CN110015896A - A kind of potassium-sodium niobate-based transparent luminescent ceramic of dysprosium doped and preparation method thereof - Google Patents
A kind of potassium-sodium niobate-based transparent luminescent ceramic of dysprosium doped and preparation method thereof Download PDFInfo
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Abstract
The invention discloses potassium-sodium niobate-based transparent luminescent ceramics of a kind of dysprosium doped and preparation method thereof.Present invention rare earth dysprosium ion doped sodium potassium niobate ceramics, prepare ceramic green with solid phase method, then sinter molding, obtain transmitance up to 52%, have the potassium-sodium niobate-based transparent luminescent ceramic of good luminous performance.Present invention process step is simple, easily operated, can obtain the higher potassium-sodium niobate-based transparent luminescent ceramic of consistency.
Description
Technical field
The invention belongs to Lead-free transparent ceramic material fields, and in particular to a kind of potassium-sodium niobate-based transparent luminescent of dysprosium doped
Ceramics and preparation method thereof.
Background technique
Important composition portion of the piezoceramic material with its stable performance, the advantages that cheap cost as piezoelectric material
Point.Compared to conventional piezoelectric, ferroelectric ceramics, transparent relaxation ferroelectric ceramic is with more excellent ferroelectricity, optical property and significant
Electrooptic effect, be expected to become the critical material in the indispensable following optical computing technology and modern advanced.Transparent hair
Light ceramic has caused the extensive concern of people as potential candidate material, such as smart phone and the new electronics of touch screen produce
The optical devices guided missile such as product and high power solid state laser, high-pressure sodium lamp.
The ferroelectricity crystalline ceramics applied at present is mainly lead zirconate titanate base ceramics, ceramics containing lead base preparation, using and
In its discarded last handling process, environment and human health can be all endangered.Thus environmentally friendly lead-free ceramics become research
Hot spot.The study found that certain leadless piezoelectric ceramics also have while its electric property obtains optimization by rear-earth-doped
The good transparency and luminescent properties.Such as: Sm2O3Modified 0.948 (K0.5Na0.5)NbO3-0.052LiSbO3、
(K0.5Na0.5)Nb1-xErxO3-x/2;Nd, Dy, Ho adulterate (K0.53Na0.47)0.942Li0.058NbO3、 (K0.5Na0.5)1- xPrxNbO3；Nd, Pr, Dy doping KNLNST have obtained good optical property and excellent rare earth ion fluorescence.Its reason
After being that rare earth ion is introduced into ceramics, the f-f electric dipole transition for having broken rare earth ion itself is prohibited, so that material has Zhuo
Optical property more；In addition, the radius of rare earth ion and alkali metal ion Na+ (0.97 Å)、K+ (1.33) radius connects
Closely, so that rare earth ion is easy to replace the position the A ion of KNN base ceramics as donor ion doping, thus, effectively mention
Its high consistency, it is hereby achieved that having fluorescence property, the multifunctional material of good transparency and excellent electric property.
Summary of the invention
It is an object of the invention to reduce to environment, the pollution of resource provides a kind of niobic acid to substitute lead base crystalline ceramics
Potassium sodium base transparent luminescent ceramic and preparation method thereof.
In order to realize above-mentioned technical purpose, the technical solution of the present invention is as follows:
A kind of preparation method of the potassium-sodium niobate-based transparent luminescent ceramic of dysprosium doped, comprising the following steps:
(1) ingredient
By chemical composition general formula xDy- (K0.5Na0.5NbO3), wherein the stoichiometric ratio of x=0.25-1mol% weighs raw material
Dy2O3, Na2CO3, K2CO3, Nb2O5, be uniformly mixed so as to obtain mixing, when weighing drug, guarantee with the drug weight of electronic balance weighing with
The actual weight of calculating is all the same before decimal point third position.
(2) ball milling
Ball-milling medium is added in the mixing of step (1), mixture is placed in ball milling in ball grinder, ball milling 8-12h.Mixing ball milling
It is to guarantee that mixing is uniform, guarantee that ceramic powder granular size is suitable, shape is suitable, the good important process of size distribution.
(3) drying sieving
It will be poured into vessel after the good material sieving of step (2) ball milling, separate wet feed and abrading-ball, and the glass that wet feed will be filled
Ware is placed in 80 °C of air dry oven dry 12 h or more, dries powder, and be ground up, sieved.
(4) pre-burning
The powder that step (3) are dried is placed in Muffle furnace and keeps the temperature 3-5h progress pre-burning at 600-850 DEG C, obtains pre-burning powder
End.Pre-burning can make ceramic particle composition fix, is uniform, be not susceptible to component segregation；Secondly, occurring that powder to a certain extent
Crystallization makes ceramic print be not susceptible to obviously deform in sintering.
(5) secondary ball milling
The powder of step (4) pre-burning continues to be put into ball grinder, is put into baking oven and dries after addition ball-milling medium ball milling 8h-12h,
Taking-up mortar grinder is simultaneously sieved.
(6) it is granulated and forms
Step (5) resulting powder is put into mortar, 3-5wt%PVA is added and is granulated, then dries, is ground after taking-up equal
It is even, be placed in the steel mould of diameter 1.0cm, depress to the green compact of 1mm thickness in the pressure of 100-300MPa.
(7) dumping
Green compact prepared by step (6) are placed in Muffle furnace, keep the temperature 2h under 800 °C, so that organic matter is sufficiently volatilized and carries out dumping.
So to carry out dumping before sintering.Dumping process should formulate its process according to product size, property, type synthesis.
(8) porcelain is sintered into
It will treated that green compact are placed on Al through step (7) dumping2O3On ceramic crucible, it is placed in Muffle furnace and is sintered, it is then natural
It is cooled to room temperature, the potassium-sodium niobate-based transparent luminescent ceramic of dysprosium doped is made.The layer overlay powder energy between crucible and green compact
It effectively prevent green compact to react with crucible.
The calcining system that this experiment uses are as follows: the print pressed is put into Muffle furnace and is sintered.In 1100-1200 DEG C
Lower sintering 8-14h, then cooled to room temperature.
(9) it tests
The sample prepared is ground to after 0.3mm and carries out the test such as scanning electron microscope, ultraviolet spectra, fluorescence property.
The step (1), raw material Dy used2O3, Na2CO3, K2CO3, Nb2O5It is that analysis is pure.
In the step (2) and (5), ball-milling medium is dehydrated alcohol, and the mass ratio of mixing and dehydrated alcohol is 1:2.
The step (2) and (5), the revolving speed of ball milling are 150 ~ 280 r/min.
The step (3) and (5) use the sieve of 600-800 mesh, obtain the powder of fine uniform.
The step (4), the heating rate in burn-in process are 3 DEG C/min.
The step (8), sintering temperature are 1100-1200 DEG C, keep the temperature 8-14h.
The study found that passing through rare earth ion Dy3+ Doped sodium potassium niobate ceramics, the sintering that can preferably improve ceramics are close
Degree reaches transparent effect, has very big facilitation to crystalline ceramics is prepared, meanwhile, introduce rare earth dysprosium ion, gained sample
With good fluorescence property.The invention adopts the above technical scheme, by preparing crystalline ceramics green compact, obtains molding consistency
High transparent luminescent ceramic.Compared with existing research achievement, the invention has the benefit that
(1) pass through rare earth ion Dy3+KNN base ceramics are adulterated, potassium-sodium niobate base transparent ceramic new system is obtained.
(2) the potassium-sodium niobate-based ceramics prepared by the method for the invention, in the crystalline ceramics for obtaining high-compactness,
Make it have good luminescent properties.
Detailed description of the invention
The present invention is further elaborated with reference to the accompanying drawings and detailed description:
Fig. 1 is xDy- (K in embodiment 10.5Na0.5NbO3) (x=0.25mol%) crystalline ceramics sample section SEM figure.
Fig. 2 is xDy- (K in embodiment 20.5Na0.5NbO3) (x=0.5mol%) crystalline ceramics sample ultraviolet spectra.KNN-
Dy(0.50mol%): xDy- (K0.5Na0.5NbO3) (x=0.5mol%).
Fig. 3 is xDy- (K in embodiment 30.5Na0.5NbO3) (x=1mol%) crystalline ceramics sample polishing after sterogram.
Fig. 4 is xDy- (K in embodiment 20.5Na0.5NbO3) xDy- (K in (x=0.5mol%) and embodiment 30.5Na0.5NbO3)
The fluorescence property figure of (x=1mol%) crystalline ceramics sample.KNN-0.5% Dy:xDy- (K0.5Na0.5NbO3) (x=0.5mol%)；
KNN-1.0% Dy:xDy- (K0.5Na0.5NbO3) (x=1mol%).
Specific embodiment
A kind of preparation method of the potassium-sodium niobate-based transparent luminescent ceramic of dysprosium doped, it is characterised in that: it includes following step
It is rapid:
(1) ingredient
By chemical composition general formula xDy- (K0.5Na0.5NbO3), wherein the stoichiometric ratio of x=0.25-1mol% weighs raw material
Dy2O3, Na2CO3, K2CO3, Nb2O5, it is uniformly mixed so as to obtain mixing, when weighing drug, it is ensured that with the drug weight of electronic balance weighing
It is all the same before decimal point third position with the actual weight of calculating.
(2) ball milling
Abrasive media is added in the mixing of step (1), mixture is placed in ball milling in ball grinder, ball milling 8-12h.Mixing ball milling
It is to guarantee that mixing is uniform, guarantee that ceramic powder granular size is suitable, shape is suitable, the good important process of size distribution.
(3) drying sieving
It will be poured into vessel after the good material sieving of step (2) ball milling, separate wet feed and abrading-ball, and the glass that wet feed will be filled
Ware is placed in 80 °C of air dry oven dry 12 h or more, dries powder, sieving.
(4) pre-burning
The powder that step (3) are dried is placed in Muffle furnace and keeps the temperature 3-5h progress pre-burning at 600-850 DEG C, obtains pre-burning powder
End.Pre-burning can make ceramic particle composition fix, is uniform, be not susceptible to component segregation;Secondly, occurring that powder to a certain extent
Crystallization makes ceramic print be not susceptible to obviously deform in sintering.
(5) secondary ball milling
The powder of step (4) pre-burning continues to be put into ball grinder, and ball-milling medium is added and carries out ball milling, is put into baking after ball milling 8h-12h
It is dried in case, taking-up mortar grinder is simultaneously sieved.
(6) it is granulated and forms
Step (5) resulting powder is put into mortar, 3-5wt%PVA is added and is granulated, then dries, is ground after taking-up equal
It is even, be placed in the steel mould of diameter 1.0cm, depress to the green compact of 1mm thickness in the pressure of 100-300MPa.
(7) dumping
Green compact prepared by step (6) are placed in Muffle furnace, keep the temperature 2h under 800 °C, so that organic matter is sufficiently volatilized and carries out dumping.
So to carry out dumping before sintering.Dumping process should formulate its mistake according to the comprehensive aspect such as product size, property, type
Journey.
(8) porcelain is sintered into
It will treated that green compact are placed on Al through step (7) dumping2O3It in ceramic crucible, is placed in Muffle furnace and is sintered, then
The potassium-sodium niobate-based transparent luminescent ceramic of dysprosium doped is made in cooled to room temperature.The layer overlay powder between crucible and green compact
Material can effectively prevent green compact to react with crucible.
(9) it tests
The sample prepared is ground to progress sintering characteristic, scanning electron microscope, ultraviolet spectra, fluorescence after being polished after 0.3mm
The test such as energy.
The step (1), raw material Dy used2O3, Na2CO3, K2CO3, Nb2O5It is that analysis is pure.
In the step (2) and (5), abrasive media is dehydrated alcohol, and the mass ratio of mixing and dehydrated alcohol is 1:2.
The step (2) and (5), the revolving speed of ball milling are 150 ~ 280 r/min.
The step (3) and (5) use the sieve of 600-800 mesh, obtain the powder of fine uniform.
The step (4), the heating rate in burn-in process are 3 DEG C/min.
The step (8), sintering temperature are 1100-1200 DEG C, keep the temperature 8-14h.
Embodiment 1
(1) ingredient
By chemical composition general formula xDy- (K0.5Na0.5NbO3), wherein the stoichiometric ratio of x=0.25mol% weighs raw material
Dy2O3, Na2CO3, K2CO3, Nb2O5, it is uniformly mixed so as to obtain mixing, when weighing drug, it is ensured that with the drug weight of electronic balance weighing
It is all the same before decimal point third position with the actual weight of calculating.
(2) ball milling
The mass ratio of the addition abrasive media dehydrated alcohol in the mixing of step (1), mixing and dehydrated alcohol is 1:2.Ball milling
Revolving speed is 280 r/min, ball milling 8h.
(3) drying sieving
It will be poured into vessel after the good material sieving of step (2) ball milling, separate wet feed and abrading-ball, and the glass that wet feed will be filled
Ware is placed in 80 °C of air dry oven dry 12 h, dries the sieve of 600 mesh of powder.
(4) pre-burning
The powder that step (3) are dried is placed in Muffle furnace and keeps the temperature 5h progress pre-burning at 850 DEG C, the heating speed in burn-in process
Rate is 3 DEG C/min, obtains preburning powder.
(5) secondary ball milling
The powder of step (4) pre-burning continues to be put into ball grinder, and abrasive media dehydrated alcohol, the matter of mixing and dehydrated alcohol is added
Amount is than being 1:2.The revolving speed of ball milling is 280 r/min, is put into baking oven after ball milling 8h and dries, taking-up mortar grinder and with 600
Purpose sieve.
(6) it is granulated and forms
Powder obtained by step (5) is put into mortar, 5wt%PVA is added and is granulated, then dries, is ground after taking-up uniform.
It weighs the powder after 0.25g is granulated to be placed in the steel mould of diameter 1.0cm, depresses to the life of 1mm thickness in the pressure of 300MPa
Base.
(7) dumping
Green compact prepared by step (6) are placed in Muffle furnace, keep the temperature 2h under 800 °C, so that organic matter is sufficiently volatilized and carries out dumping.
So to carry out dumping before sintering.Dumping process should formulate its process according to product size, property, type synthesis.
(8) porcelain is sintered into
It will treated that green compact are placed on Al through step (7) dumping2O3On ceramic crucible, it is placed in Muffle furnace at 1100 DEG C and is sintered
14h, then cooled to room temperature, is made the potassium-sodium niobate-based transparent luminescent ceramic (KNN-0.25mol%Dy) of dysprosium doped.?
Layer overlay powder can effectively prevent green compact to react with crucible between crucible and green compact.
(9) it tests
The sample prepared is ground to after 0.3mm to carry out polishing to take away and surveys sintering characteristic, scanning electron microscope, ultraviolet spectra, fluorescence
Energy.Obtaining its relative density is 95.5%, and transmitance 47%, fluorescence property is good.
XDy- (K in embodiment 10.5Na0.5NbO3) (x=0.25%) crystalline ceramics sample section SEM figure, see Fig. 1.Fig. 1
SEM picture shows that sample in cross section does not have obvious crystal boundary and stomata, and consistency is higher.
Embodiment 2
(1) ingredient
By chemical composition general formula xDy- (K0.5Na0.5NbO3), wherein the stoichiometric ratio of x=0.50mol% weighs raw material
Dy2O3, Na2CO3, K2CO3, Nb2O5, it is uniformly mixed so as to obtain mixing, when weighing drug, it is ensured that with the drug weight of electronic balance weighing
It is all the same before decimal point third position with the actual weight of calculating.
(2) ball milling
The mass ratio of the addition abrasive media dehydrated alcohol in the mixing of step (1), mixing and dehydrated alcohol is 1:2.It will mixing
Material is placed in ball milling in ball grinder, and the revolving speed of ball milling is 150 r/min, ball milling 12h.
(3) drying sieving
It will be poured into vessel after the good material sieving of step (2) ball milling, separate wet feed and abrading-ball, and the glass that wet feed will be filled
Ware is placed in 80 °C of air dry oven dry 12 h or more, powder is dried, with the sieve of 800 mesh.
(4) pre-burning
The powder that step (3) are dried is placed in Muffle furnace and keeps the temperature 5h progress pre-burning at 800 DEG C, the heating speed in burn-in process
Rate is 3 DEG C/min, obtains preburning powder.
(5) secondary ball milling
The powder of step (4) pre-burning continues to be put into ball grinder, and abrasive media dehydrated alcohol, the matter of mixing and dehydrated alcohol is added
Amount is than being 1:2.The revolving speed of ball milling is 150 r/min, is put into baking oven after ball milling 12h and dries, taking-up mortar grinder and with 600
Purpose sieve.
(6) it is granulated and forms
Powder obtained by step (5) is put into mortar, 3wt%PVA is added and is granulated, then dries, is ground after taking-up uniform.
It weighs the powder after 0.25g is granulated to be placed in the steel mould of diameter 1.0cm, depresses to the life of 1mm thickness in the pressure of 100MPa
Base.
(7) dumping
Green compact prepared by step (6) are placed in Muffle furnace, keep the temperature 2h under 800 °C, so that organic matter is sufficiently volatilized and carries out dumping.
So to carry out dumping before sintering.Dumping process should formulate its process according to product size, property, type synthesis.
(8) porcelain is sintered into
It will treated that green compact are placed on Al through step (7) dumping2O3On ceramic crucible, it is placed in Muffle furnace at 1150 DEG C and is sintered
The potassium-sodium niobate-based transparent luminescent ceramic (KNN-0.5mol%Dy) of dysprosium doped is made in 8h and then cooled to room temperature.
(9) it tests
The sample prepared is ground to after 0.3mm to carry out polishing to take away and surveys sintering characteristic, scanning electron microscope, ultraviolet spectra, fluorescence
Energy.Obtaining its relative density is 97%, and transmitance 52%, fluorescence property is good.
XDy- (K in embodiment 20.5Na0.5NbO3) ultraviolet spectra of (x=0.5mol%) crystalline ceramics sample is shown in Fig. 2；Fig. 2
The transparency that potsherd is obtained after display sintering reaches 52%.
Embodiment 3
(1) ingredient
By chemical composition general formula xDy- (K0.5Na0.5NbO3), wherein the stoichiometric ratio of x=1.0mol% weighs raw material
Dy2O3, Na2CO3, K2CO3, Nb2O5, it is uniformly mixed so as to obtain mixing, when weighing drug, it is ensured that with the drug weight of electronic balance weighing
It is all the same before decimal point third position with the actual weight of calculating.
(2) ball milling
The mass ratio of the addition abrasive media dehydrated alcohol in the mixing of step (1), mixing and dehydrated alcohol is 1:2.Ball milling
Revolving speed is 280 r/min, ball milling 8h.
(3) drying sieving
It will be poured into vessel after the good material sieving of step (2) ball milling, separate wet feed and abrading-ball, and the glass that wet feed will be filled
Ware is placed in 80 °C of air dry oven dry 12 h or more, powder is dried, with the sieve of 600 mesh.
(4) pre-burning
The powder that step (3) are dried is placed in Muffle furnace and keeps the temperature 5h progress pre-burning at 750 DEG C, the heating speed in burn-in process
Rate is 3 DEG C/min, obtains preburning powder.
(5) secondary ball milling
The powder of step (4) pre-burning continues to be put into ball grinder, and abrasive media dehydrated alcohol, the matter of mixing and dehydrated alcohol is added
Amount is than being 1:2.The revolving speed of ball milling is 280 r/min, is put into baking oven after ball milling 8h and dries, taking-up mortar grinder and with 600
Purpose sieve.
(6) it is granulated and forms
Powder obtained by step (5) is put into mortar, 5wt%PVA is added and is granulated, then dries, is ground after taking-up uniform.
It weighs the powder after 0.25g is granulated to be placed in the steel mould of diameter 1.0cm, depresses to the life of 1mm thickness in the pressure of 300MPa
Base.
(7) dumping
Green compact prepared by step (6) are placed in Muffle furnace, keep the temperature 2h under 800 °C, so that organic matter is sufficiently volatilized and carries out dumping.
So to carry out dumping before sintering.Dumping process should formulate its process according to product size, property, type synthesis.
(8) porcelain is sintered into
It will treated that green compact are placed on Al through step (7) dumping2O3On ceramic crucible, it is placed in Muffle furnace at 1200 DEG C and is sintered
14h, then cooled to room temperature, is made the potassium-sodium niobate-based transparent luminescent ceramic (KNN-1.0%Dy) of dysprosium doped.In crucible
Layer overlay powder can effectively prevent green compact to react with crucible between green compact.
(9) it tests
The sample prepared is ground to after 0.3mm to carry out polishing to take away and surveys sintering characteristic, scanning electron microscope, ultraviolet spectra, fluorescence
Energy.Obtaining its relative density is 96.4%, and transmitance 48%, fluorescence property is good.
XDy- (K in embodiment 30.5Na0.5NbO3) (x=1%) crystalline ceramics sample polishing after sterogram see Fig. 3；Fig. 3 table
Bright sample has preferable light transmittance and uniformity.
XDy- (K in embodiment 20.5Na0.5NbO3) xDy- (K in (x=0.5mol%) and embodiment 30.5Na0.5NbO3) (x=
1mol%) the fluorescence property figure of crystalline ceramics sample is shown in Fig. 4；Fig. 4 shows that sample has good shine at 472nm and 573nm
Performance.
Comparative example
(1) ingredient
By chemical composition general formula K0.5Na0.5NbO3Stoichiometric ratio weigh raw material Na2CO3, K2CO3, Nb2O5, it is uniformly mixed so as to obtain
Mixing, when weighing drug, it is ensured that with the drug weight of electronic balance weighing and the actual weight of calculating in decimal point third position
It is preceding all the same.
(2) ball milling
The mass ratio of the addition abrasive media dehydrated alcohol in the mixing of step (1), mixing and dehydrated alcohol is 1:2.Ball milling
Revolving speed is 280 r/min, ball milling 8h.
(3) drying sieving
It will be poured into vessel after the good material sieving of step (2) ball milling, separate wet feed and abrading-ball, and the glass that wet feed will be filled
Ware is placed in 80 °C of air dry oven dry 12 h or more, powder is dried, with the sieve of 600 mesh.
(4) pre-burning
The powder that step (3) are dried is placed in Muffle furnace and keeps the temperature 4h progress pre-burning at 650 DEG C, the heating speed in burn-in process
Rate is 3 DEG C/min, obtains preburning powder.
(5) secondary ball milling
The powder of step (4) pre-burning continues to be put into ball grinder, and abrasive media dehydrated alcohol, the matter of mixing and dehydrated alcohol is added
Amount is than being 1:2.The revolving speed of ball milling is 280 r/min, is put into baking oven after ball milling 8h and dries, taking-up mortar grinder and with 600
Purpose sieve.
(6) it is granulated and forms
Powder obtained by step (5) is put into mortar, 5wt%PVA is added and is granulated, then dries, is ground after taking-up uniform.
It weighs the powder after 0.25g is granulated to be placed in the steel mould of diameter 1.0cm, depresses to the life of 1mm thickness in the pressure of 300MPa
Base.
(7) dumping
Green compact prepared by step (6) are placed in Muffle furnace, keep the temperature 2h under 800 °C, so that organic matter is sufficiently volatilized and carries out dumping.
So to carry out dumping before sintering.Dumping process should formulate its process according to product size, property, type synthesis.
(8) porcelain is sintered into
It will treated that green compact are placed on Al through step (7) dumping2O3On ceramic crucible, it is placed in Muffle furnace at 1100 DEG C and is sintered
8h, then cooled to room temperature, is made pure potassium sodium niobate ceramic (KNN).The layer overlay powder between crucible and green compact
Green compact can be effectively prevent to react with crucible.
(9) it tests
The sample prepared is taken away and surveys sintering characteristic, scanning electron microscope, fluorescence property.Obtaining its relative density is 92.3%, sample
Without the transparency, and unstressed configuration performance.
By example 1-3 and comparative example it is found that dysprosium ion doping improves the consistency of potassium-sodium niobate-based ceramics, make potassium niobate
Sodium base ceramics have transparent performance and fluorescence property, are expected to realize the multifunction of potassium-sodium niobate-based ceramics.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (8)
1. a kind of preparation method of the potassium-sodium niobate-based transparent luminescent ceramic of dysprosium doped, it is characterised in that: the following steps are included:
(1) ingredient
By chemical composition general formula xDy- (K0.5Na0.5NbO3), wherein the stoichiometric ratio of x=0.25-1 mol% weighs raw material
Dy2O3, Na2CO3, K2CO3, Nb2O5, it is uniformly mixed so as to obtain mixing；
(2) ball milling
Ball-milling medium is added in the mixing of step (1), mixture is placed in ball milling in ball grinder, ball milling 8-12h；
(3) drying sieving
It will be poured into vessel after the good material sieving of step (2) ball milling, separate wet feed and abrading-ball, and the glass that wet feed will be filled
Ware is placed in 80 °C of air dry oven dry 12 h or more, dries powder, sieving；
(4) pre-burning
The powder that step (3) are dried is placed in Muffle furnace and keeps the temperature 3-5h progress pre-burning at 600-850 DEG C, obtains pre-burning powder
End；
(5) secondary ball milling
The powder of step (4) pre-burning continues to be put into ball grinder, is put into baking oven and dries after addition ball-milling medium ball milling 8h-12h,
Taking-up mortar grinder is simultaneously sieved；
(6) it is granulated and forms
Powder obtained by step (5) is put into mortar, 3-5wt%PVA is added and is granulated, then dries, is ground after taking-up equal
It is even, be placed in mold, depress to the green compact of 1mm thickness in the pressure of 100-300MPa；
(7) dumping
Green compact prepared by step (6) are placed in Muffle furnace, keep the temperature 2h under 800 °C, so that organic matter is sufficiently volatilized and carries out dumping；
(8) porcelain is sintered into
It will treated that green compact are placed on Al through step (7) dumping2O3On ceramic crucible, it is placed in Muffle furnace and is sintered, it is then naturally cold
But to room temperature, the potassium-sodium niobate-based transparent luminescent ceramic of dysprosium doped is made.
2. a kind of preparation method of the potassium-sodium niobate-based transparent luminescent ceramic of dysprosium doped according to claim 1, feature
It is: raw material Dy used in the step (1)2O3, Na2CO3, K2CO3, Nb2O5It analyzes pure.
3. a kind of preparation method of the potassium-sodium niobate-based transparent luminescent ceramic of dysprosium doped according to claim 1, feature
Be: in the step (2) and (5), ball-milling medium is dehydrated alcohol, and the mass ratio of mixing and dehydrated alcohol is 1:2.
4. a kind of preparation method of the potassium-sodium niobate-based transparent luminescent ceramic of dysprosium doped according to claim 1, feature
Be: the step (2) and (5), the revolving speed of ball milling are 150 ~ 280 r/min.
5. a kind of preparation method of the potassium-sodium niobate-based transparent luminescent ceramic of dysprosium doped according to claim 1, feature
Be: the step (3) and (5) obtain the powder of fine uniform with the sieve of 600-800 mesh.
6. a kind of preparation method of the potassium-sodium niobate-based transparent luminescent ceramic of dysprosium doped according to claim 1, feature
Be: the step (4), the heating rate in burn-in process are 3 DEG C/min.
7. a kind of preparation method of the potassium-sodium niobate-based transparent luminescent ceramic of dysprosium doped according to claim 1, feature
Be: the step (8), sintering temperature are 1100-1200 DEG C, keep the temperature 8-14h.
8. a kind of potassium-sodium niobate-based transparent luminescent ceramic of the dysprosium doped of any one of claim 1-7 the method preparation.
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| CN111099896A (en) * | 2020-01-23 | 2020-05-05 | 福州大学 | Dysprosium-doped potassium sodium niobate-based transparent ceramic for white light LED and preparation method thereof |
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| JP2013043825A (en) * | 2011-08-19 | 2013-03-04 | Shenzhen Futaihong Precision Industrial Co Ltd | Transparent ceramic, method of manufacturing the same and electronic device utilizing the transparent ceramic |
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| CN109384465A (en) * | 2018-11-19 | 2019-02-26 | 福州大学 | A kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics |
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| CN101891477A (en) * | 2010-07-23 | 2010-11-24 | 中国科学院上海硅酸盐研究所 | Method for preparing circular rod-shaped RE:YAG laser transparent ceramics |
| JP2013043825A (en) * | 2011-08-19 | 2013-03-04 | Shenzhen Futaihong Precision Industrial Co Ltd | Transparent ceramic, method of manufacturing the same and electronic device utilizing the transparent ceramic |
| CN109251030A (en) * | 2018-11-19 | 2019-01-22 | 福州大学 | A kind of holmium doping potassium-sodium niobate-strontium titanates crystalline ceramics preparation method of high optics thermometer sensor DS18B20 |
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