CN107382318A - A kind of high mechanical properties sodium potassium niobate base leadless piezoelectric ceramics material and its preparation method and application - Google Patents
A kind of high mechanical properties sodium potassium niobate base leadless piezoelectric ceramics material and its preparation method and application Download PDFInfo
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- CN107382318A CN107382318A CN201710778087.9A CN201710778087A CN107382318A CN 107382318 A CN107382318 A CN 107382318A CN 201710778087 A CN201710778087 A CN 201710778087A CN 107382318 A CN107382318 A CN 107382318A
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- potassium niobate
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- 239000000463 material Substances 0.000 title claims abstract description 130
- 239000000919 ceramic Substances 0.000 title claims abstract description 107
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000011734 sodium Substances 0.000 claims abstract description 38
- 238000005245 sintering Methods 0.000 claims abstract description 30
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims abstract description 24
- 150000001875 compounds Chemical group 0.000 claims abstract description 21
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 20
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims abstract description 18
- GNMQOUGYKPVJRR-UHFFFAOYSA-N nickel(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Ni+3].[Ni+3] GNMQOUGYKPVJRR-UHFFFAOYSA-N 0.000 claims abstract description 14
- PZFKDUMHDHEBLD-UHFFFAOYSA-N oxo(oxonickeliooxy)nickel Chemical compound O=[Ni]O[Ni]=O PZFKDUMHDHEBLD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 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 claims abstract description 12
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims abstract description 12
- UKDIAJWKFXFVFG-UHFFFAOYSA-N potassium;oxido(dioxo)niobium Chemical compound [K+].[O-][Nb](=O)=O UKDIAJWKFXFVFG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 12
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000421 cerium(III) oxide Inorganic materials 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 74
- 239000000843 powder Substances 0.000 claims description 52
- 239000002994 raw material Substances 0.000 claims description 50
- 238000000034 method Methods 0.000 claims description 38
- 238000000498 ball milling Methods 0.000 claims description 35
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 30
- 229910052709 silver Inorganic materials 0.000 claims description 30
- 239000004332 silver Substances 0.000 claims description 30
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 28
- 229910010293 ceramic material Inorganic materials 0.000 claims description 28
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 28
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 28
- 230000005684 electric field Effects 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 17
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims description 14
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 14
- 229920002545 silicone oil Polymers 0.000 claims description 14
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 14
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 14
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 12
- 239000011230 binding agent Substances 0.000 claims description 11
- 238000000465 moulding Methods 0.000 claims description 10
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 9
- 230000010287 polarization Effects 0.000 claims description 9
- 238000001514 detection method Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000003466 welding Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 229910001404 rare earth metal oxide Inorganic materials 0.000 abstract description 3
- 238000006467 substitution reaction Methods 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 230000007704 transition Effects 0.000 abstract description 3
- 239000010955 niobium Substances 0.000 description 22
- 238000005452 bending Methods 0.000 description 17
- 239000000853 adhesive Substances 0.000 description 16
- 230000001070 adhesive effect Effects 0.000 description 16
- 235000019441 ethanol Nutrition 0.000 description 16
- 238000001035 drying Methods 0.000 description 14
- 230000003014 reinforcing effect Effects 0.000 description 13
- 239000007864 aqueous solution Substances 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- 238000003786 synthesis reaction Methods 0.000 description 9
- 238000010792 warming Methods 0.000 description 9
- 238000001816 cooling Methods 0.000 description 8
- 238000009413 insulation Methods 0.000 description 8
- 238000002791 soaking Methods 0.000 description 8
- 239000012071 phase Substances 0.000 description 5
- 238000007545 Vickers hardness test Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 4
- 229910052808 lithium carbonate Inorganic materials 0.000 description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 4
- 229910052758 niobium Inorganic materials 0.000 description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 4
- 229910052573 porcelain Inorganic materials 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910010252 TiO3 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000013459 approach Methods 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
- 229910002056 binary alloy 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
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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Abstract
The invention provides a kind of high mechanical properties sodium potassium niobate base leadless piezoelectric ceramics material and its preparation method and application.Sodium potassium niobate base leadless piezoelectric ceramics material provided by the invention includes [Li0.06(K0.47‑xNa0.47+x)][(Nb0.893Sb0.057Ta0.05]O3, TMO and REO；TMO is MnO2、Fe2O3、Ni2O3、CuO、Cr2O3Or Co2O3；REO is Ce2O3、Nd2O3Or Yb2O3.The present invention passes through Li+To A positions K+、Na+And Sb5+、Ta5+To B positions Nb5+Compound substitution and transition/rare-earth oxide adulterate four kinds of mode modified synergics, improve potassium-sodium niobate-based ceramic sintering characteristic, realize the controllable preparation of the extremely low ceramic of compact of the porosity so that potassium niobate sodium-based leadless piezoelectric ceramic has good mechanical performance and piezoelectric property concurrently.
Description
Technical field
The present invention relates to lead-free piezoceramic material technical field, more particularly to a kind of potassium-sodium niobate-based nothing of high mechanical properties
Lead piezoelectric ceramics material and its preparation method and application.
Background technology
Piezoelectric ceramics is a kind of widely used functional material, and the mutual conversion of mechanical energy and electric energy can be achieved.Piezoelectricity is made pottery
Porcelain is widely used in making the devices such as ultrasonic transducer, underwater sonar detector, piezoelectric transformer, wave filter and piezoelectric buzzer
Part, there is very important status in national economy, science and technology, modern national defense.
Traditional ferroelectric piezoelectric ceramics material, mainly with Pb (Zr, Ti) O3(PZT) it is the binary system of base, ternary system pottery
Porcelain, there is excellent electric property.Piezoceramic material is used to make high performance piezoelectric ignition device, high-power piezoelectric transformer
Material, and during the purposes such as the detection of conduct underwater sonar, ultrasonic nondestructive test, mine locating, it is necessary to possess excellent mechanically performance
Adapt to the needs of big stress, dither.And traditional PZT base piezoelectric ceramics in terms of fracture toughness and bending strength it is obvious not
It can meet this requirement, therefore to piezoceramic material toughness reinforcing, there is good piezoelectric performance and mechanical performance simultaneously to obtain
Ceramic material is the current problem for being badly in need of solving.Use the side of self toughening and two-phase toughness reinforcing for the toughness reinforcing of function ceramics at present more
Formula, self toughening are to enable material tough from the bar-like grains born similar to whisker in preparation process is sintered using material
Change, two-phase toughness reinforcing refers to add Second Phase Particle in ceramic matrix or ceramic matric composite is made to reach toughness reinforcing mesh in fiber
's.With material internal, caused phase transformation and micro-crack absorb energy to reach tough to toughness reinforcing mode under stress mostly
The effect of change.For pure PZT base ceramic materials, its comprehensive mechanical performance is：Young's modulus YE=60~90GPa, Vickers hardness
HV=3.0~5.0GPa, fracture toughness KIC=0.9~1.3MPam1/2, bending strength σf=60~80MPa.By by PZT
Nanocrystalline to be mixed with micro-powder, the vickers hardness hv of the toughness reinforcing PZT ceramic materials prepared using solid-phase sintering process, fracture are tough
Property KIC, bending strength σfRespectively up to 5.11GPa, 1.33MPam1/2、93.92MPa.Although toughness reinforcing PZT base ceramic machineries
Can improve about 20%~30% relative to non-toughness reinforcing PZT sills, but the relatively conventional PZT ceramic materials of its electric property have it is bright
It is aobvious to decline.Therefore while piezoelectric ceramics comprehensive electrical performance is not greatly reduced, ceramic toughening is realized to obtain superior mechanical
Performance is the main difficult technical of current piezoceramic material toughness reinforcing.
On the other hand, (or the Pb of PbO in PZT sills3O4) content account for the 70% of raw material gross mass, this kind of material exists
Prepare, can all disseminate noxious material during use and waste treatment, the health and environment of the mankind are damaged, this obviously has
Disobey the requirement in human development and environmental protection.Therefore the lead-free piezoceramic material of development environment friendly, especially has concurrently
The lead-free ceramicses material of excellent mechanical properties and electric property is just particularly important and urgently.Countries in the world piezoelectric without
All carry out extensive work in the research and development of leaded, and achieve interim progress.In lead-free piezoceramic material system
In, (K0.5Na0.5)NbO3(KNN) base is current putative most promising material, and it has higher piezoelectricity ferro
Property and higher Curie temperature.The leadless piezoelectric material material of other systems, such as barium titanate (BaTiO3, BT) base, bismuth-sodium titanate
(Bi0.5Na0.5TiO3, BNT) and base, the piezoelectric property of bismuth layer structure be below KNN sills.Leadless piezoelectric is made pottery at present
The electric properties of porcelain especially KNN sills has excavated very fully, and the combination properties of Modified K NN base ceramic materials approaches, portion
Point performance has met or exceeded modified PZT sill.But concern of the people to leadless piezoelectric ceramics mechanical performance so far is seldom, only
There is the correlative study report on a small quantity to niobates KNN base ceramic material mechanical performances.The fracture for the KNN bases ceramics being currently known is tough
Property KICLess than 1.3MPam1/2, bending strength σfLess than 143MPa.
The content of the invention
For above-mentioned the deficiencies in the prior art, the present invention provides a kind of niobium for having high mechanical properties and good electrical performance concurrently
Sour potassium sodium base leadless piezoelectric ceramics material and its preparation method and application.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
The invention provides a kind of potassium sodium niobate piezoelectric ceramics material, [Li is included0.06(K0.47-xNa0.47+x)]
[(Nb0.893Sb0.057Ta0.05]O3, TMO and REO；
TMO is MnO2、Fe2O3、Ni2O3、CuO、Cr2O3Or Co2O3；
REO is Ce2O3、Nd2O3Or Yb2O3；
[the Li0.06(K0.47-xNa0.47+x)][(Nb0.893Sb0.057Ta0.05]O3, TMO and REO the ratio between the amount of material be
1:y:z；
Wherein,
X values are 0 or 0.01~0.10；
Y values are 0~0.004；
Z values are 0~0.0008；
It is 0 during y with z differences.
The invention provides a kind of preparation side of the sodium potassium niobate base leadless piezoelectric ceramics material described in above-mentioned technical proposal
Method, comprise the following steps：
(1) corresponding amount is weighed according to the species of each metallic element and mol ratio in sodium potassium niobate base leadless piezoelectric ceramics material
Li2CO3、K2CO3、Na2CO3、Nb2O5、Sb2O3、Ta2O5、MnO2、Fe2O3、Ni2O3、CuO、Cr2O3、Co2O3、CeO2、Nd2O3With
Yb2O3, as raw material；
(2) raw material is subjected to break process, obtains compound；
(3) pre-burning is carried out to the compound, obtains Preburning material；
(4) break process is carried out to the Preburning material, obtains fine powder material；
(5) it is compressing after mixing the fine powder material and binding agent, obtain molding mass；
(6) molding mass is sintered, obtains ceramic material；
(7) it will be polarized after silver electrode on the ceramic material in silicone oil, obtain potassium niobate sodium base leadless piezoelectricity pottery
Ceramic material.
Preferably, the break process in the step (2) is to carry out ball milling after mixing raw material and ethanol；
The mass ratio of the ethanol and raw material is (70~100):100；
The rotating speed of the ball milling is 120~300r/min；
The time of the ball milling is 1~5h.
Preferably, the temperature of the pre-burning is 890~910 DEG C；
The time of the pre-burning is 1~5h.
Preferably, the break process in the step (4) is to carry out ball milling after mixing Preburning material and ethanol；
The mass ratio of the ethanol and Preburning material is (70~100):100；
The rotating speed of the ball milling is 120~300r/min；
The time of the ball milling is 1~5h.
Preferably, the mass ratio of the fine powder material and binding agent is 100:(7~13).
Preferably, the temperature of the sintering is 1080~1150 DEG C；
The time of the sintering is 1~6h.
Preferably, the temperature of the polarization is 60~90 DEG C；
The electric-field intensity of the polarization is 2~9kV/mm；
The time of the polarization is 5~15min.
Present invention also offers the sodium potassium niobate base leadless piezoelectric ceramics material described in a kind of above-mentioned technical proposal or on
The sodium potassium niobate base leadless piezoelectric ceramics material that preparation method described in stating technical scheme any one obtains piezo-electric ignition equipment,
Application in sonar detection equipment, cleaning equipment or welding equipment.
The invention provides a kind of sodium potassium niobate base leadless piezoelectric ceramics material, [Li is included0.06(K0.47-xNa0.47+x)]
[(Nb0.893Sb0.057Ta0.05]O3, TMO and REO；TMO is MnO2、Fe2O3、Ni2O3、CuO、Cr2O3Or Co2O3；REO is Ce2O3、
Nd2O3Or Yb2O3.The present invention passes through Li+To A positions K+、Na+And Sb5+、Ta5+To B positions Nb5+Compound substitution, specific Na/K is taken in A positions
Than and transition/rare-earth oxide adulterate the specific process of four kinds of mode modified synergics, it is sinterable to solve pure KNN ceramics
Property difference problem, realize the controllable preparation of the extremely low ceramic of compact of the porosity so that obtained potassium niobate sodium base leadless piezoelectricity pottery
Ceramic material has good mechanical performance and electric property concurrently.Sodium potassium niobate base leadless piezoelectric ceramics material provided by the invention it is comprehensive
Closing piezoelectricity ferro dielectric physical property is：d33=245.1~282pC/N, kp=42.5%~45.8%, Qm=50~60, tan
δ=0.020~0.027,k31=28.6%~30.5%, Nr=3000~3200Hzm, Pr
=20.0~22.6 μ C/cm2, Ec=1.01~1.3kV/mm, ρ=4.50~4.80g/cm3；Mechanical performance is：Young's modulus YE
=89.0~98.4GPa, bending modulus Ef=74.8~221.6GPa, vickers hardness hv=3.9~5.3GPa, fracture toughness KIC
=1.53~2.0MPam1/2, bending strength σf=160.6~259MPa.The potassium niobate sodium-based leadless piezoelectric ceramic relative to
The potassium-sodium niobate-based ceramic fracture toughness K to have reported for workIC(1.3MPa·m1/2) and bending strength σf(143MPa) is respectively increased
36% and~46%；Relative to the Young's modulus Y of toughness reinforcing PZT ceramicsE(85GPa), vickers hardness hv (4.4GPa), fracture toughness
KIC(1.45MPa·m1/2), bending strength σf(93.92MPa) has been respectively increased 10%, 5%, 24%, 123%.
Present invention also offers a kind of preparation method of sodium potassium niobate base leadless piezoelectric ceramics material.Side provided by the invention
Method need not add any leaded material, green.In addition, preparation method sintering temperature provided by the invention is low, technique
It is simple pervasive, repeatability and have good stability, there is actual amplification promotional value.
Sodium potassium niobate base leadless piezoelectric ceramics material provided by the invention can meet under the conditions of big stress, high-frequency mechanical vibration
Piezoelectric device application.Such as high performance piezoelectricity ignition ceramic material needs to hit more than hundreds thousand of times repeatedly without rupturing,
High-power underwater sonar detection and large power supersonic cleaning, welding device are required to piezoceramic material and do not only have excellent electricity
Performance is learned, there is higher mechanical strength, the potassium-sodium niobate sill disclosed by the invention with high mechanical properties with greater need for it
Meet the application requirement of these field devices.
Brief description of the drawings
Fig. 1 is MnO2(y=0.0008), Fe2O3(y=0.0005), MnO2+CeO2(y=0.0008, z=0.0001) mixes
The XRD spectra of miscellaneous sodium potassium niobate base leadless piezoelectric ceramics material；
Fig. 2 is Na/K=57/43, MnO2Doping y=0.0008 ceramics sample surface SEM photograph；
Fig. 3 is Na/K=57/43, Fe2O3Doping y=0.002 ceramics sample section SEM photograph；
Fig. 4 is PZT-8 ceramic material vickers hardness test impression photos；
Fig. 5 is the sodium potassium niobate base leadless piezoelectric ceramics material vickers hardness test impression photo of the embodiment of the present invention 1.
Embodiment
The invention provides a kind of potassium niobate sodium-based leadless piezoelectric ceramic for having high mechanical properties and superior electrical performance concurrently
Material, include [Li0.06(K0.47-xNa0.47+x)][(Nb0.893Sb0.057Ta0.05]O3, TMO and REO；
TMO is MnO2、Fe2O3、Ni2O3、CuO、Cr2O3Or Co2O3；
REO is Ce2O3、Nd2O3Or Yb2O3；
[the Li0.06(K0.47-xNa0.47+x)][(Nb0.893Sb0.057Ta0.05]O3, TMO and REO the ratio between the amount of material be
1:y:z；
Wherein,
X values are 0 or 0.01~0.10；
Y values are 0~0.004；
Z values are 0~0.0008；
It is 0 during y with z differences.
The invention provides a kind of sodium potassium niobate base leadless piezoelectric ceramics material, the potassium sodium niobate piezoelectric ceramics material
For perovskite structure, [Li is included0.06(K0.47-xNa0.47+x)][(Nb0.893Sb0.057Ta0.05]O3.In the present invention, the x
It is worth for 0 or 0.01~0.10, preferably 0.05~0.1, more preferably 0.06~0.08.
In the present invention, described [Li0.06(K0.47-xNa0.47+x)][(Nb0.893Sb0.057Ta0.05]O3, TMO and REO thing
The ratio between amount of matter is 1:y:z；The y values are 0~0.004, preferably 0.0001~0.002；The z values are 0~0.0008, excellent
Elect 0.0002~0.0006 as.
The invention provides a kind of preparation side of the sodium potassium niobate base leadless piezoelectric ceramics material described in above-mentioned technical proposal
Method, comprise the following steps：
(1) corresponding amount is weighed according to the species of each metallic element and mol ratio in sodium potassium niobate base leadless piezoelectric ceramics material
Li2CO3、K2CO3、Na2CO3、Nb2O5、Sb2O3、Ta2O5、MnO2、Fe2O3、Ni2O3、CuO、Cr2O3、Co2O3、CeO2、Nd2O3With
Yb2O3, as raw material；
(2) raw material is subjected to break process, obtains compound；
(3) pre-burning is carried out to the compound, obtains Preburning material；
(4) break process is carried out to the Preburning material, obtains fine powder material；
(5) it is compressing after mixing the fine powder material and binding agent, obtain molding mass；
(6) molding mass is sintered, obtains ceramic material；
(7) it will be polarized after silver electrode on the ceramic material in silicone oil, obtain potassium niobate sodium base leadless piezoelectricity pottery
Ceramic material.
The present invention weighs pair according to the species of each metallic element and mol ratio in sodium potassium niobate base leadless piezoelectric ceramics material
The Li that should be measured2CO3、K2CO3、Na2CO3、Nb2O5、Sb2O3、Ta2O5、MnO2、Fe2O3、Ni2O3、CuO、Cr2O3、Co2O3、CeO2、
Nd2O3And Yb2O3, obtain raw material.The present invention is to the Li2CO3、K2CO3、Na2CO3、Nb2O5、Sb2O3、Ta2O5、MnO2、Fe2O3、
Ni2O3、CuO、Cr2O3、Co2O3、CeO2、Nd2O3And Yb2O3Source there is no any particular/special requirement, using people in the art
The above-mentioned substance in source known to member, it is specific such as the commercially available prod of above-mentioned material.
The present invention is to the Li2CO3、K2CO3、Na2CO3、Nb2O5、Sb2O3、Ta2O5、MnO2、Fe2O3、Ni2O3、CuO、
Cr2O3、Co2O3、CeO2、Nd2O3And Yb2O3Hybrid mode there is no any particular/special requirement, each material can be according to arbitrary suitable
Sequence carries out weighing mixing.
After obtaining raw material, the raw material is carried out break process by the present invention, obtains compound.In the present invention, the step
Suddenly the break process in (2) is preferably to carry out ball milling after mixing raw material and ethanol；The mass ratio of the ethanol and raw material is preferred
For (70~100):100, more preferably (85~95):100, most preferably 90:100；The rotating speed of the ball milling is preferably 120~
300r/min, more preferably 140~180r/min, most preferably 150~160r/min；The time of the ball milling is preferably 1~
5h, more preferably 2~4h, most preferably 3h.The present invention does not have any particular/special requirement to the concentration of the ethanol, using ability
Wet ball grinding ethanol known to field technique personnel.In the specific embodiment of the invention, the ethanol is absolute ethyl alcohol.
Processing is dried in the material that break process described in preferred pair of the present invention obtains, and obtains dry compound.At this
In invention, the temperature of the drying process is preferably 60~100 DEG C, more preferably 70~90 DEG C, most preferably 80 DEG C.The present invention
There is no any particular/special requirement to the time of the drying process, can be clean by the ethanol evaporation added in material.
After obtaining compound, the present invention carries out pre-burning to the compound, obtains Preburning material.In the present invention, it is described pre-
The temperature of burning is preferably 890~910 DEG C, more preferably 895~905 DEG C, most preferably 900 DEG C；The time of the pre-burning is preferred
For 1~5h, more preferably 2~4h, most preferably 3h.
In the present invention, the pre-burning can make raw material pre-synthesis principal crystalline phase after calcining, obtain high activity powder,
And volatile materials in raw material is excluded, shrinkage factor when reducing ceramic post sintering is to improve consistency.
After obtaining Preburning material, the present invention carries out break process to the Preburning material, obtains fine powder material.In the present invention, institute
It is preferably to carry out ball milling after mixing Preburning material and ethanol to state the break process in step (4)；The matter of the ethanol and Preburning material
Amount is than being preferably (70~100):100, more preferably (85~95):100, most preferably 90:100；The rotating speed of the ball milling is excellent
Elect 120~300r/min, more preferably 140~180r/min, most preferably 150~160r/min as；The time of the ball milling
Preferably 1~5h, more preferably 2~4h, most preferably 3h.The present invention do not have to the purity of the ethanol it is any it is special will
Ask, using wet ball grinding ethanol well-known to those skilled in the art.In the specific embodiment of the invention, the ethanol
For absolute ethyl alcohol.
Processing is dried in the material that break process described in preferred pair of the present invention obtains, and obtains dry fine powder material.At this
In invention, the temperature of the drying process is preferably 60~100 DEG C, more preferably 70~90 DEG C, most preferably 80 DEG C.The present invention
There is no any particular/special requirement to the time of the drying process, can be clean by the ethanol evaporation added in material.
In the present invention, the particle diameter of powder can be reduced by carrying out break process to the Preburning material, be easy to be molded for powder
Create conditions, while cause powder that there is higher activity, in favor of the sintering of ceramics.
After obtaining fine powder material, the present invention is compressing after mixing the fine powder material and binding agent, obtains molding mass.This hair
The bright species to the binding agent does not have any particular/special requirement, is used using ceramics shaping well-known to those skilled in the art viscous
Tie agent.The present invention does not have any particular/special requirement to the hybrid mode of the fine powder material and binding agent, can be by fine powder material
It is well mixed with binding agent.In the present invention in specific embodiment, the binding agent is preferably the PVA aqueous solution, described
The mass concentration of the PVA aqueous solution is preferably 5~10%, and more preferably 6~8%.In the present invention, the fine powder material and binding agent
Mass ratio be preferably 100:(7~13), more preferably 100:(9~11), most preferably 100:10.
In the present invention, it is described it is compressing can according to reality demand be pressed into arbitrary shape.Implement in the present invention
In example, the compressing molding mass be a diameter of 10mm, and thickness is 1.2mm disk, briquetting pressure 5MPa, during shaping
Between be 1min.In the present invention, it is described compressing preferably to carry out at room temperature.
After obtaining molding mass, the present invention is sintered to the molding mass, obtains ceramic material.In the present invention, it is described
The temperature of sintering is preferably 1080~1150 DEG C, more preferably 1090~1130 DEG C, most preferably 1100~1120 DEG C；The burning
The time of knot is preferably 1~6h, more preferably 2~4h, most preferably 3h.In the present invention, it is warming up to the sintering temperature
Speed is preferably 150~200 DEG C/h, more preferably 160~190 DEG C/h, most preferably 170~180 DEG C/h.In the present invention,
The sintering process causes molded base substrate is densified under high temperature action to form porcelain.
After obtaining ceramic material, the present invention will be polarized after silver electrode on the ceramic material in silicone oil, obtain niobium
Sour potassium sodium base leadless piezoelectric ceramics material.The present invention does not have any particular/special requirement to the method for the upper silver electrode, using this
The technique of silver electrode is carried out on ceramics known to art personnel.In the present invention, the upper silver electrode is preferably：
The silver paste of dilution is uniformly applied to the upper and lower surface of ceramics sample with banister brush, then dries silver at 200~250 DEG C so that silver
Organic matter volatilization in slurry, it is cold with stove that power-off after silver electrode is oozed in 10~30min roastings is finally incubated at a temperature of 750~800 DEG C
But.
The present invention does not have particular/special requirement to the species of silver paste and source, using silver well-known to those skilled in the art
Slurry, it is specific such as the silver paste of Shanghai Hao Yin Electron Material Co., Ltd production.The present invention does not have to the thickness of silver paste coating
Particular/special requirement, it is configured according to concrete technology requirement.In embodiments of the present invention, the thickness of silver paste coating is specific
For 10 μm.
In the present invention, the temperature for drying silver is preferably 200~250 DEG C, more preferably 210~240 DEG C, is most preferably
220~230 DEG C.The present invention is not particularly limited to the time for drying silver, can be clean i.e. by the organic matter volatilization in silver paste
Can.
In the present invention, the sintering temperature for oozing silver electrode is preferably 750~800 DEG C, more preferably 760~790 DEG C,
Most preferably 770~780 DEG C；The roasting time for oozing silver electrode is preferably 10~30min, more preferably 15~25min, most
Preferably 20min.
In the present invention, the ceramic material for coating silver electrode is specially immersed in silicone oil by described polarized in silicone oil
In, apply voltage in electrode both sides, form electric field and polarized.In the present invention, the temperature of the polarization is preferably 60~90
DEG C, more preferably 65~85 DEG C, most preferably 80 DEG C；The electric-field intensity of the polarization is preferably 2~9kV/mm, and more preferably 3
~8kV/mm, most preferably 4~6kV/mm；The time of the polarization is preferably 5~15min, more preferably 8~13min, optimal
Elect 10min as.
Present invention also offers the sodium potassium niobate base leadless piezoelectric ceramics material described in a kind of above-mentioned technical proposal or on
The sodium potassium niobate base leadless piezoelectric ceramics material that preparation method described in stating technical scheme any one obtains piezo-electric ignition equipment,
Application in sonar detection equipment, cleaning equipment or welding equipment.Potassium niobate sodium-based leadless piezoelectric ceramic material provided by the invention
Material has the feature of high mechanical properties and high electric property simultaneously, disclosure satisfy that the device under the conditions of big stress, high-frequency mechanical vibration
Part application, it is specifically hundreds thousand of secondary above without the high performance piezoelectrics igniting ceramics of rupture, high-power water if desired for hitting repeatedly
Lower sonar detection and large power supersonic cleaning, welding device etc..
With reference to embodiment to potassium sodium niobate piezoelectric ceramics material provided by the invention and its preparation method and application
It is described in detail, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
(1), from the pure Li of market buying chemistry2CO3、K2CO3、Na2CO3、Nb2O5、Sb2O3、Ta2O5、MnO2As raw material,
According to the chemical formula [Li of the sodium potassium niobate base leadless piezoelectric ceramics material of the present invention0.06(K0.47-xNa0.47+x)]
[(Nb0.893Sb0.057Ta0.05]O3+y MnO2, wherein x=0, y=0.0008 weigh raw material；Load weighted raw material is put into ball milling
In tank, after addition accounts for the absolute ethyl alcohol of above-mentioned raw materials gross weight 80%, mixed on planetary ball mill with 150r/min rotating speed
And levigate 2h；
(2), the compound after ball milling is put in crucible after 80 DEG C of drying, in 900 DEG C of pre-burnings, soaking time
3.5h；After powder addition after pre-burning synthesis accounts for the absolute ethyl alcohol of powder gross weight 80%, with the levigate 4h of 150r/min rotating speeds；
(3) pre-burning of levigate mistake, is synthesized into powder to dry at 80 DEG C, is placed in mould, is pressed into after adding suitable amount of adhesive
Required ceramic green sheet, wherein adhesive are the aqueous solution for the PVA that weight percentage is 6%, and its dosage is powder after ball milling
Expect the 10% of gross weight；
(4) ceramic green sheet, is warming up to 1100 DEG C of insulation 4h sintering by 200 DEG C/h, is naturally cooling to room temperature with stove afterwards；
(5), by silver electrode on the potsherd after sintering, in 80 DEG C of silicone oil, the direct current in electric-field intensity for 6kV/mm
Polarize 10min under electric field.
The electric parameters of the sodium potassium niobate base leadless piezoelectric ceramics material prepared according to the method described above are as follows：d33=
246pC/N, kp=43%,Tan δ=0.026；Qm=52, k31=0.293, Nr=3162Hzm, Pr=
21.63μC/cm2, Ec=1.2kV/mm and ρ=4.65g/cm3。
The mechanical performance parameter of the material is：Young's modulus YE=93.3GPa, vickers hardness hv=4.04GPa, fracture are tough
Property KIC=1.53MPam1/2, bending strength σf=199.9MPa.
Embodiment 2
(1), from the pure Li of market buying chemistry2CO3、K2CO3、Na2CO3、Nb2O5、Sb2O3、Ta2O5、MnO2As raw material,
According to the chemical formula [Li of the sodium potassium niobate base leadless piezoelectric ceramics material of the present invention0.06(K0.47-xNa0.47+x)]
[(Nb0.893Sb0.057Ta0.05]O3+y MnO2, wherein x=0.03, y=0.0008 weigh raw material；Load weighted raw material is put into
In ball grinder, after addition accounts for the absolute ethyl alcohol of above-mentioned raw materials gross weight 80%, with 150r/min rotating speed on planetary ball mill
Mixing and levigate 2h；
(2), the compound after ball milling is put in crucible after 80 DEG C of drying, in 900 DEG C of pre-burnings, soaking time
3.5h；After powder addition after pre-burning synthesis accounts for the absolute ethyl alcohol of powder gross weight 80%, with the levigate 4h of 150r/min rotating speeds；
(3) pre-burning of levigate mistake, is synthesized into powder to dry at 80 DEG C, is placed in mould, is pressed into after adding suitable amount of adhesive
Required ceramic green sheet, wherein adhesive are the aqueous solution for the PVA that weight percentage is 6%, and its dosage is powder after ball milling
Expect the 10% of gross weight；
(4) ceramic green sheet, is warming up to 1100 DEG C of insulation 4h sintering by 200 DEG C/h, is naturally cooling to room temperature with stove afterwards；
(5), by silver electrode on the potsherd after sintering, in 80 DEG C of silicone oil, the direct current in electric-field intensity for 6kV/mm
Polarize 10min under electric field.
The performance parameter of the sodium potassium niobate base leadless piezoelectric ceramics material prepared according to the method described above is as follows：d33=252pC/
N, kp=43.0%,Tan δ=0.026；k31=0.294, Pr=21.1 μ C/cm2, Ec=1.1kV/mm
With ρ=4.68g/cm3。
The mechanical performance parameter of the material is：Young's modulus YE=93.0GPa, vickers hardness hv=4.51GPa, fracture are tough
Property KIC=1.82MPam1/2, bending strength σf=220.4MPa.
Embodiment 3
(1), from the pure Li of market buying chemistry2CO3、K2CO3、Na2CO3、Nb2O5、Sb2O3、Ta2O5、MnO2As raw material,
According to the chemical formula [Li of the sodium potassium niobate base leadless piezoelectric ceramics material of the present invention0.06(K0.47-xNa0.47+x)]
[(Nb0.893Sb0.057Ta0.05]O3+y MnO2, wherein x=0.085, y=0.0008 weigh raw material；Load weighted raw material is put into
In ball grinder, after addition accounts for the absolute ethyl alcohol of above-mentioned raw materials gross weight 80%, with 140r/min rotating speed on planetary ball mill
Mixing and levigate 2h；
(2), the compound after ball milling is put in crucible after 80 DEG C of drying, in 900 DEG C of pre-burnings, soaking time
3h；After powder addition after pre-burning synthesis accounts for the absolute ethyl alcohol of powder gross weight 80%, with the levigate 4h of 140r/min rotating speeds；
(3) pre-burning of levigate mistake, is synthesized into powder to dry at 80 DEG C, is placed in mould, is pressed into after adding suitable amount of adhesive
Required ceramic green sheet, wherein adhesive are the aqueous solution for the PVA that weight percentage is 6%, and its dosage is powder after ball milling
Expect the 10% of gross weight；
(4) ceramic green sheet, is warming up to 1100 DEG C of insulation 4h sintering by 190 DEG C/h, is naturally cooling to room temperature with stove afterwards；
(5), by silver electrode on the potsherd after sintering, in 80 DEG C of silicone oil, the direct current in electric-field intensity for 6kV/mm
Polarize 10min under electric field.
The performance parameter of the sodium potassium niobate base leadless piezoelectric ceramics material prepared according to the method described above is as follows：d33=272pC/
N, kp=43.5%,Tan δ=0.025；Pr=20.8 μ C/cm2, Ec=0.95kV/mm.
The mechanical performance parameter of the material is：Young's modulus YE=90.8GPa, vickers hardness hv=4.11GPa, fracture are tough
Property KIC=1.72MPam1/2, bending strength σf=226.2MPa, bending modulus Ef=206.9GPa.
Embodiment 4
(1), from the pure Li of market buying chemistry2CO3、K2CO3、Na2CO3、Nb2O5、Sb2O3、Ta2O5、MnO2As raw material,
According to the chemical formula [Li of the sodium potassium niobate base leadless piezoelectric ceramics material of the present invention0.06(K0.47-xNa0.47+x)]
[(Nb0.893Sb0.057Ta0.05]O3+y MnO2, wherein x=0.10, y=0.0008 weigh raw material；Load weighted raw material is put into
In ball grinder, after addition accounts for the absolute ethyl alcohol of above-mentioned raw materials gross weight 90%, with 160r/min rotating speed on planetary ball mill
Mixing and levigate 2h；
(2), the compound after ball milling is put in crucible after 80 DEG C of drying, in 900 DEG C of pre-burnings, soaking time
3.5h；After powder addition after pre-burning synthesis accounts for the absolute ethyl alcohol of powder gross weight 90%, with the levigate 4h of 160r/min rotating speeds；
(3) pre-burning of levigate mistake, is synthesized into powder to dry at 80 DEG C, is placed in mould, is pressed into after adding suitable amount of adhesive
Required ceramic green sheet, wherein adhesive are the aqueous solution for the PVA that weight percentage is 6%, and its dosage is powder after ball milling
Expect the 9% of gross weight；
(4) ceramic green sheet, is warming up to 1130 DEG C of insulation 4h sintering by 200 DEG C/h, is naturally cooling to room temperature with stove afterwards；
(5), by silver electrode on the potsherd after sintering, in 80 DEG C of silicone oil, the direct current in electric-field intensity for 6kV/mm
Polarize 10min under electric field.
The performance parameter of the sodium potassium niobate base leadless piezoelectric ceramics material prepared according to the method described above is as follows：d33=260pC/
N, kp=42.5%,Tan δ=0.024；Pr=21 μ C/cm2, Ec=0.95kV/mm.
The mechanical performance parameter of the material is：Young's modulus YE=93.0GPa, vickers hardness hv=4.40GPa, fracture are tough
Property KIC=1.68MPam1/2, bending strength σf=185.1MPa.
Embodiment 5
(1), from the pure Li of market buying chemistry2CO3、K2CO3、Na2CO3、Nb2O5、Sb2O3、Ta2O5、Fe2O3As raw material,
According to the chemical formula [Li of the sodium potassium niobate base leadless piezoelectric ceramics material of the present invention0.06(K0.47-xNa0.47+x)]
[(Nb0.893Sb0.057Ta0.05]O3+y Fe2O3, wherein x=0.07, y=0.0005 weigh raw material；Load weighted raw material is put into
In ball grinder, after addition accounts for the absolute ethyl alcohol of above-mentioned raw materials gross weight 80%, with 180r/min rotating speed on planetary ball mill
Mixing and levigate 2h；
(2), the compound after ball milling is put in crucible after 70 DEG C of drying, in 900 DEG C of pre-burnings, soaking time
3.5h；After powder addition after pre-burning synthesis accounts for the absolute ethyl alcohol of powder gross weight 80%, with the levigate 4h of 180r/min rotating speeds；
(3) pre-burning of levigate mistake, is synthesized into powder to dry at 70 DEG C, is placed in mould, is pressed into after adding suitable amount of adhesive
Required ceramic green sheet, wherein adhesive are the aqueous solution for the PVA that weight percentage is 6%, and its dosage is powder after ball milling
Expect the 10% of gross weight；
(4) ceramic green sheet, is warming up to 1100 DEG C of insulation 4h sintering by 170 DEG C/h, is naturally cooling to room temperature with stove afterwards；
(5), by silver electrode on the potsherd after sintering, in 80 DEG C of silicone oil, the direct current in electric-field intensity for 6kV/mm
Polarize 10min under electric field.
The performance parameter of the sodium potassium niobate base leadless piezoelectric ceramics material prepared according to the method described above is as follows：d33=276pC/
N, kp=45.8%,Tan δ=0.026；Qm=50, k31=0.289, Pr=20.3 μ C/cm2, Nr=
3068Hz·m,Ec=1.09kV/mm.
The mechanical performance parameter of the material is：Young's modulus YE=92.4GPa, vickers hardness hv=4.95GPa, fracture are tough
Property KIC=1.80MPam1/2。
Embodiment 6
(1), from the pure Li of market buying chemistry2CO3、K2CO3、Na2CO3、Nb2O5、Sb2O3、Ta2O5、Ni2O3As raw material,
According to the chemical formula [Li of the sodium potassium niobate base leadless piezoelectric ceramics material of the present invention0.06(K0.47-xNa0.47+x)]
[(Nb0.893Sb0.057Ta0.05]O3+y Ni2O3, wherein x=0.066, y=0.0005 weigh raw material；Load weighted raw material is put
Enter in ball grinder, after addition accounts for the absolute ethyl alcohol of above-mentioned raw materials gross weight 85%, turned on planetary ball mill with 150r/min
Speed mixing and levigate 2h；
(2), the compound after ball milling is put in crucible after 70 DEG C of drying, in 900 DEG C of pre-burnings, soaking time
3.5h；After powder addition after pre-burning synthesis accounts for the absolute ethyl alcohol of powder gross weight 85%, with the levigate 4h of 150r/min rotating speeds；
(3) pre-burning of levigate mistake, is synthesized into powder to dry at 70 DEG C, is placed in mould, is pressed into after adding suitable amount of adhesive
Required ceramic green sheet, wherein adhesive are the aqueous solution for the PVA that weight percentage is 6%, and its dosage is powder after ball milling
Expect the 8% of gross weight；
(4) ceramic green sheet, is warming up to 1100 DEG C of insulation 4h sintering by 190 DEG C/h, is naturally cooling to room temperature with stove afterwards；
(5), by silver electrode on the potsherd after sintering, in 70 DEG C of silicone oil, the direct current in electric-field intensity for 6kV/mm
Polarize 10min under electric field.
The performance parameter of the sodium potassium niobate base leadless piezoelectric ceramics material prepared according to the method described above is as follows：d33=260pC/
N, kp=45.5%,Tan δ=0.021.
The mechanical performance parameter of the material is：Young's modulus YE=91.6GPa, vickers hardness hv=5.18GPa, fracture are tough
Property KIC=1.94MPam1/2。
Embodiment 7
(1), from the pure Li of market buying chemistry2CO3、K2CO3、Na2CO3、Nb2O5、Sb2O3、Ta2O5、MnO2、CeO2As
Raw material, according to the chemical formula [Li of the sodium potassium niobate base leadless piezoelectric ceramics material of the present invention0.06(K0.47-xNa0.47+x)]
[(Nb0.893Sb0.057Ta0.05]O3+y MnO2+z CeO2, wherein x=0.07, y=0.0008, z=0.0001 weighs raw material；Will
Load weighted raw material is put into ball grinder, after addition accounts for the absolute ethyl alcohol of above-mentioned raw materials gross weight 90%, on planetary ball mill
With 180r/min rotating speed mixing and levigate 2h；
(2), the compound after ball milling is put in crucible after 80 DEG C of drying, in 900 DEG C of pre-burnings, soaking time
3h；After powder addition after pre-burning synthesis accounts for the absolute ethyl alcohol of powder gross weight 90%, with the levigate 4h of 180r/min rotating speeds；
(3) pre-burning of levigate mistake, is synthesized into powder to dry at 80 DEG C, is placed in mould, is pressed into after adding suitable amount of adhesive
Required ceramic green sheet, wherein adhesive are the aqueous solution for the PVA that weight percentage is 6%, and its dosage is powder after ball milling
Expect the 8% of gross weight；
(4) ceramic green sheet, is warming up to 1100 DEG C of insulation 4h sintering by 180 DEG C/h, is naturally cooling to room temperature with stove afterwards；
(5), by silver electrode on the potsherd after sintering, in 80 DEG C of silicone oil, the direct current in electric-field intensity for 6kV/mm
Polarize 10min under electric field.
The performance parameter of the sodium potassium niobate base leadless piezoelectric ceramics material prepared according to the method described above is as follows：d33=261pC/
N, kp=42.0%,Tan δ=0.027；Qm=58, Nr=3094Hzm, Pr=22.27 μ C/cm2, Ec
=1.25kV/mm and ρ=4.54g/cm3。
The mechanical performance parameter of the material is：Young's modulus YE=90.9GPa, vickers hardness hv=4.84GPa, fracture are tough
Property KIC=1.74MPam1/2, bending strength σf=160.0MPa, bending modulus Ef=133.3GPa.
Embodiment 8
(1), from the pure Li of market buying chemistry2CO3、K2CO3、Na2CO3、Nb2O5、Sb2O3、Ta2O5、Fe2O3、CeO2As
Raw material, according to the chemical formula [Li of the sodium potassium niobate base leadless piezoelectric ceramics material of the present invention0.06(K0.47-xNa0.47+x)]
[(Nb0.893Sb0.057Ta0.05]O3+y Fe2O3+z CeO2, wherein x=0.066, y=0.0005, z=0.0001 weighs raw material；
Load weighted raw material is put into ball grinder, after addition accounts for the absolute ethyl alcohol of above-mentioned raw materials gross weight 80%, in planetary ball mill
On with the mixing of 150r/min rotating speed and levigate 2h；
(2), the compound after ball milling is put in crucible after 80 DEG C of drying, in 900 DEG C of pre-burnings, soaking time
3.5h；After powder addition after pre-burning synthesis accounts for the absolute ethyl alcohol of powder gross weight 80%, with the levigate 4h of 150r/min rotating speeds；
(3) pre-burning of levigate mistake, is synthesized into powder to dry at 80 DEG C, is placed in mould, is pressed into after adding suitable amount of adhesive
Required ceramic green sheet, wherein adhesive are the aqueous solution for the PVA that weight percentage is 6%, and its dosage is powder after ball milling
Expect the 9% of gross weight；
(4) ceramic green sheet, is warming up to 1100 DEG C of insulation 4h sintering by 180 DEG C/h, is naturally cooling to room temperature with stove afterwards；
(5), by silver electrode on the potsherd after sintering, in 80 DEG C of silicone oil, the direct current in electric-field intensity for 6kV/mm
Polarize 10min under electric field.
The performance parameter of the sodium potassium niobate base leadless piezoelectric ceramics material prepared according to the method described above is as follows：d33=267pC/
N, kp=45.7%, tan δ=0.029,Qm=52, k31=0.294, Nr=3075Hzm.
The mechanical performance parameter of the material is：Young's modulus YE=92.0GPa, vickers hardness hv=4.90GPa, fracture are tough
Property KIC=1.84MPam1/2。
According to the preparation technology of embodiment 1,5,7, MnO is obtained2(y=0.0008), Fe2O3(y=0.0005), MnO2+
CeO2The potassium sodium niobate piezoelectric ceramics material of (y=0.0008, z=0.0001) doping, and the material to obtaining carries out XRD inspections
Survey, as a result as shown in Figure 1.As shown in Figure 1, the XRD peak type knots of the potassium sodium niobate piezoelectric ceramics material of different TMO, REO doping
Structure is consistent, shows that its structure has good homogeneity, and form perovskite structure.
Na/K=57/43, MnO2Doping y=0.0008 ceramics sample surface SEM photograph it is as shown in Figure 2.Na/K
=57/43, Fe2O3Doping y=0.002 ceramics sample section SEM photograph it is as shown in Figure 3.From Fig. 2 and Fig. 3, niobium
Sour potassium sodium base leadless piezoelectric ceramics material homogeneous grain size, the porosity is extremely low, even structure is fine and close.Particularly Fig. 3 shows niobium
Complete transgranular fracture is happens is that during sour potassium sodium based leadless piezoelectric ceramics fracture, suggests that potassium-sodium niobate-based ceramics have high machine
Tool intensity and performance.
Fig. 4 is toughness reinforcing PZT-8 ceramic material vickers hardness test impression photos, and Fig. 5 is the potassium-sodium niobate of the embodiment of the present invention 1
Base leadless piezoelectric ceramics material vickers hardness test impression photo.From Fig. 4 and Fig. 5, columbate leadless provided by the invention
The area of indentation of the Vickers hardness of piezoceramic material is less than PZT-8 ceramic materials, shows the potassium-sodium niobate that the present invention obtains
The hardness of base leadless piezoelectric ceramics material is more than toughness reinforcing PZT-8 ceramics.
As seen from the above embodiment, the invention provides a kind of high mechanical properties potassium niobate sodium-based leadless piezoelectric ceramic material
Material, includes [Li0.06(K0.47-xNa0.47+x)][(Nb0.893Sb0.057Ta0.05]O3, TMO and REO；TMO is MnO2、Fe2O3、Ni2O3、
CuO、Cr2O3Or Co2O3；REO is Ce2O3、Nd2O3Or Yb2O3.The present invention passes through Li+To A positions K+、Na+And Sb5+、Ta5+To B positions
Nb5+Compound substitution and transition/rare-earth oxide adulterate four kinds of mode modified synergics, and it is sinterable to solve pure KNN ceramics
Property difference problem, realize the controllable preparation of the extremely low ceramic of compact of the porosity so that obtained potassium niobate sodium base leadless piezoelectricity pottery
Ceramic material has good mechanical performance and electric property concurrently.It can be seen from the result of embodiment, potassium niobate sodium base leadless piezoelectricity pottery
The integrated piezo ferroelectric dielectric physical property of ceramic material is：d33=245.1~282pC/N, kp=42.5%~45.8%, Qm=
50~60, tan δ=0.020~0.027,k31=28.6%~30.5%, Nr=3000~
3200Hzm, Pr=20.0~22.6 μ C/cm2, Ec=1.01~1.3kV/mm, ρ=4.50~4.80g/cm3；Mechanical performance
For：Young's modulus YE=89.0~98.4GPa, bending modulus Ef=74.8~221.6GPa, vickers hardness hv=3.9~
5.3GPa, fracture toughness KIC=1.6~2.0MPam1/2, bending strength σf=160.6~259MPa.
Present invention also offers a kind of preparation method of sodium potassium niobate base leadless piezoelectric ceramics material.Side provided by the invention
Method need not add any leaded material, green.In addition, preparation method sintering temperature provided by the invention is low, technique letter
It is single pervasive, repeatability and have good stability.
Preparation side described in sodium potassium niobate base leadless piezoelectric ceramics material provided by the invention or technical scheme any one
The potassium niobate sodium-based leadless piezoelectric ceramic that method obtains, while there is the feature of high mechanical properties and high electric property, it disclosure satisfy that
Device application under the conditions of big stress, high-frequency mechanical vibration, if desired for hitting the hundreds thousand of high-performance pressures without rupture repeatedly
Electric ignition ceramics, high-power underwater sonar detection and large power supersonic cleaning, welding device etc..
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of high mechanical properties sodium potassium niobate base leadless piezoelectric ceramics material, includes [Li0.06(K0.47-xNa0.47+x)]
[(Nb0.893Sb0.057Ta0.05]O3, TMO and REO；
TMO is MnO2、Fe2O3、Ni2O3、CuO、Cr2O3Or Co2O3；
REO is Ce2O3、Nd2O3Or Yb2O3；
[the Li0.06(K0.47-xNa0.47+x)][(Nb0.893Sb0.057Ta0.05]O3, TMO and REO the ratio between the amount of material be 1:y:
z；
Wherein,
X values are 0 or 0.01~0.10；
Y values are 0~0.004；
Z values are 0~0.0008；
It is 0 during y with z differences.
2. the preparation method of the sodium potassium niobate base leadless piezoelectric ceramics material described in claim 1, is comprised the following steps：
(1) Li of corresponding amount is weighed according to the species and mol ratio of each metallic element in potassium sodium niobate piezoelectric ceramics material2CO3、
K2CO3、Na2CO3、Nb2O5、Sb2O3、Ta2O5、MnO2、Fe2O3、Ni2O3、CuO、Cr2O3、Co2O3、CeO2、Nd2O3And Yb2O3, make
For raw material；
(2) raw material is subjected to break process, obtains compound；
(3) pre-burning is carried out to the compound, obtains Preburning material；
(4) break process is carried out to the Preburning material, obtains fine powder material；
(5) it is compressing after mixing the fine powder material and binding agent, obtain molding mass；
(6) molding mass is sintered, obtains ceramic material；
(7) it will be polarized after silver electrode on the ceramic material in silicone oil, obtain potassium niobate sodium-based leadless piezoelectric ceramic material
Material.
3. preparation method according to claim 2, it is characterised in that the break process in the step (2) is by raw material
Ball milling is carried out after being mixed with ethanol；
The mass ratio of the ethanol and raw material is (70~100):100；
The rotating speed of the ball milling is 120~300r/min；
The time of the ball milling is 1~5h.
4. preparation method according to claim 2, it is characterised in that the temperature of the pre-burning is 890~910 DEG C；
The time of the pre-burning is 1~5h.
5. preparation method according to claim 2, it is characterised in that the break process in the step (4) is by pre-burning
Ball milling is carried out after material and ethanol mixing；
The mass ratio of the ethanol and Preburning material is (70~100):100；
The rotating speed of the ball milling is 120~300r/min；
The time of the ball milling is 1~5h.
6. preparation method according to claim 2, it is characterised in that the mass ratio of the fine powder material and binding agent is 100:
(7~13).
7. preparation method according to claim 2, it is characterised in that the temperature of the sintering is 1080~1150 DEG C；
The time of the sintering is 1~6h.
8. preparation method according to claim 2, it is characterised in that the temperature of the polarization is 60~90 DEG C；
The electric-field intensity of the polarization is 2~9kV/mm；
The time of the polarization is 5~15min.
9. system described in the sodium potassium niobate base leadless piezoelectric ceramics material or claim 2~8 any one described in claim 1
The sodium potassium niobate base leadless piezoelectric ceramics material that Preparation Method obtains is in piezo-electric ignition equipment, sonar detection equipment, large power supersonic
Application in cleaning equipment or welding equipment.
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