CN110372380A - A method of the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth are prepared based on the tape casting - Google Patents

A method of the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth are prepared based on the tape casting Download PDF

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CN110372380A
CN110372380A CN201910660939.3A CN201910660939A CN110372380A CN 110372380 A CN110372380 A CN 110372380A CN 201910660939 A CN201910660939 A CN 201910660939A CN 110372380 A CN110372380 A CN 110372380A
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holmium
lithium
tape casting
bismuth
sodium niobate
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吴啸
鲁齐铃
林锦锋
林枞
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Fuzhou University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
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    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B3/00Producing shaped articles from the material by using presses; Presses specially adapted therefor
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    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract

The invention discloses a kind of methods for preparing the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth based on the tape casting, prepare Ho first3+、Li+、Bi5+Adulterate (K0.5Na0.5)NbO3Powder carries out pressureless sintering by casting molding processes at 1170~1200 DEG C, can be prepared by the 0.5Ho-KNN-6LB luminescence transparent ceramics of no miscellaneous phase, compact structure, uniform small grains.The sample has the multi-functional characteristics such as good translucency and up-conversion luminescence.Present device simple process, easily operated, high production efficiency, and ceramic thickness is controllable, can prepare multi-functional ferroelectricity crystalline ceramics, further expand the preparation method of the Quito KNN function crystalline ceramics.

Description

It is a kind of that the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth are prepared based on the tape casting Method
Technical field
The present invention relates to Lead-free transparent ceramic material fields, more particularly to one kind to prepare holmium/lithium/bismuth based on the tape casting and be modified The method of potassium-sodium niobate luminescence transparent ceramics.
Background technique
The ferroelectricity crystalline ceramics that shines is a kind of multifunctional material, not only has excellent ferroelectricity, piezoelectricity, fluorescence, transparent etc. Characteristic, also have both excellent mechanical performance, chemical stability and high temperature resistant, it is corrosion-resistant the advantages that, be widely used in intelligent electricity Son/optical device, such as electronic curtain, optical filter, photoswitch, optical modulator etc..1971, Haertling and Land The first ferroelectricity crystalline ceramics in the world: the lead zirconate titanate (PLZT) of La doped has been prepared using hot pressed sintering, has been had excellent Electrooptic effect and good light transmittance, enable ferroelectricity crystalline ceramics fast development.But lead base crystalline ceramics has high Lead content (more than 60wt%), the volatilization of lead can cause certain injury to human body and environment in preparation process.Therefore, it develops Environmentally friendly lead-free replaces leaded ferroelectricity transparent ceramic material commercial to be at present trend of the times.
Potassium-sodium niobate (K0.5Na0.5)NbO3 (KNN) base ceramics are a kind of materials for being expected to substitution lead base crystalline ceramics.KNN Base ceramics Curie temperature with higher and preferable electromechanical coupling characteristics, it is also more deep to its research at present.Preparation The forming method of KNN base ceramics includes dry-pressing formed and tape casting, wherein tape casting be it is a kind of be suitable for preparing it is single-phase or The more effective technique of complex phase ceramic thin slice is conducive to the thickness for controlling potsherd, relatively thin potsherd can be prepared; There is apparatus and process simple, high production efficiency simultaneously, can operate continuously and flaw size is small, steady performance.But Research in terms of the tape casting prepares ferroelectricity crystalline ceramics is almost without report, and mainly have following reason: 1. in preparation process In generally require that a large amount of organic matter is added, need strict control technological parameter, be otherwise easy for generate cracking, curling, thickness Phenomena such as unevenly and being not easily stripped;2. needing to formulate a suitable sintering procedure, because having in sintering process a large amount of Organic matter volatilization and alkali metal ion volatilization, will affect sintering effect;3. the potsherd compactness being prepared is poor, gas Hole is big and more, and through meeting after ceramics significant divergence occurs at internal porosity for light, opaque so as to cause ceramics.
Summary of the invention
In order to solve the above-mentioned technical problem, new KNN base ferroelectricity crystalline ceramics is developed, the purpose of the present invention is to provide one The method that kind prepares the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth based on the tape casting.Tool can be prepared by the method There are the 0.5Ho-KNN-6LB Lead-free transparent ceramics of excellent light transmittance and up-conversion luminescence performance.
In order to realize above-mentioned technical purpose, the technical solution of the present invention is as follows:
A method of the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth are prepared based on the tape casting, comprising the following steps:
(1) ingredient: raw material is weighed by following mass ratio, is then uniformly mixed so as to obtain mixture;Ho2O3 : K2CO3 : Na2CO3 : Li2CO3 : Bi2O3 : Nb2O5 = 0.0071 : 0.26 : 0.1998 : 0.0167 : 0.1052 : 1;
(2) ball milling: above-mentioned mixture being fitted into ball grinder and carries out 10~12 h of ball milling, and after ball milling, mixture is dried, Then mixture is put into mortar again and is ground;
(3) pre-burning: the mixture after grinding is added in crucible, after being compacted, is placed in Muffle furnace, is warming up to 800~850 DEG C and keep the temperature 3~5 h and carry out pre-burning, then crucible is taken out after cooled to room temperature again, powder is made, chemical composition is logical Formula is 0.005Ho-0.94 (K0.5Na0.5)NbO3-0.06LiBiO3
(4) slurrying: by the above-mentioned powder by pre-burning and dispersing agent triethanolamine dehydrated alcohol and butanone in the mixed solvent 8~12 h are stirred, plasticiser polyethylene glycol, dibutyl phthalate and the stirring of binder polyvinyl butyral are added later Uniformly mixed slurry is prepared in 8~12 h, then continue in draught cupboard stirring evaporate solvent, until slurry reduce to 20~30 mL;Prepare powder required when slurry, triethanolamine, polyethylene glycol, dibutyl phthalate, polyvinyl alcohol contracting The mass ratio of butyraldehyde be 1: x: y1: y2: z, wherein x=0.03~0.05, y1=0.03~0.05, y2= 0.03~0.05, z=0.08~0.10;
(5) it is cast: above-mentioned slurry is cast on casting machine, cutter height is 600~700 μm, is used after its drying Blade is removed, and curtain coating object is made;
(6) tabletting: above-mentioned curtain coating object is cut into slices, and is stacked to 10~30 thickness, is placed in mold, in 200~300 MPa Pressure depress to the green compact of 0.5~1.0 mm of thickness;
(7) dumping: above-mentioned green compact are placed in Muffle furnace, in 700~850 DEG C of at a temperature of heat preservation 1~3 h progress dumping, so Afterwards again by it with furnace cooled to room temperature;
(8) it is sintered: will be placed in Muffle furnace by the green compact of step (7) processing, 5~8 h are sintered at 1170~1200 DEG C, so Cooled to room temperature is afterwards to get the 0.5Ho-KNN-6LB crystalline ceramics prepared based on the tape casting.
As a preferred embodiment of the above technical solution, in the step (2), abrasive media is ethyl alcohol, the weight of mixture and ethyl alcohol Amount is than being 1: 2~1: 3.
As a preferred embodiment of the above technical solution, in the step (2), rotational speed of ball-mill is 250~380 rpm.
As a preferred embodiment of the above technical solution, in the step (2), drying temperature is 80~85 DEG C.
As a preferred embodiment of the above technical solution, in the step (3), the heating rate of pre-burning is 3~5 DEG C/min.
As a preferred embodiment of the above technical solution, in the step (4), the volume ratio of in the mixed solvent dehydrated alcohol and butanone It is 2: 1.
As a preferred embodiment of the above technical solution, in the step (6), wafer cutting die diameter is 12 mm.
As a preferred embodiment of the above technical solution, in the step (8), the heating rate of sintering is 0.5~1 DEG C/min.
As a preferred embodiment of the above technical solution, the raw material Ho2O3、K2CO3、Na2CO3、Li2CO3、Bi2O3And Nb2O5? It is pure to analyze.
In conclusion the invention has the following advantages:
1, the present invention is joined using casting molding processes by suitable technology by using the ceramic composition of 0.5Ho-KNN-6LB Number controls available thinner thickness and the higher unleaded luminescence transparent ceramics of consistency, the ceramics have good translucency and The characteristics such as up-conversion luminescence, alternative part lead base crystalline ceramics promote environmental protection.
2, present invention process equipment is simple, easily operated, high production efficiency, and ceramic thickness is controllable, can prepare more Function ferroelectricity luminescence transparent ceramics, have further expanded the preparation method of KNN base ferroelectricity crystalline ceramics.
Detailed description of the invention
The present invention is further elaborated with reference to the accompanying drawings and detailed description:
Fig. 1 is the XRD diagram for the 0.5Ho-KNN-6LB crystalline ceramics sample that embodiment 3 obtains;
Fig. 2 is the SEM figure for the 0.5Ho-KNN-6LB crystalline ceramics sample that embodiment 3 obtains;
Fig. 3 is the entity photo for the 0.5Ho-KNN-6LB crystalline ceramics sample that embodiment 3 obtains;
Fig. 4 is the optical transmittance figure for the 0.5Ho-KNN-6LB crystalline ceramics sample that embodiment 3 obtains;
Fig. 5 is the up-conversion luminescence spectrogram for the 0.5Ho-KNN-6LB crystalline ceramics sample that embodiment 3 obtains.
Specific embodiment
Explanation is further explained to the present invention below in conjunction with attached drawing.
Present embodiment is only explanation of the invention, is not limitation of the present invention, those skilled in the art As long as any change that member is made after having read specification of the invention is within the scope of the claims, all will be by special The protection of sharp method.
Embodiment 1
A method of the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth are prepared based on the tape casting, comprising the following steps:
(1) ingredient: raw material is weighed by following mass ratio, is then uniformly mixed so as to obtain mixture;Ho2O3 : K2CO3 : Na2CO3 : Li2CO3 : Bi2O3 : Nb2O5 = 0.0071 : 0.26 : 0.1998 : 0.0167 : 0.1052 : 1;
(2) ball milling: being fitted into 10 h of ball milling in ball grinder for above-mentioned mixture, and 300 rpm of rotational speed of ball-mill, ball-milling medium is ethyl alcohol, The weight ratio of mixture and ethyl alcohol is 1: 2.5, after ball milling, mixture is placed in baking oven and is dried with 85 DEG C of temperature It is dry, then mixture is put into mortar again and is ground;
(3) pre-burning: the mixture after grinding is added in crucible, after being compacted, is placed in Muffle furnace, with the liter of 3 DEG C/min Warm rate is warming up to 800 DEG C and keeps the temperature 3 h pre-burnings, then again takes out crucible after cooled to room temperature, 0.5Ho- is made KNN-6LB powder;
(4) slurrying: by the above-mentioned powder by pre-burning and dispersing agent triethanolamine dehydrated alcohol and butanone in the mixed solvent 8 h are stirred, plasticiser polyethylene glycol, dibutyl phthalate and binder polyvinyl butyral are added later and stirs 8 h Uniformly mixed slurry is prepared, then continuing stirring in draught cupboard evaporates solvent, until slurry is reduced to 20 mL; Prepare the quality of powder required when slurry, triethanolamine, polyethylene glycol, dibutyl phthalate, polyvinyl butyral Than being 1: x: y1: y2: z, wherein x=0.03, y1=0.03, y2=0.03, z=0.08, in the mixed solvent The volume ratio of dehydrated alcohol and butanone is 2: 1;
(5) it is cast: above-mentioned slurry is cast on casting machine, cutter height is 600 μm, covers crystallising dish with anti-gray Dirt is scraped down after its drying with blade, and curtain coating object is made;
(6) above-mentioned curtain coating object: being cut into the disk of 12 mm of diameter by tabletting with wafer cutting die, and is folded thickness 10, is placed in mold In, the green compact of about 0.5 mm of thickness are depressed in the pressure of 200 MPa;
(7) dumping: being placed in above-mentioned green compact in crucible and cover, be then placed in Muffle furnace, 700 DEG C at a temperature of keep the temperature 2 H carries out dumping, then again by it with furnace cooled to room temperature;
(8) it is sintered: will be placed in Muffle furnace by the green compact of step (7) processing, 5 h are sintered at 1170 DEG C, it is then naturally cold But to room temperature to get the 0.5Ho-KNN-6LB crystalline ceramics prepared based on the tape casting.
Performance test:
Ceramics sample is polished to 0.3 mm, tests its light transmittance, test result shows the light transmittance when wavelength is about 900 nm It is 38%.
Embodiment 2
A method of the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth are prepared based on the tape casting, comprising the following steps:
(1) ingredient: raw material is weighed by following mass ratio, is then uniformly mixed so as to obtain mixture;Ho2O3 : K2CO3 : Na2CO3 : Li2CO3 : Bi2O3 : Nb2O5 = 0.0071 : 0.26 : 0.1998 : 0.0167 : 0.1052 : 1;
(2) ball milling: being fitted into 10 h of ball milling in ball grinder for above-mentioned mixture, and 380 rpm of rotational speed of ball-mill, ball-milling medium is ethyl alcohol, The weight ratio of mixture and ethyl alcohol is 1: 2.5, after ball milling, mixture is placed in baking oven and is dried with 85 DEG C of temperature It is dry, then mixture is put into mortar again and is ground;
(3) pre-burning: the mixture after above-mentioned grinding is added in crucible, after being compacted, is placed in Muffle furnace, with 3 DEG C/min Heating rate be warming up to 800 DEG C and keep the temperature 4 h pre-burnings, then crucible is taken out after cooled to room temperature again, be made 0.5Ho-KNN-6LB powder;
(4) slurrying: by the above-mentioned powder by pre-burning and dispersing agent triethanolamine dehydrated alcohol and butanone in the mixed solvent 10 h are stirred, plasticiser polyethylene glycol, dibutyl phthalate and binder polyvinyl butyral stirring 10 are added later Uniformly mixed slurry is prepared in h, and then continuing stirring in draught cupboard evaporates solvent, until slurry is reduced to 25 mL; Prepare the quality of powder required when slurry, triethanolamine, polyethylene glycol, dibutyl phthalate, polyvinyl butyral Than being 1: x: y1: y2: z, wherein x=0.03, y1=0.04, y2=0.04, z=0.08, in the mixed solvent The volume ratio of dehydrated alcohol and butanone is 2: 1;
(5) it is cast: above-mentioned slurry is cast on casting machine, cutter height is 700 μm, covers crystallising dish with anti-gray Dirt is scraped down after its drying with blade, and curtain coating object is made;
(6) above-mentioned curtain coating object: being cut into the disk of 12 mm of diameter by tabletting with wafer cutting die, and is folded thickness 15, is placed in mold In, the green compact of about 0.8 mm of thickness are depressed in the pressure of 250 MPa;
(7) dumping: being placed in above-mentioned green compact in crucible and cover, be then placed in Muffle furnace, 750 DEG C at a temperature of keep the temperature 2 H carries out dumping, then again by it with furnace cooled to room temperature;
(8) it is sintered: will be placed in Muffle furnace by the green compact of step (7) processing, 5 h are sintered at 1180 DEG C, it is then naturally cold But to room temperature to get the 0.5Ho-KNN-6LB crystalline ceramics prepared based on the tape casting.
Performance test:
Ceramics sample is polished to 0.3 mm, tests its light transmittance, test result shows the light transmittance when wavelength is about 900 nm It is 40%.
Embodiment 3
A method of the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth are prepared based on the tape casting, comprising the following steps:
(1) ingredient: raw material is weighed by following mass ratio, is then uniformly mixed so as to obtain mixture;Ho2O3 : K2CO3 : Na2CO3 : Li2CO3 : Bi2O3 : Nb2O5 = 0.0071 : 0.26 : 0.1998 : 0.0167 : 0.1052 : 1;
(2) ball milling: above-mentioned mixture is fitted into progress 12 h of ball milling in ball grinder, 300 rpm of rotational speed of ball-mill, ball-milling medium is second The weight ratio of alcohol, mixture and ethyl alcohol is 1: 2.5, after ball milling, by mixture be placed in baking oven with 85 DEG C of temperature into Mixture, is then put into mortar again and grinds by row drying;
(3) pre-burning: the mixture after above-mentioned grinding is added in crucible, after being compacted, is placed in Muffle furnace, with 3 DEG C/min Heating rate be warming up to 850 DEG C and keep the temperature 4 h pre-burnings, then crucible is taken out after cooled to room temperature again, be made 0.5Ho-KNN-6LB powder;
(4) slurrying: by the above-mentioned powder by pre-burning and dispersing agent triethanolamine dehydrated alcohol and butanone in the mixed solvent 12 h are stirred, plasticiser polyethylene glycol, dibutyl phthalate and binder polyvinyl butyral stirring 12 are added later Uniformly mixed slurry is prepared in h, and then continuing stirring in draught cupboard evaporates solvent, until slurry is reduced to 25 mL; Prepare the quality of powder required when slurry, triethanolamine, polyethylene glycol, dibutyl phthalate, polyvinyl butyral Than being 1: x: y1: y2: z, wherein x=0.04, y1=0.03, y2=0.03, z=0.09, in the mixed solvent The volume ratio of dehydrated alcohol and butanone is 2: 1;
(5) it is cast: above-mentioned slurry is cast on casting machine, cutter height is 700 μm, covers crystallising dish with anti-gray Dirt is scraped down after its drying with blade, and curtain coating object is made;
(6) above-mentioned curtain coating object: being cut into the disk of 12 mm of diameter by tabletting with wafer cutting die, and is folded thickness 20, is placed in mold In, the green compact of about 1.0 mm of thickness are depressed in the pressure of 250 MPa;
(7) dumping: being placed in above-mentioned green compact in crucible and cover, be then placed in Muffle furnace, 800 DEG C at a temperature of keep the temperature 2 H carries out dumping, then again by it with furnace cooled to room temperature;
(8) it is sintered: will be placed in Muffle furnace by the green compact of step (7) processing, 5 h are sintered at 1190 DEG C, it is then naturally cold But to room temperature to get the 0.5Ho-KNN-6LB crystalline ceramics prepared based on the tape casting.
Performance test:
By ceramics sample wear down and it is polished to 0.3 mm, is then tested.
The XRD diagram for the 0.5Ho-KNN-6LB crystalline ceramics sample that embodiment 3 obtains, SEM figure, entity photo, optics penetrate Rate figure and up-conversion luminescence spectrogram difference are as shown in Figs. 1-5.Fig. 1 shows to obtain the ceramics sample with counterfeit cube of calcium titanium Mine structure, and the purity of phase is relatively high;Fig. 2 shows that the sample has well-regulated square crystal grain, and of uniform size and structure causes It is close;The sample photo shown from Fig. 3, it can be seen that sample is relatively transparent, can see beneath text more visiblely by sample Word, but casting technique uncontrollable factor is more, makes sample slightly bending and fleck occurs in surface;Fig. 4 shows that sample is thrown Light transmittance figure after light, it can be seen that light transmittance is ~ 40% when wavelength is about 900 nm, basically reaches the level of crystalline ceramics; Fig. 5 shows that there is acquired sample good Upconversion luminescence to show stronger green light under the excitation of 980 nm And red emission, it is a kind of preferable transparent up-conversion luminescent material.
Embodiment 4
A method of the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth are prepared based on the tape casting, comprising the following steps:
(1) ingredient: raw material is weighed by following mass ratio, is then uniformly mixed so as to obtain mixture;Ho2O3 : K2CO3 : Na2CO3 : Li2CO3 : Bi2O3 : Nb2O5 = 0.0071 : 0.26 : 0.1998 : 0.0167 : 0.1052 : 1;
(2) ball milling: being fitted into 12 h of ball milling in ball grinder for above-mentioned mixture, and 380 rpm of rotational speed of ball-mill, ball-milling medium is ethyl alcohol, The weight ratio of mixture and ethyl alcohol is 1: 2.5, after ball milling, mixture is placed in baking oven and is dried with 85 DEG C of temperature It is dry, then mixture is put into mortar again and is ground;
(3) pre-burning: the mixture after above-mentioned grinding is added in crucible, after being compacted, is placed in Muffle furnace, with 3 DEG C/min Heating rate be warming up to 850 DEG C and keep the temperature 3 h pre-burnings, then crucible is taken out after cooled to room temperature again, be made 0.5Ho-KNN-6LB powder;
(4) slurrying: by the above-mentioned powder by pre-burning and dispersing agent triethanolamine dehydrated alcohol and butanone in the mixed solvent 12 h are stirred, plasticiser polyethylene glycol, dibutyl phthalate and binder polyvinyl butyral stirring 12 are added later Uniformly mixed slurry is prepared in h, and then continuing stirring in draught cupboard evaporates solvent, until slurry is reduced to 20 mL; Prepare the quality of powder required when slurry, triethanolamine, polyethylene glycol, dibutyl phthalate, polyvinyl butyral Than being 1: x: y1: y2: z, wherein x=0.04, y1=0.04, y2=0.04, z=0.09, in the mixed solvent The volume ratio of dehydrated alcohol and butanone is 2: 1;
(5) it is cast: above-mentioned slurry is cast on casting machine, cutter height is 600 μm, covers crystallising dish with anti-gray Dirt is scraped down after its drying with blade, and curtain coating object is made;
(6) above-mentioned curtain coating object: being cut into the disk of 12 mm of diameter by tabletting with wafer cutting die, and is folded thickness 20, is placed in mold In, the green compact of about 0.8 mm of thickness are depressed in the pressure of 250 MPa;
(7) dumping: being placed in above-mentioned green compact in crucible and cover, be then placed in Muffle furnace, 800 DEG C at a temperature of keep the temperature 2 H carries out dumping, then again by it with furnace cooled to room temperature;
(8) it is sintered: will be placed in Muffle furnace by the green compact of step (7) processing, 5 h are sintered at 1200 DEG C, it is then naturally cold But to room temperature to get the 0.5Ho-KNN-6LB crystalline ceramics prepared based on the tape casting.
Performance test:
Ceramics sample is polished to 0.3 mm, tests its light transmittance, test result shows the light transmittance when wavelength is about 900 nm It is 35%.

Claims (9)

1. a kind of method for preparing the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth based on the tape casting, comprising the following steps:
(1) ingredient: raw material is weighed by following mass ratio, is then uniformly mixed so as to obtain mixture;Ho2O3 : K2CO3 : Na2CO3 : Li2CO3 : Bi2O3 : Nb2O5 = 0.0071 : 0.26 : 0.1998 : 0.0167 : 0.1052 : 1;
(2) ball milling: above-mentioned mixture is fitted into 10~12 h of ball milling in ball grinder, after ball milling, mixture is dried, then Mixture is put into mortar again and is ground;
(3) pre-burning: the mixture after grinding is added in crucible, after being compacted, is placed in Muffle furnace, is warming up to 800~850 DEG C and keep the temperature 3~5 h and carry out pre-burning, then crucible is taken out after cooled to room temperature again, powder is made, chemical composition is logical Formula is 0.005Ho-0.94 (K0.5Na0.5)NbO3-0.06LiBiO3, abbreviation 0.5Ho-KNN-6LB powder;
(4) slurrying: by the above-mentioned powder by pre-burning and dispersing agent triethanolamine dehydrated alcohol and butanone in the mixed solvent 8~12 h are stirred, plasticiser polyethylene glycol, dibutyl phthalate and the stirring of binder polyvinyl butyral are added later Uniformly mixed slurry is prepared in 8~12 h, then continue in draught cupboard stirring evaporate solvent, until slurry reduce to 20~30 mL;Prepare powder required when slurry, triethanolamine, polyethylene glycol, dibutyl phthalate, polyvinyl alcohol contracting The mass ratio of butyraldehyde be 1: x: y1: y2: z, wherein x=0.03~0.05, y1=0.03~0.05, y2= 0.03~0.05, z=0.08~0.10;
(5) it is cast: above-mentioned slurry is cast on casting machine, cutter height is 600~700 μm, is used after its drying Blade scrapes down, and curtain coating object is made;
(6) tabletting: above-mentioned curtain coating object is cut into slices, and is stacked to 10~30 thickness, is placed in mold, in 200~300 MPa Pressure depress to the green compact of 0.5~1.0 mm of thickness;
(7) dumping: above-mentioned green compact are placed in Muffle furnace, in 700~850 DEG C of at a temperature of heat preservation 1~3 h progress dumping, so Afterwards again by it with furnace cooled to room temperature;
(8) it is sintered: will be placed in Muffle furnace by the green compact of step (7) processing, 5~8 h are sintered at 1170~1200 DEG C, so Cooled to room temperature is afterwards to get the 0.5Ho-KNN-6LB crystalline ceramics prepared based on the tape casting.
2. a kind of the tape casting that is based on according to claim 1 prepares the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth Method, it is characterised in that: in the step (2), abrasive media is ethyl alcohol, the weight ratio of mixture and ethyl alcohol is 1: 2~ 1: 3。
3. a kind of the tape casting that is based on according to claim 1 prepares the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth Method, it is characterised in that: in the step (2), rotational speed of ball-mill be 250~380 rpm.
A kind of the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth are prepared based on the tape casting 4. according to claim 1 Method, it is characterised in that: in the step (2), drying temperature is 80~85 DEG C.
A kind of the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth are prepared based on the tape casting 5. according to claim 1 Method, it is characterised in that: in the step (3), the heating rate of pre-burning is 3~5 DEG C/min.
6. a kind of the tape casting that is based on according to claim 1 prepares the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth Method, it is characterised in that: in the step (4), the volume ratio of in the mixed solvent dehydrated alcohol and butanone is 2: 1.
A kind of the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth are prepared based on the tape casting 7. according to claim 1 Method, it is characterised in that: in the step (6), wafer cutting die diameter is 12 mm.
A kind of the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth are prepared based on the tape casting 8. according to claim 1 Method, it is characterised in that: in the step (8), the heating rate of sintering is 0.5~1 DEG C/min.
A kind of the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth are prepared based on the tape casting 9. according to claim 1 Method, it is characterised in that: the raw material Ho2O3、K2CO3、Na2CO3、Li2CO3、Bi2O3And Nb2O5It is that analysis is pure.
CN201910660939.3A 2019-07-22 2019-07-22 A method of the modified potassium-sodium niobate luminescence transparent ceramics of holmium/lithium/bismuth are prepared based on the tape casting Pending CN110372380A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113149647A (en) * 2021-06-06 2021-07-23 福州大学 Ytterbium and up-conversion rare earth luminescent ion double-doped potassium-sodium niobate thick film
CN113185287A (en) * 2021-03-30 2021-07-30 南昌大学 Potassium sodium niobate-lithium niobate piezoelectric crystal and preparation method thereof

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FR2283873A1 (en) * 1974-09-04 1976-04-02 Nippon Telegraph & Telephone HOT PRESSED FERROELECTRIC TRANSPARENT CERAMICS
CN102060540A (en) * 2009-11-16 2011-05-18 中国科学院福建物质结构研究所 Method for preparing Re:YAG polycrystalline transparent ceramic by using different molding modes
CN108840677A (en) * 2018-07-27 2018-11-20 福州大学 A kind of preparation method of holmium doped sodium potassium niobate crystalline ceramics

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FR2283873A1 (en) * 1974-09-04 1976-04-02 Nippon Telegraph & Telephone HOT PRESSED FERROELECTRIC TRANSPARENT CERAMICS
CN102060540A (en) * 2009-11-16 2011-05-18 中国科学院福建物质结构研究所 Method for preparing Re:YAG polycrystalline transparent ceramic by using different molding modes
CN108840677A (en) * 2018-07-27 2018-11-20 福州大学 A kind of preparation method of holmium doped sodium potassium niobate crystalline ceramics

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113185287A (en) * 2021-03-30 2021-07-30 南昌大学 Potassium sodium niobate-lithium niobate piezoelectric crystal and preparation method thereof
CN113149647A (en) * 2021-06-06 2021-07-23 福州大学 Ytterbium and up-conversion rare earth luminescent ion double-doped potassium-sodium niobate thick film

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Application publication date: 20191025