CN107216130B - A kind of preparation method of PHT-PNN piezoceramic material - Google Patents
A kind of preparation method of PHT-PNN piezoceramic material Download PDFInfo
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Abstract
A kind of preparation method of PHT-PNN piezoceramic material 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 successively dried, calcined and cooled down, obtains hafnium lead titanates-lead nickle niobate powder；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 to pre-synthesis dry mash to be granulated, green body is made in obtained granule；Dumping, furnace cooling and high temperature sintering are carried out to green body and obtain PHT-PNN piezoceramic material.Preparation method of the 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 fields, and in particular to a kind of PHT-PNN piezoelectric ceramics material
The preparation method of material.
Background technique
Piezoelectric ceramics is a kind of functional material that can mutually convert mechanical energy and electric energy, by its preferable mechanical property
Can be with stable piezoelectric property the advantages that, the high-tech areas such as aviation, medical treatment, communication and detection have been widely used in it.
According to working principle, the application range of piezoelectric ceramics is broadly divided into two aspects of piezoelectric vibrator and energy converter.In piezoelectric vibrator
The application of aspect mainly has oscillator, resonator, filter, piezoelectric transformer and deferred mount etc.；In terms of energy converter
Using mainly thering is underwater acoustic transducer, high power altrasonic transducer, medical transducer, ultrasonic, piezo-electric motor and piezoelectricity to drive
Dynamic device etc..The different application of piezoelectric ceramics has different requirements to its performance, such as: as piezoelectric vibrator in use, needing to press
Electroceramics has preferable frequency stability and higher mechanical quality factor；As energy converter, then piezoelectric ceramics is required to have
There are biggish piezoelectric modulus and electromechanical coupling factor.But for the underwater acoustic transducer of novel big displacement driver, efficient transmission
And medical ultrasonic sensor, the piezoelectric ceramics piezoelectric modulus value developed at present is still lower, is not able to satisfy next-generation drive
Or demand of the energy converter to 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 process and doping
Property etc. has done a large amount of work, studies the Pb (B that more a kind of material is complex perovskite structure at present1B2)O3System；
Wherein B1To be cationic at a low price, such as: Mg2+、Zn2+、Fe3+、Ni2+And Sc3+Deng；B2For high-valence cationic, such as: Nb5+、Ta5+、Ti4+
And W6+Deng.Representative 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 process is complicated, sintering condition is more demanding, and piezoelectric constant d33It is difficult to dash forward
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 process, can get piezoelectric constant d33Greater than 850pC/
The high-performance of N.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of PHT-PNN piezoceramic material, utilize the preparation method
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 material, 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, calcines 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 ratio weigh respectively
Lead oxide powder Pb3O4, titanium dioxide powder TiO2, hafnium oxide powder HfO2And niobic acid nickel powder body obtained in step 1
NiNb2O6, then ball-milling treatment will be carried out after the mixing of weighed all materials, matrix mixed powder is obtained, finally by matrix mixed powder
Material is successively dried, is calcined and cooling treatment, and hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O is obtained3-Pb(NiNb)O3；
Step 3 weighs fluorination powder for lithium LiF, will be through the lead titanates of hafnium made from step 2-lead nickle niobate powder Pb (TiHf)
O3-Pb(NiNb)O3After carrying out ball-milling treatment, then drying processing after mixing with fluorination powder for lithium LiF, pre-synthesis dry powder is obtained
Material；
Step 4 prepares PVA solution, and PVA solution is added to the pre-synthesis dry mash obtained through step 3 and is granulated, then
Selection granule is handled by sieving, green body is made after dry-pressing formed processing in obtained granule later；
Step 5 first obtains green body progress dumping processing to through step 4, then carries out furnace cooling processing, then at high temperature
It is sintered, finally obtains PHT-PNN piezoceramic material.
The features of the present invention also characterized in that:
Step 1 is specifically implemented according to the following steps:
Step 1.1 is that 1:2.5~3.5 weigh basic nickel carbonate powder NiCO respectively according to molar ratio3-2Ni(OH)2-
4H2O and niobium oxide powder Nb2O5；
Step 1.2, by basic nickel carbonate powder NiCO weighed in step 1.13-2Ni(OH)2-4H2O and niobium oxide powder
Nb2O5It mixes, is subsequently poured into planetary ball mill, then add dehydrated alcohol and abrading-ball into planetary ball mill, warp
After ball-milling treatment, uniformly mixed mixed powder is obtained；
The mixed powder obtained through step 1.2 is placed in baking oven and carries out drying and processing by step 1.3, obtains mixed powder
Material；
Step 1.4 pours into the mixed powder material obtained through step 1.3 in crucible, and by mixed powder material in crucible
Compacting, then lid is covered on crucible, make to form confined space in crucible, the crucible be placed in chamber type electric resistance furnace later,
Mixed powder material under the conditions of air atmosphere and 1050 DEG C~1150 DEG C temperature in calcining at constant temperature crucible, heating rate control exist
3 DEG C/min~5 DEG C/min, calcination time control is 1.5h~2.5h；
Step 1.5, after the completion of the calcining in step 1.4, crucible is taken out from chamber type electric resistance furnace, it is naturally cold to crucible
But room temperature is arrived, forms niobic acid nickel presoma powder NiNb in crucible2O6。
In step 1.2: the dosage of ball-milling medium dehydrated alcohol, which is every gram, to ball milling powder will be added 0.6ml~1.2ml
Dehydrated alcohol；Abrading-ball using diameter 3mm~5mm zirconia ball, and ball material mass ratio be (1.5~3): 1；When 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 the following steps:
Step 2.1, according to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric ratio weighs oxygen respectively
Change lead powder body Pb3O4, titanium oxide powder TiO2, hafnium oxide powder HfO2And niobic acid nickel powder body NiNb obtained in step 12O6,
Form matrix mixed powder；
The matrix mixed powder and abrading-ball that obtain through step 2.1 are added in ball grinder by step 2.2 together, then to ball
Dehydrated alcohol is added in grinding jar, after ball-milling treatment, obtains matrix mixed powder；
The matrix mixed powder obtained through step 2.2 is placed in baking oven and carries out drying and processing by step 2.3, obtains matrix
Mixed powder material；
Step 2.4 pours into the matrix mixed powder material obtained through step 2.3 in crucible, and by matrix mixed powder material
In crucible and compacting, then lid is covered on crucible, make to form confined space in crucible, which is placed in chamber type electric resistance furnace
In, the matrix mixed powder material under the conditions of air atmosphere and 750 DEG C~900 DEG C temperature 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, after the completion of the calcining in step 2.4, crucible is taken out from chamber type electric resistance furnace, keeps crucible naturally cold
But room temperature is arrived, forms hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O in crucible3-Pb(NiNb)O3。
In step 2.2: during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol is every gram and wants to ball milling powder
The dehydrated alcohol of 0.6ml~1.2ml is added；Zirconia ball of the abrading-ball using diameter 3mm~5mm, and ball material mass ratio are as follows:
(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 the following steps:
Step 3.1 weighs fluorination powder for lithium LiF, and the mole of fluorination powder for lithium LiF 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 weighed in step 3.1 and hafnium lead titanates-lead nickle niobate powder Pb (TiHf)
O3-Pb(NiNb)O3It is added in ball grinder after mixing, then adds abrading-ball and dehydrated alcohol into ball grinder, after ball-milling treatment,
Obtain pre-synthesis powder；
The pre-synthesis powder obtained through step 3.2 is placed in baking oven and carries out drying and processing by step 3.3, obtains pre-synthesis
Dry mash.
In step 3.2: during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol is every gram and wants to ball milling powder
The dehydrated alcohol of 0.6ml~1.2ml is added；Abrading-ball is using the zirconia ball of diameter 3mm~5mm, 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 the following steps:
Step 4.1 weighs PVA and is dissolved in the water, and makes the PVA solution that mass percent concentration is 4%~7%；
Step 4.2, by the PVA solution made through step 4.1 be added in the pre-synthesis dry mash obtained through step 3 into
Row granulation processing, obtains granule；
The PVA solution of 0.1ml~0.2ml to be added in every gram of pre-synthesis dry mash；
Step 4.3, after step 4.2, by the granule of forming cross aperture be 80 mesh sieve, reject wherein partial size it is biggish
Granule；
Step 4.4, by the obtained granule dry-pressing formed system under the pressure of 90Mpa~110Mpa after step 4.3 sieving
At green body.
Step 5 is specifically implemented according to the following steps:
Step 5.1, under the conditions of 600 DEG C~700 DEG C, to through step 4 obtain green body carry out dumping processing, it is then cold with furnace
But to room temperature；
Step 5.2, will through step 5.1, treated that green body 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 rate, Isothermal sinter 1.5h~2.5h to get
To PHT-PNN piezoceramic material.
The process of dumping in step 5.1 specifically:
Under air atmosphere, chamber type electric resistance furnace is warming up to 120 DEG C with 2.5 DEG C/min~3.5 DEG C/min rate, constant temperature
0.5h is continuously heating to 600 DEG C~700 DEG C, constant temperature 2h later with 2.5 DEG C/min~3.5 DEG C/min rate, i.e. completion green body
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, pass through technique that is simple, being easily achieved
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 preparation method of the invention can be used for piezoelectric constant d33Have higher
It is required that device, such as: novel big displacement driver, the underwater acoustic transducer of efficient transmission, medical ultrasonic sensor, have very
Big economic and social benefit.
Specific embodiment
The present invention is described in detail With reference to embodiment.
A kind of preparation method of PHT-PNN piezoceramic material of the present invention, is specifically implemented according to the 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；It is calcined after mixed powder is dried, obtains niobic acid nickel presoma powder NiNb2O6, specifically
It follows the steps below to implement:
Step 1.1 is that 1:2.5~3.5 weigh basic nickel carbonate powder NiCO respectively according to molar ratio3-2Ni(OH)2-
4H2O and niobium oxide powder Nb2O5；
Wherein, basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2The purity of O is 99.9%, niobium oxide powder Nb2O5's
Purity is 99.9%；
Step 1.2, by basic nickel carbonate powder NiCO weighed in step 1.13-2Ni(OH)2-4H2O and niobium oxide powder
Nb2O5It mixes, is subsequently poured into planetary ball mill, then add dehydrated alcohol and abrading-ball into planetary ball mill, warp
After ball-milling treatment, uniformly mixed mixed powder is obtained；
During ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol, which is every gram, will be added 0.6ml to ball milling powder
The dehydrated alcohol of~1.2ml；Zirconia ball of the abrading-ball using diameter 3mm~5mm, and ball material mass ratio are as follows: (1.5~3):
1；Ball-milling Time is 10h~14h；
The mixed powder obtained through step 1.2 is placed in baking oven and carries out drying and processing by step 1.3, obtains mixed powder
Material；
Wherein, the temperature control of drying is 80 DEG C~100 DEG C；
Step 1.4 pours into the mixed powder material obtained through step 1.3 in crucible, and by mixed powder material in crucible
Compacting, then lid is covered on crucible, make to form confined space in crucible, the crucible be placed in chamber type electric resistance furnace later,
Mixed powder material under the conditions of air atmosphere and 1050 DEG C~1150 DEG C temperature in calcining at constant temperature crucible, heating rate control exist
3 DEG C/min~5 DEG C/min, calcination time control is 1.5h~2.5h；
Step 1.5, after the completion of the calcining in step 1.4, crucible is taken out from chamber type electric resistance furnace, it is naturally cold to crucible
But room temperature is arrived, forms niobic acid nickel presoma powder NiNb in crucible2O6。
Step 2, elder generation are according to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric ratio weigh respectively
Lead oxide powder Pb3O4, titanium dioxide powder TiO2, hafnium oxide powder HfO2And niobic acid nickel powder body obtained in step 1
NiNb2O6, then ball-milling treatment will be carried out after the mixing of weighed all materials, matrix mixed powder is obtained, finally by matrix mixed powder
Material is successively dried, is calcined and cooling treatment, and hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O is obtained3-Pb(NiNb)O3,
It is specifically implemented according to the following steps:
Step 2.1, according to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric ratio weighs oxygen respectively
Change lead powder body Pb3O4, titanium oxide powder TiO2, hafnium oxide powder HfO2And 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%；
The matrix mixed powder and abrading-ball that obtain through step 2.1 are added in ball grinder by step 2.2 together, then to ball
Dehydrated alcohol is added in grinding jar, after ball-milling treatment, obtains uniformly mixed matrix mixed powder；
During ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol are as follows: every gram to ball milling powder will be added 0.6ml
The dehydrated alcohol of~1.2ml；Abrading-ball using diameter 3mm~5mm zirconia ball, and ball material mass ratio be (1.5~3):
1；Ball-milling Time is 10h~14h；
The matrix mixed powder obtained through step 2.2 is placed in baking oven and carries out drying and processing by step 2.3, obtains matrix
Mixed powder material；
Wherein, the temperature control of drying is 80 DEG C~100 DEG C；
Step 2.4 pours into the matrix mixed powder material obtained through step 2.3 in crucible, and by matrix mixed powder material
In crucible and compacting, then lid is covered on crucible, make to form confined space in crucible, which is placed in chamber type electric resistance furnace
In, the matrix mixed powder material under the conditions of air atmosphere and 750 DEG C~900 DEG C temperature 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, after the completion of the calcining in step 2.4, crucible is taken out from chamber type electric resistance furnace, keeps crucible naturally cold
But room temperature is arrived, forms hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O in crucible3-Pb(NiNb)O3。
Step 3 weighs fluorination powder for lithium LiF, will be through the lead titanates of hafnium made from step 2-lead nickle niobate powder Pb (TiHf)
O3-Pb(NiNb)O3After carrying out ball-milling treatment, then drying processing after mixing with fluorination powder for lithium LiF, pre-synthesis dry powder is obtained
Material, is specifically implemented according to the following steps:
Step 3.1 weighs fluorination powder for lithium LiF, and the mole of fluorination powder for lithium LiF 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 weighed in step 3.1 and hafnium lead titanates-lead nickle niobate powder Pb (TiHf)
O3-Pb(NiNb)O3It is added in ball grinder after mixing, then adds abrading-ball and dehydrated alcohol into ball grinder, after ball-milling treatment,
Obtain pre-synthesis powder；
During ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol, which is every gram, will be added 0.6ml to ball milling powder
The dehydrated alcohol of~1.2ml；Abrading-ball using diameter 3mm~5mm zirconia ball, and ball material mass ratio be (1.5~3):
1；Ball-milling Time is 10h~14h；
The pre-synthesis powder obtained through step 3.2 is placed in baking oven and carries out drying and processing by step 3.3, obtains pre-synthesis
Dry mash；
Wherein, the temperature control of drying is 80 DEG C~100 DEG C；
Step 4 prepares PVA solution, and PVA solution is added to the pre-synthesis dry mash obtained through step 3 and is granulated, then
Selection granule is handled by sieving, green body is made in obtained granule after dry-pressing formed processing later, specifically according to following step
It is rapid to implement:
Step 4.1 weighs PVA and is dissolved in the water, and makes the PVA solution that mass percent concentration is 4%~7%；
Step 4.2, by the PVA solution made through step 4.1 be added in the pre-synthesis dry mash obtained through step 3 into
Row granulation processing, obtains granule；
Wherein, the PVA solution of 0.1ml~0.2ml to be added in every gram of pre-synthesis dry mash；
Step 4.3, after step 4.2, by the granule of forming cross aperture be 80 mesh sieve, reject wherein partial size it is biggish
Granule；
Step 4.4, by the obtained granule dry-pressing formed system under the pressure of 90Mpa~110Mpa after step 4.3 sieving
At green body；
Wherein, green body is Ф 10mm × (0.5~1.5) mm cylindrical type green body；
Step 5 first obtains green body progress dumping processing to through step 4, then carries out furnace cooling processing, then at high temperature
It is sintered, finally obtains PHT-PNN piezoceramic material, be specifically implemented according to the following steps:
Step 5.1, under the conditions of 600 DEG C~700 DEG C, to through step 4 obtain green body carry out dumping processing, it is then cold with furnace
But to room temperature；
Dumping process is specific as follows:
Under air atmosphere, chamber type electric resistance furnace is warming up to 120 DEG C with 2.5 DEG C/min~3.5 DEG C/min rate, constant temperature
0.5h is continuously heating to 600 DEG C~700 DEG C, constant temperature 2h later with 2.5 DEG C/min~3.5 DEG C/min rate, i.e. completion green body
Dumping；
Step 5.2, will through step 5.1, treated that green body 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 rate, Isothermal sinter 1.5h~2.5h to get
To high performance fluorination lithium doping hafnium lead titanates-lead nickle niobate piezoceramic material, i.e. PHT-PNN piezoceramic material.
Embodiment 1
It is that 1:2.5 weighs basic nickel carbonate powder NiCO respectively according to molar ratio3-2Ni(OH)2-4H2O and niobium oxide powder
Nb2O5, wherein basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2The purity of O is 99.9%, niobium oxide powder Nb2O5It is pure
Degree is 99.9%；By weighed basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5It is blended in one
It rises, is subsequently poured into planetary ball mill, then add dehydrated alcohol and abrading-ball into planetary ball mill, after ball-milling treatment,
Uniformly mixed mixed powder is obtained, during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol is every gram to ball milling
Powder will be added the dehydrated alcohol of 0.6ml, and abrading-ball is using the zirconia ball of diameter 3mm~5mm, and ball material mass ratio is
1.5:1, Ball-milling Time 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 added on crucible
Lid lid makes to form confined space in crucible, the crucible is placed in chamber type electric resistance furnace later, in air atmosphere and 1050 DEG C
Mixed powder material under the conditions of temperature in calcining at constant temperature crucible, heating rate control are in 3 DEG C/min, calcination time control
2.5h；After the completion of calcining, crucible is taken out from chamber type electric resistance furnace, room temperature is naturally cooled to crucible, is formed in crucible
Niobic acid nickel presoma powder NiNb2O6；
According to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric ratio 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 dehydrated alcohol is added into ball grinder, through ball milling
After processing, uniformly mixed matrix mixed powder is obtained, during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol is every
Gram the dehydrated alcohol that 0.6ml to be added to ball milling powder；Zirconia ball of the abrading-ball using diameter 3mm~5mm, and ball material
Mass ratio is 1.5:1, Ball-milling Time 10h；Obtained matrix mixed powder is placed in the baking oven that temperature is 80 DEG C and is dried
Dry-cure obtains matrix mixed powder material；Obtained matrix mixed powder material is poured into crucible, and by matrix mixed powder material
In crucible and compacting, then lid is covered on crucible, make to form confined space in crucible, which is placed in chamber type electric resistance furnace
In, the matrix mixed powder material under the conditions of air atmosphere and 750 DEG C of temperature in calcining at constant temperature crucible, heating rate is controlled 3
DEG C/min, calcination time control is 2.5h；After the completion of calcining, crucible is taken out from chamber type electric resistance furnace, keeps crucible naturally cold
But room temperature is arrived, forms hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O in crucible3-Pb(NiNb)O3；
Fluorination powder for lithium LiF is weighed, the mole of fluorination powder for lithium LiF is hafnium lead titanates-lead nickle niobate powder Pb
(TiHf)O3-Pb(NiNb)O3The 1.0% of mole；By weighed fluorination powder for lithium LiF and hafnium lead titanates-lead nickle niobate powder
Pb(TiHf)O3-Pb(NiNb)O3It is added in ball grinder after mixing, then adds abrading-ball and dehydrated alcohol into ball grinder, through ball
Mill processing after, obtain pre-synthesis powder, during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol are as follows: every gram to ball
The dehydrated alcohol of 0.6ml will be added in milling material；Abrading-ball is using the zirconia ball of diameter 3mm~5mm, and ball material mass ratio is
1.5:1；Ball-milling Time is 10h；It is to carry out drying and processing in 80 DEG C of baking ovens that obtained pre-synthesis powder, which is placed in temperature, is obtained pre-
Synthesize dry mash；
It weighs PVA to be dissolved in the water, makes the PVA solution that mass percent concentration is 4%；The PVA made is molten
Liquid, which is added in pre-synthesis dry mash, carries out granulation processing, obtains granule, wherein to be added in every gram of pre-synthesis dry mash
The PVA solution of 0.1ml；The granule of forming is crossed into the sieve that aperture is 80 mesh, rejects the wherein biggish granule of partial size；After being sieved
Obtained granule is dry-pressing formed under the pressure of 90Mpa to be made green body, wherein green body is the cylinder parison of Ф 10mm × 0.5mm
Body；
Under the conditions of 600 DEG C, dumping processing is carried out to green body is obtained, then cools to room temperature with the furnace；The process of dumping has
Body are as follows: under air atmosphere, chamber type electric resistance furnace is warming up to 120 DEG C with the rate of 2.5 DEG C/min, constant temperature 0.5h, later with 2.5
DEG C/rate of min is continuously heating to 600 DEG C, constant temperature 2h, i.e. completion green body dumping；
Will treated that green body is put into chamber type electric resistance furnace, under air atmosphere, with the rate of 2.5 DEG C/min by box electricity
Resistance furnace is warming up to 1100 DEG C, and Isothermal sinter 1.5h is to get arriving PHT-PNN piezoceramic material.
Embodiment 2
It is that 1:2.8 weighs basic nickel carbonate powder NiCO respectively according to molar ratio3-2Ni(OH)2-4H2O and niobium oxide powder
Nb2O5, wherein basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2The purity of O is 99.9%, niobium oxide powder Nb2O5It is pure
Degree is 99.9%；By weighed basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5It is blended in one
It rises, is subsequently poured into planetary ball mill, then add dehydrated alcohol and abrading-ball into planetary ball mill, after ball-milling treatment,
Uniformly mixed mixed powder is obtained, during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol is every gram to ball milling
The dehydrated alcohol of 0.8ml will be added in powder；Abrading-ball using diameter 3mm~5mm zirconia ball, and ball material mass ratio be 2:
1；Ball-milling Time is 11h；It is to carry out drying and processing in 85 DEG C of baking ovens that obtained mixed powder, which is placed in temperature, obtains mixed powder
Material；Obtained mixed powder material is poured into crucible, and by mixed powder material in crucible and compacting, then covers lid on crucible
Son makes to form confined space in crucible, the crucible is placed in chamber type electric resistance furnace later, 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；To
After the completion of calcining, crucible is taken out from chamber type electric resistance furnace, crucible is made to naturally cool to room temperature, before forming niobic acid nickel in crucible
Drive body powder NiNb2O6；
According to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric ratio 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 dehydrated alcohol is added into ball grinder, through ball milling
After processing, uniformly mixed matrix mixed powder is obtained, during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol is every
Gram the dehydrated alcohol that 0.8ml to be added to ball milling powder；Zirconia ball of the abrading-ball using diameter 3mm~5mm, 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 is 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 covered on crucible, make to form confined space in crucible, which is placed in chamber type electric resistance furnace
In, the matrix mixed powder material under the conditions of air atmosphere and 800 DEG C of temperature in calcining at constant temperature crucible, heating rate control exists
3.5 DEG C/min, calcination time control is 2h；After the completion of calcining, crucible is taken out from chamber type electric resistance furnace, keeps crucible naturally cold
But room temperature is arrived, forms hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O in crucible3-Pb(NiNb)O3；
Fluorination powder for lithium LiF is weighed, the mole of fluorination powder for lithium LiF is hafnium lead titanates-lead nickle niobate powder Pb
(TiHf)O3-Pb(NiNb)O3The 2.0% of mole；By weighed fluorination powder for lithium LiF and hafnium lead titanates-lead nickle niobate powder
Pb(TiHf)O3-Pb(NiNb)O3It is added in ball grinder after mixing, then adds abrading-ball and dehydrated alcohol into ball grinder, through ball
Mill processing after, obtain pre-synthesis powder, during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol are as follows: every gram to ball
The dehydrated alcohol of 0.8ml will be added in milling material；Abrading-ball is using the zirconia ball of diameter 3mm~5mm, 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, is obtained pre-
Synthesize dry mash；
It weighs PVA to be dissolved in the water, makes the PVA solution that mass percent concentration is 5%；The PVA made is molten
Liquid, which is added in pre-synthesis dry mash, carries out granulation processing, obtains granule, wherein to be added in every gram of pre-synthesis dry mash
The PVA solution of 0.15ml；The granule of forming is crossed into the sieve that aperture is 80 mesh, rejects the wherein biggish granule of partial size；It will sieving
The granule obtained afterwards is dry-pressing formed under the pressure of 95Mpa to be made green body, wherein green body is the cylinder parison of Ф 10mm × 1mm
Body；
Under the conditions of 650 DEG C, dumping processing is carried out to green body is obtained, then cools to room temperature with the furnace；The process of dumping has
Body are as follows: under air atmosphere, chamber type electric resistance furnace is warming up to 120 DEG C, constant temperature 0.5h with the rate of 3 DEG C/min, later with 3 DEG C/
The rate of min is continuously heating to 650 DEG C, constant temperature 2h, i.e. completion green body dumping；
Will treated that green body is put into chamber type electric resistance furnace, under air atmosphere, with the rate of 3 DEG C/min by box resistance
Furnace is warming up to 1150 DEG C, Isothermal sinter 2h, i.e. PHT-PNN piezoceramic material.
Embodiment 3
It is that 1:3 weighs basic nickel carbonate powder NiCO respectively according to molar ratio3-2Ni(OH)2-4H2O and niobium oxide powder
Nb2O5, wherein basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2The purity of O is 99.9%, niobium oxide powder Nb2O5It is pure
Degree is 99.9%；By weighed basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5It is blended in one
It rises, is subsequently poured into planetary ball mill, then add dehydrated alcohol and abrading-ball into planetary ball mill, after ball-milling treatment,
Obtain uniformly mixed mixed powder, during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol are as follows: every gram to ball milling
The dehydrated alcohol of 1.0ml will be added in powder；Abrading-ball is using the zirconia ball of diameter 3mm~5mm, and ball material mass ratio is
2.5:1；Ball-milling Time is 12h；It is to carry out drying and processing in 90 DEG C of baking ovens that obtained mixed powder, which is placed in temperature, is mixed
Dry mash；Obtained mixed powder material is poured into crucible, and mixed powder material is covered in crucible and compacting, then on crucible
Lid makes to form confined space in crucible, the crucible is placed in chamber type electric resistance furnace later, 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 are 2h in 4 DEG C/min, calcination time control；To
After the completion of calcining, crucible is taken out from chamber type electric resistance furnace, crucible is made to naturally cool to room temperature, before forming niobic acid nickel in crucible
Drive body powder NiNb2O6；
According to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric ratio 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 dehydrated alcohol is added into ball grinder, through ball milling
After processing, uniformly mixed matrix mixed powder is obtained, during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol is every
Gram the dehydrated alcohol that 1.0ml to be added to ball milling powder；Zirconia ball of the abrading-ball using diameter 3mm~5mm, and ball material
Mass ratio is 2:1；Ball-milling Time is 12h；It is to carry out at drying in 90 DEG C of baking ovens that obtained matrix mixed powder, which is placed in temperature,
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 covers lid on crucible, made to form confined space in crucible, which is placed in chamber type electric resistance furnace,
Matrix mixed powder material under the conditions of air atmosphere and 850 DEG C of temperature in calcining at constant temperature crucible, heating rate control 4 DEG C/
Min, calcination time control are 2h；After the completion of calcining, crucible is taken out from chamber type electric resistance furnace, crucible is made to naturally cool 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, the mole of fluorination powder for lithium LiF is hafnium lead titanates-lead nickle niobate powder Pb
(TiHf)O3-Pb(NiNb)O3The 3.0% of mole；By weighed fluorination powder for lithium LiF and hafnium lead titanates-lead nickle niobate powder
Pb(TiHf)O3-Pb(NiNb)O3It is added in ball grinder after mixing, then adds abrading-ball and dehydrated alcohol into ball grinder, through ball
Mill processing after, obtain pre-synthesis powder, during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol are as follows: every gram to ball
Milling material will be added the dehydrated alcohol of 1.0ml, and abrading-ball is using the zirconia ball of diameter 3mm~5mm, and ball material mass ratio is
2:1；Ball-milling Time is 12h；It is to carry out drying and processing in 90 DEG C of baking ovens that obtained pre-synthesis powder, which is placed in temperature, obtains pre- conjunction
At dry mash；
It weighs PVA to be dissolved in the water, makes the PVA solution that mass percent concentration is 5.5%；The PVA that will be made
Solution, which is added in pre-synthesis dry mash, carries out granulation processing, obtains granule, wherein to be added in every gram of pre-synthesis dry mash
The PVA solution of 0.18ml；The granule of forming is crossed into the sieve that aperture is 80 mesh, rejects the wherein biggish granule of partial size；It will sieving
The granule obtained afterwards is dry-pressing formed under the pressure of 100Mpa to be made green body, wherein green body is the cylinder parison of Ф 10mm × 1mm
Body；
Under the conditions of 680 DEG C, dumping processing is carried out to green body is obtained, then cools to room temperature with the furnace；The process of dumping
Specifically: under air atmosphere, chamber type electric resistance furnace is warming up to 120 DEG C with the rate of 3 DEG C/min, constant temperature 0.5h, later with 3
DEG C/rate of min is continuously heating to 680 DEG C, constant temperature 2h, i.e. completion green body dumping；
Will treated that green body is put into chamber type electric resistance furnace, under air atmosphere, with the rate of 23 DEG C/min by box electricity
Resistance furnace is warming up to 1200 DEG C, Isothermal sinter 1.5h, i.e. PHT-PNN piezoceramic material.
Embodiment 4
It is that 1:3 weighs basic nickel carbonate powder NiCO respectively according to molar ratio3-2Ni(OH)2-4H2O and niobium oxide powder
Nb2O5, wherein basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2The purity of O is 99.9%, niobium oxide powder Nb2O5It is pure
Degree is 99.9%；By weighed basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5It is blended in one
It rises, is subsequently poured into planetary ball mill, then add dehydrated alcohol and abrading-ball into planetary ball mill, after ball-milling treatment,
Obtain uniformly mixed mixed powder, during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol are as follows: every gram to ball milling
The dehydrated alcohol of 0.9ml will be added in powder；Abrading-ball is using the zirconia ball of diameter 3mm~5mm, 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 added on crucible
Lid lid makes to form confined space in crucible, the crucible is placed in chamber type electric resistance furnace later, in air atmosphere and 1125 DEG C
Mixed powder material under the conditions of temperature in calcining at constant temperature crucible, heating rate control are in 4.5 DEG C/min, calcination time control
1.5h；After the completion of calcining, crucible is taken out from chamber type electric resistance furnace, so that crucible is naturally cooled to room temperature, is formed in crucible
Niobic acid nickel presoma powder NiNb2O6；
According to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric ratio 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 dehydrated alcohol is added into ball grinder, through ball milling
After processing, uniformly mixed matrix mixed powder, during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol are obtained are as follows:
Every gram of the dehydrated alcohol that 0.9ml to be added to ball milling powder；Zirconia ball of the abrading-ball using diameter 3mm~5mm, and ball
Material mass ratio is 2.5:1；Ball-milling Time is 13h；Obtained matrix mixed powder is placed in the baking oven that temperature is 95 DEG C and is 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 in crucible and compacting, then lid is covered on crucible, makes to form confined space in crucible, which is placed in box resistance
In furnace, matrix mixed powder material under the conditions of air atmosphere and 850 DEG C of temperature in calcining at constant temperature crucible, heating rate control exists
4.5 DEG C/min, calcination time control is 1.5h；After the completion of calcining, crucible is taken out from chamber type electric resistance furnace, keeps crucible natural
It is 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, the mole of fluorination powder for lithium LiF is hafnium lead titanates-lead nickle niobate powder Pb
(TiHf)O3-Pb(NiNb)O3The 4.0% of mole；By weighed fluorination powder for lithium LiF and hafnium lead titanates-lead nickle niobate powder
Pb(TiHf)O3-Pb(NiNb)O3It is added in ball grinder after mixing, then adds abrading-ball and dehydrated alcohol into ball grinder, through ball
Mill processing after, obtain pre-synthesis powder, during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol are as follows: every gram to ball
The dehydrated alcohol of 0.9ml will be added in milling material；Abrading-ball is using the zirconia ball of diameter 3mm~5mm, 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；
It weighs PVA to be dissolved in the water, makes the PVA solution that mass percent concentration is 6%；The PVA made is molten
Liquid, which is added in pre-synthesis dry mash, carries out granulation processing, obtains granule, wherein to be added in every gram of pre-synthesis dry mash
The PVA solution of 0.2ml；The granule of forming is crossed into the sieve that aperture is 80 mesh, rejects the wherein biggish granule of partial size；After being sieved
Obtained granule is dry-pressing formed under the pressure of 100Mpa to be made green body；Wherein, green body is the cylinder parison of Ф 10mm × 1.5mm
Body；
Under the conditions of 700 DEG C, dumping processing is carried out to green body is obtained, then cools to room temperature with the furnace；The process of dumping has
Body are as follows: under air atmosphere, chamber type electric resistance furnace is warming up to 120 DEG C with the rate of 3.5 DEG C/min, constant temperature 0.5h, later with 3.5
DEG C/rate of min is continuously heating to 700 DEG C, constant temperature 2h, i.e. completion green body dumping；
Will treated that green body is put into chamber type electric resistance furnace, under air atmosphere, with the rate of 3.5 DEG C/min by box electricity
Resistance furnace is warming up to 1225 DEG C, Isothermal sinter 2h, i.e. PHT-PNN piezoceramic material.
Embodiment 5
It is that 1:3.5 weighs basic nickel carbonate powder NiCO respectively according to molar ratio3-2Ni(OH)2-4H2O and niobium oxide powder
Nb2O5, wherein basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2The purity of O is 99.9%, niobium oxide powder Nb2O5It is pure
Degree is 99.9%；By weighed basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5It is blended in one
It rises, is subsequently poured into planetary ball mill, then add dehydrated alcohol and abrading-ball into planetary ball mill, after ball-milling treatment,
Obtain uniformly mixed mixed powder, during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol are as follows: every gram to ball milling
The dehydrated alcohol of 1.2ml will be added in powder；Abrading-ball using diameter 3mm~5mm zirconia ball, and ball material mass ratio be 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 mixed powder material is covered in crucible and compacting, then on crucible
Lid makes to form confined space in crucible, the crucible is placed in chamber type electric resistance furnace later, 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 are 1.5h in 5 DEG C/min, calcination time control；
After the completion of calcining, crucible is taken out from chamber type electric resistance furnace, crucible is made to naturally cool to room temperature, forms niobic acid nickel in crucible
Presoma powder NiNb2O6；
According to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric ratio weighs lead oxide powder respectively
Pb3O4, titanium oxide powder TiO2, hafnium oxide powder HfO2And 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 dehydrated alcohol is added into ball grinder,
After ball-milling treatment, uniformly mixed matrix mixed powder, during ball-milling treatment, the use of ball-milling medium dehydrated alcohol are obtained
Amount are as follows: every gram of the dehydrated alcohol that ml to be added to ball milling powder；Abrading-ball using diameter 3mm~5mm zirconia ball, and
Ball material mass ratio is 3:1；Ball-milling Time is 14h；It is to dry in 100 DEG C of baking ovens that obtained matrix mixed powder, which is placed in temperature,
Dry-cure obtains matrix mixed powder material；Obtained matrix mixed powder material is poured into crucible, and by matrix mixed powder material
In crucible and compacting, then lid is covered on crucible, make to form confined space in crucible, which is placed in chamber type electric resistance furnace
In, the matrix mixed powder material under the conditions of air atmosphere and 900 DEG C of temperature in calcining at constant temperature crucible, heating rate is controlled 5
DEG C/min, calcination time control is 1.5h；After the completion of calcining, crucible is taken out from chamber type electric resistance furnace, keeps crucible naturally cold
But room temperature is arrived, forms hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O in crucible3-Pb(NiNb)O3；
Fluorination powder for lithium LiF is weighed, the mole of fluorination powder for lithium LiF is hafnium lead titanates-lead nickle niobate powder Pb
(TiHf)O3-Pb(NiNb)O3The 5.0% of mole；By weighed fluorination powder for lithium LiF and hafnium lead titanates-lead nickle niobate powder
Pb(TiHf)O3-Pb(NiNb)O3It is added in ball grinder after mixing, then adds abrading-ball and dehydrated alcohol into ball grinder, through ball
Mill processing after, obtain pre-synthesis powder, during ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol are as follows: every gram to ball
The dehydrated alcohol of 1.2ml will be added in milling material；Abrading-ball is using the zirconia ball of diameter 3mm~5mm, 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；
It weighs PVA to be dissolved in the water, makes the PVA solution that mass percent concentration is 7%；The PVA made is molten
Liquid, which is added in pre-synthesis dry mash, carries out granulation processing, obtains granule, wherein to be added in every gram of pre-synthesis dry mash
The PVA solution of 0.2ml；The granule of forming is crossed into the sieve that aperture is 80 mesh, rejects the wherein biggish granule of partial size；After being sieved
Obtained granule is dry-pressing formed under the pressure of 110Mpa to be made green body, and green body is the cylindrical type green body of Ф 10mm × 1.5mm；
Under the conditions of 700 DEG C, dumping processing is carried out to green body is obtained through step 4, then cools to room temperature with the furnace；Dumping
Process specifically: under air atmosphere, chamber type electric resistance furnace is warming up to 120 DEG C, constant temperature 0.5h with the rate of 3.5 DEG C/min, it
700 DEG C, constant temperature 2h are continuously heating to the rate of 3.5 DEG C/min afterwards, i.e. completion green body dumping；
Will treated that green body is put into chamber type electric resistance furnace, under air atmosphere, with the rate of 3.5 DEG C/min by box electricity
Resistance furnace is warming up to 1250 DEG C, Isothermal sinter 1.5h, i.e. PHT-PNN piezoceramic material.
Utilize a kind of PHT-PNN piezoelectric ceramics material that the preparation method of PHT-PNN piezoceramic material is prepared of the present invention
Material, after by silver metallized processing, polarize 20min under the polarized electric field of 2kV/cm~3kV/cm, then under room temperature
It stands again for 24 hours, tests its piezoelectric property later, see Table 1 for details for specific test result.
The different embodiments of table 1 prepare hafnium lead titanates-lead nickle niobate piezoelectric ceramics piezoelectric property parameters
A kind of preparation method of PHT-PNN piezoceramic material 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 (7)
1. a kind of preparation method of PHT-PNN piezoceramic material, which is characterized in that be specifically implemented according to the following steps:
Step 1, by basic nickel carbonate powder NiCO3-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5It is carried out at ball milling after mixing
Reason forms mixed powder, calcines 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 ratio weigh oxidation respectively
Lead powder body Pb3O4, titanium dioxide powder TiO2, hafnium oxide powder HfO2And niobic acid nickel powder body NiNb obtained in step 12O6,
Ball-milling treatment is carried out after weighed all materials are mixed again, obtains matrix mixed powder, successively by matrix mixed powder finally
It dried, calcined and cooling treatment, obtain hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O3-Pb(NiNb)O3；
The step 2 is specifically implemented according to the following steps:
Step 2.1, according to 0.51Pb (Ti0.7Hf0.3)O3-0.49Pb(Ni1/3Nb2/3)O3Stoichiometric ratio weighs lead oxide respectively
Powder Pb3O4, titanium oxide powder TiO2, hafnium oxide powder HfO2And niobic acid nickel powder body NiNb obtained in step 12O6, formed
Matrix mixed powder；
The matrix mixed powder and abrading-ball that obtain through step 2.1 are added in ball grinder by step 2.2 together, then to ball grinder
Middle addition dehydrated alcohol obtains matrix mixed powder after ball-milling treatment；
The matrix mixed powder obtained through step 2.2 is placed in baking oven and carries out drying and processing by step 2.3, obtains matrix mixing
Dry mash；
Step 2.4 pours into the matrix mixed powder material obtained through step 2.3 in crucible, and by matrix mixed powder material in earthenware
It is compacted in crucible, then covers lid on crucible, made to form confined space in crucible, which is placed in chamber type electric resistance furnace,
Matrix mixed powder material under the conditions of air atmosphere and 750 DEG C~900 DEG C temperature 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, after the completion of the calcining in step 2.4, crucible is taken out from chamber type electric resistance furnace, naturally cools to crucible
Room temperature forms hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O in crucible3-Pb(NiNb)O3；
Step 3 weighs fluorination powder for lithium LiF, will be through the lead titanates of hafnium made from step 2-lead nickle niobate powder Pb (TiHf) O3-Pb
(NiNb)O3After carrying out ball-milling treatment, then drying processing after mixing with fluorination powder for lithium LiF, pre-synthesis dry mash is obtained；
The step 3 is specifically implemented according to the following steps:
Step 3.1 weighs fluorination powder for lithium LiF, and the mole of fluorination powder for lithium LiF 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 weighed in step 3.1 and hafnium lead titanates-lead nickle niobate powder Pb (TiHf) O3-Pb
(NiNb)O3It is added in ball grinder after mixing, then addition abrading-ball and dehydrated alcohol obtain after ball-milling treatment into ball grinder
Pre-synthesis powder；
The pre-synthesis powder obtained through step 3.2 is placed in baking oven and carries out drying and processing by step 3.3, obtains pre-synthesis dry powder
Material；
Step 4 prepares PVA solution, and PVA solution is added to the pre-synthesis dry mash obtained through step 3 and is granulated, then is passed through
Sieving processing selection granule, is made green body after dry-pressing formed processing for obtained granule later；
Step 5 first obtains green body progress dumping processing to through step 4, then carries out furnace cooling processing, then carry out at high temperature
Sintering processes finally obtain PHT-PNN piezoceramic material；
The step 5 is specifically implemented according to the following steps:
Step 5.1, under the conditions of 600 DEG C~700 DEG C, to through step 4 obtain green body carry out dumping processing, then cool to the furnace
Room temperature；
Step 5.2, will through step 5.1, treated that green body 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 the rate of~3.5 DEG C/min, and Isothermal sinter 1.5h~2.5h is to get arriving
PHT-PNN piezoceramic material.
2. a kind of preparation method of PHT-PNN piezoceramic material according to claim 1, which is characterized in that the step
Rapid 1 is specifically implemented according to the following steps:
Step 1.1 is that 1:2.5~3.5 weigh basic nickel carbonate powder NiCO respectively according to molar ratio3-2Ni(OH)2-4H2O and
Niobium oxide powder Nb2O5；
Step 1.2, by basic nickel carbonate powder NiCO weighed in step 1.13-2Ni(OH)2-4H2O and niobium oxide powder Nb2O5
It mixes, is subsequently poured into planetary ball mill, then add dehydrated alcohol and abrading-ball into planetary ball mill, through ball milling
After processing, uniformly mixed mixed powder is obtained；
The mixed powder obtained through step 1.2 is placed in baking oven and carries out drying and processing by step 1.3, obtains mixed powder material；
Step 1.4 pours into the mixed powder material obtained through step 1.3 in crucible, and by mixed powder material in crucible and compacting,
Lid is covered on crucible again, makes to form confined space in crucible, the crucible is placed in chamber type electric resistance furnace later, Yu great Qi
Mixed powder material under the conditions of atmosphere and 1050 DEG C~1150 DEG C temperature in calcining at constant temperature crucible, heating rate control 3 DEG C/
Min~5 DEG C/min, calcination time control are 1.5h~2.5h；
Step 1.5, after the completion of the calcining in step 1.4, crucible is taken out from chamber type electric resistance furnace, is naturally cooled to crucible
Room temperature forms niobic acid nickel presoma powder NiNb in crucible2O6。
3. a kind of preparation method of PHT-PNN piezoceramic material according to claim 2, which is characterized in that the step
In rapid 1.2:
During the ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol, which is every gram, will be added 0.6ml to ball milling powder
The dehydrated alcohol of~1.2ml；Abrading-ball using diameter 3mm~5mm zirconia ball, and ball material mass ratio be (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 material according to claim 1, which is characterized in that the step
In rapid 2.2:
During ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol be every gram to ball milling powder to be added 0.6ml~
The dehydrated alcohol of 1.2ml；Zirconia ball of the abrading-ball using diameter 3mm~5mm, and ball material mass ratio are as follows: (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.
5. a kind of preparation method of PHT-PNN piezoceramic material according to claim 1, which is characterized in that the step
In rapid 3.2:
During ball-milling treatment, the dosage of ball-milling medium dehydrated alcohol be every gram to ball milling powder to be added 0.6ml~
The dehydrated alcohol of 1.2ml；Abrading-ball using diameter 3mm~5mm zirconia ball, and ball material mass ratio be (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.
6. a kind of preparation method of PHT-PNN piezoceramic material according to claim 1, which is characterized in that the step
Rapid 4 are specifically implemented according to the following steps:
Step 4.1 weighs PVA and is dissolved in the water, and makes the PVA solution that mass percent concentration is 4%~7%；
The PVA solution made through step 4.1 is added in the pre-synthesis dry mash obtained through step 3 and makes by step 4.2
Grain processing, obtains granule；
The PVA solution of 0.1ml~0.2ml to be added in every gram of pre-synthesis dry mash；
Step 4.3, after step 4.2, the granule of forming is crossed into the sieve that aperture is 80 mesh, rejects the wherein biggish group of partial size
Grain；
Base is made by obtained granule is dry-pressing formed under the pressure of 90Mpa~110Mpa after step 4.3 sieving in step 4.4
Body.
7. a kind of preparation method of PHT-PNN piezoceramic material according to claim 1, which is characterized in that described
In step 5.1, the dumping process is specific as follows:
Under air atmosphere, chamber type electric resistance furnace is warming up to 120 DEG C with 2.5 DEG C/min~3.5 DEG C/min rate, constant temperature
0.5h is continuously heating to 600 DEG C~700 DEG C, constant temperature 2h later with 2.5 DEG C/min~3.5 DEG C/min rate, i.e. completion green body
Dumping.
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| CN110818410B (en) * | 2019-11-12 | 2021-09-21 | 西安电子科技大学 | High-temperature PIN-PHT piezoelectric ceramic and preparation method thereof |
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