CN101062864A - Niobic acid sodium potassium lithium radical leadless piezo-electric ceramic and preparation method thereof - Google Patents
Niobic acid sodium potassium lithium radical leadless piezo-electric ceramic and preparation method thereof Download PDFInfo
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- CN101062864A CN101062864A CN200710099675.6A CN200710099675A CN101062864A CN 101062864 A CN101062864 A CN 101062864A CN 200710099675 A CN200710099675 A CN 200710099675A CN 101062864 A CN101062864 A CN 101062864A
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- general formula
- acid sodium
- sintering
- potassium
- niobic acid
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- 239000000919 ceramic Substances 0.000 title claims abstract description 36
- 239000002253 acid Substances 0.000 title abstract description 12
- 238000002360 preparation method Methods 0.000 title description 14
- 239000000463 material Substances 0.000 claims abstract description 18
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052709 silver Inorganic materials 0.000 claims abstract description 13
- 239000004332 silver Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011575 calcium Substances 0.000 claims abstract description 7
- 239000010949 copper Substances 0.000 claims abstract description 7
- 239000011777 magnesium Substances 0.000 claims abstract description 7
- 239000011135 tin Substances 0.000 claims abstract description 7
- 239000010936 titanium Substances 0.000 claims abstract description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 6
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 6
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 6
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052788 barium Inorganic materials 0.000 claims abstract description 5
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000010941 cobalt Substances 0.000 claims abstract description 5
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052802 copper Inorganic materials 0.000 claims abstract description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 5
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 5
- 239000010703 silicon Substances 0.000 claims abstract description 5
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052718 tin Inorganic materials 0.000 claims abstract description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 5
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000010955 niobium Substances 0.000 claims description 25
- 238000005245 sintering Methods 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 21
- 239000011734 sodium Substances 0.000 claims description 20
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 12
- 230000010287 polarization Effects 0.000 claims description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 7
- 238000000748 compression moulding Methods 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 238000012856 packing Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 229920002545 silicone oil Polymers 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 6
- 229910052744 lithium Inorganic materials 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 239000010937 tungsten Substances 0.000 claims description 5
- 239000004411 aluminium Substances 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 3
- UTBYQPSPFXHANA-UHFFFAOYSA-N [K].[Na].[Li] Chemical group [K].[Na].[Li] UTBYQPSPFXHANA-UHFFFAOYSA-N 0.000 abstract description 4
- 230000008878 coupling Effects 0.000 abstract description 3
- 238000010168 coupling process Methods 0.000 abstract description 3
- 238000005859 coupling reaction Methods 0.000 abstract description 3
- -1 ferric Chemical compound 0.000 abstract description 3
- 230000005621 ferroelectricity Effects 0.000 abstract 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- 229910052758 niobium Inorganic materials 0.000 description 7
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 6
- 238000000465 moulding Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 4
- 235000015320 potassium carbonate Nutrition 0.000 description 4
- 235000017550 sodium carbonate Nutrition 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- 229910052715 tantalum Inorganic materials 0.000 description 4
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Inorganic materials [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 3
- 229910052765 Lutetium Inorganic materials 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- UKDIAJWKFXFVFG-UHFFFAOYSA-N potassium;oxido(dioxo)niobium Chemical compound [K+].[O-][Nb](=O)=O UKDIAJWKFXFVFG-UHFFFAOYSA-N 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001778 solid-state sintering Methods 0.000 description 1
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Abstract
The invention discloses a preparing method of niobic acid sodium potassium lithium group leadless piezoelectric ceramic in green energy source material domain, which comprises the following steps: expressing component of niobic acid sodium potassium lithium group as non-stoichiometric ratio general formula (NaaKbLic)(NbxTaySbz)O3 or -nM; expressing a, b, c as A bit element; expressing x, y, z as mole fraction of B bit element; setting the selective rage as (0<=a<=1. 5, 0<=b<=1. 5, 0<c<=1. 5, 1<a+b+c<=3, 0<x<=1. 5, 0<=y<=1. 5, 0<=z<=1. 5, 1<(a+b+c)/(x+y+z)<=3 or 0. 2<(a+b+c)/(x+y+z)<1, 0<n<=1); choosing M from the oxide or composite oxide of calcium, copper, manganese, barium, yttrium, strontium, titanium, zirconium, lanthanum, magnesium, aluminum, silicon, ferric, cobalt, nickel, silver, tin, antimony and wolfram; adopting commercial raw material; balling; baking; caking under normal pressure; getting the product. This invention possesses good ferro-electricity property, which electromechanical coupling factor Kp can reach 10-50%.
Description
Technical field
The invention belongs to environmentally friendly field of energy source materials, a kind of potassium-sodium niobate lithium radical leadless piezo-electric ceramic material and preparation method thereof particularly is provided.
Background technology
The piezoceramic material of widespread use at present is Pb (Ti, Zr) O
3(PZT), PbTiO
3-PbZrO
3-ABO
3(ABO
3Be the composite perofskite type ferroelectrics) and PbTiO
3On the lead base pottery, wherein Qian massfraction is approximately 70%.This class pottery produce, use and discarded last handling process in cause serious harm all can for the mankind and ecotope, the exploitation leadless piezoelectric material material is imperative.The leadless piezoelectric ceramics of having reported at present has tungsten bronze structure ceramic systems, potassium niobate base ceramic systems, bismuth laminated ceramic systems and barium titanate ceramics system, and wherein the columbate leadless piezoelectric ceramics is to be hopeful to replace one of system that contains lead piezoelectric ceramics most.2004 document 1 (Nature, 2004 Vol 432, p 84-87) reported the piezoelectric property of the niobate base lead-free piezoelectric ceramic of lithium, tantalum and the common modification of antimony, can reach 416pC/N through the piezoelectric constant of the textured ceramic of template preparation.But for normal pressure-sintered and without the potassium-sodium niobate pottery of any modification, (Applied Physics Letter.2004, Vol 85, report that p412) its piezoelectric constant has only 97pC/N according to document 3.Document 4 (Applied Physics Letter.2005, Vol 59, p241-244) and document 5 (Applied Physics Letter.2006, Vol 88, p212) reported by adding the piezoelectric property that modifying element can improve potassium-sodium niobate base pottery effectively, document 7 (Journal of American Society.1962, Vol 45, p209-13) and document 8 (MaterialsScience Forum.2005, p475-479) report advanced preparation technologies such as utilizing hot pressed sintering and discharge plasma sintering, obtained well behaved dense ceramic material.By means such as element modified and optimal preparation technology, the piezoelectric property of unleaded potassium-sodium niobate base pottery is significantly improved, and is constantly approaching actual application level, and the patent content published of this field is as follows at present.Patent CN1609047A discloses crystallization orientation ceramic and preparation method, and this ceramic general formula is: { Li
x(K
1-yNa
y)
1-x{ Nb
1-z-wTa
zSb
wO
3, 0≤x≤0.2,0≤y≤1,0≤z≤0.4 wherein, 0≤w≤0.2, x+z+w>0 is characterized in that based on potassium-sodium niobate, add modifying elements such as lithium, tantalum, antimony, and be made into stupalith on this basis, do not comprise polycrystalline ceramic with texture structure.Patent CN1810711A discloses a kind of high curie point niobic acid sodium potassium lithium radical leadless piezo-electric ceramic and preparation method, and the general formula of pottery can be expressed as: (1-u) [(1-z) (Li
xNa
yK
1-x-y) NbO
3+ zMTiO
3]+uMnO
2Wherein x, y, z represent respective element material shared atomic percent in each constituent element in the compound ion, and all total atom numbers and be 1,0.01≤x≤0.2,0.2≤y≤0.7,0.01≤z≤0.25,0≤u≤0.05, it is characterized in that on the basis of niobic acid sodium potassium lithium the titanate or the oxide compound that add one or more Mg, Ca, Sr, Ba carry out modification.Patent CN1884198A discloses niobium tantalic acid sodium potassium based leadless piezoelectric ceramics and preparation method, its feature with based on niobium tantalic acid sodium potassium, the general formula of base-material is: (K
1-xNa
x) (Nb
1-yTa
y) O
3X=0.1~0.9 wherein, y=0.01~0.30), add Cu on this basis
2+, Sb
5+, Sn
4+, Li
+In any or appoint several modifications of carrying out.Patent CN1511802A discloses a class multi constituent niobate lead-free piezoelectric ceramics, and its claim composition is: (Li
xNa
yK
1-x-y) (Nb
1-zR
z) O
3Or add one or more LMnO on this basis
3, in the formula, 0<x≤0.3,0<y<1,0<(x+y)<1,0≤z≤0.4, R is Ta or Sb or both compound ions, L is Y, Er, Ho, Dy, Tm, Lu, Yb, Lu, Nd, Sm rare earth metals element, LMnO
3Adding proportion be 0-17wt%, (Li
xNa
yK
1-x-y) (Nb
1-zR
z) O
3Ratio be 83-17wt%.The feature of this patent is based on niobic acid sodium potassium lithium, at first by Ta, Sb Nb is carried out the B position and replaces, and carries out the rare earth metals element doping then.Patent CN1644562A discloses potassium-sodium niobate system leadless piezoelectric ceramics and preparation method thereof.Though patent CN1388089A has reported that with Na, Li, Nb and O element be the perovskite structure compound that main component constitutes, its general formula is: (1-u) [(1-z) Na
1-xLi
x)
1-yK
y] (Nb
1-zTa
z) O
3-nM1M2O
3, wherein, 0.02≤x≤0.3,0≤y≤0.2,0≤z≤0.2,0≤n≤0.1, M1 is a divalent metal, M2 is a tetravalent metal, but its interpolation element not only has tantalum, also have other metallic elements, and the molar fraction of potassium is between 0~0.2.Up to the present the common trait of disclosed patent be exactly the general formula of stupalith be ABO
3, A position atomic mole fraction sum is 1, that is to say that they all belong to the stoichiometric ratio category.Patent CN1919791A discloses potassium-sodium niobate based leadless piezoelectric ceramics and the intermediate frequency resonator thereof of a kind of high Qm, it is characterized in that based on potassium-sodium niobate, and its general formula is (Na
xK
1-x+ δ) Nb
1+zO
3+ wmolCuO, 0≤x in the formula≤1,0≤δ≤0.1,0≤z≤0.2,0≤w≤0.1, doped with Cu O realizes high resonance then.Though the disclosure patent is the patent that present unique A of relating to position atomic mole fraction sum comprises a part of non-stoichiometric composition, does not contain elemental lithium, its piezoelectric constant is on the low side only to be 90~120.
Summary of the invention
The object of the present invention is to provide a kind of niobic acid sodium potassium lithium radical pottery and preparation method thereof with high piezoelectric constant.Patent is at the niobate base lead-free piezoelectric ceramic piezoelectric constant d of present ordinary sinter method preparation
33Lower defective provides a kind of composition design with niobic acid sodium potassium lithium radical leadless piezo-electric ceramic of high piezoelectric constant, and this composition relates to the non-stoichiometric category, its piezoelectric constant d
33Be not less than 150pC/N.
The moiety of a kind of niobic acid sodium potassium lithium radical pottery provided by the invention can be used general formula (Na
aK
bLic) (Nb
xTa
ySb
z) O
3Expression, wherein a, b, c represent that A position composition element, x, y, z represent the molar fraction of B position composition element, the range of choice of numerical value is: 0≤a≤1.5,0≤b≤1.5,0<c≤1.5,1<a+b+c≤3,0<x≤1.5,0≤y≤1.5,0≤z≤1.5,1<(a+b+c)/(x+y+z)≤3 or 0.2<(a+b+c)/(x+y+z)<1.
The present invention also provides a kind of piezoelectric ceramics that a kind of or a kind of hotchpotch is formed that adds on the basis of above-mentioned general formula, with general formula (Na
aK
bLic) (Nb
xTa
ySb
z) O
3-nM represents, 0≤a≤1.5,0≤b≤1.5,0<c≤1.5 wherein, 1<a+b+c≤3,0<x≤1.5,0≤y≤1.5,0≤z≤1.5,1<(a+b+c)/(x+y+z)≤3 or 0.2<(a+b+c)/(x+y+z)<1,0<n≤1, M is at least a in the oxide compound of calcium, copper, manganese, barium, yttrium, strontium, titanium, zirconium, lanthanum, magnesium, aluminium, silicon, iron, cobalt, nickel, silver, tin, antimony and tungsten or the composite oxides, n represents the molar fraction of M component.
Preparation method of the present invention is a batching after according to the non-stoichiometric general formula raw materials by weight being weighed, and confected materials is that medium carries out batch mixing in the mode of ball milling or vibration with the dehydrated alcohol, and the time is 1-8 hour, and oven dry obtains dry powder; With the dry powder roasting, maturing temperature 500-900 ℃, be incubated 1-10 hour, carry out the synthetic of niobate; With the compression moulding in the mould of φ 5-30mm of packing into of pre-burning synthetic powder, put sintering in the sintering oven then into, under 600-1200 ℃ of temperature in the atmosphere, heat preservation sintering 1-5 hour; Potassium-sodium niobate series piezoelectric ceramic disk is coated with roasting silver electrode, polarizes in silicone oil, the polarization temperature is 80-200 ℃, and the time is 10-60min, and voltage is 1-10kV/mm, carries out every electrical performance testing after polarization is finished.
Non-stoichiometric general formula of the present invention is: (Na
aK
bLic) (Nb
xTa
ySb
z) O
3Expression, wherein a, b, c represent that A position composition element, x, y, z represent the molar fraction of B position composition element, the range of choice of numerical value is: 0≤a≤1.5,0≤b≤1.5,0<c≤1.5,1<a+b+c≤3,0<x≤1.5,0≤y≤1.5,0≤z≤1.5,1<(a+b+c)/(x+y+z)≤3 or 0.2<(a+b+c)/(x+y+z)<1; Perhaps, (Na
aK
bLic) (Nb
xTa
ySb
z) O
3-nM represents, 0≤a≤1.5,0≤b≤1.5,0<c≤1.5 wherein, 1<a+b+c≤3,0<x≤1.5,0≤y≤1.5,0≤z≤1.5,1<(a+b+c)/(x+y+z)≤3 or 0.2<(a+b+c)/(x+y+z)<1,0<n≤1, M is at least a in the oxide compound of calcium, copper, manganese, barium, yttrium, strontium, titanium, zirconium, lanthanum, magnesium, aluminium, silicon, iron, cobalt, nickel, silver, tin, antimony and tungsten or the composite oxides, n represents the molar fraction of M component.
The polynary system piezoelectric ceramics that the present invention proposes has following advantage:
(1) good piezoelectric property, its piezoelectric constant d
33Be not less than 150pC/N;
(2) good ferroelectric performance is shown in the ferroelectric hysteresis loop figure of Fig. 1 piezoelectric ceramics sample;
(3) electromechanical coupling factor Kp reaches 10-50%; Having reached can the actual performance index of using.
Description of drawings
Fig. 1 is ferroelectric hysteresis loop figure.
Embodiment:
Piezoelectric ceramics sample of the present invention utilizes the solid-phase sintering process preparation, and its process comprises grinding batch mixing, roasting synthetic in advance niobate, fine grinding, adds technical process such as caking agent, moulding, solid state sintering, grind away, quilt silver, polarization.Be specially: according to (NbxTaySbz) O of general formula (NaaKbLic)
3Batching after-nM weighs raw materials by weight, confected materials is that medium carries out batch mixing in the mode of ball milling or vibration with the dehydrated alcohol, the time dries and obtains dry powder after being 1-8 hour; With the dry powder roasting, maturing temperature 500-900 ℃, be incubated 1-10 hour, carry out the synthetic of niobate; With the compression moulding in the mould of φ 5-30mm of packing into of pre-burning synthetic powder, put sintering in the sintering oven then into, under 600-1200 ℃ of temperature in the atmosphere, heat preservation sintering 1-5 hour; Potassium-sodium niobate series piezoelectric ceramic disk is coated with roasting silver electrode, polarizes in silicone oil, the polarization temperature is 80-200 ℃, and the time is 10-60min, and voltage is 1-10kV/mm.After finishing, polarization carries out every electrical performance testing.
Exemplifying following embodiment is specified the present invention.
Provide 2-3 specific examples below.
Example 1: at first raw material is pressed equation (Na
0.569Kb
0.485Li
0.40) (Nb
0.850Ta
1.5) O
3Carry out weighing, the quality of each material is: 0.7912g yellow soda ash, 0.9255g salt of wormwood, 0.1255g Quilonum Retard 3.5581g Niobium Pentxoxide, 6.5713g tantalum pentoxide.Raw material and put into ball grinder, adding the 30ml dehydrated alcohol is medium, and ball milling is 1 hour under 160 rev/mins rotating speed, shift the material oar and 80 ℃ dry 8 hours down.Powder after will drying then was 500 ℃ of roasting temperatures 10 hours.The compression moulding in the mould of φ 20mm of packing into of pre-burning synthetic powder.Put the powder after the moulding in sintering oven sintering then, under 600 ℃ of temperature in the atmosphere, heat preservation sintering 5 hours.Potassium-sodium niobate series piezoelectric ceramic disk is coated with roasting silver electrode, polarizes in silicone oil, temperature progressively is raised to 100 ℃ by room temperature during polarization, is 10 minutes in the 1kV/mm time then.
Example two: at first raw material is pressed equation (Na
0.716Kb
0.630Li
0.823) (Nb
0.220Ta
0.213Sb
0.421) O
3Carry out weighing, the concrete quality of each material is: 0.2395g yellow soda ash, 0.3722g salt of wormwood, 1.2197g Niobium Pentxoxide, 2.4293g tantalum pentoxide, 0.1520g Quilonum Retard, 2.45126 antimonous oxides.Raw material and put into ball grinder, adding the 30ml dehydrated alcohol is medium, and ball milling is 1 hour under 160 rev/mins rotating speed, shift the material oar and 80 ℃ dry 8 hours down.Powder after will drying then was 900 ℃ of roasting temperatures 1 hour.The compression moulding in the mould of φ 5mm of packing into of pre-burning synthetic powder.Put the powder after the moulding in sintering oven sintering then, under 1200 ℃ of temperature in the atmosphere, heat preservation sintering 5 hours.Potassium-sodium niobate series piezoelectric ceramic disk is coated with roasting silver electrode, polarizes in silicone oil, temperature progressively is raised to 80 ℃ by room temperature during polarization, is 10 minutes in the 2kV/mm time then.
Example three: at first raw material is pressed equation (Na
0.456Kb
0.630Li
0.412) (Nb
0.360Ta
0.213Sb
0.421) O
3-0.045-CaO carries out weighing, and the concrete quality of each material is: 0.4295g yellow soda ash, 0.6522g salt of wormwood, 3.1197g Niobium Pentxoxide, 4.7164g tantalum pentoxide, 0.3521g Quilonum Retard, 6.3124 antimonous oxides, 0.1211g calcium oxide.Raw material and put into ball grinder, adding the 30ml dehydrated alcohol is medium, and ball milling is 8 hours under 160 rev/mins rotating speed, shift the material oar and 80 ℃ dry 8 hours down.Powder after will drying then was 700 ℃ of roasting temperatures 3 hours.The compression moulding in the mould of φ 16mm of packing into of pre-burning synthetic powder.Put the powder after the moulding in sintering oven sintering then, under 1020 ℃ of temperature in the atmosphere, heat preservation sintering 5 hours.Potassium-sodium niobate series piezoelectric ceramic disk is coated with roasting silver electrode, polarizes in silicone oil, temperature progressively is raised to 200 ℃ by room temperature during polarization, is 60 minutes in the 1kV/mm time then.
Example four: at first raw material is pressed equation (Na
0.463Kb
0.620Li
0.420) (Nb
0.126Ta
0.713Sb
0.421) O
3-0.036-SrO carries out weighing, and the concrete quality of each material is: 0.2395g yellow soda ash, 0.3722g salt of wormwood, 1.2197g Niobium Pentxoxide, 11.3164g tantalum pentoxide, 0.2525g Quilonum Retard, 6.0671 antimonous oxides, 0.3311g strontium oxide.Raw material and put into ball grinder, adding the 30ml dehydrated alcohol is medium, and ball milling is 6 hours under 160 rev/mins rotating speed, shift the material oar and 80 ℃ dry 8 hours down.Powder after will drying then was 750 ℃ of roasting temperatures 4 hours.The compression moulding in the mould of φ 30mm of packing into of pre-burning synthetic powder.Put the powder after the moulding in sintering oven sintering then, under 1040 ℃ of temperature in the atmosphere, heat preservation sintering 3 hours.Potassium-sodium niobate series piezoelectric ceramic disk is coated with roasting silver electrode, polarizes in silicone oil, temperature progressively is raised to 100 ℃ by room temperature during polarization, is 20 minutes in the 10kV/mm time then.
Provided several preferred embodiments of the present invention in the following table.D wherein
33, Kp, ε, tan δ represent piezoelectric constant, electromechanical coupling factor, specific inductivity and dielectric loss respectively.
Embodiment:
Sample | Sintering temperature (℃) | a | b | c | x | y | z | n | Element | d 33(pC/N) |
1 | 1050 | 0.000 | 1.500 | 0.010 | 1.000 | 0.000 | 0.000 | 0.000 | Do not have | 165 |
2 | 1060 | 0.525 | 0.485 | 0.010 | 0.100 | 0.000 | 0.820 | 0.000 | Do not have | 191 |
3 | 1040 | 0.569 | 0.485 | 0.040 | 0.850 | 1.500 | 0.000 | 0.000 | Do not have | 230 |
4 | 1070 | 0.530 | 0.490 | 0.055 | 1.500 | 0.000 | 0.000 | 0.000 | Do not have | 243 |
5 | 1060 | 0.540 | 0.490 | 0.070 | 0.100 | 0.000 | 1.500 | 0.000 | Do not have | 187 |
6 | 1130 | 0.550 | 1.500 | 0.080 | 0.140 | 0.040 | 1.205 | 0.000 | Do not have | 247 |
7 | 1040 | 0.612 | 0.560 | 0.021 | 0.160 | 0.600 | 0.600 | 0.000 | Do not have | 160 |
8 | 970 | 0.740 | 0.570 | 0.640 | 0.149 | 0.400 | 0.101 | 0.000 | Do not have | 304 |
9 | 1090 | 0.760 | 0.580 | 0.650 | 0.180 | 0.210 | 0.360 | 0.000 | Do not have | 210 |
10 | 1050 | 0.800 | 0.620 | 0.760 | 0.200 | 0.680 | 0.631 | 0.000 | Do not have | 185 |
11 | 1130 | 0.716 | 0.630 | 0.823 | 0.220 | 0.213 | 0.421 | 0.000 | Do not have | 176 |
12 | 900 | 0.100 | 0.710 | 0.954 | 0.260 | 0.362 | 0.325 | 1.000 | Mg | 190 |
13 | 980 | 1.100 | 0.630 | 1.000 | 0.360 | 0.412 | 0.541 | 0.450 | Ca | 178 |
14 | 1160 | 1.200 | 0.600 | 1.200 | 0.950 | 0.060 | 0.214 | 0.692 | Sr | 216 |
15 | 1120 | 1.500 | 0.000 | 1.500 | 0.160 | 0.860 | 0.258 | 0.250 | Ba | 203 |
16 | 940 | 0.542 | 0.531 | 0.042 | 0.213 | 0.080 | 0.165 | 0.564 | Cu | 195 |
17 | 1160 | 1.300 | 0.501 | 0.006 | 0.546 | 0.094 | 0.370 | 0.587 | Mn | 234 |
18 | 1130 | 1.500 | 0.000 | 1.400 | 0.800 | 0.758 | 0.140 | 0.366 | Y | 212 |
19 | 1040 | 0.055 | 0.251 | 0.354 | 0.945 | 1.450 | 0.885 | 0.450 | Ti | 248 |
20 | 1080 | 0.015 | 0.250 | 0.956 | 0.150 | 0.250 | 1.230 | 1.000 | Zr | 173 |
21 | 1180 | 1.500 | 0.000 | 1.430 | 0.160 | 0.763 | 0.140 | 0.680 | La | 201 |
22 | 1000 | 0.325 | 0.982 | 1.215 | 0.544 | 0.250 | 1.032 | 0.460 | Al | 186 |
23 | 1170 | 0.256 | 0.248 | 1.341 | 0.135 | 0.065 | 0.968 | 0.853 | Si | 215 |
24 | 980 | 0.464 | 0.780 | 0.896 | 0.160 | 0.386 | 0.352 | 0.574 | Fe | 224 |
25 | 1130 | 0.768 | 0.512 | 1.500 | 0.165 | 0.452 | 0.481 | 0.056 | Co | 258 |
26 | 1040 | 0.257 | 1.156 | 1.356 | 0.089 | 0.847 | 0.150 | 0.745 | Ni | 196 |
27 | 1000 | 0.348 | 0.257 | 1.224 | 0.202 | 0.460 | 0.147 | 0.032 | Ag | 185 |
28 | 1050 | 1.266 | 0.000 | 1.047 | 0.308 | 0.068 | 0.572 | 0.227 | Sn | 168 |
29 | 1090 | 0.209 | 0.636 | 0.350 | 0.453 | 0.758 | 0.142 | 0.792 | Sb | 210 |
30 | 1180 | 0.503 | 0.967 | 0.706 | 0.569 | 0.066 | 0.459 | 0.358 | W | 225 |
Claims (4)
1, a kind of potassium-sodium niobate lithium radical leadless piezo-electric ceramic with high tension performance is characterized in that, with non-stoichiometric general formula (Na
aK
bLi
c) (Nb
xTa
ySb
z) O
3Expression, wherein a, b, c represent that A position composition element, x, y, z represent the molar fraction of B position composition element, the range of choice of numerical value is: 0≤a≤1.5,0≤b≤1.5,0<c≤1.5,1<a+b+c≤3,0<x≤1.5,0≤y≤1.5,0≤z≤1.5,1<(a+b+c)/(x+y+z)≤3 or 0.2<(a+b+c)/(x+y+z)<1.
2, according to claim 1 leadless piezoelectric ceramics, it is characterized in that, add one or more hotchpotchs and formed piezoelectric ceramics, with non-stoichiometric general formula (Na
aK
bLi
c) (Nb
xTa
ySb
z) O
3-nM represents, 0≤a≤1.5,0≤b≤1.5,0<c≤1.5 wherein, 1<a+b+c≤3,0<x≤1.5,0≤y≤1.5,0≤z≤1.5,1<(a+b+c)/(x+y+z)≤3 or 0.2<(a+b+c)/(x+y+z)<1,0<n≤1, n represents the molar fraction of M component, M is at least a in the oxide compound of calcium, copper, manganese, barium, yttrium, strontium, titanium, zirconium, lanthanum, magnesium, aluminium, silicon, iron, cobalt, nickel, silver, tin, antimony and tungsten or the composite oxides.
3. method for preparing claim 1 or 2 described leadless piezoelectric ceramicss, it is characterized in that, according to the non-stoichiometric general formula with weigh back batching of raw materials by weight, confected materials is that medium carries out batch mixing in the mode of ball milling or vibration with the dehydrated alcohol, time is 1-8 hour, and oven dry obtains dry powder; With the dry powder roasting, maturing temperature 500-900 ℃, be incubated 1-10 hour, carry out the synthetic of niobate; With the compression moulding in the mould of φ 5-30mm of packing into of pre-burning synthetic powder, put sintering in the sintering oven then into, under 600-1200 ℃ of temperature in the atmosphere, heat preservation sintering 1-5 hour; Potassium-sodium niobate series piezoelectric ceramic disk is coated with roasting silver electrode, polarizes in silicone oil, the polarization temperature is 80-200 ℃, and the time is 10-60min, and voltage is 1-10kV/mm, carries out every electrical performance testing after polarization is finished.
4, in accordance with the method for claim 3, it is characterized in that described non-stoichiometric general formula is: (Na
aK
bLi
c) (Nb
xTa
ySb
z) O
3Expression, wherein a, b, c represent that A position composition element, x, y, z represent the molar fraction of B position composition element, the range of choice of numerical value is: 0≤a≤1.5,0≤b≤1.5,0<c≤1.5,1<a+b+c≤3,0<x≤1.5,0≤y≤1.5,0≤z≤1.5,1<(a+b+c)/(x+y+z)≤3 or 0.2<(a+b+c)/(x+y+z)<1; Perhaps, (Na
aK
bLi
c) (Nb
xTa
ySb
z) O
3-nM represents, 0≤a≤1.5,0≤b≤1.5,0<c≤1.5 wherein, 1<a+b+c≤3,0<x≤1.5,0≤y≤1.5,0≤z≤1.5,1<(a+b+c)/(x+y+z)≤3 or 0.2<(a+b+c)/(x+y+z)<1,0<n≤1, M is at least a in the oxide compound of calcium, copper, manganese, barium, yttrium, strontium, titanium, zirconium, lanthanum, magnesium, aluminium, silicon, iron, cobalt, nickel, silver, tin, antimony and tungsten or the composite oxides, n represents the molar fraction of M component.
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