CN109384465A - A kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics - Google Patents
A kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics, is related to no lead base piezoelectric material field.The present invention is by Sm2O3, Na2CO3, K2CO3, Nb2O5According to, by dry-pressing compression molding, the sinter molding at 1150~1170 DEG C obtains near infrared region highest light transmittance up to 61% samarium doping potassium-sodium niobate crystalline ceramics after the ratio mixing of 0.007~0.079:0.199:0.26:1 of weight ratio.The present invention adulterates (K by adopting the above technical scheme, by Sm0.5Na0.5)NbO3, the high xSm- (K of available molding consistency0.5Na0.5)NbO3Crystalline ceramics, prepared ceramics have counterfeit cubic structure and higher light transmittance；And the good combination of ferroelectricity, optics and photoluminescence property, achieves multifunction；xSm-(K0.5Na0.5)NbO3Part lead base crystalline ceramics can be substituted, problem of environmental pollution is not only reduced, while can also ensure that good electric property.
Description
Technical field
The present invention relates to no lead base piezoelectric material field more particularly to a kind of preparations of samarium doping potassium-sodium niobate crystalline ceramics
Method.
Background technique
Ferroelectric ceramics refer to certain dielectrics can spontaneous polarization, spontaneous polarization energy reorientation shows under the action of an external electric field
As claiming ferroelectric effect.Main ferroelectric ceramics system has barium titanate-calcium stannate and barium titanate-barium zirconate system high dielectric constant ferroelectricity
Ceramics, the barium titanate-low ferroelectric ceramics of bismuth stannate system change in dielectric constant rate, barium titanate-calcium zirconate-niobium zirconium acid bismuth and metatitanic acid
It barium-barium stannate system high pressure ferroelectric ceramics and more bismuth titanates and its makes pottery with the system solid solution low loss ferro-electricity of the compositions such as strontium titanates
Porcelain etc..The characteristic of ferroelectric ceramics determines its purposes.Using its high dielectric constant, capacitor, the height of large capacity can be made
Frequency button capacitor, high-voltage capacitor, stacked capacitor and semiconductor ceramic capacitor etc., capacitance may be up to 0.45 μ F/
cm2。
Transparent ferroelectric ceramics is found a view in photoelectron, pyroelectric electric device, photoswitch, optical printer, colour camera
The fields such as device, reflected displaying device and the storage of photoelectricity ferroelectricity image cause extensive research.Ferroelectricity crystalline ceramics combines iron
The electrology characteristic of electric body and the transparency of material, are exploited for adaptive optics, optical integrated circuit, optical resonantor and micro-
Wave device.For comprehensively considering for environmental pollution and climate change etc., people start widely to study a kind of novel
The response of bloom electric frequency and holographic storage material.Currently, plumbum-based material has been widely used in the application of photoelectric controller,
Including some piezoelectric membranes.In all photoelectric controllers, the first ferroelectricity crystalline ceramics is lead lanthanum zirconate titanate in the world
(PLZT), light transmittance is in near-infrared up to 70%.But since the oxide of lead can generate volatilization in process, to human body
And environmental pollution.
(K0.5Na0.5)NbO3 (KNN) ceramic Curie temperature height and big electromechanical coupling factor are that a kind of performance is more excellent
Lead-free ferroelectric material.Pure KNN usually has the orthorhombic crystal phase of low symmetry, and is difficult to be made up of traditional approach
Crystalline ceramics, although the ceramic photoelectric properties of traditional KNN are very good, light transmittance is low, and dielectric constant is low, bad mechanical strength.
Summary of the invention
In view of this, the present invention provides a kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics, tapping can be prepared
The crystalline ceramics that the characteristics such as electricity/dielectric, optics and luminescence generated by light are integrated, and production process is pollution-free.
The present invention is a kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics, comprising the following steps:
(1) ingredient: by Sm2O3, Na2CO3, K2CO3, Nb2O5According to the ratio of 0.007~0.079:0.199:0.26:1 of weight ratio
Ball milling is carried out after example mixing, obtains mixed powder；
The process of ball milling can refine powder, while various materials being mixed more evenly, wet-milling can be used, in mixture
Middle addition ball-milling medium is simultaneously fitted into progress 9~12 h of ball milling in ball grinder, and the revolving speed of ball milling is 150~280 r/min, and ball milling is situated between
Matter can be ethyl alcohol, Er2O3、Na2CO3、K2CO3、Nb2O5、La2O3Gross mass and ethyl alcohol weight ratio be 1:2~1:3.Ball milling
After, mixture is dried, drying temperature is 80~85 DEG C；
(2) pre-burning: the mixture after above-mentioned grinding is added in crucible, after being compacted, is placed in Muffle furnace, is warming up to 800
~850 DEG C and 3~6 h of heat preservation carry out pre-burning, and the heating rate of pre-burning is 3~5 DEG C/min, then again after cooled to room temperature
Crucible is taken out.Pre-burning is to improve purity, and despumation makes stable crystal form get off, at the same can also reduce burn eventually when
Between, the process of pre-burning is that solid-state reaction occurs to will affect so the time of pre-burning is critically important in the preparation process of transparent glass
The growth of crystal grain into next step sintering process；
(3) secondary ball milling: the mixed powder Jing Guo pre-burning is subjected to ball milling, sieving, obtaining chemical composition general formula is xSm-
(K0.5Na0.5)NbO3Powder, x=0.5~6%；
Toward above-mentioned after ball-milling medium is added in the mixture of pre-burning, then it is loaded into ball grinder and carries out ball milling, ball milling
Revolving speed is 150~280 r/min, and Ball-milling Time is 7~10 h, after ball milling, mixture is dried at 80~85 DEG C, then
Obtaining chemical composition general formula after the sieving of the sieve of 80~100 mesh again is xSm- (K0.5Na0.5)NbO3Powder；
(4) tabletting: granulating agent is added in the powder, and the polyethylene that mass fraction is 5~12 wt% can be used in granulating agent
Then alcoholic solution is placed in baking oven dry, drying temperature 90-130 by poly-vinyl alcohol solution after powder is uniformly mixed again
DEG C, then the sieving of the sieve through 80~100 mesh, xSm- (K is made0.5Na0.5)NbO3Pellet；It will under the pressure of 200~300 MPa
xSm-(K0.5Na0.5)NbO3Pellet is pressed into the green compact of 0.8~1.5 mm of thickness；Above-mentioned green compact are placed in pallet and are covered, so
After be put into Muffle furnace, 700~850 DEG C at a temperature of heat preservation 1~3 h carry out dumping, then again by it with furnace natural cooling
To room temperature；
(5) it is sintered: by the xSm- (K0.5Na0.5)NbO3Green compact keep the temperature 6~9 h at 1150 ~ 1170 DEG C, obtain samarium doping niobium
Sour potassium sodium crystalline ceramics.
The present invention adulterates (K by adopting the above technical scheme, by Sm0.5Na0.5)NbO3, available molding consistency is high
xSm-(K0.5Na0.5)NbO3Crystalline ceramics, prepared ceramics have counterfeit cubic structure and higher light transmittance；And ferroelectricity,
The good combination of optics and photoluminescence property, achieves multifunction；xSm-(K0.5Na0.5)NbO3Part lead can be substituted
Base transparent ceramic not only reduces problem of environmental pollution, while can also ensure that good electric property.
Detailed description of the invention
Fig. 1 is the Sm- (K provided in the embodiment of the present invention 40.5Na0.5)NbO3The XRD diagram of crystalline ceramics sample；
Fig. 2 is the Sm- (K provided in the embodiment of the present invention 40.5Na0.5)NbO3The light transmittance figure of crystalline ceramics sample；
Fig. 3 is the Sm- (K provided in the embodiment of the present invention 40.5Na0.5)NbO3Sterogram after the polishing of crystalline ceramics sample；
Fig. 4 is the Sm- (K provided in the embodiment of the present invention 40.5Na0.5)NbO3The SEM of crystalline ceramics sample schemes；
Fig. 5 is the Sm- (K provided in the embodiment of the present invention 40.5Na0.5)NbO3The luminescent spectrum of crystalline ceramics sample.
Specific embodiment
The present invention will be described in detail With reference to embodiment.
Embodiment 1
A kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics, comprising the following steps:
(1) ingredient: by 0.07g Sm2O3, 1.99g Na2CO3, 2.6g K2CO3, 10g Nb2O5Ball milling is carried out after mixing, is obtained
Mixed powder；
Ball milling: adding mixture into ball-milling medium, is fitted into progress 9 h of ball milling in ball grinder, and rotational speed of ball-mill is 150 r/min, ball
After mill, mixture is placed in baking oven and is dried with 85 DEG C of temperature, and then mixture is put into mortar again and is ground
Mill, abrasive media are ethyl alcohol, and the weight ratio of mixture and ethyl alcohol is 1:3.
(2) pre-burning: the mixture after above-mentioned grinding is added in crucible, after being compacted, is placed in Muffle furnace, with 3 DEG C/
The heating rate of min, which is warming up to 800 DEG C and keeps the temperature 3 h, carries out pre-burning, then again takes out crucible after cooled to room temperature.
(3) secondary ball milling: toward above-mentioned after ball-milling medium is added in the mixture of pre-burning, then it is loaded into ball grinder
In, carry out 7 h of ball milling, the revolving speed of ball milling is 150 r/min, after ball milling, mixture is dried, is then sieved again through sieve
Afterwards, it can be prepared by powder, chemical composition general formula is 0.005Sm- (K0.5Na0.5)NbO3；
(4) tabletting: the poly-vinyl alcohol solution that 5 wt% are added toward above-mentioned powder is uniformly mixed, and is then placed in again in baking oven at 90 DEG C
It is dry, then through being sieved through 80 mesh screens；Treated, and powder is added in mold, depresses to thickness 0.8 in the pressure of 200 MPa
The green compact of mm；Above-mentioned green compact are placed in pallet and are covered, are then placed in Muffle furnace, 700 DEG C at a temperature of keep the temperature 1 h into
Row dumping, then again by it with furnace cooled to room temperature；Obtain 0.005Sm- (K0.5Na0.5)NbO3Green compact.
(5) it is sintered: green compact being placed in Muffle furnace, 6 h are sintered at 1150 DEG C, then cooled to room temperature
Samarium doping potassium-sodium niobate crystalline ceramics is made.
Performance test
By ceramics sample wear down and it is polished to 0.3 mm, surveys its light transmittance, test result shows the light transmission when wavelength is 900 nm
Rate is 58%.Its relative dielectric constant is 1115.
Embodiment 2
A kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics, comprising the following steps:
(1) ingredient: by 0.112g Sm2O3, 1.99g Na2CO3, 2.6g K2CO3, 10g Nb2O5Ball milling is carried out after mixing, is obtained
Mixed powder；
Ball milling: adding mixture into ball-milling medium, is fitted into progress ball milling 12h in ball grinder, and rotational speed of ball-mill is 280 r/min, ball
After mill, mixture is placed in baking oven and is dried with 80 DEG C of temperature, and then mixture is put into mortar again and is ground
Mill, abrasive media are ethyl alcohol, and the weight ratio of mixture and ethyl alcohol is 1:2.
(2) pre-burning: the mixture after above-mentioned grinding is added in crucible, after being compacted, is placed in Muffle furnace, with 5 DEG C/
The heating rate of min, which is warming up to 850 DEG C and keeps the temperature 6 h, carries out pre-burning, then again takes out crucible after cooled to room temperature.
(3) secondary ball milling: toward above-mentioned after ball-milling medium is added in the mixture of pre-burning, then it is loaded into ball grinder
In, carry out 10 h of ball milling, the revolving speed of ball milling is 150 r/min, after ball milling, mixture is dried, then again through sieve mistake
After sieve, powder can be prepared by, chemical composition general formula is 0.008Sm- (K0.5Na0.5)NbO3；
(4) tabletting: the poly-vinyl alcohol solution that 12 wt% are added toward above-mentioned powder is uniformly mixed, and is then placed in baking oven again 130
DEG C drying, then through being sieved through 100 mesh screens；Treated, and powder is added in mold, depresses to thickness 1.5 in the pressure of 300MPa
The green compact of mm；Above-mentioned green compact are placed in pallet and are covered, are then placed in Muffle furnace, 850 DEG C at a temperature of keep the temperature 3 h into
Row dumping, then again by it with furnace cooled to room temperature；Obtain 0.008Sm- (K0.5Na0.5)NbO3Green compact.
(5) it is sintered: green compact being placed in Muffle furnace, 9 h are sintered at 1170 DEG C, then cooled to room temperature
Samarium doping potassium-sodium niobate crystalline ceramics is made.
Performance test
By ceramics sample wear down and it is polished to 0.3 mm, surveys its light transmittance, test result shows the light transmission when wavelength is 900 nm
Rate is 60%.Its relative dielectric constant is 1122.
Embodiment 3
A kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics, comprising the following steps:
(1) ingredient: by 0.79g Sm2O3, 1.99g Na2CO3, 2.6g K2CO3, 10g Nb2O5Ball milling is carried out after mixing, is obtained
Mixed powder；
Ball milling: adding mixture into ball-milling medium, is fitted into progress ball milling 10h, rotational speed of ball-mill 250r/min, ball milling in ball grinder
After, mixture is placed in baking oven and is dried with 83 DEG C of temperature, and then mixture is put into mortar again and is ground,
Abrasive media is ethyl alcohol, and the weight ratio of mixture and ethyl alcohol is 1:2.5.
(2) pre-burning: the mixture after above-mentioned grinding is added in crucible, after being compacted, is placed in Muffle furnace, with 4 DEG C/
The heating rate of min, which is warming up to 820 DEG C and keeps the temperature 4 h, carries out pre-burning, then again takes out crucible after cooled to room temperature.
(3) secondary ball milling: toward above-mentioned after ball-milling medium is added in the mixture of pre-burning, then it is loaded into ball grinder
In, carry out 8 h of ball milling, the revolving speed of ball milling is 200 r/min, after ball milling, mixture is dried, is then sieved again through sieve
Afterwards, it can be prepared by powder, chemical composition general formula is 0.06Sm- (K0.5Na0.5)NbO3；
(4) tabletting: the poly-vinyl alcohol solution that 10 wt% are added toward above-mentioned powder is uniformly mixed, and is then placed in baking oven again 110
DEG C drying, then through being sieved through 90 mesh screens；Treated, and powder is added in mold, depresses to thickness 1.0 in the pressure of 250MPa
The green compact of mm；Above-mentioned green compact are placed in pallet and are covered, are then placed in Muffle furnace, 820 DEG C at a temperature of keep the temperature 2 h into
Row dumping, then again by it with furnace cooled to room temperature；Obtain 0.06Sm- (K0.5Na0.5)NbO3Green compact.
(5) it is sintered: green compact being placed in Muffle furnace, 8 h are sintered at 1160 DEG C, then cooled to room temperature
Samarium doping potassium-sodium niobate crystalline ceramics is made.
Performance test
By sample wear down and it is polished to 0.3 mm, surveys its light transmittance, test result shows that light transmittance is when wavelength is 900 nm
55%.Its relative dielectric constant is 1074.
Embodiment 4
A kind of preparation method of Er ions potassium-sodium niobate-strontium titanates crystalline ceramics, comprising the following steps:
(1) ingredient: by 0.21g Sm2O3, 1.99g Na2CO3, 2.6g K2CO3, 10g Nb2O5Ball milling is carried out after mixing, is obtained
Mixed powder.
Ball milling: adding mixture into ball-milling medium, is fitted into progress 10 h of ball milling in ball grinder, and rotational speed of ball-mill is 200 r/
Min, after ball milling, mixture is placed in baking oven and is dried with 85 DEG C of temperature, and then mixture is put into mortar again
It is ground, abrasive media is ethyl alcohol, and the weight ratio of mixture and ethyl alcohol is 1:3.
(2) pre-burning: the mixture after above-mentioned grinding is added in crucible, after being compacted, is placed in Muffle furnace, with 3.5
DEG C/heating rate of min is warming up to 850 DEG C and keeps the temperature 4 h and carry out pre-burning, then crucible is taken after cooled to room temperature again
Out.
(3) secondary ball milling: toward above-mentioned after ball-milling medium is added in the mixture of pre-burning, then it is loaded into ball grinder
In, 8 h of ball milling is carried out, after ball milling, mixture is dried, then again after sieve is sieved, can be prepared by powder, chemistry
Composition general formula is 0.015Sm- (K0.5Na0.5)NbO3。
(4) tabletting: the poly-vinyl alcohol solution that 6 wt% are added toward above-mentioned powder is uniformly mixed, and is then placed in baking oven and is done again
Dry, drying temperature is 100 DEG C, then the net through sieving 100 mesh is sieved；Treated, and powder is added in mold, in the pressure of 250 MPa
Depress to the green compact of 1.2 mm of thickness；Above-mentioned green compact are placed in pallet and are covered, are then placed in Muffle furnace, at 800 DEG C
At a temperature of keep the temperature 2 h carry out dumping, then again by it with furnace cooled to room temperature.
(5) it is sintered: treated green compact being placed in Muffle furnace, 7 h are sintered at 1160 DEG C, are then naturally cooled to
Room temperature can be prepared by samarium doping potassium-sodium niobate crystalline ceramics.
Performance test
By ceramics sample wear down and it is polished to 0.3 mm, surveys its light transmittance, test result shows the light transmission when wavelength is 900 nm
Rate is 61%.Its relative dielectric constant is 1136.
0.015Sm- (the K that embodiment 4 obtains0.5Na0.5)NbO3The XRD diagram of crystalline ceramics sample, light transmittance figure, polishing
Sterogram, SEM and fluorescence emission spectra afterwards is distinguished as shown in Figs. 1-5.Fig. 1 shows, obtained ceramics sample is pure counterfeit
Cubic perovskite structure, almost without miscellaneous phase appearance；The potsherd light transmittance figure obtained after Fig. 2 display sintering, near infrared region
Light transmittance reach 62%；Ceramics sample figure after Fig. 3 display polishing, it can be seen that sample has good light transmittance, surveys with Fig. 2
Test result is consistent；The surface SEM of the potsherd obtained after Fig. 4 display sintering, it can be seen that crystallite dimension is tiny (< 400 nm)
And be evenly distributed, shape reduces the scattering of light, maintains higher light transmittance close to the higher Cubic structure of symmetry；
Fig. 5 shows that the sample has preferable photoluminescence property, under the excitation of 407 nm, can generate4G5/2→6H5/2
(562 nm)、4G5/2→6H7/2 (598 nm)、4G5/2→6H9/2 (645 nm) three kinds of transition, respectively two green lights and a tangerine
Light emitting.
The raw material Sm2O3, Na2CO3, K2CO3And Nb2O5It is that analysis is pure.
The present invention adulterates (K by adopting the above technical scheme, by Sm0.5Na0.5)NbO3, available molding consistency is high
xSm-(K0.5Na0.5)NbO3Crystalline ceramics, prepared ceramics have counterfeit cubic structure and higher light transmittance；And ferroelectricity,
The good combination of optics and photoluminescence property, achieves multifunction；xSm-(K0.5Na0.5)NbO3Part lead can be substituted
Base transparent ceramic not only reduces problem of environmental pollution, while can also ensure that good electric property, transparent for environmentally friendly piezoelectricity
The industrialized production of ceramic material has established theory and practice basis.
Present invention process step is simple, reproducible, easily operated, can be applied to the smart phone and touch screen of environment-friendly type
Etc. new electronic product and adaptive optics, optical integrated circuit, the devices such as optical resonantor.
The present invention is not limited to above-mentioned specific embodiment, and the invention may be variously modified and varied.All foundations
Technical spirit of the invention should be included in the present invention to embodiment of above any modification, equivalent replacement, improvement and so on
Protection scope.
Claims (9)
1. a kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics, which comprises the following steps:
(1) ingredient: by Sm2O3, Na2CO3, K2CO3, Nb2O5, it is 0.007~0.079:0.199:0.26:1's according to weight ratio
Ball milling is carried out after ratio mixing, obtains mixed powder；
(2) pre-burning: by the mixed powder in 800~850 DEG C of progress pre-burnings；
(3) secondary ball milling: the mixed powder Jing Guo pre-burning is subjected to ball milling, sieving, obtaining chemical composition general formula is xSm-
(K0.5Na0.5)NbO3Powder, x=0.5~6%；
(4) tabletting: granulating agent is added in the powder, and xSm- (K is made0.5Na0.5)NbO3Pellet is obtained by tabletting, dumping
xSm-(K0.5Na0.5)NbO3Green compact；
(5) it is sintered: by the xSm- (K0.5Na0.5)NbO3Green compact keep the temperature 6~9 h at 1150 ~ 1170 DEG C, obtain samarium doping niobium
Sour potassium sodium crystalline ceramics.
2. a kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics according to claim 1, which is characterized in that step
(1), the revolving speed of ball milling described in step (3) is 150~280 r/min.
3. a kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics according to claim 2, which is characterized in that step
(1) time of the ball milling is 9~12 h.
4. a kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics according to claim 3, which is characterized in that step
(3) time of the ball milling is 7~10 h.
5. a kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics according to claim 1, which is characterized in that step
(4) dumping described in is in 700~850 DEG C of 1~3 h of heat preservation.
6. a kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics according to claim 5, which is characterized in that step
(4) pressure that the tabletting described in is is in 200~300 MPa.
7. a kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics according to claim 6, which is characterized in that described
xSm-(K0.5Na0.5)NbO3Green compact with a thickness of 0.8~1.5 mm.
8. a kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics according to claim 1, which is characterized in that step
(2) heating rate of the pre-burning is 3~5 DEG C/min.
9. a kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics according to claim 1, which is characterized in that step
(3) aperture of the sieve of the sieving is 80~100 mesh.
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| CN115159983B (en) * | 2022-07-01 | 2023-03-10 | 中国科学院上海硅酸盐研究所 | Sodium niobate-based relaxor antiferroelectric ceramic material and preparation method thereof |
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