CN105601286A - Erbium ytterbium-doped potassium lithium tantalite niobate ceramic and preparation method thereof - Google Patents
Erbium ytterbium-doped potassium lithium tantalite niobate ceramic and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses an erbium ytterbium-doped potassium lithium tantalite niobate ceramic and a preparation method thereof. The method is as below: weighing potassium carbonate, lithium carbonate, tantalum oxide and niobium oxide powder in the molar ratio of 0.6:0.4:0.5:0.5; and adding erbium oxide (Er2O3) powder in accordance with the doping concentration of Er<3+> being 1.0 mol% and adding ytterbium oxide powder in accordance with the doping concentration of Yb<3+> being 0.1mol%-2.0mol%. The method uses a solid phase reaction for preparation of erbium ytterbium-doped potassium lithium tantalite niobate ceramic in a groundbreaking way, fills the gaps in this research home and abroad, and realizes controllable sintering of erbium ytterbium-doped ceramic; and the ceramic has high sintering density, and good formation effect.
Description
Technical field
The present invention relates to a kind of erbium ytterbium tantalum doping potassium niobate lithium pottery and preparation method thereof, belong to ceramic material technology neckTerritory.
Background technology
Utilize the solid state light emitter of transition effects acquisition short-wave long light-emitting on rare earth ion in High-Density Holographic Storage, panchromatic aobviousShow, the extensive use in the field such as photoetching and spectroscopy promoted the progress of various rare earth ion doped materials. Rare earth Er3+ToolHaving good red-green glow up-conversion luminescence performance is the study hotspot in rare earth luminescence field. Rare Earth Y b3+There is large 980nmNear photoabsorption cross-section and and the good advantage of other ion ability matching degree, be widely used in rare earth ion sensitized luminescence,Work to strengthen rare earth luminescence. Meanwhile, on rare earth ion switch technology to host material require lowly, can make rare earthIon doping is realized Laser output as working-laser material in crystal, glass or even liquid.
Potassium tantalate-niobate lithium (K1-yLiyTa1-xNbxO3, KLTN) and be potassium tantalate lithium (K1-xLixTaO3) and lithium potassium niobate (K1- xLixNbO3) solid solution, be at potassium tantalate-niobate (KTa1-xNbxO3) develop by substitute element modification on the basis of crystal.Ca-Ti ore type potassium tantalate-niobate lithium is opened at photoelectricity because have large diffraction efficiency, fast response time and special mechanism of ammonium fixationThere is very large application prospect in pass and Hologram Storage field. Tungsten bronze type potassium tantalate-niobate lithium has outstanding second harmonic generation propertyCan, be mainly used in laser freuqency doubling field. The work in our early stage is carried out rear-earth-doped and frequency to potassium tantalate-niobate crystalline lithiumThe research of changing in rate. The preparation of potassium tantalate-niobate lithium is more difficult, and growth conditions is had relatively high expectations, and therefore needs to develop neomorphMaterial carry out rear-earth-doped research.
Summary of the invention
Object: for solving the deficiencies in the prior art, the present invention carries out erbium ytterbium tantalum doping potassium niobate lithium pottery has been carried out to groupPoint and the research of manufacture craft, a kind of erbium ytterbium tantalum doping potassium niobate lithium pottery and preparation method thereof is provided.
Technical scheme: for solving the problems of the technologies described above, the technical solution used in the present invention is:
The preparation method of erbium ytterbium tantalum doping potassium niobate lithium pottery, is characterized in that, utilizes solid reaction process, comprises the following steps:Step 1) batching: potash (K2CO3), lithium carbonate (Li2CO3), tantalum oxide (Ta2O5), niobium oxide (Nb2O5) powder is according to 0.6:The molar ratio weigh batching of 0.4:0.5:0.5, and be Er according to doping content respectively3+1.0mol% adds erbium oxide(Er2O3) powder and doping content be Yb3+: 0.1mol%-2.0mol% adds ytterbium oxide powder;
The K wherein using2CO3、Li2CO3、Ta2O5And Nb2O5The molar ratio of powder is erbium ytterbium tantalum doping potassium niobate lithium potteryThe primary condition of preparation success or failure.
Step 2), grind, obtain powder;
Step 3), compressing tablet: use hydraulic press powder is pressed into material piece;
Pre-burning: pack material piece into corundum crucible, put into Muffle furnace, be warming up to 100 DEG C with 150 DEG C/h, and keep 30min;Be warming up to 800-950 DEG C with 150 DEG C/h, and keep 6-10h; Be cooled to room temperature with 200 DEG C/h, complete pre-burning process. This processMake raw material carry out sufficient chemical reaction.
Step 4), regrind: the material piece after pre-burning is placed in agate mortar, smashs to pieces, grinds; Add anhydrous secondAlcohol, is ground to absolute ethanol volatilizes clean, repeatedly repeats; Splash into certain polyvinyl alcohol (PVA) solution, be ground to polyethyleneAlcoholic solution volatilization is clean; Add again absolute ethyl alcohol, be ground to absolute ethanol volatilizes clean, put into drying baker and dry;
Step 5), compressing tablet granulation: powder is pressed into material piece, places some hours;
Sieve: material piece is smashed to pieces, through 150 orders and the screening of 200 object sieves, obtained the raw material of granularity between 75 μ m～106 μ mParticle; To obtain evengranular crystal grain.
Step 6), sintering: by step 5) process the feed particles that obtains and take 0.8g/ part, compressing tablet; Pack corundum crucible into,Put into Muffle furnace, be warming up to 100 DEG C with 150 DEG C/h, and keep 30min; Be warming up to 500～600 DEG C with 150 DEG C/h, and protectHold 4～6h, carry out mixed powder binder removal; Be warming up to 1180～1190 DEG C with 150 DEG C/h, and keep 4～6h; Fall with 200 DEG C/hTemperature, to room temperature, completes sintering process, obtains erbium ytterbium tantalum doping potassium niobate lithium pottery.
Step 1) in, the purity of potash, lithium carbonate, tantalum oxide, niobium oxide, erbium oxide and ytterbium oxide is all not less than99.9%. In embodiment, the doping content of preferential oxidation ytterbium is Yb3+Doping 0.5mol%, 1.0mol% and 2.0mol%.
Step 2) in, grind and specifically refer to: mixed powder is put into agate mortar, grind; Add absolute ethyl alcoholGrind, until absolute ethanol volatilizes is clean, repeat to add absolute ethyl alcohol grinding operation three times, to ensure that powder can grind and mixEvenly, the powder after grinding is put into corundum crucible, put into drying baker and dry, the pottery growth mixed powder that obtains being dried.This step in triplicate object is to make raw material fully grind and mix.
Step 3) in, in compressing tablet process, hydraulic press pressure is 20Pa, keeps one minute.
Step 4) in, regrind specifically refers to: the material piece after pre-burning is placed in agate mortar, smashs to pieces, be ground toWithout bulky grain; Add 10ml absolute ethyl alcohol, grind more than one hour, until absolute ethanol volatilizes is clean, repeat to add 10ml withoutTwice of water-ethanol grinding operation; Splash into concentration and be 20 of 5% polyvinyl alcohol (PVA) solution, be ground to solution evaporation clean; AddEnter 10ml absolute ethyl alcohol, be ground to absolute ethanol volatilizes clean, put into drying baker and dry.
Material piece after pre-burning is carried out to regrind process, and add therein 20 of polyvinyl alcohol (PVA) solution to riseAdhesive effect, object is to make the raw material sintering in follow-up sintering process, obtain more uniform more greatly crystal grain.
Erbium ytterbium tantalum doping potassium niobate lithium pottery provided by the invention, adopts above-mentioned erbium ytterbium tantalum doping potassium niobate lithium potteryPreparation method makes, and crystal structure is Tetragonal tungsten bronze type.
Beneficial effect: in the present invention, that utilizes solid reaction process initiative prepares erbium ytterbium tantalum doping potassium niobate lithium pottery, fills outMend the blank in this research both at home and abroad; Can realize the controlled sintering of erbium ytterbium doped ceramics, and ceramic sintered compactSpend very highly, become porcelain effect fine. The relative technique of the method is simple in addition, does not use special equipment, does not need special atmosphere growth,The features such as environmentally safe. The method has played heavy for extensive preparation and the application of rear-earth-doped potassium tantalate-niobate lithium potteryThe impetus of wanting. Utilize ripe solid reacting method can carry out the preparation of potassium tantalate-niobate lithium pottery, and technique is simple, becomesThis is lower, and sample physical and chemical performance is stable, and in addition, the rare earth ion of the higher concentration that can adulterate in pottery, conveniently carries outThe structure of high concentration rare earth ion doping pottery and luminescent properties research. Therefore the present invention utilizes solid phase reaction method to carry out rare earthEr3+/Yb3+The potassium tantalate-niobate lithium pottery preparation technology of doping, and obtained good achievement.
Brief description of the drawings
Fig. 1 is the preparation flow figure of erbium ytterbium tantalum doping potassium niobate lithium pottery;
Fig. 2 is the powder X-ray RD ideograph of erbium ytterbium tantalum doping potassium niobate lithium ceramics sample;
Fig. 3 is SEM surface and cross-section morphology figure: (a) (b) of erbium ytterbium tantalum doping potassium niobate lithium ceramics sample1mol％Er3+/0.5mol％Yb3+:KLTN；(c)(d)1mol％Er3+/1mol％Yb3+:KLTN；(e)(f)1mol％Er3+/2mol％Yb3+: KLTN pottery;
Fig. 4 is the up-conversion fluorescence spectrogram of erbium ytterbium tantalum doping potassium niobate lithium ceramics sample under 975nm laser excitation.
Detailed description of the invention
Below in conjunction with example, the present invention is illustrated:
Embodiment 1:
As shown in Figure 1, erbium tantalum doping potassium niobate lithium pottery is prepared by following steps:
One, batching: the potash (K that purity is 99.99%2CO3), lithium carbonate (Li2CO3), tantalum oxide (Ta2O5) and niobium oxide(Nb2O5) powder weighs three parts of 10g batchings according to the molar ratio of 0.6:0.4:0.5:0.5, in every part of raw material according to Er3+RubYou ratio 1mol% adds erbium oxide (Er2O3) powder, in first part of raw material respectively according to Yb3+Molar ratio 0.5mol% addsEnter ytterbium oxide (Yb2O3) powder is mixed with ceramic raw materials;
Two, grind: mixed powder is put into agate mortar, be ground to without large particle. Add 10ml absolute ethyl alcohol, grindMill is more than one hour, until absolute ethanol volatilizes is clean. This operation will be in triplicate, to ensure that powder can grind and mix allEven. Powder after grinding is put into corundum crucible, put into drying baker and dry, obtain dry mixed-powder raw material;
Three, compressing tablet: use hydraulic press that powder is pressed into the material piece that diameter is 30mm, hydraulic press pressure is 20Pa, keeps a pointClock. Pre-burning: pack material piece into corundum crucible, put into Muffle furnace, be warming up to 100 DEG C with 150 DEG C/h, and keep 30min. With150 DEG C/h is warming up to 800-950 DEG C, and keeps 6-10h. Be cooled to room temperature with 200 DEG C/h, complete pre-burning process;
Four, regrind: the material piece after pre-burning is placed in agate mortar, smashs to pieces, be ground to without bulky grain. Add 10ml withoutWater-ethanol, grinds more than one hour, until absolute ethanol volatilizes is clean, this operation repeats twice. Splash into concentration and be 5% poly-second20 of enol (PVA) solution, are ground to solution evaporation clean. Add 10ml absolute ethyl alcohol, be ground to absolute ethanol volatilizes clean,Putting into drying baker dries;
Five, compressing tablet granulation: powder is pressed into the material piece that diameter is 30mm, places some hours. Sieve: material piece is smashed to pieces,Through 150 orders and the screening of 200 object sieves, obtain the feed particles of granularity between 75 μ m～106 μ m. The excessive process again of particle is groundMill sieves again. The granulation of compressing tablet again that particle is too small, then smashs to pieces after sieve, repeats this and is operated to all powders and all accords withClose granularity requirements;
Six, sintering: by step 5) process the feed particles that obtains and take 0.8g/ part, compressing tablet, diameter is 13.5mm; Pack corundum intoCrucible, puts into Muffle furnace, is warming up to 100 DEG C with 150 DEG C/h, and keeps 30min; Be warming up to 500～600 DEG C with 150 DEG C/h,And keep 4～6h, carry out mixed powder binder removal; Be warming up to 1180 DEG C with 150 DEG C/h, and keep 4～6h; Lower the temperature with 200 DEG C/hTo room temperature, complete sintering process, obtain erbium ytterbium tantalum doping potassium niobate lithium pottery.
Seven, pottery is characterized, comprise that X-ray diffraction (XRD), SEM (SEM) and 975nm exciteConversion fluorescence spectrum.
Embodiment 2: present embodiment and embodiment 1 difference are in step 1, change Yb3+Concentration is 1.0mol%.
Embodiment 3: present embodiment and embodiment 1 difference are in step 1, change Yb3+Concentration is 2.0mol%.
Embodiment 4: present embodiment and embodiment 1 difference are in step 1, along with the increasing of rare earth ytterbium ion concentrationAdd, sintering temperature rises to 1190 DEG C by 1180 DEG C.
The pictorial diagram of preparing sample, is respectively Yb3+Doping content is 0.5mol%, the sample of 1.0mol% and 2.0mol%Product, Yb3+Doping content is that the color sample of 2.0mol% is turned to be yellow a little, illustrates that sintering temperature is higher a little.
Fig. 2 is the powder X-ray RD ideograph that makes sample, and the diffraction pattern of pottery does not increase and occurs with rear-earth-doped concentrationObviously change. This diffraction pattern shows that pottery has tungsten bronze crystal structure, and ceramic structure cell belongs to 4mm point group, P4/mbmSpace group, ceramic cell parameter is
Fig. 3 Er3+/Yb3+: SEM surface and the cross-section morphology figure of KLTN ceramics sample, sample Yb3+ConcentrationBe respectively 0.5mol%, 1.0mol% and 2.0mol%. Can find out from left-hand face photo, sample grain shape is inhomogeneous,Large-size particle is still cuboid, but the mean size of crystal grain is obviously than singly mixing Er3+KLTN sample little, and mixAssorted Yb3+Uniform crystal particles variation after concentration increases, crystallite dimension diminishes, and sintering effect reduces. Can from the section photograph on right sideFind out, the transgranular fracture phenomenon of sample is more obvious, illustrates that the rising of doping with rare-earth ions concentration has affected ceramic knotCrystalline condition. Experimental result shows, along with the rising of doping with rare-earth ions concentration, the desirable sintering temperature of pottery reduces. PotteryThe demonstration of low power SEM photo, the rear-earth-doped concentration of sample is higher, and the porosity is also higher. This is mainly because actual sintered temperature is inclined to one sideHeight, while making sintering, the component volatilization of sample is more serious, causes pore to increase.
Fig. 4 is the up-conversion fluorescence spectrogram that utilizes 975nm semiconductor laser to excite, and crystal has very strong at 548nm placeGreen emitting, has emitting red light at 665nm place, at 850nm place substantially without infraluminescence. And, three duplicate samples at this point,Along with doping Yb3+The increase of concentration, up-conversion fluorescence intensity increases thereupon, and red light-emitting intensity becomes compared with green luminescence intensityMore greatly.
Below disclose the present invention with preferred embodiment, so it is not intended to limiting the invention, and all employings are equal to replacementOr the technical scheme that equivalent transformation mode obtains, within all dropping on protection scope of the present invention.
Claims (7)
1. the preparation method of erbium ytterbium tantalum doping potassium niobate lithium pottery, is characterized in that, utilizes solid reaction process, comprises following stepRapid:
Step 1), batching: potash, lithium carbonate, tantalum oxide, niobium oxide powder are according to the molar ratio of 0.6:0.4:0.5:0.5Weigh batching, and be Er according to doping content respectively3+It is Yb that 1.0mol% adds erbium oxide powder and doping content3+:0.1mol%-2.0mol% adds ytterbium oxide powder;
Step 2), grind, obtain powder;
Step 3), compressing tablet: use hydraulic press that powder is pressed into material piece;
Pre-burning: pack material piece into corundum crucible, put into Muffle furnace, be warming up to 100 DEG C with 150 DEG C/h, and keep 30min;Be warming up to 800-950 DEG C with 150 DEG C/h, and keep 6-10h; Be cooled to room temperature with 200 DEG C/h, complete pre-burning process;
Step 4), regrind: the material piece after pre-burning is placed in agate mortar, smashs to pieces, grind; Add absolute ethyl alcohol, grindBe milled to absolute ethanol volatilizes clean, repeatedly repeat; Splash into certain polyvinyl alcohol (PVA) solution, be ground to polyvinyl alcohol moltenLiquid volatilization is clean; Add again absolute ethyl alcohol, be ground to absolute ethanol volatilizes clean, put into drying baker and dry;
Step 5), compressing tablet granulation: powder is pressed into material piece, places some hours;
Sieve: material piece is smashed to pieces, through 150 orders and the screening of 200 object sieves, obtained the raw material of granularity between 75 μ m～106 μ mParticle;
Step 6), sintering: the feed particles that step 5) processing is obtained takes 0.8g/ part, compressing tablet; Pack corundum crucible into, put intoIn Muffle furnace, be warming up to 100 DEG C with 150 DEG C/h, and keep 30min; Be warming up to 500～600 DEG C with 150 DEG C/h, and keep 4～6h, carries out mixed powder binder removal; Be warming up to 1180～1190 DEG C with 150 DEG C/h, and keep 4～6h; Be cooled to chamber with 200 DEG C/hTemperature, completes sintering process, obtains erbium ytterbium tantalum doping potassium niobate lithium pottery.
2. the preparation method of erbium tantalum doping potassium niobate lithium pottery according to claim 1, is characterized in that: in step 1),The purity of potash, lithium carbonate, tantalum oxide, niobium oxide, erbium oxide and ytterbium oxide is all not less than 99.9%.
3. the preparation method of erbium ytterbium tantalum doping potassium niobate lithium pottery according to claim 1, is characterized in that: step 2)In, grind and specifically refer to: mixed powder is put into agate mortar, grind; Add absolute ethyl alcohol to grind, until anhydrous secondAlcohol volatilization is clean, repeats to add absolute ethyl alcohol grinding operation three times, to ensure that powder can grind and mix, by after grindingPowder is put into corundum crucible, puts into drying baker and dries, the pottery growth mixed powder that obtains being dried.
4. the preparation method of erbium ytterbium tantalum doping potassium niobate lithium pottery according to claim 1, is characterized in that: step 3)In, in compressing tablet process, hydraulic press pressure is 20Pa, keeps one minute.
5. the preparation method of erbium tantalum doping potassium niobate lithium pottery according to claim 1, is characterized in that: in step 4),Regrind specifically refers to: the material piece after pre-burning is placed in agate mortar, smashs to pieces, be ground to without bulky grain; Add 10mlAbsolute ethyl alcohol, grinds more than one hour, until absolute ethanol volatilizes is clean, repeats to add 10ml absolute ethyl alcohol grinding operation twoInferior; Splash into concentration and be 20 of 5% poly-vinyl alcohol solutions, be ground to solution evaporation clean; Add 10ml absolute ethyl alcohol, be ground toAbsolute ethanol volatilizes is clean, puts into drying baker and dries.
6. erbium ytterbium tantalum doping potassium niobate lithium pottery, adopts the erbium ytterbium tantalum doping potassium niobate lithium pottery described in claim 1-5 any oneThe preparation method of porcelain makes.
7. erbium ytterbium tantalum doping potassium niobate lithium pottery according to claim 1, is characterized in that: described erbium ytterbium doping tantalum niobic acidPotassium lithium pottery is Tetragonal tungsten bronze crystal structure.
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| CN107176837A (en) * | 2017-05-31 | 2017-09-19 | 哈尔滨理工大学 | A kind of preparation method of ultra-high dielectric coefficient potassium tantalate-niobate ceramics |
| CN114014653A (en) * | 2021-12-10 | 2022-02-08 | 山东省科学院新材料研究所 | Preparation method of potassium tantalate niobate ceramic chip with adjustable dielectric constant |
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| CN107176837B (en) * | 2017-05-31 | 2019-12-06 | 哈尔滨理工大学 | Preparation method of potassium tantalate niobate ceramic with ultrahigh dielectric constant |
| CN114014653A (en) * | 2021-12-10 | 2022-02-08 | 山东省科学院新材料研究所 | Preparation method of potassium tantalate niobate ceramic chip with adjustable dielectric constant |
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Application publication date: 20160525 |