CN107216149A - A kind of transparent lead-free piezoceramic material and preparation method thereof - Google Patents
A kind of transparent lead-free piezoceramic material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to field of non-metallic materials, and more particularly to a kind of transparent lead-free piezoceramic material and preparation method thereof.The transparent lead-free piezoceramic material and preparation method thereof, devises a kind of new lead-free piezoceramic material, consisting of (Na1‑x‑y‑ zKzLiyCax)Nb1‑xSnxO3(wherein x=0.02~0.08, y=0.02~0.10, z=0.35~0.55), the material easy-sintering, the transmitance to light is high, and piezoelectric property is good.A kind of method of new two-step sintering is employed, i.e., vacuum pressed is sintered at a lower temperature first, oxygen pressure sintering is then led under nominal sintering temperature, effect is better than common pressure sintering method.
Description
Technical field
The present invention relates to field of non-metallic materials, and more particularly to a kind of transparent lead-free piezoceramic material and its preparation side
Method.
Background technology
Potassium-sodium niobate ((Na0.5K0.5)NbO3Or KNN) leadless piezoelectric monocrystalline has big optical index, high photoelectric coefficient
With two grades of Clock Multiplier Factors, optics field is can be widely applied to, and because it does not include heavy metal element lead, with zirconium metatitanic acid
Lead system (such as lead lanthanum zirconate titanate) piezoelectric is compared, more environmentally friendly.But, the monocrystalline production process time is long, high to equipment requirement,
Energy consumption is big, thus price is costly, and due to the difference of kalium ion and natrium ion property, composition is easily inclined in single crystal growth process
Analysis, it is difficult to prepare the uniform large size single crystal of composition.Potassium sodium niobate ceramic also has good ferroelectricity, piezoelectricity and pyroelectric
Can, and easily prepare.However, the scattering due to crystal grain boundary, stomata etc. to light, the ceramics are general opaque, it is impossible to be used for
Optical field.
The problem of being difficult transparent for potassium sodium niobate piezoelectric ceramics, the technical scheme developed at present mainly includes following two
Kind：1) by doping, component is adjusted, makes its more easy-sintering, but existing Adjusted Option is while translucency is improved, often
The raising of piezoelectric property is helpless to, or even reduces piezoelectric property；2) crystallite dimension is reduced by pressure sintering, improves fine and close
Degree, but effect is sometimes still less desirable.
The content of the invention
It is an object of the invention to provide a kind of transparent lead-free piezoceramic material, improve light transmission rate, at the same also compared with
Piezoelectric property has been significantly increased.
The second object of the present invention is to provide a kind of preparation method of transparent lead-free piezoceramic material, it is possible to increase thoroughly
The consistency of bright lead-free piezoceramic material, preparation method is simple to operate.
The present invention is solved its technical problem and realized using following technical scheme：
The invention provides a kind of transparent lead-free piezoceramic material, the chemical formula of transparent lead-free piezoceramic material
(Na1-x-y-zKzLiyCax)Nb1-xSnxO3(wherein x=0.02~0.08, y=0.02~0.10, z=0.35~0.55).
The present invention also provides a kind of preparation method of transparent lead-free piezoceramic material, according to chemical formula (Na1-x-y- zKzLiyCax)Nb1-xSnxO3, wherein x=0.02~0.08, y=0.02~0.10, z=0.35~0.55, in Na, K, Li,
Ca, Nb and Sn mol ratio calculate oxide spinel sodium, potassium carbonate, lithium carbonate, calcium carbonate, niobium pentaoxide and tin oxide
Mass fraction, according to the mass fraction of plurality of raw materials weigh sodium carbonate, potassium carbonate, lithium carbonate, calcium carbonate, niobium pentaoxide,
And tin oxide, calcine and be made after load weighted plurality of raw materials is mixed.
Present invention has the advantages that：
The transparent lead-free piezoceramic material that the present invention is provided, the chemical formula (Na of transparent lead-free piezoceramic material1-x-y- zKzLiyCax)Nb1-xSnxO3(wherein x=0.02~0.08, y=0.02~0.10, z=0.35~0.55).By right
(Na0.5K0.5)NbO3Adulterate LiNbO3And CaSnO3, light transmission rate is not only substantially increased, while also greatly improving
Piezoelectric property.
The present invention provides a kind of preparation method of transparent lead-free piezoceramic material, to oxide spinel sodium, potassium carbonate, carbonic acid
Lithium, calcium carbonate, niobium pentaoxide and tin oxide, calcining are made.In pressure sintering process, two-step method is employed, i.e., first
Vacuum pressed is sintered at a lower temperature, and oxygen pressure sintering is then led under nominal sintering temperature, transparent lead-free piezoelectricity is improved
Ceramic material consistency, effect is better than common pressure sintering method.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to institute in embodiment
The accompanying drawing needed to use is briefly described.
Fig. 1 is the profile scanning electron microscope for the transparent lead-free piezoceramic material that the embodiment of the present invention 1 is prepared；
Fig. 2 is the piezoelectric property figure for the transparent lead-free piezoceramic material that the embodiment of the present invention 2 is prepared；
Fig. 3 is each component for the transparent lead-free piezoceramic material that the embodiment of the present invention 3 is prepared to its transmitance
Influence figure；
When Fig. 4 is that the embodiment of the present invention 4 prepares transparent lead-free piezoceramic material, shadow of the sintering method to ceramic transmitance
Ring.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, are the conventional production that can be obtained by commercially available purchase
Product.
In the description of the invention, it is necessary to which explanation, term " first ", " second " etc. are only used for distinguishing description, without
It is understood that to indicate or imply relative importance.
A kind of transparent lead-free piezoceramic material of the embodiment of the present invention and preparation method thereof is specifically described below.
A kind of transparent lead-free piezoceramic material provided in an embodiment of the present invention.
A kind of transparent lead-free piezoceramic material, its chemical formula is (Na1-x-y-zKzLiyCax)Nb1-xSnxO3, wherein x=
0.02~0.08, y=0.02~0.10, z=0.35~0.55.
Above-mentioned transparent lead-free piezoceramic material is mainly made up of plurality of raw materials.Many of raw material includes：Sodium carbonate,
Potassium carbonate, lithium carbonate, calcium carbonate, niobium pentaoxide and tin oxide.
Niobium pentaoxide (Nb2O5), it is white powdered.It is water insoluble, be insoluble in acid, can be dissolved in melting potassium acid sulfate or
In the carbonate of alkali metal, hydroxide.As draw niobic acid Ni-monocrystal, special optical glass processed, high and low frequency capacitor and
Piezo ceramic element.It is also used for producing the various niobium alloys that ferro-niobium and special steel need.It is to produce niobium and its raw material of compound.
Also serve as catalyst, refractory material.
By niobium pentaoxide (Nb2O5) be used to manufacture transparent lead-free piezoelectric ceramics, transparent lead-free piezoelectricity can be effectively improved
The light transmission rate of ceramics, while also greatly improving piezoelectric property.
Tin oxide (chemical formula：SnO2, formula weight：150.71) white, faint yellow or light gray is cubic, six sides or orthorhombic system
Powder.1630 DEG C of fusing point, 1800 DEG C of boiling point.It is simultaneously a kind of outstanding transparent conductive material.It is first and put it into commercial operation
Transparent conductive material, in order to improve its electric conductivity and stability, is often doped and uses, such as SnO2：Sb、SnO2：F etc..
By tin oxide (SnO2) be used to manufacture transparent lead-free piezoelectric ceramics, it can further improve transparent lead-free piezoelectricity pottery
The light transmission rate of porcelain.
Sodium carbonate (Na2CO3), molecular weight 105.99.The purity of chemicals is more more than 99.5% (mass fraction), is called
Soda ash, but classification belongs to salt, is not belonging to alkali.In international trade also known as soda or sode ash.It is that a kind of important organic chemical industry is former
Material, is mainly used in the production of plate glass, glassware and ceramic glaze.Life washing, acids is also widely used in neutralize and eat
Product processing etc..
Potassium carbonate (K2CO3) white crystalline powder.Density 2.428g/cm3.891 DEG C of fusing point, is decomposed, average molecular during boiling point
Amount 138.21.Water is dissolved in, the aqueous solution is in alkalescence, insoluble in ethanol, acetone and ether.Hygroscopicity is strong, and exposure can inhale in atmosphere
Carbon dioxide and moisture are received, is changed into saleratus, should pack.Hydrate has a water thing, two water things, three water things.Carbonic acid
Aqueous solutions of potassium is in alkalescence.Insoluble in ethanol and ether.
Choose tin oxide, niobium pentaoxide, sodium carbonate, potassium carbonate etc. and transparent lead-free piezoelectric ceramics material is prepared as raw material
Material, be conducive to obtaining the ceramic material of larger optical index, high photoelectric coefficient and two grades of Clock Multiplier Factors, it is to avoid traditional
Heavy metal element lead in piezoelectric ceramics, the harm brought to environment and human body is more environmentally friendly.
Some embodiments of the present invention also provide a kind of preparation method of transparent lead-free piezoceramic material.Including following
Step：
S1, according to chemical formula (Na1-x-y-zKzLiyCax)Nb1-xSnxO3, wherein x=0.02~0.08, y=0.02~
0.10, z=0.35~0.55, in Na, K, Li, Ca, Nb and Sn mol ratio calculate oxide spinel sodium, potassium carbonate, carbonic acid
Lithium, calcium carbonate, the mass fraction of niobium pentaoxide and tin oxide, sodium carbonate, carbon are weighed according to the mass fraction of plurality of raw materials
Sour potassium, lithium carbonate, calcium carbonate, niobium pentaoxide and tin oxide, calcine after load weighted plurality of raw materials is mixed and are made.
Specifically, corresponding oxide spinel sodium, potassium carbonate, lithium carbonate, calcium carbonate, five are calculated according to above-mentioned chemical formula
The mol ratio of two niobiums and tin oxide is aoxidized, the mass fraction of each raw material is then calculated again, and then correspondence weighs material carbon
Sour sodium, potassium carbonate, lithium carbonate, calcium carbonate, niobium pentaoxide and tin oxide, in case follow-up calcining step.
Further, 700~950 DEG C of calcining heat.Specifically, by each above-mentioned raw material by weighing, mixing, grind
Mill, dry, after be placed in high temperature furnace and calcine, and select 700~950 DEG C of calcining heat.Within the scope of above-mentioned temperature, not only
It can calcine and obtain good transparent lead-free piezoceramic material, and not result in the waste of the energy.
Further, during to each above-mentioned raw material by grinding, the average grain diameter of each raw material is ground to by selection
Less than 5 μm.When the average grain diameter of each raw material is respectively less than 5 μm, the melting homogenizing of each raw material in calcining is advantageously allowed.
Further, the obtained transparent lead-free piezoceramic material of calcining is pulverized powder material, particle diameter is less than 1 μm.
Transparent lead-free piezoceramic material made from above-mentioned calcining is ground to form into dusty material of the particle diameter less than 1 μm contributes to
Follow-up sheeting operation.
S2, add adhesive in dusty material obtained above, granulation compacting obtains flaky material.
Specifically, organic binder is added in above-mentioned dusty material, by granulation, be compressed into tablet form.
In an optional embodiment of the invention, above-mentioned organic binder selection polyvinyl butyral resin.
Polyvinyl butyral resin is dissolved in methanol, normal propyl alcohol, isopropanol, n-amyl alcohol, phenmethylol, butanol, diacetone alcohol, and the third two
Alcohol ether/methyl ether/propyl ether, acetone, MEK, cyclohexanone, dichloromethane, chloroform, methyl acetate, ethyl acetate, butyl acetate,
Acetic acid etc..With excellent flexibility and flexibility.
Obtained dusty material is bonded using polyvinyl butyral resin, performance is stable, adhesive effect is good, to powder
The pollution of powder material is small, in follow-up high-temperature process, it is readily volatilized fall, so as to provide favourable guarantee for follow-up operation.
It should be understood that in other optional embodiments of the invention, above-mentioned organic binder can also be according to actual need
Select other adhesives commonly used in the art.
Further, above-mentioned sheet sample is handled in high temperature furnace, organic binder is reacted completely and vapor away.
It should be understood that specific treatment temperature when being handled in above-mentioned high temperature furnace, can be according to specifically chosen different
Bonding agent, selects suitable temperature to carry out high-temperature process.
S3, vacuum hotpressing processing is carried out to above-mentioned flaky material obtain the first material, temperature is 950~1050 DEG C, pressure
More than 5MPa.
Specifically, in an optional embodiment of the invention, the sheet sample of organic binder will be removed, is put into Vacuum Heat
Press in sintering furnace, first vacuumize, open heating after pressure is less than 100Pa, programming rate is not higher than 20 DEG C/min, final temperature
For 950~1050 DEG C, then start pressurization, pressure is more than 5MPa.
S4, carry out hot pressed sintering under oxygen atmosphere to the first above-mentioned material, wherein the pressure of oxygen is that 1 standard is big
Air pressure, 1080~1180 DEG C of sintering temperature, pressure is more than 5MPa during sintering.
Specifically, in an optional embodiment of the invention, the sample that above-mentioned process vacuum hotpressing is handled is in purity oxygen
Hot pressed sintering under atmosphere, pressure is more than 5MPa, and oxygen pressure is 1 standard atmospheric pressure, 1080~1180 DEG C of sintering temperature.
By above-mentioned step, in pressure sintering process, two-step method is employed, i.e., vacuum adds at a lower temperature first
Pressure sintering, then leads to oxygen pressure sintering under nominal sintering temperature, and effect is better than common pressure sintering method, what sintering was obtained
The compact structure of transparent lead-free piezoceramic material, without obvious stomata.
S5, the transparent lead-free piezoceramic material sanding and polishing that will be obtained by hot pressed sintering.
It should be understood that above-mentioned polishing and polishing can select the common polishing of this area according to the actual needs, throw
The specific method of light.
The feature and performance to the present invention are described in further detail with reference to embodiments：
Embodiment 1
A kind of transparent lead-free piezoceramic material that the present embodiment is provided.
Chemical formula (the Na of the transparent lead-free piezoceramic material0.61K0.35Li0.02Ca0.02)Nb0.98Sn0.02O3。
The transparent lead-free piezoceramic material is made by following steps：To sodium carbonate, potassium carbonate, lithium carbonate, calcium carbonate,
Niobium pentaoxide and tin oxide, weigh, mix, grind, dry, by average grain diameter control in below 5m.Mixed-powder is existed
Calcined in high temperature furnace, temperature is 700 DEG C.Powder after calcining is placed in ball mill and grinds, dry, average grain diameter is controlled in 1 μ
Below m.Polyvinyl butyral resin organic binder is added in above-mentioned powder, by granulation, is compressed into tablet form.By above-mentioned sheet
Sample is handled in high temperature furnace, organic binder is reacted completely and is vapored away.The sheet sample of organic binder will be removed, be put into
In vacuum sintering funace, first vacuumize, open heating after pressure is less than 100Pa, programming rate is not higher than 20 DEG C/min, most
Finishing temperature is 950 DEG C, then starts pressurization, and pressure is more than 5MPa.The sample that above-mentioned process vacuum hotpressing is handled is in purity oxygen
Hot pressed sintering under atmosphere, pressure is more than 5MPa, and oxygen pressure is 1 standard atmospheric pressure, 1080 DEG C of sintering temperature.By above-mentioned sample two
Face sanding and polishing, that is, transparent lead-free piezoelectric ceramics needed for obtaining.
Embodiment 2
A kind of transparent lead-free piezoceramic material that the present embodiment is provided.
Chemical formula (the Na of the transparent lead-free piezoceramic material0.27K0.55Li0.10Ca0.08)Nb0.92Sn0.08O3。
The transparent lead-free piezoceramic material is made by following steps：To sodium carbonate, potassium carbonate, lithium carbonate, calcium carbonate,
Niobium pentaoxide and tin oxide, weigh, mix, grind, dry, by average grain diameter control in below 5m.Mixed-powder is existed
Calcined in high temperature furnace, temperature is 950 DEG C.Powder after calcining is placed in ball mill and grinds, dry, average grain diameter is controlled in 1 μ
Below m.Polyvinyl butyral resin organic binder is added in above-mentioned powder, by granulation, is compressed into tablet form.By above-mentioned sheet
Sample is handled in high temperature furnace, organic binder is reacted completely and is vapored away.The sheet sample of organic binder will be removed, be put into
In vacuum sintering funace, first vacuumize, open heating after pressure is less than 100Pa, programming rate is not higher than 20 DEG C/min, most
Finishing temperature is 1050 DEG C, then starts pressurization, and pressure is more than 5MPa.The sample that above-mentioned process vacuum hotpressing is handled is in purity oxygen
Hot pressed sintering under atmosphere, pressure is more than 5MPa, and oxygen pressure is 1 standard atmospheric pressure, 1180 DEG C of sintering temperature.By above-mentioned sample two
Face sanding and polishing, that is, transparent lead-free piezoelectric ceramics needed for obtaining.
Embodiment 3
A kind of transparent lead-free piezoceramic material that the present embodiment is provided.
Chemical formula (the Na of the transparent lead-free piezoceramic material0.5K0.4Li0.05Ca0.05)Nb0.95Sn0.05O3。
The transparent lead-free piezoceramic material is made by following steps：To sodium carbonate, potassium carbonate, lithium carbonate, calcium carbonate,
Niobium pentaoxide and tin oxide, weigh, mix, grind, dry, by average grain diameter control in below 5m.Mixed-powder is existed
Calcined in high temperature furnace, temperature is 800 DEG C.Powder after calcining is placed in ball mill and grinds, dry, average grain diameter is controlled in 1 μ
Below m.Polyvinyl butyral resin organic binder is added in above-mentioned powder, by granulation, is compressed into tablet form.By above-mentioned sheet
Sample is handled in high temperature furnace, organic binder is reacted completely and is vapored away.The sheet sample of organic binder will be removed, be put into
In vacuum sintering funace, first vacuumize, open heating after pressure is less than 100Pa, programming rate is not higher than 20 DEG C/min, most
Finishing temperature is 1000 DEG C, then starts pressurization, and pressure is more than 5MPa.The sample that above-mentioned process vacuum hotpressing is handled is in purity oxygen
Hot pressed sintering under atmosphere, pressure is more than 5MPa, and oxygen pressure is 1 standard atmospheric pressure, 1100 DEG C of sintering temperature.By above-mentioned sample two
Face sanding and polishing, that is, transparent lead-free piezoelectric ceramics needed for obtaining.
Embodiment 4
A kind of transparent lead-free piezoceramic material that the present embodiment is provided.
The chemical formula Na of the transparent lead-free piezoceramic material0.45K0.45Li0.06Ca0.04)Nb0.96Sn0.04O3。
The transparent lead-free piezoceramic material is made by following steps：To sodium carbonate, potassium carbonate, lithium carbonate, calcium carbonate,
Niobium pentaoxide and tin oxide, weigh, mix, grind, dry, by average grain diameter control in below 5m.Mixed-powder is existed
Calcined in high temperature furnace, temperature is 900 DEG C.Powder after calcining is placed in ball mill and grinds, dry, average grain diameter is controlled in 1 μ
Below m.Polyvinyl butyral resin organic binder is added in above-mentioned powder, by granulation, is compressed into tablet form.By above-mentioned sheet
Sample is handled in high temperature furnace, organic binder is reacted completely and is vapored away.The sheet sample of organic binder will be removed, be put into
In vacuum sintering funace, first vacuumize, open heating after pressure is less than 100Pa, programming rate is not higher than 20 DEG C/min, most
Finishing temperature is 1000 DEG C, then starts pressurization, and pressure is more than 5MPa.The sample that above-mentioned process vacuum hotpressing is handled is in purity oxygen
Hot pressed sintering under atmosphere, pressure is more than 5MPa, and oxygen pressure is 1 standard atmospheric pressure, 1100 DEG C of sintering temperature.By above-mentioned sample two
Face sanding and polishing, that is, transparent lead-free piezoelectric ceramics needed for obtaining.
Experimental example one
Embodiments of the invention 1 are prepared with transparent lead-free piezoceramic material and is scanned Electronic Speculum sign.Obtain
The profile scanning electron microscope of bright lead-free piezoceramic material.Specifically, it refer to Fig. 1.It can be seen that the present embodiment system
For obtaining, transparent lead-free piezoceramic material compactness is good, and density reaches more than the 99% of solid density.Dense micro-structure, nothing
Obvious stomata.
Experimental example two
Embodiments of the invention 2 are prepared with transparent lead-free piezoceramic material and investigates piezoelectric property.Specifically, test
Embodiments of the invention 2 prepare the piezoelectric coefficient d of transparent lead-free piezoceramic material33.Specifically, it refer to Fig. 2.From figure
In as can be seen that the present embodiment prepare transparent lead-free piezoceramic material piezoelectric property it is good, piezoelectric coefficient d33Reach
More than 250pC/N.Fig. 2 compares individually doping LiNbO3With LiNbO3、CaSnO3Piezoelectric modulus pair when two kinds of materials are co-doped with
Than two groups of data are all from optimal doping ratio, it is seen that the LiNbO that this programme is used3、CaSnO3The side that two kinds of materials are co-doped with
Case can significantly improve piezoelectric property.
Experimental example three
Embodiments of the invention 3 are prepared with transparent lead-free piezoceramic material and investigates transmitance.Specifically, this is tested
The embodiment 3 of invention prepares the transmitance of transparent lead-free piezoceramic material.Fig. 3 is refer to, Fig. 3 compares independent doping
LiNbO3With LiNbO3、CaSnO3Transmitance contrast when two kinds of materials are co-doped with, thickness of sample 0.5mm, two groups of data are all from most
Good doping ratio, and employ identical sintering scheme, i.e., a traditional step pressure sintering scheme, it is seen that this programme is used
LiNbO3、CaSnO3The scheme that two kinds of materials are co-doped with can significantly improve the transmitance of ceramics.
Experimental example four
Embodiments of the invention 4 are prepared with transparent lead-free piezoceramic material and traditional sintering method progress pair
Than.Specifically, Fig. 4 is refer to, is sintered using 2 steps, ceramic transmitance can be significantly improved.Embodiment 4 prepares transparent lead-free
Piezoceramic material, thickness is 0.5mm, and (400~760nm) optimum transmission (is better than for 16~47% in visible-range
The 15 of conventional pressurized sintering~45%), the transmitance at near-infrared 2500nm (is sintered more than 80% better than conventional pressurized
69%).
In summary, transparent lead-free piezoceramic material for providing of the present invention and preparation method thereof, is devised a kind of new
Lead-free piezoceramic material, consisting of (Na1-x-y-zKzLiyCax)Nb1-xSnxO3(wherein x=0.02~0.08, y=0.02~
0.10, z=0.35~0.55), the material easy-sintering, the transmitance to light is high, and piezoelectric property is good.Employ a kind of two new steps
The method of sintering, i.e., vacuum pressed is sintered at a lower temperature first, and oxygen pressure sintering, effect are then led under nominal sintering temperature
Fruit is better than common pressure sintering method.
Embodiments described above is a part of embodiment of the invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of transparent lead-free piezoceramic material, it is characterised in that the chemical formula of the transparent lead-free piezoceramic material
(Na1-x-y-zKzLiyCax)Nb1-xSnxO3, wherein x=0.02~0.08, y=0.02~0.10, z=0.35~0.55.
2. transparent lead-free piezoceramic material according to claim 1, it is characterised in that the transparent lead-free piezoelectric ceramics
Material is mainly made up of plurality of raw materials, and the plurality of raw materials includes：Sodium carbonate, potassium carbonate, lithium carbonate, calcium carbonate, five oxidations two
Niobium and tin oxide.
3. a kind of preparation method of transparent lead-free piezoceramic material, it is characterised in that according to chemical formula (Na1-x-y-zKzLiyCax)
Nb1-xSnxO3, wherein x=0.02~0.08, y=0.02~0.10, z=0.35~0.55, in Na, K, Li, Ca, Nb and
Sn mol ratio calculates the quality point of oxide spinel sodium, potassium carbonate, lithium carbonate, calcium carbonate, niobium pentaoxide and tin oxide
Number, the sodium carbonate, the potassium carbonate, the lithium carbonate, the carbon are weighed according to the mass fraction of the plurality of raw materials
Sour calcium, the niobium pentaoxide and the tin oxide, calcine after the load weighted plurality of raw materials is mixed and are made.
4. the preparation method of transparent lead-free piezoceramic material according to claim 3, it is characterised in that calcining heat
700~950 DEG C.
5. the preparation method of transparent lead-free piezoceramic material according to claim 4, it is characterised in that the carbonic acid
Sodium, the potassium carbonate, the lithium carbonate, the calcium carbonate, the niobium pentaoxide and the tin oxide average grain diameter it is equal
Less than 5 μm.
6. the preparation method of transparent lead-free piezoceramic material according to claim 5, it is characterised in that calcining is made
The transparent lead-free piezoceramic material pulverize powder material, particle diameter is less than 1 μm.
7. the preparation method of transparent lead-free piezoceramic material according to claim 6, it is characterised in that in the powder
Adhesive is added in material, granulation compacting obtains flaky material.
8. the preparation method of transparent lead-free piezoceramic material according to claim 7, it is characterised in that to the sheet
Material carries out vacuum hotpressing processing and obtains the first material, and temperature is 950~1050 DEG C, and pressure is more than 5MPa.
9. the preparation method of transparent lead-free piezoceramic material according to claim 8, it is characterised in that to described first
Material carries out hot pressed sintering under oxygen atmosphere, and the pressure of the oxygen is 1 standard atmospheric pressure, sintering temperature 1080~1180
DEG C, pressure is more than 5MPa.
10. the preparation method of transparent lead-free piezoceramic material according to claim 9, it is characterised in that will be through overheat
The transparent lead-free piezoceramic material sanding and polishing that pressure sintering is obtained.
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