CN100556852C - Modification PZT piezoelectric ceramics that a kind of nano-powder directly adds and preparation method thereof - Google Patents
Modification PZT piezoelectric ceramics that a kind of nano-powder directly adds and preparation method thereof Download PDFInfo
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- 239000011858 nanopowder Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 45
- 239000000919 ceramic Substances 0.000 title claims abstract description 44
- 230000004048 modification Effects 0.000 title claims abstract description 38
- 238000012986 modification Methods 0.000 title claims abstract description 38
- 150000001875 compounds Chemical class 0.000 claims abstract description 47
- 239000000463 material Substances 0.000 claims abstract description 42
- 239000000654 additive Substances 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 28
- 238000005516 engineering process Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000005338 frosted glass Substances 0.000 claims description 47
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 31
- 238000000498 ball milling Methods 0.000 claims description 28
- 239000008367 deionised water Substances 0.000 claims description 28
- 229910021641 deionized water Inorganic materials 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 28
- 238000005507 spraying Methods 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000003643 water by type Substances 0.000 claims description 28
- 230000000996 additive effect Effects 0.000 claims description 24
- 229910052749 magnesium Inorganic materials 0.000 claims description 17
- 229910052799 carbon Inorganic materials 0.000 claims description 16
- 238000005469 granulation Methods 0.000 claims description 15
- 230000003179 granulation Effects 0.000 claims description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 14
- 239000011230 binding agent Substances 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 14
- 229910052748 manganese Inorganic materials 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 238000000465 moulding Methods 0.000 claims description 14
- 238000012856 packing Methods 0.000 claims description 14
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 14
- 238000010298 pulverizing process Methods 0.000 claims description 14
- 238000005096 rolling process Methods 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 14
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 229910052787 antimony Inorganic materials 0.000 claims description 5
- 238000010304 firing Methods 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical class [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052451 lead zirconate titanate Inorganic materials 0.000 abstract description 7
- 230000002349 favourable effect Effects 0.000 abstract description 3
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- 230000033228 biological regulation Effects 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 description 13
- 239000007788 liquid Substances 0.000 description 12
- 238000002156 mixing Methods 0.000 description 12
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- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 10
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- 229910002113 barium titanate Inorganic materials 0.000 description 3
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
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- 229910052746 lanthanum Inorganic materials 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 2
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Abstract
The present invention relates to a kind of nano-powder raw material and directly add modified lead zirconate titanate (PZT) piezoelectric ceramics of preparation and preparation method thereof, adopt the micro-powder in the nano-powder replacement prescription, and in compound, directly add the nano-component powder additives, calcined temperature reduces by 50 ℃～200 ℃, become to burn temperature and can reduce by 50 ℃～100 ℃, but the crystalline phase of comprehensive regulation pre-sintered sample and material property, and the electric property that becomes to burn piezoelectric ceramics; The Curie temperature that the nano-powder that becomes to burn about 1200 ℃ directly adds the modification piezoelectric ceramics has improved 50～100 ℃, and the high/low-temperature impact stability is superior: T
C=350～400 ℃; ε=350～800; Kp=0.48～0.60, dielectric-constant adjustable; Material technology is stable, favorable reproducibility.Piezoceramic material of the present invention can be applicable to the production of ceramic discriminator, wave filter equifrequent components and parts.
Description
Technical field
The present invention relates to a kind of piezoelectric ceramics and preparation method thereof, refer in particular to direct modification Pb-based lanthanumdoped zirconate titanates (PZT) piezoelectric ceramics that adds of a kind of nano-powder and preparation method thereof, function of dominant ceramics processing field.
Background technology
Before and after nineteen forty-two, barium titanate ceramics are successively discovered by the U.S., USSR (Union of Soviet Socialist Republics) and Japanese scientist, become first kind of piezoceramic material with application prospect after French Curie's brother's discovery " piezoelectric effect ".Nineteen forty-seven, first piezoelectric ceramic devices-barium titanate (BT) sound pick-up has been born.At the beginning of the fifties, performance obviously is better than Pb-based lanthanumdoped zirconate titanates (PZT) piezoceramic material of barium titanate and succeeds in developing.From then on, the development of piezoelectric ceramics has entered the new stage.The sixties is to the seventies, and the research of piezoelectric ceramics is deepened continuously, and occurred based on Pb-based lanthanumdoped zirconate titanates, with the improved three component system of multiple element, four-component-system piezoelectric ceramics.These excellent material performance are made simply, and are with low cost, are widely used.
Pb-based lanthanumdoped zirconate titanates (PZT) piezoelectric ceramics is that a class can be with the ceramic material of mechanical energy and the mutual conversion of electric energy.Be widely used in national defense construction, scientific research, industrial production and and the closely-related many fields of people's lives in.Yet because plumbous oxide can volatilize in the synthetic preparation process of PZT high temperature, thereby environment and HUMAN HEALTH are had a negative impact.In order to overcome lead base piezoelectric ceramics shortcoming in this respect, there is considerable researcher to drop into research to leadless piezoelectric ceramics, and material and device that suitable low and middle-end is used have been developed, but the Application Areas of piezoelectric property being had relatively high expectations in part, leadless piezoelectric ceramics still has very large gap from practical application, needs to continue to improve its performance index aspect electromechanical coupling factor, piezoelectric constant and Qm.At present, leadless piezoelectric ceramics does not still have the possibility that replaces the lead base piezoelectric ceramics fully, is still having many work to do aspect reduction lead base piezoelectric ceramics sintering temperature, the plumbous volatilization of inhibition and its piezoelectric property of continuation raising.
Nano material is meant the ultra-micro powder of particle size＜100nm, big because of its specific surface area, surface energy is high, the surface atom ratio height of particle, surface atom ligancy deficiency also have and other atom bonded tendencies, so nanoparticle has very high chemically reactive.In sintering process, use nano-powder can effectively reduce ceramic sintering temperature, the carrying out of acceleration of sintering process.In addition because nano-powder, on the surface and inside have a large amount of lattice imperfections, therefore introducing nano-powder in the ceramic post sintering process will exert an influence to dielectric properties such as the specific inductivity of pottery and dielectric losses.
In view of the remarkable effect of nano-powder to improvement material sintering character and adjusting defective etc., there has been both at home and abroad considerable researcher to prepare the lead zirconate titanate powder of total composition, comprised hydrothermal method, sol-gel method, metallo-organic decomposition process and mechanochemical method etc. with diverse ways; But, the lead zirconate titanate powder that adopts the part component is a feedstock production piezoelectric and to the piezoelectric Study on Influence also seldom, and there is the high problem of product cost in this method, and using value is little aspect industrialization.On the other hand, the nano-powder price of the single raw material of Pb-based lanthanumdoped zirconate titanates system has dropped to industrialization acceptable level, under the parameter prerequisite of improving the critical process process, adopt these commercial nano-powder raw materials, under the constant substantially prerequisite of technical process, by nano-powder the part of respective components micro-powder is substituted, the adjusting process system prepares the piezoelectric ceramics electric property and can be in harmonious proportion the research work that improves and seldom report.Particularly, this technology is applied to the lead zirconate-titanate ceramic field that frequency element is used, and the acquisition nano-powder directly adds the industrialization technology and the correlated frequency component products of modification lead zirconate-titanate ceramic piezoelectric ceramics material preparation, that have good piezoelectric property and does not appear in the newspapers as yet.
Summary of the invention
The present invention seeks to use lead zirconate-titanate ceramic at the needs aspect raising frequency stability of temperature and the high/low-temperature impact characteristic, propose a kind of nano-powder and directly add modified lead zirconate titanate (PZT) piezoelectric ceramics of preparation and preparation method thereof at the frequency element that with the Pb-based lanthanumdoped zirconate titanates is basic components.With Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3System is a research object, replaces Pb with a certain proportion of nano-powder
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3Corresponding micro-powder in the composition, reducing calcined temperature and adjusting pre-imitation frosted glass crystalline phase and form under the prerequisite, the collaborative one-tenth that reduces lead zirconate-titanate ceramic burns temperature, the dielectric properties of comprehensive regulation material, acquisition has tunable dielectric constant, has the nano powder modified lead titanate piezoelectric ceramics of the frequency element of high high/low-temperature impact performance, and forms industrialization.
A kind of nano-powder directly adds the Pb-based lanthanumdoped zirconate titanates binary piezoelectric ceramics of modification preparation, and the prescription composition formula is: Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, wherein A is one or both among Mg, Ca, Sr, the Ba, and B is one or both of Mn, Zn, Ni, Sb, Mg, and C is one or both of Sb, Nb, W; 0＜x≤0.12,0＜Y≤0.15,0＜Z≤0.25.
A kind of nano-powder directly adds the preparation method of the lead titanate piezoelectric ceramics of modification preparation, may further comprise the steps:
1), compound preparation and low temperature presintering technology: by prescription composition formula Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, weighing main raw material Pb
3O
4, ZrO
2, TiO
2And each component, add nano-powder component additive and be mixed with compound; Weight ratio by compound and deionized water is 2: 0.5～1.5 adding deionized waters, mixes 24～72h at rotating speed 300r/min rolling ball milling; The ball milling material is in 100～250 ℃ of oven dry 12～36h; With the compound alumina crucible of packing into of oven dry, at 750～950 ℃ of calcining 1～12h down, synthetic Pb-based lanthanumdoped zirconate titanates is principal crystalline phase mutually, contains small amounts of Pb ZrO
3And PbTiO
3The nano-powder of crystalline phase adds pre-imitation frosted glass;
2), pre-imitation frosted glass is pulverized slurrying, granulating and forming and become firing technique: the weight ratio of adding pre-imitation frosted glass and deionized water by nano-powder is 2: 0.5～1.0 adding deionized waters, pulverizes 24～48h in rotating speed 300r/min ball mill; Weight in the pre-imitation frosted glass after pulverizing is 100%, and the weight percent concentration of adding 10～20% is 5～20% polyvinyl alcohol solution, is mixed with spraying drying nano modification slip, and the slip spraying drying obtains the dried granulation powder; The knobble of diameter 25mm, thickness 0.6～0.8mm is made in dry-pressing under 100～150Mpa pressure, or is pressed into that 25 * 40mm is square, the dice of thickness 0.6～0.8mm; Molding mass is incubated 24～72h at 750～850 ℃ of following binder removals; Being incubated 1～12h down at 1050～1300 ℃ afterwards becomes to burn promptly;
Described nano-powder component additive is a nano-TiO
2, nanometer ZrO
2, nano-MgO, nanometer CaCO
3, nanometer SrCO
3Or nanometer BaCO
3In one or more.The addition of described nano-powder component additive is: the weight of nano-powder component additive account for this component additive correspondence the raw material gross weight 10～100%.
A kind of typical frequency element that the present invention adopts consists of with the prescription that nano-powder directly adds the lead lanthanum zirconate titanate (PLZT) electrooptical ceramics material of modification preparation: Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, x=0.10 wherein, Y=0.026, Z=0.074, A are Mg, and B is Mn, and C is Nb.The addition of described nano-powder component additive is: nano-TiO
2Powder additives accounts for total TiO
255% of weight; Nanometer ZrO
2Powder additives accounts for total ZrO
235% of weight; The nano-MgO powder additives accounts for 80% of total MgO weight.
The present invention who adopts above-mentioned prescription and technology to form need carry out pre-burning in the temperature range than low 50 ℃-200 ℃ of traditional technology, be that pure PZT is obviously different mutually with the pre-imitation frosted glass of traditional technology, and the present invention obtains PZT mutually for principal crystalline phase, contains small amounts of Pb ZrO
3And PbTiO
3The nano-powder of crystalline phase adds pre-imitation frosted glass; Pulverize afterwards, spray and become to burn operation, become to burn temperature and reduce by 50 ℃～100 ℃ than traditional technology, the piezoceramic material of acquisition has superior dielectric properties: ε=350～800; Kp=0.48～0.60, dielectric-constant adjustable; Material technology is stable, favorable reproducibility.The modification PZT piezoelectric ceramics that such nano-powder directly adds preparation is a kind of material that has development prospect, invested in plant production.
The present invention has compared following advantage with the PZT piezoelectric ceramics of traditional method preparation:
1) reduced the calcined temperature and the sintering temperature of lead titanate piezoelectric ceramics, saved the energy, reduced the pollution of plumbous volatilization environment.
2) low temperature presintering and the follow-up one-tenth firing technique of employing nano-powder component compound make full use of the effect of nano-powder to promoting that crystalline phase is synthetic and defective is regulated and control, and have improved the electric property of piezoelectric ceramics.The nano modification lead titanate piezoelectric ceramics Curie temperature of burning till about 1200 ℃ is at T
C=350～400 ℃, the same component pottery for preparing than traditional technology has improved 50-100 ℃
3) lead lanthanum zirconate titanate (PLZT) electrooptical ceramics material that obtains has higher dielectric constant ε, electromechanical coupling factor K
pLower dielectric loss Tan δ, frequency-temperature coefficient effectively is controlled in the use range.
4) stable, the favorable reproducibility of material technology, the high/low-temperature impact stability of the frequency element of making is superior.
Description of drawings
Fig. 1 is different amount TiO
2The thing phase composite of sample behind 1150 ℃ of sintering of nanometer replacement.Be single cubic phase Pb (Zr as can be seen behind the sintering
0.58Ti
0.42) O
3
Fig. 2 (a), Fig. 2 (b), Fig. 2 (c) are TiO behind the differing temps sintering
2Nanometer replaces the cross-section morphology (20000x) of sample.Fig. 2 (a) is 1200 ℃ in 20% a replacement sample, and Fig. 2 (b) is 1150 ℃ in 50% a replacement sample, and Fig. 2 (c) is 1100 ℃ in 80% a replacement sample.Sample density behind the sintering is higher as we can see from the figure, and grain size is more even.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment 1:
According to prescription Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, wherein A is Mg, and B is Mn, and C is Nb; X=0.10, Y=0.026, Z=0.074.Pb in molar ratio
3O
4: micron (MgCO
3)
4Mg (OH)
25H
2O: ZrO
2: (micron TiO
2: nano-TiO
2): MnCO
3: Nb
2O
5=0.3000: 0.02: 0.5260: (0.2844: 0.1896): weighing in 0.0333: 0.0333, preparation meets the compound that nano-powder component additive is formed and comprised to prescription; Weight ratio by compound and deionized water is 2: 1.0 adding deionized waters, at rotating speed 300r/min rolling ball milling mixing 36h; The ball milling material is in 180 ℃ of oven dry 24h; With the compound alumina crucible of packing into of oven dry, at 890 ℃ of calcining 2h down, synthetic PZT is principal crystalline phase mutually, contains small amounts of Pb ZrO
3And PbTiO
3The nano-powder of crystalline phase adds pre-imitation frosted glass.Pre-imitation frosted glass is 2: 1.0 adding deionized waters by the weight ratio of pre-imitation frosted glass and deionized water, pulverizes 24h in rotating speed 300r/min ball mill; After the ball mill pulverizing, adding polyvinyl alcohol concentration by the 15wt% weight ratio is the liquid of 15wt%, preparation spraying drying nano modification slip, and the slip spraying drying obtains the dried granulation powder; The knobble of diameter 25mm, thickness 0.6～0.8mm is made in dry-pressing under 100～150Mpa pressure, or is pressed into that 25 * 40mm is square, the dice of thickness 0.6～0.8mm.Molding mass is incubated 50h at 850 ℃ of following binder removals; Be incubated 3h down at 1210 ℃ afterwards and become to burn, promptly obtaining principal crystalline phase is the nano modification piezoceramic material of the present invention of PZT phase.
Embodiment 2:
According to prescription Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, wherein A is Mg, and B is Mn, and C is Nb; X=0.10, Y=0.026, Z=0.074.Pb in molar ratio
3O
4: micron (MgCO
3)
4Mg (OH)
25H
2O: ZrO
2: (micron TiO
2: nano-TiO
2): MnCO
3: Nb
2O
5=0.3000: 0.02: 0.5260: (0.1896: 0.2844): weighing in 0.0333: 0.0333, preparation meets the compound that nano-powder component additive is formed and comprised to prescription; Weight ratio by compound and deionized water is 2: 1.0 adding deionized waters, at rotating speed 300r/min rolling ball milling mixing 36h; The ball milling material is in 180 ℃ of oven dry 24h; With the compound alumina crucible of packing into of oven dry, at 845 ℃ of calcining 5h down, synthetic PZT is principal crystalline phase mutually, contains small amounts of Pb ZrO
3And PbTiO
3The nano-powder of crystalline phase adds pre-imitation frosted glass.Pre-imitation frosted glass is 2: 1.0 adding deionized waters by the weight ratio of pre-imitation frosted glass and deionized water, pulverizes 24h in rotating speed 300r/min ball mill; After the ball mill pulverizing, adding polyvinyl alcohol concentration by the 15wt% weight ratio is the liquid of 15wt%, preparation spraying drying nano modification slip, and the slip spraying drying obtains the dried granulation powder; The knobble of diameter 25mm, thickness 0.6～0.8mm is made in dry-pressing under 100～150Mpa pressure, or is pressed into that 25 * 40mm is square, the dice of thickness 0.6～0.8mm.Molding mass is incubated 50h at 850 ℃ of following binder removals; Be incubated 7h down at 1175 ℃ afterwards and become to burn, promptly obtaining principal crystalline phase is the nano modification piezoceramic material of the present invention of PZT phase.
Embodiment 3:
According to prescription Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, wherein A is Mg, and B is Mn, and C is Nb; X=0.10, Y=0.026, Z=0.074.Pb in molar ratio
3O
4: micron (MgCO
3)
4Mg (OH)
25H
2O: ZrO
2: (micron TiO
2: nano-TiO
2): MnCO
3: Nb
2O
5=0.3000: 0.02: 0.5260: (0.0948: 0.3792): weighing in 0.0333: 0.0333, preparation meets the compound that nano-powder component additive is formed and comprised to prescription; Weight ratio by compound and deionized water is 2: 1.0 adding deionized waters, at rotating speed 300r/min rolling ball milling mixing 36h; The ball milling material is in 180 ℃ of oven dry 24h; With the compound alumina crucible of packing into of oven dry, at 800 ℃ of calcining 10h down, synthetic PZT is principal crystalline phase mutually, contains small amounts of Pb ZrO
3And PbTiO
3The nano-powder of crystalline phase adds pre-imitation frosted glass.Pre-imitation frosted glass is 2: 1.0 adding deionized waters by the weight ratio of pre-imitation frosted glass and deionized water, pulverizes 24h in rotating speed 300r/min ball mill; After the ball mill pulverizing, adding polyvinyl alcohol concentration by the 15wt% weight ratio is the liquid of 15wt%, preparation spraying drying nano modification slip, and the slip spraying drying obtains the dried granulation powder; The knobble of diameter 25mm, thickness 0.6～0.8mm is made in dry-pressing under 100～150Mpa pressure, or is pressed into that 25 * 40mm is square, the dice of thickness 0.6～0.8mm.Molding mass is incubated 50h at 850 ℃ of following binder removals; Be incubated 9h down at 1130 ℃ afterwards and become to burn, promptly obtaining principal crystalline phase is the nano modification piezoceramic material of the present invention of PZT phase.
Embodiment 4:
According to prescription Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, wherein A is Mg, and B is Mn, and C is Nb; X=0.10, Y=0.026, Z=0.074.Pb in molar ratio
3O
4: (micron (MgCO
3)
4Mg (OH)
25H
2O: nano-MgO): ZrO
2: micron TiO
2: MnCO
3: Nb
2O
5=0.3000: (0.012: 0.04): 0.5260: 0.4740: 0.0333: 0.0333 weighing, preparation meets the compound that nano-powder component additive is formed and comprised to prescription; Weight ratio by compound and deionized water is 2: 1.0 adding deionized waters, at rotating speed 300r/min rolling ball milling mixing 36h; The ball milling material is in 180 ℃ of oven dry 24h; With the compound alumina crucible of packing into of oven dry, at 900 ℃ of calcining 2h down, synthetic PZT is principal crystalline phase mutually, contains small amounts of Pb ZrO
3And PbTiO
3The nano-powder of crystalline phase adds pre-imitation frosted glass.Pre-imitation frosted glass is 2: 1.0 adding deionized waters by the weight ratio of pre-imitation frosted glass and deionized water, pulverizes 24h in rotating speed 300r/min ball mill; After the ball mill pulverizing, adding polyvinyl alcohol concentration by the 15wt% weight ratio is the liquid of 15wt%, preparation spraying drying nano modification slip, and the slip spraying drying obtains the dried granulation powder; The knobble of diameter 25mm, thickness 0.6～0.8mm is made in dry-pressing under 100～150Mpa pressure, or is pressed into that 25 * 40mm is square, the dice of thickness 0.6～0.8mm.Molding mass is incubated 50h at 850 ℃ of following binder removals; Be incubated 3h down at 1225 ℃ afterwards and become to burn, promptly obtaining principal crystalline phase is the nano modification piezoceramic material of the present invention of PZT phase.
Embodiment 5:
According to prescription Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, wherein A is Mg, and B is Mn, and C is Nb; X=0.10, Y=0.026, Z=0.074.Pb in molar ratio
3O
4: (micron (MgCO
3)
4Mg (OH)
25H
2O: nano-MgO): ZrO
2: micron TiO
2: MnCO
3: Nb
2O
5=0.3000: (0.004: 0.08): 0.5260: 0.4740: 0.0333: 0.0333 weighing, preparation meets the compound that nano-powder component additive is formed and comprised to prescription; Weight ratio by compound and deionized water is 2: 1.0 adding deionized waters, at rotating speed 300r/min rolling ball milling mixing 36h; The ball milling material is in 180 ℃ of oven dry 24h; With the compound alumina crucible of packing into of oven dry, at 860 ℃ of calcining 4h down, synthetic PZT is principal crystalline phase mutually, contains small amounts of Pb ZrO
3And PbTiO
3The nano-powder of crystalline phase adds pre-imitation frosted glass.Pre-imitation frosted glass is 2: 1.0 adding deionized waters by the weight ratio of pre-imitation frosted glass and deionized water, pulverizes 24h in rotating speed 300r/min ball mill; After the ball mill pulverizing, adding polyvinyl alcohol concentration by the 15wt% weight ratio is the liquid of 15wt%, preparation spraying drying nano modification slip, and the slip spraying drying obtains the dried granulation powder; The knobble of diameter 25mm, thickness 0.6～0.8mm is made in dry-pressing under 100～150Mpa pressure, or is pressed into that 25 * 40mm is square, the dice of thickness 0.6～0.8mm.Molding mass is incubated 50h at 850 ℃ of following binder removals; Be incubated 4h down at 1200 ℃ afterwards and become to burn, promptly obtaining principal crystalline phase is the nano modification piezoceramic material of the present invention of PZT phase.
Embodiment 6:
According to prescription Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, wherein A is Mg, and B is Mn, and C is Nb; X=0.10, Y=0.026, Z=0.074.Pb in molar ratio
3O
4: (micron (MgCO
3)
4Mg (OH)
25H
2O: nano-MgO): ZrO
2: (micron TiO
2: nano-TiO
2): MnCO
3: Nb
2O
5=0.3000: (0.012: 0.04): 0.5260: (0.2844: 0.1896): weighing in 0.0333: 0.0333, preparation meets the compound that nano-powder component additive is formed and comprised to prescription; Weight ratio by compound and deionized water is 2: 1.0 adding deionized waters, at rotating speed 300r/min rolling ball milling mixing 36h; The ball milling material is in 180 ℃ of oven dry 24h; With the compound alumina crucible of packing into of oven dry, at 875 ℃ of calcining 3h down, synthetic PZT is principal crystalline phase mutually, contains small amounts of Pb ZrO
3And PbTiO
3The nano-powder of crystalline phase adds pre-imitation frosted glass.Pre-imitation frosted glass is 2: 1.0 adding deionized waters by the weight ratio of pre-imitation frosted glass and deionized water, pulverizes 24h in rotating speed 300r/min ball mill; After the ball mill pulverizing, adding polyvinyl alcohol concentration by the 15wt% weight ratio is the liquid of 15wt%, preparation spraying drying nano modification slip, and the slip spraying drying obtains the dried granulation powder; The knobble of diameter 25mm, thickness 0.6～0.8mm is made in dry-pressing under 100～150Mpa pressure, or is pressed into that 25 * 40mm is square, the dice of thickness 0.6～0.8mm.Molding mass is incubated 50h at 850 ℃ of following binder removals; Be incubated 4h down at 1200 ℃ afterwards and become to burn, promptly obtaining principal crystalline phase is the nano modification piezoceramic material of the present invention of PZT phase.
Embodiment 7:
According to prescription Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
I/3C
2/3)
Y+ZO
3, wherein A is Mg, and B is Mn, and C is Nb; X=0.10, Y=0.026, Z=0.074.In molar ratio (micron (MgCO
3)
4Mg (OH)
25H
2O: nano-MgO): ZrO
2: (micron TiO
2: nano-TiO
2): MnCO
3: Nb
2O
5=0.3000: (0.008: 0.06): 0.5260: (0.1896: 0.2844): weighing in 0.0333: 0.0333, preparation meets the compound that nano-powder component additive is formed and comprised to prescription; Weight ratio by compound and deionized water is 2: 1.0 adding deionized waters, at rotating speed 300r/min rolling ball milling mixing 36h; The ball milling material is in 180 ℃ of oven dry 24h; With the compound alumina crucible of packing into of oven dry, at 830 ℃ of calcining 5h down, synthetic PZT is principal crystalline phase mutually, contains small amounts of Pb ZrO
3And PbTiO
3The nano-powder of crystalline phase adds pre-imitation frosted glass.Pre-imitation frosted glass is 2: 1.0 adding deionized waters by the weight ratio of pre-imitation frosted glass and deionized water, pulverizes 24h in rotating speed 300r/min ball mill; After the ball mill pulverizing, adding polyvinyl alcohol concentration by the 15wt% weight ratio is the liquid of 15wt%, preparation spraying drying nano modification slip, and the slip spraying drying obtains the dried granulation powder; The knobble of diameter 25mm, thickness 0.6～0.8mm is made in dry-pressing under 100～150Mpa pressure, or is pressed into that 25 * 40mm is square, the dice of thickness 0.6～0.8mm.Molding mass is incubated 50h at 850 ℃ of following binder removals; Be incubated 6h down at 1160 ℃ afterwards and become to burn, promptly obtaining principal crystalline phase is the nano modification piezoceramic material of the present invention of PZT phase.
Embodiment 8:
According to prescription Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, wherein A is Mg, and B is Mn, and C is Nb; X=0.10, Y=0.026, Z=0.074.Pb in molar ratio
3O
4: (micron (MgCO
3)
4Mg (OH)
25H
2O: nano-MgO): ZrO
2: (micron TiO
2: nano-TiO
2): MnCO
3: Nb
2O
5=0.3000: (0.004: 0.08): 0.5260: (0.0948: 0.3792): weighing in 0.0333: 0.0333, preparation meets the compound that nano-powder component additive is formed and comprised to prescription; Weight ratio by compound and deionized water is 2: 1.0 adding deionized waters, at rotating speed 300r/min rolling ball milling mixing 36h; The ball milling material is in 180 ℃ of oven dry 24h; With the compound alumina crucible of packing into of oven dry, at 790 ℃ of calcining 9h down, synthetic PZT is principal crystalline phase mutually, contains small amounts of Pb ZrO
3And PbTiO
3The nano-powder of crystalline phase adds pre-imitation frosted glass.Pre-imitation frosted glass is 2: 1.0 adding deionized waters by the weight ratio of pre-imitation frosted glass and deionized water, pulverizes 24h in rotating speed 300r/min ball mill; After the ball mill pulverizing, adding polyvinyl alcohol concentration by the 15wt% weight ratio is the liquid of 15wt%, preparation spraying drying nano modification slip, and the slip spraying drying obtains the dried granulation powder; The knobble of diameter 25mm, thickness 0.6～0.8mm is made in dry-pressing under 100～150Mpa pressure, or is pressed into that 25 * 40mm is square, the dice of thickness 0.6～0.8mm.Molding mass is incubated 50h at 850 ℃ of following binder removals; Be incubated 8h down at 1100 ℃ afterwards and become to burn, promptly obtaining principal crystalline phase is the nano modification piezoceramic material of the present invention of PZT phase.
Embodiment 9:
According to prescription Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, wherein A is Mg, and B is Mn, and C is Sb; X=0.10, Y=0.12, Z=0.03.Pb in molar ratio
3O
4: micron (MgCO
3)
4Mg (OH)
25H
2O: ZrO
2: (micron TiO
2: nano-TiO
2): MnCO
3: Sb
2O
3=0.3000: 0.02: 0.6200: (0.172: 0.258): weighing in 0.05: 0.05, preparation meets the compound that nano-powder component additive is formed and comprised to prescription; Weight ratio by compound and deionized water is 2: 1.0 adding deionized waters, at rotating speed 300r/min rolling ball milling mixing 36h; The ball milling material is in 180 ℃ of oven dry 24h; With the compound alumina crucible of packing into of oven dry, at 860 ℃ of calcining 5h down, synthetic PZT is principal crystalline phase mutually, contains small amounts of Pb ZrO
3And PbTiO
3The nano-powder of crystalline phase adds pre-imitation frosted glass.Pre-imitation frosted glass is 2: 1.0 adding deionized waters by the weight ratio of pre-imitation frosted glass and deionized water, pulverizes 24h in rotating speed 300r/min ball mill; After the ball mill pulverizing, adding polyvinyl alcohol concentration by the 15wt% weight ratio is the liquid of 15wt%, preparation spraying drying nano modification slip, and the slip spraying drying obtains the dried granulation powder; The knobble of diameter 25mm, thickness 0.6～0.8mm is made in dry-pressing under 100～150Mpa pressure, or is pressed into that 25 * 40mm is square, the dice of thickness 0.6～0.8mm.Molding mass is incubated 50h at 850 ℃ of following binder removals; Be incubated 7h down at 1175 ℃ afterwards and become to burn, promptly obtaining principal crystalline phase is the nano modification piezoceramic material of the present invention of PZT phase.
Embodiment 10:
According to prescription Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, wherein A is Mg, and B is Mn, and C is Sb; X=0.10, Y=0.02, Z=0.22.Pb in molar ratio
3O
4: micron (MgCO
3)
4Mg (OH)
25H
2O: ZrO
2: (micron TiO
2: nano-TiO
2): MnCO
3: Sb
2O
3=0.3000: 0.02: 0.5200: (0.248: 0.372): weighing in 0.080: 0.080, preparation meets the compound that nano-powder component additive is formed and comprised to prescription; Weight ratio by compound and deionized water is 2: 1.0 adding deionized waters, at rotating speed 300r/min rolling ball milling mixing 36h; The ball milling material is in 180 ℃ of oven dry 24h; With the compound alumina crucible of packing into of oven dry, at 840 ℃ of calcining 6h down, synthetic PZT is principal crystalline phase mutually, contains small amounts of Pb ZrO
3And PbTiO
3The nano-powder of crystalline phase adds pre-imitation frosted glass.Pre-imitation frosted glass is 2: 1.0 adding deionized waters by the weight ratio of pre-imitation frosted glass and deionized water, pulverizes 24h in rotating speed 300r/min ball mill; After the ball mill pulverizing, adding polyvinyl alcohol concentration by the 15wt% weight ratio is the liquid of 15wt%, preparation spraying drying nano modification slip, and the slip spraying drying obtains the dried granulation powder; The knobble of diameter 25mm, thickness 0.6～0.8mm is made in dry-pressing under 100～150Mpa pressure, or is pressed into that 25 * 40mm is square, the dice of thickness 0.6～0.8mm.Molding mass is incubated 50h at 850 ℃ of following binder removals; Be incubated 8h down at 1160 ℃ afterwards and become to burn, promptly obtaining principal crystalline phase is the nano modification piezoceramic material of the present invention of PZT phase.
Embodiment 11:
According to prescription Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, wherein A is Sr, and B is Mg, and C is Sb; X=0.02, Y=0.026, Z=0.074.Pb in molar ratio
3O
4: SrCO
3: ZrO
2: (micron TiO
2: nano-TiO
2): (MgCO
3)
4Mg (OH)
25H
2O: Sb
2O
3=0.3267: 0.020: 0.5260: (0.1896: 0.2844): weighing in 0.0067: 0.0333, preparation meets the compound that nano-powder component additive is formed and comprised to prescription; Weight ratio by compound and deionized water is 2: 1.0 adding deionized waters, at rotating speed 300r/min rolling ball milling mixing 36h; The ball milling material is in 180 ℃ of oven dry 24h; With the compound alumina crucible of packing into of oven dry, at 830 ℃ of calcining 5h down, synthetic PZT is principal crystalline phase mutually, contains small amounts of Pb ZrO
3And PbTiO
3The nano-powder of crystalline phase adds pre-imitation frosted glass.Pre-imitation frosted glass is 2: 1.0 adding deionized waters by the weight ratio of pre-imitation frosted glass and deionized water, pulverizes 24h in rotating speed 300r/min ball mill; After the ball mill pulverizing, adding polyvinyl alcohol concentration by the 15wt% weight ratio is the liquid of 15wt%, preparation spraying drying nano modification slip, and the slip spraying drying obtains the dried granulation powder; The knobble of diameter 25mm, thickness 0.6～0.8mm is made in dry-pressing under 100～150Mpa pressure, or is pressed into that 25 * 40mm is square, the dice of thickness 0.6～0.8mm.Molding mass is incubated 50h at 850 ℃ of following binder removals; Be incubated 4h down at 1180 ℃ afterwards and become to burn, promptly obtaining principal crystalline phase is the nano modification piezoceramic material of the present invention of PZT phase.
Embodiment 12:
According to prescription Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, wherein A is Ca, and B is Sb, and C is Nb; X=0.02, Y=0.013, Z=0.037.Pb in molar ratio
3O
4: CaCO
3: ZrO
2: (micron TiO
2: nano-TiO
2): Sb
2O
3: Nb
2O
5=0.3267: 0.02: 0.5130: (0.1748: 0.2622): weighing in 0.0083: 0.0167, preparation meets the compound that nano-powder component additive is formed and comprised to prescription; Weight ratio by compound and deionized water is 2: 1.0 adding deionized waters, at rotating speed 300r/min rolling ball milling mixing 36h; The ball milling material is in 180 ℃ of oven dry 24h; With the compound alumina crucible of packing into of oven dry, at 840 ℃ of calcining 5h down, synthetic PZT is principal crystalline phase mutually, contains small amounts of Pb ZrO
3And PbTiO
3The nano-powder of crystalline phase adds pre-imitation frosted glass.Pre-imitation frosted glass is 2: 1.0 adding deionized waters by the weight ratio of pre-imitation frosted glass and deionized water, pulverizes 24h in rotating speed 300r/min ball mill; After the ball mill pulverizing, adding polyvinyl alcohol concentration by the 15wt% weight ratio is the liquid of 15wt%, preparation spraying drying nano modification slip, and the slip spraying drying obtains the dried granulation powder; The knobble of diameter 25mm, thickness 0.6～0.8mm is made in dry-pressing under 100～150Mpa pressure, or is pressed into that 25 * 40mm is square, the dice of thickness 0.6～0.8mm.Molding mass is incubated 50h at 850 ℃ of following binder removals; Be incubated 4h down at 1190 ℃ afterwards and become to burn, promptly obtaining principal crystalline phase is the nano modification piezoceramic material of the present invention of PZT phase.
Claims (4)
1. a nano-powder directly adds the lead titanate piezoelectric ceramics that modification prepares, and it is characterized in that: the prescription composition formula is: Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, wherein A is one or both among Mg, Ca, Sr or the Ba, and B is one or both of Mn, Zn, Ni, Sb or Mg, and C is one or both of Sb, Nb or W; 0＜x≤0.12,0＜Y≤0.15,0＜Z≤0.25; Add nano-powder component additive during the preparation compound, nano-powder component additive is a nano-TiO
2, nanometer ZrO
2, nano-MgO, nanometer CaCO
3, nanometer SrCO
3Or nanometer BaCO
3In one or more, addition be the weight of nano-powder component additive account for the pairing raw material gross weight of this component additive 10～100%.
2. lead titanate piezoelectric ceramics according to claim 1 is characterized in that: described prescription composition formula is Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, x=0.10 wherein, Y=0.026, Z=0.074, A are Mg, and B is Mn, and C is Nb.
3. lead titanate piezoelectric ceramics according to claim 1 is characterized in that: a kind of typical addition of described nano-powder component additive is: nano-TiO
2Powder additives accounts for total TiO
255% of weight; Nanometer ZrO
2Powder additives accounts for total ZrO
235% of weight; The nano-MgO powder additives accounts for 80% of total MgO weight.
4. one kind is directly added the preparation method of the lead titanate piezoelectric ceramics of modification preparation as the arbitrary described nano-powder of claim 1-3, it is characterized in that: may further comprise the steps:
1) compound preparation and low temperature presintering technology: by prescription composition formula Pb
1-XA
X(Zr
0.5+YTi
0.4+Z) (B
1/3C
2/3)
Y+ZO
3, weighing main raw material Pb
3O
4, ZrO
2, TiO
2And each component, add nano-powder component additive and be mixed with compound; Weight ratio by compound and deionized water is 2: 0.5～1.5 adding deionized waters, mixes 24～72h at rotating speed 300r/min rolling ball milling; The ball milling material is in 100～250 ℃ of oven dry 12～36h; With the compound alumina crucible of packing into of oven dry, at 750～950 ℃ of calcining 1～12h down, synthetic Pb-based lanthanumdoped zirconate titanates is principal crystalline phase mutually, contains small amounts of Pb ZrO
3And PbTiO
3The nano-powder of crystalline phase adds pre-imitation frosted glass;
2) pre-imitation frosted glass is pulverized slurrying, granulating and forming and become firing technique: the weight ratio of adding pre-imitation frosted glass and deionized water by nano-powder is 2: 0.5～1.0 adding deionized waters, pulverizes 24～48h in rotating speed 300r/min ball mill; Weight in the pre-imitation frosted glass after pulverizing is 100%, and the weight percent concentration of adding 10～20% is 5～20% polyvinyl alcohol solution, is mixed with spraying drying nano modification slip, and the slip spraying drying obtains the dried granulation powder; The granulation powder is made molding mass, at 750～850 ℃ of following binder removals, insulation 24～72h; Being incubated 1～12h down at 1050～1300 ℃ afterwards becomes to burn promptly.
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| CN101302105B (en) * | 2008-06-30 | 2010-09-29 | 陕西师范大学 | Lead niobium antimonite-containing five-element piezoelectric ceramics material for driver and preparation thereof |
| CN101948309B (en) * | 2010-08-20 | 2013-08-21 | 暨南大学 | PPSMZT-doped piezoelectric ceramic, preparation method thereof and use thereof |
| CN102503420A (en) * | 2011-10-21 | 2012-06-20 | 佛山市亿强电子有限公司 | Piezoelectric ceramics and preparation process thereof |
| CN102515759A (en) * | 2011-12-12 | 2012-06-27 | 中国振华集团红云器材厂 | High-electromechanical coupling coefficient piezoelectric ceramic material and manufacturing method thereof |
| CN102815942A (en) * | 2012-04-20 | 2012-12-12 | 汕头市创新科技电子有限公司 | Piezoelectric ceramic material and piezoelectric ceramic vibrator manufactured by same |
| CN102795854B (en) * | 2012-08-28 | 2013-12-11 | 中国船舶重工集团公司第七一五研究所 | High-power density piezoceramic material and method for preparing same |
| CN103588478A (en) * | 2013-11-15 | 2014-02-19 | 中船重工海声科技有限公司 | Lead titanate piezoelectric ceramics and preparation method |
| CN104446521B (en) * | 2014-11-07 | 2016-05-25 | 东莞思威特电子有限公司 | A kind of technique that reduces PZT piezoelectricity material powder calcining heat |
| CN105948744B (en) * | 2016-05-01 | 2019-01-04 | 林尔福 | A kind of preparation method of the piezoceramic material for frequency converter |
| CN109336593A (en) * | 2018-10-19 | 2019-02-15 | 海鹰企业集团有限责任公司 | A kind of high-temperature resistant piezoelectric ceramic and its preparation process |
| CN109503157B (en) * | 2018-12-17 | 2021-08-31 | 贵州振华红云电子有限公司 | Piezoelectric ceramic with high density and high piezoelectric constant |
| CN110862262B (en) * | 2019-12-05 | 2022-04-29 | 湖南嘉业达电子有限公司 | High-performance piezoelectric ceramic applied to sound element and manufacturing method thereof |
| CN112645709A (en) * | 2020-12-25 | 2021-04-13 | 湖南瀚德微创医疗科技有限公司 | PZT-based piezoelectric ceramic and preparation method thereof |
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