CN103467096B - Novel potassium sodium niobate-based leadless piezoelectric ceramics and preparation method thereof - Google Patents
Novel potassium sodium niobate-based leadless piezoelectric ceramics and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a novel potassium sodium niobate-based leadless piezoelectric ceramics and a preparation method thereof. The potassium sodium niobate-based leadless piezoelectric ceramics which is higher in density, excellent in piezoelectric property and environment-friendly is prepared by adjusting the components of the potassium sodium niobate-based leadless piezoelectric ceramics and adopting the technologies such as microwave sintering, silver roasting, polarization, etc. The novel potassium sodium niobate-based leadless piezoelectric ceramics is prepared from the raw materials of chemical pure Na2CO3, K2CO3, Li2CO3, Nb2O5, Ta2O5 and Sb2O3, and the additives of chemical pure ZnO, ZnCO3 or 5ZnO.4CO2.6H2O; the composition of the leadless piezoelectric ceramics is expressed as the chemical formula: (Na 0.52 K0.46 Li 0.06) (Nb 0.86 Tb 0.08 Sb 0.06) O(3+x) ZnO, wherein x is equal to 0.00-0.05.
Description
Technical field
The present invention relates to a kind of piezoceramic material, particularly relate to a kind of potassium niobate sodium-based leadless piezoelectric ceramic and preparation method thereof.
Background technology
Piezoelectric ceramics is that a class is at the widely used new and high technology material of electron trade.But use Pb-based lanthanumdoped zirconate titanates Pb (Zr, Ti) O on a large scale at present
3base piezoelectric ceramic (being called PZT base piezoelectric ceramic), in PZT base piezoelectric ceramic, Pb content is up to more than 60wt. %, all can work the mischief to human body health and living environment thereof in its preparation, use, waste procedures.Therefore research and develop piezoelectric property excellent, eco-friendly leadless piezoelectric ceramics is urgent, to have an important social effect problem.
In leadless piezoelectric ceramics system, potassium-sodium niobate (K, Na) NbO
3based leadless piezoelectric ceramics (being called KNN base piezoelectric ceramic), because it has higher Curie temperature and good electromechanical coupling performance, is considered to one of candidate material of the most potential replacement lead base piezoelectric ceramics.But the KNN ceramic dense degree prepared by conventional sintering technique is not high, and piezoelectric property is also poor.Its reason mainly contain following some: KNbO
3-NaNbO
3the phase equilibrium temperature of sosoloid is below 1140 DEG C; Basic metal in KNN pottery easily volatilizees when sintering at relatively high temperatures, causes the actual constituent nonstoichiometry formula of pottery, easily forms second-phase and reduces its piezoelectric property; Higher sintering temperature and longer soaking time, easily make the portion crystal of pottery occur abnormal growth phenomenon, make the distribution of crystal grain occur the two poles of the earth distribution situation.
Be expected to overcome above-mentioned shortcoming by measure such as adjustment preparation technology or doping vario-property etc.The sintering method of current preparation KNN pottery mainly contains hot pressed sintering, discharge plasma sintering etc.Although these sintering technologies can improve the density of stupalith, its apparatus expensive, the shape of sample and quantity are all subject to strict restriction, are not suitable for suitability for industrialized production.Current research data shows, the factor affecting KNN base pottery alkali metal volatilization in sintering process mainly contains sintering temperature and sintering time.The sintering temperature of conventional sintering technique is higher, and sintering time is long, is unfavorable for the sintering of KNN base pottery, therefore the piezoelectric constant of KNN pottery prepared of conventional sintering technique
d 33only have 80 pC/N.
Summary of the invention
The present invention seeks to the deficiency in order to solve the problems of the technologies described above existence, providing that a kind of density is high, integrated piezo excellent performance and potassium niobate sodium-based leadless piezoelectric ceramic of environmental protection and preparation method thereof.
The technical solution adopted in the present invention is: by adjusting the composition of potassium niobate sodium-based leadless piezoelectric ceramic, adopt microwave sintering, preparation technology such as roasting silver, polarization etc., in lower sintering temperature and shorter sintering time, prepare that density is higher, piezoelectric property is excellent and the potassium niobate sodium-based leadless piezoelectric ceramic of environmental protection.The present invention is raw materials used is chemical pure Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3, additive is chemical pure ZnO, ZnCO
3or 5ZnO4CO
26H
2o; The one-tenth of this pottery is grouped into useful chemical formula and is expressed as: (Na
0.52k
0.46li
0.06) (Nb
0.86ta
0.08sb
0.06) O
3+
xznO, wherein,
x=0.00 ~ 0.05.
The technological process that microwave sintering of the present invention prepares potassium niobate sodium-based leadless piezoelectric ceramic is:
Step one, the present invention is raw materials used is chemical pure Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3, additive is chemical pure ZnO, ZnCO
3or 5ZnO4CO
26H
2o; Raw material is pressed chemical formula (Na
0.52k
0.46li
0.06) (Nb
0.86ta
0.08sb
0.06) O
3+
xznO(
x=0.00 ~ 0.05) proportioning carries out weighing, preparing burden, with dehydrated alcohol as ball-milling medium, with planetary ball mill ball milling 4 ~ 8 h, then slurry to be placed in loft drier 100 DEG C dry 8 h after obtain dry powder;
Step 2, step one gained dry powder is put into temperature programmed control box-type furnace, with speed continuous warming to 800 ~ 900 DEG C of 5 DEG C/min, insulation 4 ~ 6 h, synthesize potassium-sodium niobate-based ceramic powder;
Step 3, add the polyvinyl alcohol of 5wt.% as binding agent using in step 2 gained ceramic powder, stir, put into mould, with Manual tablet pressing machine compression moulding under 200MPa;
Temperature programmed control box-type furnace put into by step 4, biscuit step 3 suppressed, and rises to 650 DEG C with the temperature rise rate of 10 DEG C/min, and insulation 60min carries out binder removal, is then cooled to room temperature;
Step 5, the ceramics sample after step 4 binder removal is placed in microwave agglomerating furnace, at 1000 ~ 1100 DEG C of temperature, is incubated the densification sintering that 20 ~ 60 min carry out ceramics sample;
Step 6, to polish to ceramic plate with 600 order sand paper, after polishing, coat silver slurry, be heated to 520 DEG C in temperature programmed control box-type furnace at two surface uniforms, being incubated 20 min, to carry out roasting silver-colored; Put into silicone oil after ceramic plate after roasting silver to polarize, poling temperature is: 80 ~ 100 DEG C; Polarizing voltage is 3 ~ 5 kV/mm; Polarization time is 20 min; Obtain this potassium niobate sodium-based leadless piezoelectric ceramic.
Raw material in described step one will dry 10 h, in order to thoroughly get rid of the moisture in raw material at 120 DEG C before weighing.
In described step one, ball-milling medium is dehydrated alcohol and zirconia ball, and the mass ratio of raw material, dehydrated alcohol and zirconia ball is: 1:1:2, and drum's speed of rotation is 250-300 r/min.
In described step 5, microwave sintering warming machine is made as: the temperature rise rate before 1000 DEG C is 25 DEG C/min; 1000 DEG C of later temperature rise rates are 15 DEG C/min.
The invention has the advantages that, add excess alkali metal K and Na by 8 drift angles at perovskite structure, to compensate the volatilization of K, Na in sintering process, keep the perovskite structure of ceramic crystal; By adding ZnO, ZnCO
3or 5ZnO4CO
26H
2o, to reduce the sintering temperature of pottery, thus improves density and the mechanical quality factor of pottery.
Present invention employs Microwave Sintering Techniques, microwave sintering is a kind of energy-efficient sintering method, has following advantage compared with sintering with conventional solid: heating rate is fast, and soaking time is short, inhibits alkali-metal volatilization in sintering process; Micro-wave energy directly penetrates the sample of certain depth, heats at different depths simultaneously, does not need heat transfer process, avoids the abnormal growth of ceramic crystalline grain in sintering process, can prepare the stupalith of uniform crystal particles distribution at a lower temperature; By regulating the output rating of microwave, can make the heating state of sample that inertialess occurs immediately and changing, be convenient to automatically control and operate continuously; The thermal inertia of microwave sintering is little, energy fast cooling after terminating, and heat utilization rate is high; Can sintering time be shortened simultaneously, thus suppress the uniformity coefficient of alkali-metal volatilization and regulation and control ceramic crystalline grain.Employing this method makes preparation cycle shorten, thus is more conducive to suitability for industrialized production.
The present invention adopts and puts into temperature programmed control box-type furnace at the biscuit suppressed, and rises to 650 DEG C with the temperature rise rate of 10 DEG C/min, and insulation 60min carries out binder removal, and binder decomposed is volatilized; Adopt roasting silver process, prepare silver electrode at ceramic plate two ends; Adopt polarization process, make piezoelectric ceramics have better piezoelectric property.
To invention has been electrical performance testing, performance index are as follows: piezoelectric constant
d 33be 221 ~ 305 pC/N; Planar electromechanical coupling factor
k pbe 24 ~ 48%; Mechanical quality factor
q mbe 110 ~ 214; Specific inductivity
ε rbe 694 ~ 872; Dielectric loss tan
δbe 0.024 ~ 0.04; Relative density
ρ rbe 86.8 ~ 96.5%; Remnant polarization
p rbe 15.6 ~ 28.6 μ C/cm
2; Curie temperature
t cit is 442 ~ 464 DEG C.
The present invention is different from traditional piezoelectric ceramics, and not leaded and any objectionable impurities, is not only beneficial to the healthy of the producer, and to environment without any pollution.
Embodiment
Following examples understand the present invention in detail.
Embodiment 1:
With chemical pure Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3be raw material with ZnO, according to chemical formula (Na
0.52k
0.46li
0.06) (Nb
0.86ta
0.08sb
0.06) O
3+
xznO, gets
x=0.005, prepare burden; Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3, each raw material of ZnO mass ratio be: 306:356:46:1267:196:97:5.To prepare burden 50 g by the mass ratio of above raw material, using dehydrated alcohol as ball-milling medium, with planetary ball mill batch mixing 4 h, rotating speed is 250 rpm, and slip dries 8 h at 100 DEG C.Dry powder is incubated 4 h at 800 DEG C, synthesizes potassium-sodium niobate-based ceramic powder.The polyvinyl alcohol (PVA) of 5wt.% is added, compression moulding under 200MPa in powder.First use conventional sintering method to rise to 650 DEG C with the temperature rise rate of 10 DEG C/min, be incubated 60 min and carry out binder removal, be cooled to room temperature.And then by microwave sintering method at 1100 DEG C of insulation 30min, the temperature rise rate before 1000 DEG C is 25 DEG C/min; 1000 DEG C of later temperature rise rates are 15 DEG C/min.Upper and lower two surfaces of burned ceramics sample are parallel to be polished and evenly coats silver slurry afterwards, puts into box-type furnace, at 520 DEG C, is incubated 30min, carry out roasting silver-colored.Roast silver-colored ceramic plate to put into silicone oil and be heated to 80 ~ 100 DEG C, under 3 ~ 5kV/mm voltage, keep 20min to polarize, after static 24 h, carry out electrical performance testing.Result is as follows:
| d 33(pC/N) | k p(%) | Q m | ε r | tan δ | ρ r(%) | P r(μC/cm 2) | T c(℃) |
| 290 | 32 | 110 | 723 | 0.036 | 92.4 | 23.4 | 445 |
embodiment 2:
With chemical pure Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3be raw material with ZnO, according to chemical formula (Na
0.52k
0.46li
0.06) (Nb
0.86ta
0.08sb
0.06) O
3+
xznO, gets
x=0.010, prepare burden; Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3, each raw material of ZnO mass ratio be: 305:355:46:1265:196:97:9.To prepare burden 50 g by the mass ratio of above raw material, using dehydrated alcohol as ball-milling medium, with planetary ball mill batch mixing 4 h, rotating speed is 250 rpm, and slip dries 8 h at 100 DEG C.Dry powder is incubated 4 h at 800 DEG C, synthesizes potassium-sodium niobate-based ceramic powder.The polyvinyl alcohol (PVA) of 5wt.% is added, compression moulding under 200MPa in powder.First use conventional sintering method to rise to 650 DEG C with the temperature rise rate of 10 DEG C/min, be incubated 60 min and carry out binder removal, be cooled to room temperature.And then by microwave sintering method at 1050 DEG C of insulation 30min, the temperature rise rate before 1000 DEG C is 25 DEG C/min; 1000 DEG C of later temperature rise rates are 15 DEG C/min.Upper and lower two surfaces of burned ceramics sample are parallel to be polished and evenly coats silver slurry afterwards, puts into box-type furnace, at 520 DEG C, is incubated 30min, carry out roasting silver-colored.Roast silver-colored ceramic plate to put into silicone oil and be heated to 80 ~ 100 DEG C, under 3 ~ 5kV/mm voltage, keep 20min to polarize, after static 24 h, carry out electrical performance testing.Result is as follows:
| d 33(pC/N) | k p(%) | Q m | ε r | tan δ | ρ r(%) | P r(μC/cm 2) | T c(℃) |
| 305 | 48 | 195 | 865 | 0.028 | 94.5 | 28.6 | 464 |
embodiment 3:
With chemical pure Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3be raw material with ZnO, according to chemical formula (Na
0.52k
0.46li
0.06) (Nb
0.86ta
0.08sb
0.06) O
3+
xznO, gets
x=0.015, prepare burden; Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3, each raw material of ZnO mass ratio be: 305:354:46:1262:196:97:13.5.To prepare burden 50 g by the mass ratio of above raw material, using dehydrated alcohol as ball-milling medium, with planetary ball mill batch mixing 4 h, rotating speed is 250 rpm, and slip dries 8 h at 100 DEG C.Dry powder is incubated 4 h at 800 DEG C, synthesizes potassium-sodium niobate-based ceramic powder.The polyvinyl alcohol (PVA) of 5wt.% is added, compression moulding under 200MPa in powder.First use conventional sintering method to rise to 650 DEG C with the temperature rise rate of 10 DEG C/min, be incubated 60 min and carry out binder removal, be cooled to room temperature.And then by microwave sintering method at 1020 DEG C of insulation 30min, the temperature rise rate before 1000 DEG C is 25 DEG C/min; 1000 DEG C of later temperature rise rates are 15 DEG C/min.Upper and lower two surfaces of burned ceramics sample are parallel to be polished and evenly coats silver slurry afterwards, puts into box-type furnace, at 520 DEG C, is incubated 30min, carry out roasting silver-colored.Roast silver-colored ceramic plate to put into silicone oil and be heated to 80 ~ 100 DEG C, under 3 ~ 5kV/mm voltage, keep 20min to polarize, after static 24 h, carry out electrical performance testing.Result is as follows:
| d 33(pC/N) | k p(%) | Q m | ε r | tan δ | ρ r(%) | P r(μC/cm 2) | T c(℃) |
| 296 | 43 | 210 | 765 | 0.024 | 96.5 | 28.6 | 452 |
embodiment 4:
With chemical pure Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3be raw material with ZnO, according to chemical formula (Na
0.52k
0.46li
0.06) (Nb
0.86ta
0.08sb
0.06) O
3+
xznO, gets
x=0.020, prepare burden; Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3, each raw material of ZnO mass ratio be: 304:354:46:1259:196:96:18.To prepare burden 50 g by the mass ratio of above raw material, using dehydrated alcohol as ball-milling medium, with planetary ball mill batch mixing 4 h, rotating speed is 250 rpm, and slip dries 8 h at 100 DEG C.Dry powder is incubated 4 h at 800 DEG C, synthesizes potassium-sodium niobate-based ceramic powder.The polyvinyl alcohol (PVA) of 5wt.% is added, compression moulding under 200MPa in powder.First use conventional sintering method to rise to 650 DEG C with the temperature rise rate of 10 DEG C/min, be incubated 60 min and carry out binder removal, be cooled to room temperature.And then by microwave sintering method at 1000 DEG C of insulation 30min, the temperature rise rate before 1000 DEG C is 25 DEG C/min; 1000 DEG C of later temperature rise rates are 15 DEG C/min.Upper and lower two surfaces of burned ceramics sample are parallel to be polished and evenly coats silver slurry afterwards, puts into box-type furnace, at 520 DEG C, is incubated 30min, carry out roasting silver-colored.Roast silver-colored ceramic plate to put into silicone oil and be heated to 80 ~ 100 DEG C, under 3 ~ 5kV/mm voltage, keep 20min to polarize, after static 24 h, carry out electrical performance testing.Result is as follows:
| d 33(pC/N) | k p(%) | Q m | ε r | tan δ | ρ r(%) | P r(μC/cm 2) | T c(℃) |
| 285 | 38 | 212 | 716 | 0.032 | 91.7 | 22.5 | 447 |
embodiment 5:
With chemical pure Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3be raw material with ZnO, according to chemical formula (Na
0.52k
0.46li
0.06) (Nb
0.86ta
0.08sb
0.06) O
3+
xznO, gets
x=0.025, prepare burden; Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3, each raw material of ZnO mass ratio be: 303:353:46:1256:194:96:22.To prepare burden 50 g by the mass ratio of above raw material, using dehydrated alcohol as ball-milling medium, with planetary ball mill batch mixing 4 h, rotating speed is 250 rpm, and slip dries 8 h at 100 DEG C.Dry powder is incubated 4 h at 800 DEG C, synthesizes potassium-sodium niobate-based ceramic powder.The polyvinyl alcohol (PVA) of 5wt.% is added, compression moulding under 200MPa in powder.First use conventional sintering method to rise to 650 DEG C with the temperature rise rate of 10 DEG C/min, be incubated 60 min and carry out binder removal, be cooled to room temperature.And then by microwave sintering method at 1000 DEG C of insulation 30min, the temperature rise rate before 1000 DEG C is 25 DEG C/min; 1000 DEG C of later temperature rise rates are 15 DEG C/min.Upper and lower two surfaces of burned ceramics sample are parallel to be polished and evenly coats silver slurry afterwards, puts into box-type furnace, at 520 DEG C, is incubated 30min, carry out roasting silver-colored.Roast silver-colored ceramic plate to put into silicone oil and be heated to 80 ~ 100 DEG C, under 3 ~ 5kV/mm voltage, keep 20min to polarize, after static 24 h, carry out electrical performance testing.Result is as follows:
| d 33(pC/N) | k p(%) | Q m | ε r | tan δ | ρ r(%) | P r(μC/cm 2) | T c(℃) |
| 221 | 24 | 214 | 694 | 0.038 | 86.8 | 15.6 | 442 |
embodiment 6:
With chemical pure Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3be raw material with ZnO, according to chemical formula (Na
0.52k
0.46li
0.06) (Nb
0.86ta
0.08sb
0.06) O
3+
xznO, gets
x=0.010, prepare burden; Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3, each raw material of ZnO mass ratio be: 305:355:46:1265:196:97:9.To prepare burden 50 g by the mass ratio of above raw material, using dehydrated alcohol as ball-milling medium, with planetary ball mill batch mixing 4 h, rotating speed is 250 rpm, and slip dries 8 h at 100 DEG C.Dry powder is incubated 4 h at 800 DEG C, synthesizes potassium-sodium niobate-based ceramic powder.The polyvinyl alcohol (PVA) of 5wt.% is added, compression moulding under 200MPa in powder.First use conventional sintering method to rise to 650 DEG C with the temperature rise rate of 10 DEG C/min, be incubated 60 min and carry out binder removal, be cooled to room temperature.And then by microwave sintering method at 1050 DEG C of insulation 50min, the temperature rise rate before 1000 DEG C is 25 DEG C/min; 1000 DEG C of later temperature rise rates are 15 DEG C/min.Upper and lower two surfaces of burned ceramics sample are parallel to be polished and evenly coats silver slurry afterwards, puts into box-type furnace, at 520 DEG C, is incubated 30min, carry out roasting silver-colored.Roast silver-colored ceramic plate to put into silicone oil and be heated to 80 ~ 100 DEG C, under 3 ~ 5kV/mm voltage, keep 20min to polarize, after static 24 h, carry out electrical performance testing.Result is as follows:
| d 33(pC/N) | k p(%) | Q m | ε r | tan δ | ρ r(%) | P r(μC/cm 2) | T c(℃) |
| 292 | 36 | 196 | 872 | 0.034 | 91.4 | 26.7 | 454 |
embodiment 7:
With chemical pure Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3be raw material with ZnO, according to chemical formula (Na
0.52k
0.46li
0.06) (Nb
0.86ta
0.08sb
0.06) O
3+
xznO, gets
x=0.010, prepare burden; Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3, each raw material of ZnO mass ratio be: 305:355:46:1265:196:97:9.To prepare burden 50 g by the mass ratio of above raw material, using dehydrated alcohol as ball-milling medium, with planetary ball mill batch mixing 4 h, rotating speed is 250 rpm, and slip dries 8 h at 100 DEG C.Dry powder is incubated 4 h at 800 DEG C, synthesizes potassium-sodium niobate-based ceramic powder.The polyvinyl alcohol (PVA) of 5wt.% is added, compression moulding under 200MPa in powder.First use conventional sintering method to rise to 650 DEG C with the temperature rise rate of 10 DEG C/min, be incubated 60 min and carry out binder removal, be cooled to room temperature.And then by microwave sintering method at 1050 DEG C of insulation 60min, the temperature rise rate before 1000 DEG C is 25 DEG C/min; 1000 DEG C of later temperature rise rates are 15 DEG C/min.Upper and lower two surfaces of burned ceramics sample are parallel to be polished and evenly coats silver slurry afterwards, puts into box-type furnace, at 520 DEG C, is incubated 30min, carry out roasting silver-colored.Roast silver-colored ceramic plate to put into silicone oil and be heated to 80 ~ 100 DEG C, under 3 ~ 5kV/mm voltage, keep 20min to polarize, after static 24 h, carry out electrical performance testing.Result is as follows:
| d 33(pC/N) | k p(%) | Q m | ε r | tan δ | ρ r(%) | P r(μC/cm 2) | T c(℃) |
| 278 | 33 | 190 | 782 | 0.040 | 88.4 | 22.4 | 448 |
Claims (2)
1. a potassium niobate sodium-based leadless piezoelectric ceramic, is characterized in that: raw materials used is chemical pure Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3, additive is chemical pure ZnO, ZnCO
3or 5ZnO4CO
26H
2o; The one-tenth of this pottery is grouped into useful chemical formula and is expressed as: (Na
0.52k
0.46li
0.06) (Nb
0.86ta
0.08sb
0.06) O
3+
xznO, wherein,
x=0.00 ~ 0.05; Preparation method is:
Step one, raw material is pressed chemical formula (Na
0.52k
0.46li
0.06) (Nb
0.86ta
0.08sb
0.06) O
3+
xznO, wherein,
x=0.00 ~ 0.05, proportioning carry out weighing, preparing burden, with dehydrated alcohol as ball-milling medium, with planetary ball mill ball milling 4 ~ 8 h, then slurry to be placed in loft drier 100 DEG C dry 8 h after obtain dry powder; Step 2, step one gained dry powder is put into temperature programmed control box-type furnace, with speed continuous warming to 800 ~ 900 DEG C of 5 DEG C/min, insulation 4 ~ 6 h, synthesize potassium-sodium niobate-based ceramic powder; Step 3, add the polyvinyl alcohol of 5wt.% as binding agent using in step 2 gained ceramic powder, stir, put into mould, with Manual tablet pressing machine compression moulding under 200MPa; Temperature programmed control box-type furnace put into by step 4, biscuit step 3 suppressed, and rises to 650 DEG C with the temperature rise rate of 10 DEG C/min, and insulation 60min carries out binder removal, is then cooled to room temperature; Step 5, the ceramics sample after step 4 binder removal is placed in microwave agglomerating furnace, at 1000 ~ 1100 DEG C of temperature, is incubated the densification sintering that 20 ~ 60 min carry out ceramics sample; Step 6, to polish to ceramic plate with 600 order sand paperings, after polishing, coat silver slurry, be heated to 520 DEG C in temperature programmed control box-type furnace at two surface uniforms, being incubated 20 min, to carry out roasting silver-colored; Put into silicone oil after ceramic plate after roasting silver to polarize, poling temperature is: 80 ~ 100 DEG C; Polarizing voltage is: at 3 ~ 5 kV/mm; Polarization time is: 20 min; Obtain this potassium niobate sodium-based leadless piezoelectric ceramic.
2. potassium niobate sodium-based leadless piezoelectric ceramic according to claim 1, is characterized in that: Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3, ZnO mass ratio is: 306:356:46:1267:196:97:5.
3. potassium niobate sodium-based leadless piezoelectric ceramic according to claim 1, is characterized in that: Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3, ZnO mass ratio is: 304:354:46:1259:196:96:18.
4. potassium niobate sodium-based leadless piezoelectric ceramic according to claim 1, is characterized in that: Na
2cO
3, K
2cO
3, Li
2cO
3, Nb
2o
5, Ta
2o
5, Sb
2o
3, ZnO mass ratio is: 305:355:46:1265:196:97:9.
5. potassium niobate sodium-based leadless piezoelectric ceramic according to claim 1, is characterized in that: the raw material in step one will dry 10 h at 120 DEG C before weighing.
6. potassium niobate sodium-based leadless piezoelectric ceramic according to claim 1, is characterized in that: in step 5, microwave sintering warming machine is made as: the temperature rise rates before 1000 DEG C are 25 DEG C/min; 1000 DEG C of later temperature rise rates are 15 DEG C/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310423852.7A CN103467096B (en) | 2013-09-17 | 2013-09-17 | Novel potassium sodium niobate-based leadless piezoelectric ceramics and preparation method thereof |
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| CN104016674B (en) * | 2014-06-17 | 2015-09-16 | 河南科技大学 | A kind of barium titanate-based lead-free piezoelectric ceramic and preparation method thereof |
| CN106242568B (en) * | 2016-07-22 | 2019-03-22 | 郑州大学 | A kind of microwave synthesis method of potassium-sodium niobate leadless piezoelectric ceramic |
| CN106291142B (en) * | 2016-09-19 | 2022-04-29 | 河南感联智能科技有限公司 | Piezoelectric ceramic and piezoelectric semiconductor test piece diversity polarization experimental system |
| CN107176837B (en) * | 2017-05-31 | 2019-12-06 | 哈尔滨理工大学 | Preparation method of potassium tantalate niobate ceramic with ultrahigh dielectric constant |
| CN109206137A (en) * | 2018-11-19 | 2019-01-15 | 福州大学 | A kind of preparation method of potassium-sodium niobate-zinc titanate strontium crystalline ceramics |
| CN109721352B (en) * | 2019-03-16 | 2021-08-20 | 信阳师范学院 | Sodium bismuth titanate-based lead-free piezoelectric ceramic prepared by adopting microwave material scientific workstation and preparation method thereof |
| CN113461422B (en) * | 2021-08-03 | 2022-05-31 | 四川大学 | High-voltage anti-fatigue potassium-sodium niobate-based lead-free piezoelectric ceramic and preparation method thereof |
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