ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is (1.5~3)：
1；Ball-milling Time is 10h~14h；
Step 2.3, the matrix mixed powder obtained through step 2.2 is placed in baking oven carries out drying and processing, obtain matrix
Mixed powder material；
Wherein, the temperature control of drying is 80 DEG C~100 DEG C；
Step 2.4, the matrix mixed powder material obtained through step 2.3 poured into crucible, and by matrix mixed powder material
Lid is capped in crucible and compacting, then on crucible, makes to form confined space in crucible, the crucible is positioned over chamber type electric resistance furnace
In, in the matrix mixed powder material under air atmosphere and 750 DEG C~900 DEG C temperature conditionss in calcining at constant temperature crucible, heating rate
Control is 1.5h~2.5h in 3 DEG C/min~5 DEG C/min, calcination time control；
Step 2.5, treat calcining in step 2.4 after the completion of, crucible is taken out from chamber type electric resistance furnace, makes crucible naturally cold
But room temperature is arrived, hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O is formed in crucible3-Pb(NiNb)O3。
Step 3, weigh fluorination powder for lithium LiF, will be through hafnium lead titanates made from step 2-lead nickle niobate powder Pb (TiHf)
O3-Pb(NiNb)O3Carried out after being mixed with fluorination powder for lithium LiF after ball-milling treatment, then drying processing, obtain pre-synthesis dry powder
Material, specifically implements according to following steps：
Step 3.1, fluorination powder for lithium LiF is weighed, fluorination powder for lithium LiF mole is hafnium lead titanates-lead nickle niobate powder
Body Pb (TiHf) O3-Pb(NiNb)O3The 1.0%~5.0% of mole；
Step 3.2, by fluorination powder for lithium LiF and the hafnium lead titanates weighed in step 3.1-lead nickle niobate powder Pb (TiHf)
O3-Pb(NiNb)O3It is added to after mixing in ball grinder, then abrading-ball and absolute ethyl alcohol is added into ball grinder, after ball-milling treatment,
Obtain pre-synthesis powder；
During ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol treats that ball milling powder will add 0.6ml for every gram
~1.2ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is (1.5~3)：
1；Ball-milling Time is 10h~14h；
Step 3.3, the pre-synthesis powder obtained through step 3.2 is placed in baking oven carries out drying and processing, obtain pre-synthesis
Dry mash；
Wherein, the temperature control of drying is 80 DEG C~100 DEG C；
Step 4, preparation PVA solution, PVA solution are added to the pre-synthesis dry mash obtained through step 3 and granulated, then
By the processing selection granule that sieves, idiosome is made in obtained granule after dry-pressing formed processing afterwards, specifically according to following step
It is rapid to implement：
Step 4.1, weigh PVA and be dissolved in the water, make the PVA solution that mass percent concentration is 4%~7%；
Step 4.2, the PVA solution made through step 4.1 is added in the pre-synthesis dry mash obtained through step 3
Row granulation is handled, and obtains granule；
Wherein, 0.1ml~0.2ml PVA solution is added in every gram of pre-synthesis dry mash；
Step 4.3, through after step 4.2, the granule of shaping is crossed into the sieve that aperture is 80 mesh, wherein particle diameter is rejected larger
Granule；
Step 4.4, will be sieved through step 4.3 after obtained granule in dry-pressing formed system under 90Mpa~110Mpa pressure
Into idiosome；
Wherein, idiosome is Ф 10mm × (0.5~1.5) mm cylindrical type idiosome；
Step 5, dumping processing first is carried out to obtaining idiosome through step 4, then carry out furnace cooling processing, then at high temperature
It is sintered, finally gives PHT-PNN piezoceramic materials, specifically implement according to following steps：
Step 5.1, under the conditions of 600 DEG C~700 DEG C, to through step 4 obtain idiosome carry out dumping processing, it is then cold with stove
But to room temperature；
Dumping process is specific as follows：
In under air atmosphere, chamber type electric resistance furnace is warming up to by 120 DEG C, constant temperature with 2.5 DEG C/min~3.5 DEG C/min speed
0.5h, is continuously heating to 600 DEG C~700 DEG C, constant temperature 2h completes idiosome with 2.5 DEG C/min~3.5 DEG C/min speed afterwards
Dumping；
Step 5.2, the idiosome after being handled through step 5.1 is put into chamber type electric resistance furnace, under air atmosphere, with 2.5 DEG C/
Chamber type electric resistance furnace is warming up to 1100 DEG C~1250 DEG C by min~3.5 DEG C/min speed, and Isothermal sinter 1.5h~2.5h is produced
To high performance fluorination lithium doping hafnium lead titanates-lead nickle niobate piezoceramic material, i.e. PHT-PNN piezoceramic materials.
Embodiment 1
It is 1 according to mol ratio：2.5 weigh basic nickel carbonate powder NiCO respectively3-2Ni(OH)2-4H2O and niobium oxide powder
Nb2O5, wherein, basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2O purity is 99.9%, niobium oxide powder Nb2O5It is pure
Spend for 99.9%；By the basic nickel carbonate powder NiCO weighed3-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5It is blended in one
Rise, be subsequently poured into planetary ball mill, then absolute ethyl alcohol and abrading-ball are added into planetary ball mill, after ball-milling treatment,
Well mixed mixed powder is obtained, during ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol treats ball milling for every gram
Powder will add 0.6ml absolute ethyl alcohol, and abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is
1.5：1, Ball-milling Time is 10h；Obtained mixed powder is placed in the baking oven that temperature is 80 DEG C and carries out drying and processing, is mixed
Close dry mash；Obtained mixed powder material is poured into crucible, and by mixed powder material in crucible and compacting, then on crucible plus
Lid lid, makes to form confined space in crucible, the crucible is positioned in chamber type electric resistance furnace afterwards, in air atmosphere and 1050 DEG C
Mixed powder material under temperature conditionss in calcining at constant temperature crucible, heating rate is controlled in 3 DEG C/min, and calcination time control is
2.5h；Wait after the completion of calcining, crucible is taken out from chamber type electric resistance furnace, treats that crucible naturally cools to room temperature, formed in crucible
Niobic acid nickel presoma powder NiNb2O6；
According to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric proportion weighs lead oxide powder respectively
Pb3O4, titanium oxide powder TiO2, hafnium oxide powder HfO2And obtained niobic acid nickel powder body NiNb2O6, form matrix mixed powder
Body, wherein, Pb3O4The purity of powder is 99.9%, TiO2The purity of powder is 99.9%, HfO2The purity of powder is 99.9%；
Obtained matrix mixed powder and abrading-ball are added in ball grinder together, then absolute ethyl alcohol is added into ball grinder, through ball milling
After processing, well mixed matrix mixed powder is obtained, during ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol is every
Gram treat that ball milling powder will add 0.6ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material
Mass ratio is 1.5：1, Ball-milling Time is 10h；Obtained matrix mixed powder is placed in the baking oven that temperature is 80 DEG C and dried
Dry-cure, obtains matrix mixed powder material；Obtained matrix mixed powder material is poured into crucible, and by matrix mixed powder material
Lid is capped in crucible and compacting, then on crucible, makes to form confined space in crucible, the crucible is positioned over chamber type electric resistance furnace
In, in the matrix mixed powder material under air atmosphere and 750 DEG C of temperature conditionss in calcining at constant temperature crucible, heating rate is controlled 3
DEG C/min, calcination time control is 2.5h；Wait after the completion of calcining, crucible is taken out from chamber type electric resistance furnace, makes crucible naturally cold
But room temperature is arrived, hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O is formed in crucible3-Pb(NiNb)O3；
Fluorination powder for lithium LiF is weighed, fluorination powder for lithium LiF mole is hafnium lead titanates-lead nickle niobate powder Pb
(TiHf)O3-Pb(NiNb)O3The 1.0% of mole；By fluorination powder for lithium LiF and hafnium lead titanates-the lead nickle niobate powder weighed
Pb(TiHf)O3-Pb(NiNb)O3It is added to after mixing in ball grinder, then abrading-ball and absolute ethyl alcohol is added into ball grinder, through ball
After mill processing, pre-synthesis powder is obtained, during ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol is：Every gram is treated ball
Milling material will add 0.6ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is
1.5：1；Ball-milling Time is 10h；Obtained pre-synthesis powder is placed in temperature to carry out drying and processing in 80 DEG C of baking ovens, obtains pre-
Synthesize dry mash；
Weigh PVA to be dissolved in the water, make the PVA solution that mass percent concentration is 4%；The PVA made is molten
Liquid is added to progress granulation processing in pre-synthesis dry mash, obtains granule, wherein, to be added in every gram of pre-synthesis dry mash
0.1ml PVA solution；The granule of shaping is crossed into the sieve that aperture is 80 mesh, the wherein larger granule of particle diameter is rejected；After sieving
Idiosome is made in dry-pressing formed under 90Mpa pressure in obtained granule, wherein, idiosome is Ф 10mm × 0.5mm cylindrical type embryo
Body；
Under the conditions of 600 DEG C, dumping processing is carried out to obtaining idiosome, room temperature is then cooled to the furnace；The process tool of dumping
Body is：In under air atmosphere, chamber type electric resistance furnace is warming up to by 120 DEG C, constant temperature 0.5h, afterwards with 2.5 with 2.5 DEG C/min speed
DEG C/min speed is continuously heating to 600 DEG C, constant temperature 2h completes idiosome dumping；
Idiosome after processing is put into chamber type electric resistance furnace, under air atmosphere, with 2.5 DEG C/min speed by box electricity
Resistance stove is warming up to 1100 DEG C, and Isothermal sinter 1.5h obtains PHT-PNN piezoceramic materials.
Embodiment 2
It is 1 according to mol ratio：2.8 weigh basic nickel carbonate powder NiCO respectively3-2Ni(OH)2-4H2O and niobium oxide powder
Nb2O5, wherein, basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2O purity is 99.9%, niobium oxide powder Nb2O5It is pure
Spend for 99.9%；By the basic nickel carbonate powder NiCO weighed3-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5It is blended in one
Rise, be subsequently poured into planetary ball mill, then absolute ethyl alcohol and abrading-ball are added into planetary ball mill, after ball-milling treatment,
Well mixed mixed powder is obtained, during ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol treats ball milling for every gram
Powder will add 0.8ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is 2：
1；Ball-milling Time is 11h；Obtained mixed powder is placed in temperature to carry out drying and processing in 85 DEG C of baking ovens, mixed powder is obtained
Material；Obtained mixed powder material is poured into crucible, and by mixed powder material in crucible and compacting, then the capping lid on crucible
Son, makes to form confined space in crucible, the crucible is positioned in chamber type electric resistance furnace afterwards, in air atmosphere and 1080 DEG C of temperature
Under the conditions of mixed powder material in calcining at constant temperature crucible, heating rate control is 2h in 3.5 DEG C/min, calcination time control；Treat
After the completion of calcining, crucible is taken out from chamber type electric resistance furnace, crucible is naturally cooled to room temperature, formed in crucible before niobic acid nickel
Drive body powder NiNb2O6；
According to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric proportion weighs lead oxide powder respectively
Pb3O4, titanium oxide powder TiO2, hafnium oxide powder HfO2And obtained niobic acid nickel powder body NiNb2O6, form matrix mixed powder
Body, wherein, Pb3O4The purity of powder is 99.9%, TiO2The purity of powder is 99.9%, HfO2The purity of powder is 99.9%；
Obtained matrix mixed powder and abrading-ball are added in ball grinder together, then absolute ethyl alcohol is added into ball grinder, through ball milling
After processing, well mixed matrix mixed powder is obtained, during ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol is every
Gram treat that ball milling powder will add 0.8ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material
Mass ratio is 2：1；Ball-milling Time is 11h；Obtained matrix mixed powder is placed in the baking oven that temperature is 85 DEG C and dried
Processing, obtains matrix mixed powder material；Obtained matrix mixed powder material is poured into crucible, and matrix mixed powder material is existed
Crucible and compacting, then lid is capped on crucible, make to form confined space in crucible, the crucible is positioned over chamber type electric resistance furnace
In, in the matrix mixed powder material under air atmosphere and 800 DEG C of temperature conditionss in calcining at constant temperature crucible, heating rate control exists
3.5 DEG C/min, calcination time control is 2h；Wait after the completion of calcining, crucible is taken out from chamber type electric resistance furnace, makes crucible naturally cold
But room temperature is arrived, hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O is formed in crucible3-Pb(NiNb)O3；
Fluorination powder for lithium LiF is weighed, fluorination powder for lithium LiF mole is hafnium lead titanates-lead nickle niobate powder Pb
(TiHf)O3-Pb(NiNb)O3The 2.0% of mole；By fluorination powder for lithium LiF and hafnium lead titanates-the lead nickle niobate powder weighed
Pb(TiHf)O3-Pb(NiNb)O3It is added to after mixing in ball grinder, then abrading-ball and absolute ethyl alcohol is added into ball grinder, through ball
After mill processing, pre-synthesis powder is obtained, during ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol is：Every gram is treated ball
Milling material will add 0.8ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is
2：1；Ball-milling Time is 11h；Obtained pre-synthesis powder is placed in the baking oven that temperature is 85 DEG C and carries out drying and processing, obtains pre-
Synthesize dry mash；
Weigh PVA to be dissolved in the water, make the PVA solution that mass percent concentration is 5%；The PVA made is molten
Liquid is added to progress granulation processing in pre-synthesis dry mash, obtains granule, wherein, to be added in every gram of pre-synthesis dry mash
0.15ml PVA solution；The granule of shaping is crossed into the sieve that aperture is 80 mesh, the wherein larger granule of particle diameter is rejected；Will sieving
Idiosome is made in dry-pressing formed under 95Mpa pressure in the granule obtained afterwards, wherein, idiosome is Ф 10mm × 1mm cylindrical type embryo
Body；
Under the conditions of 650 DEG C, dumping processing is carried out to obtaining idiosome, room temperature is then cooled to the furnace；The process tool of dumping
Body is：In under air atmosphere, chamber type electric resistance furnace is warming up to 120 DEG C with 3 DEG C/min speed, constant temperature 0.5h, afterwards with 3 DEG C/
Min speed is continuously heating to 650 DEG C, and constant temperature 2h completes idiosome dumping；
Idiosome after processing is put into chamber type electric resistance furnace, under air atmosphere, with 3 DEG C/min speed by box resistance
Stove is warming up to 1150 DEG C, Isothermal sinter 2h, i.e. PHT-PNN piezoceramic materials.
Embodiment 3
It is 1 according to mol ratio：3 weigh basic nickel carbonate powder NiCO respectively3-2Ni(OH)2-4H2O and niobium oxide powder
Nb2O5, wherein, basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2O purity is 99.9%, niobium oxide powder Nb2O5It is pure
Spend for 99.9%；By the basic nickel carbonate powder NiCO weighed3-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5It is blended in one
Rise, be subsequently poured into planetary ball mill, then absolute ethyl alcohol and abrading-ball are added into planetary ball mill, after ball-milling treatment,
Well mixed mixed powder is obtained, during ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol is：Every gram is treated ball milling
Powder will add 1.0ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is
2.5：1；Ball-milling Time is 12h；Obtained mixed powder is placed in temperature to carry out drying and processing in 90 DEG C of baking ovens, mixed
Dry mash；Obtained mixed powder material is poured into crucible, and by mixed powder material in crucible and compacting, then the capping on crucible
Lid, makes to form confined space in crucible, the crucible is positioned in chamber type electric resistance furnace afterwards, in air atmosphere and 1100 DEG C of temperature
Mixed powder material under the conditions of degree in calcining at constant temperature crucible, heating rate control is 2h in 4 DEG C/min, calcination time control；Treat
After the completion of calcining, crucible is taken out from chamber type electric resistance furnace, crucible is naturally cooled to room temperature, formed in crucible before niobic acid nickel
Drive body powder NiNb2O6；
According to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric proportion weighs lead oxide powder respectively
Pb3O4, titanium oxide powder TiO2, hafnium oxide powder HfO2And obtained niobic acid nickel powder body NiNb2O6, form matrix mixed powder
Body, wherein, Pb3O4The purity of powder is 99.9%, TiO2The purity of powder is 99.9%, HfO2The purity of powder is 99.9%；
Obtained matrix mixed powder and abrading-ball are added in ball grinder together, then absolute ethyl alcohol is added into ball grinder, through ball milling
After processing, well mixed matrix mixed powder is obtained, during ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol is every
Gram treat that ball milling powder will add 1.0ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material
Mass ratio is 2：1；Ball-milling Time is 12h；Obtained matrix mixed powder is placed in temperature to carry out at drying in 90 DEG C of baking ovens
Reason, obtains matrix mixed powder material；Obtained matrix mixed powder material is poured into crucible, and by matrix mixed powder material in earthenware
It is compacted in crucible, then lid is capped on crucible, is made to form confined space in crucible, the crucible is positioned in chamber type electric resistance furnace,
In the matrix mixed powder material under air atmosphere and 850 DEG C of temperature conditionss in calcining at constant temperature crucible, heating rate control 4 DEG C/
Min, calcination time control is 2h；Wait after the completion of calcining, crucible is taken out from chamber type electric resistance furnace, crucible is naturally cooled to room
Temperature, forms hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O in crucible3-Pb(NiNb)O3。
Fluorination powder for lithium LiF is weighed, fluorination powder for lithium LiF mole is hafnium lead titanates-lead nickle niobate powder Pb
(TiHf)O3-Pb(NiNb)O3The 3.0% of mole；By fluorination powder for lithium LiF and hafnium lead titanates-the lead nickle niobate powder weighed
Pb(TiHf)O3-Pb(NiNb)O3It is added to after mixing in ball grinder, then abrading-ball and absolute ethyl alcohol is added into ball grinder, through ball
After mill processing, pre-synthesis powder is obtained, during ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol is：Every gram is treated ball
Milling material will add 1.0ml absolute ethyl alcohol, and abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is
2：1；Ball-milling Time is 12h；Obtained pre-synthesis powder is placed in temperature to carry out drying and processing in 90 DEG C of baking ovens, pre- conjunction is obtained
Into dry mash；
Weigh PVA to be dissolved in the water, make the PVA solution that mass percent concentration is 5.5%；By the PVA made
Solution is added to progress granulation processing in pre-synthesis dry mash, obtains granule, wherein, to be added in every gram of pre-synthesis dry mash
0.18ml PVA solution；The granule of shaping is crossed into the sieve that aperture is 80 mesh, the wherein larger granule of particle diameter is rejected；Will sieving
Idiosome is made in dry-pressing formed under 100Mpa pressure in the granule obtained afterwards, wherein, idiosome is Ф 10mm × 1mm cylindrical type embryo
Body；
Under the conditions of 680 DEG C, to carrying out dumping processing through obtaining idiosome, room temperature is then cooled to the furnace；The process of dumping
Specially：In under air atmosphere, chamber type electric resistance furnace is warming up to by 120 DEG C, constant temperature 0.5h, afterwards with 3 with 3 DEG C/min speed
DEG C/min speed is continuously heating to 680 DEG C, constant temperature 2h completes idiosome dumping；
Idiosome after processing is put into chamber type electric resistance furnace, under air atmosphere, with 23 DEG C/min speed by box electricity
Resistance stove is warming up to 1200 DEG C, Isothermal sinter 1.5h, i.e. PHT-PNN piezoceramic materials.
Embodiment 4
It is 1 according to mol ratio：3 weigh basic nickel carbonate powder NiCO respectively3-2Ni(OH)2-4H2O and niobium oxide powder
Nb2O5, wherein, basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2O purity is 99.9%, niobium oxide powder Nb2O5It is pure
Spend for 99.9%；By the basic nickel carbonate powder NiCO weighed3-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5It is blended in one
Rise, be subsequently poured into planetary ball mill, then absolute ethyl alcohol and abrading-ball are added into planetary ball mill, after ball-milling treatment,
Well mixed mixed powder is obtained, during ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol is：Every gram is treated ball milling
Powder will add 0.9ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is
2.5：1；Ball-milling Time is 13h；Obtained mixed powder is placed in the baking oven that temperature is 95 DEG C and carries out drying and processing, is mixed
Close dry mash；Obtained mixed powder material is poured into crucible, and by mixed powder material in crucible and compacting, then on crucible plus
Lid lid, makes to form confined space in crucible, the crucible is positioned in chamber type electric resistance furnace afterwards, in air atmosphere and 1125 DEG C
Mixed powder material under temperature conditionss in calcining at constant temperature crucible, heating rate is controlled in 4.5 DEG C/min, and calcination time control is
1.5h；Wait after the completion of calcining, crucible is taken out from chamber type electric resistance furnace, crucible is naturally cooled to room temperature, formed in crucible
Niobic acid nickel presoma powder NiNb2O6；
According to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric proportion weighs lead oxide powder respectively
Pb3O4, titanium oxide powder TiO2, hafnium oxide powder HfO2And obtained niobic acid nickel powder body NiNb2O6, form matrix mixed powder
Body, wherein, Pb3O4The purity of powder is 99.9%, TiO2The purity of powder is 99.9%, HfO2The purity of powder is 99.9%；
Obtained matrix mixed powder and abrading-ball are added in ball grinder together, then absolute ethyl alcohol is added into ball grinder, through ball milling
After processing, well mixed matrix mixed powder is obtained, during ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol is：
Every gram is treated that ball milling powder will add 0.9ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball
It is 2.5 to expect mass ratio：1；Ball-milling Time is 13h；Obtained matrix mixed powder is placed in the baking oven that temperature is 95 DEG C and carried out
Drying and processing, obtains matrix mixed powder material；Obtained matrix mixed powder material is poured into crucible, and by matrix mixed powder
Material is capped lid in crucible and compacting, then on crucible, makes to form confined space in crucible, the crucible is positioned over into box resistance
In stove, in the matrix mixed powder material under air atmosphere and 850 DEG C of temperature conditionss in calcining at constant temperature crucible, heating rate control exists
4.5 DEG C/min, calcination time control is 1.5h；Wait after the completion of calcining, crucible is taken out from chamber type electric resistance furnace, make crucible natural
Room temperature is cooled to, hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O is formed in crucible3-Pb(NiNb)O3；
Fluorination powder for lithium LiF is weighed, fluorination powder for lithium LiF mole is hafnium lead titanates-lead nickle niobate powder Pb
(TiHf)O3-Pb(NiNb)O3The 4.0% of mole；By fluorination powder for lithium LiF and hafnium lead titanates-the lead nickle niobate powder weighed
Pb(TiHf)O3-Pb(NiNb)O3It is added to after mixing in ball grinder, then abrading-ball and absolute ethyl alcohol is added into ball grinder, through ball
After mill processing, pre-synthesis powder is obtained, during ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol is：Every gram is treated ball
Milling material will add 0.9ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is
2.5：1；Ball-milling Time is 13h；Obtained pre-synthesis powder is placed in the baking oven that temperature is 95 DEG C and carries out drying and processing, is obtained
Pre-synthesis dry mash；
Weigh PVA to be dissolved in the water, make the PVA solution that mass percent concentration is 6%；The PVA made is molten
Liquid is added to progress granulation processing in pre-synthesis dry mash, obtains granule, wherein, to be added in every gram of pre-synthesis dry mash
0.2ml PVA solution；The granule of shaping is crossed into the sieve that aperture is 80 mesh, the wherein larger granule of particle diameter is rejected；After sieving
Idiosome is made in dry-pressing formed under 100Mpa pressure in obtained granule；Wherein, idiosome is Ф 10mm × 1.5mm cylindrical type embryo
Body；
Under the conditions of 700 DEG C, dumping processing is carried out to obtaining idiosome, room temperature is then cooled to the furnace；The process tool of dumping
Body is：In under air atmosphere, chamber type electric resistance furnace is warming up to by 120 DEG C, constant temperature 0.5h, afterwards with 3.5 with 3.5 DEG C/min speed
DEG C/min speed is continuously heating to 700 DEG C, constant temperature 2h completes idiosome dumping；
Idiosome after processing is put into chamber type electric resistance furnace, under air atmosphere, with 3.5 DEG C/min speed by box electricity
Resistance stove is warming up to 1225 DEG C, Isothermal sinter 2h, i.e. PHT-PNN piezoceramic materials.
Embodiment 5
It is 1 according to mol ratio：3.5 weigh basic nickel carbonate powder NiCO respectively3-2Ni(OH)2-4H2O and niobium oxide powder
Nb2O5, wherein, basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2O purity is 99.9%, niobium oxide powder Nb2O5It is pure
Spend for 99.9%；By the basic nickel carbonate powder NiCO weighed3-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5It is blended in one
Rise, be subsequently poured into planetary ball mill, then absolute ethyl alcohol and abrading-ball are added into planetary ball mill, after ball-milling treatment,
Well mixed mixed powder is obtained, during ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol is：Every gram is treated ball milling
Powder will add 1.2ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is 3：
1；Ball-milling Time is 14h；Obtained mixed powder is placed in the baking oven that temperature is 100 DEG C and carries out drying and processing, is mixed
Dry mash；Obtained mixed powder material is poured into crucible, and by mixed powder material in crucible and compacting, then the capping on crucible
Lid, makes to form confined space in crucible, the crucible is positioned in chamber type electric resistance furnace afterwards, in air atmosphere and 1150 DEG C of temperature
Mixed powder material under the conditions of degree in calcining at constant temperature crucible, heating rate control is 1.5h in 5 DEG C/min, calcination time control；
Wait after the completion of calcining, crucible is taken out from chamber type electric resistance furnace, crucible is naturally cooled to room temperature, niobic acid nickel is formed in crucible
Presoma powder NiNb2O6；
According to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric proportion weighs lead oxide powder respectively
Pb3O4, titanium oxide powder TiO2, hafnium oxide powder HfO2And the niobic acid nickel powder body NiNb obtained in step 12O6, form matrix
Mixed powder, wherein, Pb3O4The purity of powder is 99.9%, TiO2The purity of powder is 99.9%, HfO2The purity of powder is
99.9%；Obtained matrix mixed powder and abrading-ball are added in ball grinder together, then add into ball grinder absolute ethyl alcohol,
After ball-milling treatment, well mixed matrix mixed powder, during ball-milling treatment, the use of ball-milling medium absolute ethyl alcohol are obtained
Measure and be：Every gram is treated that ball milling powder will add ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and
Ball material mass ratio is 3：1；Ball-milling Time is 14h；Obtained matrix mixed powder is placed in temperature to be dried in 100 DEG C of baking ovens
Dry-cure, obtains matrix mixed powder material；Obtained matrix mixed powder material is poured into crucible, and by matrix mixed powder material
Lid is capped in crucible and compacting, then on crucible, makes to form confined space in crucible, the crucible is positioned over chamber type electric resistance furnace
In, in the matrix mixed powder material under air atmosphere and 900 DEG C of temperature conditionss in calcining at constant temperature crucible, heating rate is controlled 5
DEG C/min, calcination time control is 1.5h；Wait after the completion of calcining, crucible is taken out from chamber type electric resistance furnace, makes crucible naturally cold
But room temperature is arrived, hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O is formed in crucible3-Pb(NiNb)O3；
Fluorination powder for lithium LiF is weighed, fluorination powder for lithium LiF mole is hafnium lead titanates-lead nickle niobate powder Pb
(TiHf)O3-Pb(NiNb)O3The 5.0% of mole；By fluorination powder for lithium LiF and hafnium lead titanates-the lead nickle niobate powder weighed
Pb(TiHf)O3-Pb(NiNb)O3It is added to after mixing in ball grinder, then abrading-ball and absolute ethyl alcohol is added into ball grinder, through ball
After mill processing, pre-synthesis powder is obtained, during ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol is：Every gram is treated ball
Milling material will add 1.2ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is
3：1；Ball-milling Time is 14h；Obtained pre-synthesis powder is placed in the baking oven that temperature is 100 DEG C and carries out drying and processing, is obtained
Pre-synthesis dry mash；
Weigh PVA to be dissolved in the water, make the PVA solution that mass percent concentration is 7%；The PVA made is molten
Liquid is added to progress granulation processing in pre-synthesis dry mash, obtains granule, wherein, to be added in every gram of pre-synthesis dry mash
0.2ml PVA solution；The granule of shaping is crossed into the sieve that aperture is 80 mesh, the wherein larger granule of particle diameter is rejected；After sieving
Idiosome is made in dry-pressing formed under 110Mpa pressure in obtained granule, and idiosome is Ф 10mm × 1.5mm cylindrical type idiosome；
Under the conditions of 700 DEG C, dumping processing is carried out to obtaining idiosome through step 4, room temperature is then cooled to the furnace；Dumping
Process is specially：In under air atmosphere, chamber type electric resistance furnace is warming up to 120 DEG C with 3.5 DEG C/min speed, constant temperature 0.5h, it
700 DEG C are continuously heating to 3.5 DEG C/min speed afterwards, constant temperature 2h completes idiosome dumping；
Idiosome after processing is put into chamber type electric resistance furnace, under air atmosphere, with 3.5 DEG C/min speed by box electricity
Resistance stove is warming up to 1250 DEG C, Isothermal sinter 1.5h, i.e. PHT-PNN piezoceramic materials.
The PHT-PNN piezoelectric ceramics materials prepared using a kind of preparation method of PHT-PNN piezoceramic materials of the invention
Material, after by silver metallized processing, polarize 20min under 2kV/cm~3kV/cm polarized electric field, then under room temperature condition
24h is stood again, its piezoelectric property is tested afterwards, and specific test result refers to table 1.
Be the same as Example does not prepare the piezoelectric property parameters of hafnium lead titanates-lead nickle niobate piezoelectric ceramics to table 1
A kind of preparation method of PHT-PNN piezoceramic materials of the present invention, passes through technique that is simple and being easily achieved
Fluorination lithium doping hafnium lead titanates-lead nickle niobate piezoceramic material of high tension performance is prepared, as can be seen from Table 1：It is pressed
Electric constant d33Reach as high as 957pC/N.
Claims (10)
1. a kind of preparation method of PHT-PNN piezoceramic materials, it is characterised in that specifically implement according to following steps：
Step 1, by basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5Carried out after mixing at ball milling
Reason, forms mixed powder, is calcined after mixed powder is dried, obtain niobic acid nickel presoma powder NiNb2O6；
Step 2, elder generation are according to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric proportion weigh oxidation respectively
Lead powder body Pb3O4, titanium dioxide powder TiO2, hafnium oxide powder HfO2And the niobic acid nickel powder body NiNb obtained in step 12O6,
Ball-milling treatment is carried out after all materials weighed are mixed again, matrix mixed powder is obtained, finally mixed powder by matrix successively
Dried, calcined and cooling treatment, obtain hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O3-Pb(NiNb)O3；
Step 3, weigh fluorination powder for lithium LiF, will be through hafnium lead titanates made from step 2-lead nickle niobate powder Pb (TiHf) O3-Pb
(NiNb)O3Carried out after being mixed with fluorination powder for lithium LiF after ball-milling treatment, then drying processing, obtain pre-synthesis dry mash；
Step 4, preparation PVA solution, PVA solution are added to the pre-synthesis dry mash obtained through step 3 and granulated, then passed through
Sieving processing selection granule, is made idiosome by obtained granule after dry-pressing formed processing afterwards；
Step 5, dumping processing first is carried out to obtaining idiosome through step 4, then carry out furnace cooling processing, then carry out at high temperature
Sintering processes, finally give PHT-PNN piezoceramic materials.
2. a kind of preparation method of PHT-PNN piezoceramic materials according to claim 1, it is characterised in that the step
Rapid 1 specifically implements according to following steps：
Step 1.1, according to mol ratio be 1：2.5~3.5 weigh basic nickel carbonate powder NiCO respectively3-2Ni(OH)2-4H2O and
Niobium oxide powder Nb2O5；
Step 1.2, by the basic nickel carbonate powder NiCO weighed in step 1.13-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5
Mix, be subsequently poured into planetary ball mill, then absolute ethyl alcohol and abrading-ball are added into planetary ball mill, through ball milling
After processing, well mixed mixed powder is obtained；
Step 1.3, the mixed powder obtained through step 1.2 is placed in baking oven carries out drying and processing, obtain mixed powder material；
Step 1.4, the mixed powder material obtained through step 1.3 poured into crucible, and by mixed powder material in crucible and compacting,
Lid is capped on crucible again, makes to form confined space in crucible, the crucible is positioned in chamber type electric resistance furnace afterwards, in air
Mixed powder material under atmosphere and 1050 DEG C~1150 DEG C temperature conditionss in calcining at constant temperature crucible, heating rate control 3 DEG C/
Min~5 DEG C/min, calcination time control is 1.5h~2.5h；
Step 1.5, treat calcining in step 1.4 after the completion of, crucible is taken out from chamber type electric resistance furnace, treats that crucible is naturally cooled to
Room temperature, forms niobic acid nickel presoma powder NiNb in crucible2O6。
3. a kind of preparation method of PHT-PNN piezoceramic materials according to claim 2, it is characterised in that the step
In rapid 1.2：
During the ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol treats that ball milling powder will add 0.6ml for every gram
~1.2ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is (1.5~3)：
1；Ball-milling Time is 10h~14h；
In the step 1.3, the temperature control of drying is 80 DEG C~100 DEG C.
4. a kind of preparation method of PHT-PNN piezoceramic materials according to claim 1, it is characterised in that the step
Rapid 2 specifically implement according to following steps：
Step 2.1, according to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric proportion weighs lead oxide respectively
Powder Pb3O4, titanium oxide powder TiO2, hafnium oxide powder HfO2And the niobic acid nickel powder body NiNb obtained in step 12O6, formed
Matrix mixed powder；
Step 2.2, the matrix mixed powder and abrading-ball that are obtained through step 2.1 be added in ball grinder together, then to ball grinder
Middle addition absolute ethyl alcohol, after ball-milling treatment, obtains matrix mixed powder；
Step 2.3, the matrix mixed powder obtained through step 2.2 is placed in baking oven carries out drying and processing, obtain matrix mixing
Dry mash；
Step 2.4, the matrix mixed powder material obtained through step 2.3 poured into crucible, and by matrix mixed powder material in earthenware
It is compacted in crucible, then lid is capped on crucible, is made to form confined space in crucible, the crucible is positioned in chamber type electric resistance furnace,
In the matrix mixed powder material under air atmosphere and 750 DEG C~900 DEG C temperature conditionss in calcining at constant temperature crucible, heating rate control
In 3 DEG C/min~5 DEG C/min, calcination time control is 1.5h~2.5h；
Step 2.5, treat calcining in step 2.4 after the completion of, crucible is taken out from chamber type electric resistance furnace, crucible is naturally cooled to
Room temperature, forms hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O in crucible3-Pb(NiNb)O3。
5. a kind of preparation method of PHT-PNN piezoceramic materials according to claim 4, it is characterised in that the step
In rapid 2.2：
During ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol for every gram treat ball milling powder to add 0.6ml~
1.2ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is：(1.5~3)：1；
Ball-milling Time is 10h~14h；
In the step 2.3, the temperature control of drying is 80 DEG C~100 DEG C.
6. a kind of preparation method of PHT-PNN piezoceramic materials according to claim 1, it is characterised in that the step
Rapid 3 specifically implement according to following steps：
Step 3.1, fluorination powder for lithium LiF is weighed, fluorination powder for lithium LiF mole is hafnium lead titanates-lead nickle niobate powder Pb
(TiHf)O3-Pb(NiNb)O3The 1.0%~5.0% of mole；
Step 3.2, by fluorination powder for lithium LiF and the hafnium lead titanates weighed in step 3.1-lead nickle niobate powder Pb (TiHf) O3-Pb
(NiNb)O3It is added to after mixing in ball grinder, then abrading-ball and absolute ethyl alcohol is added into ball grinder, after ball-milling treatment, obtains
Pre-synthesis powder；
Step 3.3, the pre-synthesis powder obtained through step 3.2 is placed in baking oven carries out drying and processing, obtain pre-synthesis dry powder
Material.
7. a kind of preparation method of PHT-PNN piezoceramic materials according to claim 6, it is characterised in that the step
In rapid 3.2：
During ball-milling treatment, the consumption of ball-milling medium absolute ethyl alcohol for every gram treat ball milling powder to add 0.6ml~
1.2ml absolute ethyl alcohol；Abrading-ball uses diameter 3mm~5mm zirconia ball, and ball material mass ratio is (1.5~3)：1；
Ball-milling Time is 10h~14h；
In the step 3.3, the temperature control of drying is 80 DEG C~100 DEG C.
8. a kind of preparation method of PHT-PNN piezoceramic materials according to claim 1, it is characterised in that the step
Rapid 4 specifically implement according to following steps：
Step 4.1, weigh PVA and be dissolved in the water, make the PVA solution that mass percent concentration is 4%~7%；
Step 4.2, the PVA solution made through step 4.1 is added in the pre-synthesis dry mash obtained through step 3 and made
Grain processing, obtains granule；
0.1ml~0.2ml PVA solution is added in every gram of pre-synthesis dry mash；
Step 4.3, through after step 4.2, the granule of shaping is crossed into the sieve that aperture is 80 mesh, the wherein larger group of particle diameter is rejected
Grain；
Step 4.4, will be sieved through step 4.3 after obtained granule embryo is made in dry-pressing formed under 90Mpa~110Mpa pressure
Body.
9. a kind of preparation method of PHT-PNN piezoceramic materials according to claim 1, it is characterised in that the step
Rapid 5 specifically implement according to following steps：
Step 5.1, under the conditions of 600 DEG C~700 DEG C, to through step 4 obtain idiosome carry out dumping processing, then cool to the furnace
Room temperature；
Step 5.2, the idiosome after being handled through step 5.1 is put into chamber type electric resistance furnace, under air atmosphere, with 2.5 DEG C/min
Chamber type electric resistance furnace is warming up to 1100 DEG C~1250 DEG C by~3.5 DEG C/min speed, and Isothermal sinter 1.5h~2.5h obtains
PHT-PNN piezoceramic materials.
10. the preparation method of a kind of PHT-PNN piezoceramic materials according to claim 9, it is characterised in that described
In step 5.1, the dumping process is specific as follows：
In under air atmosphere, chamber type electric resistance furnace is warming up to by 120 DEG C, constant temperature with 2.5 DEG C/min~3.5 DEG C/min speed
0.5h, is continuously heating to 600 DEG C~700 DEG C, constant temperature 2h completes idiosome with 2.5 DEG C/min~3.5 DEG C/min speed afterwards
Dumping.
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