CN100448796C - Low temperature synthesized no-lead piezoelectric Mg doped sodium potassium niobate ceramic and its prepn process - Google Patents
Low temperature synthesized no-lead piezoelectric Mg doped sodium potassium niobate ceramic and its prepn process Download PDFInfo
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- CN100448796C CN100448796C CNB2007101189078A CN200710118907A CN100448796C CN 100448796 C CN100448796 C CN 100448796C CN B2007101189078 A CNB2007101189078 A CN B2007101189078A CN 200710118907 A CN200710118907 A CN 200710118907A CN 100448796 C CN100448796 C CN 100448796C
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- 239000000919 ceramic Substances 0.000 title claims abstract description 40
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims description 5
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 239000011734 sodium Substances 0.000 claims abstract description 23
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 10
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 7
- 229910052709 silver Inorganic materials 0.000 claims abstract description 7
- 239000004332 silver Substances 0.000 claims abstract description 7
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 5
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 15
- 239000011777 magnesium Substances 0.000 claims description 12
- 230000010287 polarization Effects 0.000 claims description 9
- 238000000748 compression moulding Methods 0.000 claims description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- OGWLTJRQYVEDMR-UHFFFAOYSA-F tetramagnesium;tetracarbonate Chemical compound [Mg+2].[Mg+2].[Mg+2].[Mg+2].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O OGWLTJRQYVEDMR-UHFFFAOYSA-F 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 244000137852 Petrea volubilis Species 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 229920002545 silicone oil Polymers 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 235000015895 biscuits Nutrition 0.000 claims description 2
- 238000002156 mixing Methods 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000009740 moulding (composite fabrication) Methods 0.000 abstract 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 6
- UKDIAJWKFXFVFG-UHFFFAOYSA-N potassium;oxido(dioxo)niobium Chemical compound [K+].[O-][Nb](=O)=O UKDIAJWKFXFVFG-UHFFFAOYSA-N 0.000 description 6
- 238000001272 pressureless sintering Methods 0.000 description 5
- 238000000465 moulding Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- LBSANEJBGMCTBH-UHFFFAOYSA-N manganate Chemical compound [O-][Mn]([O-])(=O)=O LBSANEJBGMCTBH-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The low temperature synthesized no-lead piezoelectric Mg doped sodium potassium niobate ceramic as one kind of environment friendly material has the composition formula of (NaaKbLic)NbO3+xMgO, where, a, b, c and x are the molar fractions of Na, K, Li, Mg separately, a is 0.20-0.80, b is 0.20-0.80, c is 0.00-0.30, and x is 0.00-0.30. Its preparation process includes the technological steps of mixing material, roasting, forming, sintering, coating silver, polarizing, etc. The low temperature synthesized no-lead piezoelectric Mg doped sodium potassium niobate ceramic of the present invention has the advantages of sintering temperature effectively lowered to 800-1040 deg.c and high performance.
Description
Technical field
The invention belongs to the environmentally friendly material of function ceramics field, a kind of low temperature synthetic no-lead piezoelectric Mg doped sodium potassium niobate ceramic and preparation method thereof is provided especially.
Background technology
Piezoelectric ceramics is important, the widely used hi-tech material of a class, but at present extensive what use is the lead base piezoelectric ceramics, and the mankind and ecotope are brought serious harm.The research and development leadless piezoelectric ceramics become one urgent, have a problem of society and economic implications.In the leadless piezoelectric ceramics system, niobate lead-free piezoelectric ceramics (K, Na) NbO
3, because of it has high Curie temperature and piezoelectric property, be considered to one of material of the most promising replacement lead base piezoelectric ceramics, by adjusting preparation technology or measure such as element modified is expected to improve its performance.At present the main technique of this ceramic systems of preparation has: pressure sintering, forge hot, discharge plasma sintering etc., these complex process equipment, production cost are higher.Traditional non-pressure sintering technology is not owing to need special experimental installation, and is with low cost and receive much concern.But present data shows that the roasting synthesis temperature of pressureless sintering is very high, discloses the titanate MTiO that adds divalent metal in the potassium-sodium niobate system as patent CN1810711A
3(M is at least a among Ca, Mg, Ba and the Sr) and MnO
2, its sintering temperature all is higher than 1050 ℃, and after adding titanate, the piezoelectric property of material is unsatisfactory.Patent CN1919791A discloses in the potassium-sodium niobate system and has added CuO, though the Q of material
mHigher, but other piezoelectric property such as piezoelectric constant are lower, and sintering temperature is also more than 1050 ℃.Patent CN1511802A adds Ta or Sb in the potassium-sodium niobate system, disclose class general formula (Li
xNa
yK
1-x-y) (Nb
1-zR
z) O
3The multi constituent niobate lead-free piezoelectric ceramics of (wherein R is Ta or Sb) expression, sintering temperature is 1100-1200 ℃, the piezoelectric constant of this type of material is up to 150pC/N.Patent CN1958511A adds Ta and Sb simultaneously in the potassium-sodium niobate system, though the piezoelectric property of material obviously improves, sintering temperature is still more than 1050 ℃.
Table 1 has compared the sintering temperature and the performance of the potassium sodium niobate piezoelectric ceramics of the pressureless sintering preparation that relates in low sintering potassium niobate sodium-based leadless piezoelectric ceramic provided by the present invention and other patent.
The potassium niobate sodium-based leadless piezoelectric ceramic performance of table 1 pressureless sintering relatively
| Patent | The doping composition | Sintering temperature (℃) | d 33(pC/N) |
| CN1511802A | Ta, Sb and rare earth class manganate | 1100-1200 | 120-157 |
| CN1699280A | Ta, Sb and SrTiO 3 | 1100-1250 | Below 120 |
| CN1810711A | MnO 2And titanates of alkali-earth metals | 1070-1190 | 30-222 |
| CN1919791A | CuO | 1050-1130 | 90-120 |
| CN1958511A | Ta、Sb | 1085-1220 | 109-252 |
| The present invention | Mg | 800-1000 | 120-231 |
In sum, the pressureless sintering temperature of the leadless piezoelectric ceramics of better performances all is higher than 1050 ℃ at present.And in the relevant patent of being found, there is no in the potassium-sodium niobate system by adding MgO, MgCO
3And magnesium basic carbonate reduces the report of pressureless sintering temperature.
Summary of the invention
The object of the present invention is to provide a kind of low temperature synthesized no-lead piezoelectric Mg doped sodium potassium niobate ceramic and preparation method, and the pottery that makes have piezoelectricity preferably, can practical planar electromechanical coupling factor k
p
The present invention adopts traditional non-pressure sintering technology, has synthesized potassium niobate sodium-based leadless piezoelectric ceramic in lower sintering temperature 800-1040 ℃ scope, and sintering temperature is lower than present document and patent report value.This pottery is formed with general formula (Na
aK
bLi
c) NbO
3+ xMgO represents that wherein a, b, c, x represent the molar fraction of Na, K, Li, Mg component respectively.The scope of numerical value is: 0.20≤a≤0.80,0.20≤b≤0.80,0.00＜c≤0.30,0.00＜x≤0.30.
The preparation process of low-temperature sintered ceramics of the present invention is:
(1) raw material is pressed general formula (Na respectively
aK
bLi
c) NbO
3The proportioning of+xMgO is carried out weighing, batching, uses dehydrated alcohol to be medium, and after 1-8 hour, oven dry obtains dry powder with the planetary ball mill ball milling; A, b, c, x represent the molar fraction of Na, K, Li, Mg component respectively in the general formula, and the scope of numerical value is: 0.20≤a≤0.80,0.20≤b≤0.80,0.00＜c≤0.30,0.00＜x≤0.30; Magnesium-doped element is respectively with MgO, MgCO
3Or magnesium basic carbonate is that raw material adds;
(2) dry powder is warming up to 500-900 ℃ continuously in the temperature programmed control box-type furnace, is incubated 1-10 hour, carry out the synthetic of niobate;
(3) in the roasting powder of preparation, behind the adding binding agent, put into mould, with oil press compression moulding under 100-500MPa;
(4) biscuit of compression moulding is put into the temperature programmed control box-type furnace, be warming up to 800-1040 ℃ continuously, sintering 1-4 hour, be cooled to room temperature;
(5) ceramic disks that makes with the polishing of 600 order fine sandpapers, be coated with roasting silver electrode on two surfaces afterwards, make and put into polarization device behind the silver-colored ceramic plate, silicone oil is heated to 100-200 ℃, under 1-5kV/mm voltage, keep 10-60min, make the adulterated potassium niobate sodium-based leadless piezoelectric ceramic of magnesium.Measure the density and the piezoelectric property thereof of sintered specimen under the differing temps; Obtain the piezoelectric ceramics finished product of excellent property.
Raw material of the present invention adopts commercial Na
2CO
3(99.8%), K
2CO
3(99%), Li
2CO
3(99.5%) and Nb
2O
5(99.95%), with commercial 98% MgO, 99% MgCO
3Or (molecular formula is 5MgO4CO to contain the magnesium basic carbonate of 44%MgO
26H
2O) be added ingredients.
The invention has the advantages that, by doped with Mg O, MgCO
3Or magnesium basic carbonate effectively reduces the sintering temperature of potassium niobate sodium-based leadless piezoelectric ceramic, synthesized the ceramics sample of excellent property in 800-1040 ℃ low temperature range.
Embodiment
The invention provides a kind of method of effective reduction potassium niobate sodium-based leadless piezoelectric ceramic sintering temperature.Its preparation method comprises mixing raw material, roasting, moulding, sintering, quilt silver, polarization.
Exemplify basic inventive embodiment below.
Embodiment 1:
According to (Na
0.263K
0.772Li
0.057) NbO
3+ 0.044MgO (a=0.263, b=0.772, c=0.057, x=0.044) prescription is with electronic balance difference weighing 0.3195 gram Na
2CO
3, 1.2227 gram K
2CO
3, 0.0483 gram Li
2CO
3, 2.9122 gram Nb
2O
5And 0.0406 gram MgO, as medium, with planetary ball mill grinding batch mixing 8 hours, rotating speed was 100rpm with dehydrated alcohol, slip obtains the siccative powder 50 ℃ of oven dry.Dry powder is incubated 9 hours through 500 ℃, carries out the synthetic of niobate.Get powder 0.3 and restrain in the mould of the Φ 10mm that packs into compression moulding.The disk of moulding is put into temperature programmed control box-type furnace sintering, carries out sintering under 1040 ℃, is incubated 1 hour, is cooled to room temperature and makes ceramic disks.After the polishing of 600 order fine sandpapers, be coated with roasting silver electrode on two surfaces and make by silver-colored ceramic plate, put into polarization device, silicone oil is heated to 100 ℃, keeps 10min to polarize under 5kV/mm voltage, cools to room temperature again, finishes polarization.
Embodiment 2:
According to (Na
0.539K
0.467Li
0.114) NbO
3+ 0.187MgO (a=0.539, b=0.467, c=0.114, x=0.187) prescription is with electronic balance difference weighing 0.7163 gram Na
2CO
3, 0.8092 gram K
2CO
3, 0.1056 gram Li
2CO
3, 2.7093 gram Nb
2O
5And 0.1977 the gram MgCO
3, as medium, use planetary ball mill grinding batch mixing 4 hours with dehydrated alcohol, rotating speed is 250rpm, slip obtains the siccative powder 120 ℃ of oven dry.Dry powder is incubated 4 hours through 650 ℃, carries out the synthetic of niobate.Get powder 0.3 and restrain in the mould of the Φ 10mm that packs into compression moulding.The disk of moulding is put into temperature programmed control box-type furnace sintering, carries out sintering under 960 ℃, is incubated 2 hours, is cooled to room temperature and makes ceramic disks.After the polishing of 600 order fine sandpapers, be coated with roasting silver electrode on two surfaces and make by silver-colored ceramic plate, put into polarization device, silicone oil is heated to 150 ℃, keeps 30min to polarize under 3kV/mm voltage, cools to room temperature again, finishes polarization.
Embodiment 3:
According to (Na
0.539K
0.467Li
0.001) NbO
3+ 0.187MgO (a=0.674, b=0.318, c=0.001, x=0.3) prescription is with electronic balance difference weighing 0.7199 gram Na
2CO
3, 0.8132 gram K
2CO
3, 0.009 gram Li
2CO
3, 2.7229 gram Nb
2O
5And 0.0380 gram magnesium basic carbonate, as medium, with planetary ball mill grinding batch mixing 1 hour, rotating speed was 450rpm with dehydrated alcohol, slip obtains the siccative powder 200 ℃ of oven dry.Dry powder is incubated 1 hour through 900 ℃, carries out the synthetic of niobate.Get powder 0.3 and restrain in the mould of the Φ 10mm that packs into compression moulding.The disk of moulding is put into temperature programmed control box-type furnace sintering, carries out sintering under 800 ℃, is incubated 4 hours, is cooled to room temperature and makes ceramic disks.After the polishing of 600 order fine sandpapers, be coated with roasting silver electrode on two surfaces and make by silver-colored ceramic plate, put into polarization device, silicone oil is heated to 200 ℃, keeps 60min to polarize under 1kV/mm voltage, cools to room temperature again, finishes polarization.
The concrete prescription of other embodiment sees Table 2, and table 3 is the piezoelectric constant (d of the corresponding prescription of table 2 under different firing temperatures
33) value.
The prescription of table 2 magnesium doping leadless piezoelectric ceramics
| Sample number into spectrum | a | b | c | x |
| 01 | 0.2 | 0.8 | 0.001 | 0.026 |
| 02 | 0.263 | 0.772 | 0.057 | 0.044 |
| 03 | 0.329 | 0.683 | 0.019 | 0.044 |
| 04 | 0.395 | 0.624 | 0.057 | 0.026 |
| 05 | 0.405 | 0.587 | 0.114 | 0.132 |
| 06 | 0.472 | 0.504 | 0.173 | 0.187 |
| 07 | 0.539 | 0.467 | 0.114 | 0.187 |
| 08 | 0.591 | 0.416 | 0.173 | 0.132 |
| 09 | 0.643 | 0.361 | 0.235 | 0.215 |
| 10 | 0.674 | 0.318 | 0.3 | 0.3 |
| 11 | 0.756 | 0.275 | 0.235 | 0.3 |
| 12 | 0.8 | 0.2 | 0.3 | 0.215 |
Piezoelectric constant d under the different sintering temperatures of table 3
33(pC/N)
Claims (2)
1, a kind of low temperature synthetic no-lead piezoelectric Mg doped sodium potassium niobate ceramic is characterized in that: it is (Na that material is formed general formula
aK
bLi
c) NbO
3+ xMgO, wherein a, b, c, x represent the molar fraction of Na, K, Li, Mg component respectively, the scope of numerical value is: 0.20≤a≤0.80,0.20≤b≤0.80,0.00＜c≤0.30,0.00＜x≤0.30; Magnesium-doped element is respectively with MgO, MgCO
3Or magnesium basic carbonate is that raw material adds.
2, a kind of method for preparing the described piezoelectric ceramics of claim 1 is characterized in that, preparation technology is:
(1) raw material is pressed general formula (Na respectively
aK
bLi
c) NbO
3The proportioning of+xMgO is carried out weighing, batching, uses dehydrated alcohol to be medium, uses planetary ball mill ball milling 1-8 hour, and rotating speed is 100-450rpm, obtains dry powder 50-200 ℃ of oven dry;
(2) dry powder is warming up to 500-900 ℃ continuously in the temperature programmed control box-type furnace, is incubated 1-10 hour, carry out the synthetic of niobate;
(3) in the roasting powder of preparation, behind the adding binding agent, put into mould, with oil press compression moulding under 100-500MPa;
(4) biscuit of compression moulding is put into the temperature programmed control box-type furnace, be warming up to 800-1040 ℃ continuously, reduce to room temperature after sintering 1-4 hour;
(5) ceramic disks that makes with the polishing of 600 order fine sandpapers, be coated with roasting silver electrode on two surfaces afterwards, make and put into polarization device behind the silver-colored ceramic plate, silicone oil is heated to 100-200 ℃, under 1-5kV/mm voltage, keep 10-60min, make no-lead piezoelectric Mg doped sodium potassium niobate ceramic.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101537494B (en) * | 2009-04-29 | 2010-07-28 | 北京科技大学 | Method for preparing nickel particle dispersion barium calcium zirconate titanate piezoelectric composite material |
| CN102070337B (en) * | 2010-10-29 | 2012-12-05 | 景德镇陶瓷学院 | Low-temperature sintered potassium sodium niobate lead-free piezoelectric ceramic and preparation method thereof |
| KR20160111476A (en) * | 2014-01-29 | 2016-09-26 | 캐논 가부시끼가이샤 | Piezoelectric ceramic, method for producing the same, piezoelectric element, multilayer piezoelectric element, liquid ejection head, liquid ejecting apparatus, ultrasonic motor, optical device, vibrating apparatus, dust-removing apparatus, imaging apparatus, and electronic device |
| CN105669193A (en) * | 2014-11-20 | 2016-06-15 | 中国科学院声学研究所 | K-Na-Li niobate barium titanate-based lead-free piezoelectric ceramic and low-temperature sintering preparation method thereof |
| CN104698294B (en) * | 2015-03-17 | 2018-03-06 | 中国科学院上海硅酸盐研究所 | A kind of device of dynamic measurement piezoelectric high-temperature piezoelectric coefficient |
| CN104698295A (en) * | 2015-03-17 | 2015-06-10 | 中国科学院上海硅酸盐研究所 | Method for dynamically measuring high-temperature piezoelectric coefficients of piezoelectric material |
| CN107185558B (en) * | 2017-05-16 | 2019-09-03 | 浙江师范大学 | A kind of photocatalysis hydrogen production catalyst and preparation method thereof |
| CN110981479B (en) * | 2020-01-10 | 2022-03-01 | 陕西科技大学 | High-breakdown ferroelectric ceramic and preparation method thereof |
| CN111995396A (en) * | 2020-07-20 | 2020-11-27 | 南昌航空大学 | Method for utilizing oxygen ion conductivity of magnesium modified sodium niobate ceramic |
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| WO2006117990A1 (en) * | 2005-04-28 | 2006-11-09 | Murata Manufacturing Co., Ltd. | Piezoelectric ceramic composition, process for producing said piezoelectric ceramic composition, and piezoelectric ceramic electronic component |
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| WO2006117990A1 (en) * | 2005-04-28 | 2006-11-09 | Murata Manufacturing Co., Ltd. | Piezoelectric ceramic composition, process for producing said piezoelectric ceramic composition, and piezoelectric ceramic electronic component |
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| Title |
|---|
| （K0.5Na0.5）NbO3－LiNbO3无铅压电陶瓷的烧结特性和压电性能研究. 唐福生等.无机材料学报，第22卷第2期. 2007 |
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