CN105347796A - Erbium-doped potassium lithium tantalate niobate ceramic and preparation method thereof - Google Patents
Erbium-doped potassium lithium tantalate niobate ceramic and preparation method thereof Download PDFInfo
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- CN105347796A CN105347796A CN201510848616.9A CN201510848616A CN105347796A CN 105347796 A CN105347796 A CN 105347796A CN 201510848616 A CN201510848616 A CN 201510848616A CN 105347796 A CN105347796 A CN 105347796A
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Abstract
The invention discloses erbium-doped potassium lithium tantalate niobate ceramic and a preparation method thereof. The preparation method comprises the steps that potassium carbonate powder, lithium carbonate powder, tantalum oxide powder and niobium oxide powder are weighed and mixed according to the mole ratio of 0.6:0.4:0.5:0.5, erbium oxide powder is added according to the Er<3+> mono doping concentration of 0.1 mol%-1.0 mol%, the erbium-doped potassium lithium tantalate niobate ceramic is creatively prepared through a solid phase reaction method, and the green body on the research at home and abroad is filled. Existing erbium-doped ceramic sintering is controllable, high in density and good in ceramic forming effect.
Description
Technical field
The present invention relates to a kind of Er ions potassium tantalate-niobate lithium pottery and preparation method thereof, belong to technical field of ceramic material.
Background technology
The solid state light emitter utilizing rare earth ion upconversion mechanism to obtain short-wave long light-emitting facilitates the progress of various rare earth ion doped material in the widespread use in the fields such as High-Density Holographic Storage, total colouring, photoetching and spectroscopy.Rare earth Er
3+there is the study hotspot that excellent red-green glow up-conversion luminescence performance is rare earth luminescence field.Meanwhile, on rare earth ion, the requirement of switch technology to substrate material is low, can make rare earth ion dopedly in crystal, glass or even liquid, to realize Laser output as working-laser material.
Potassium tantalate-niobate lithium (K
1-yli
yta
1-xnb
xo
3, KLTN) and be potassium tantalate lithium (K
1-xli
xtaO
3) and lithium potassium niobate (K
1-xli
xnbO
3) Solid solution, be at potassium tantalate-niobate (KTa
1-xnb
xo
3) crystal basis on developed by substitute element modification.Perovskite typed potassium tantalate-niobate lithium is because have large diffraction efficiency, fast time of response and special mechanism of ammonium fixation has very large application prospect at optoelectronic switch and Hologram Storage field.Tungsten bronze type potassium tantalate-niobate lithium has outstanding second_harmonic generation performance, is mainly used in laser freuqency doubling field.We carry out research that is rear-earth-doped and frequency upooaversion to potassium tantalate-niobate crystalline lithium at the work in early stage.The preparation of potassium tantalate-niobate lithium is more difficult, requires higher to growth conditions, therefore needs the material developing new shape to carry out rear-earth-doped research.
Summary of the invention
Object: for solving the deficiencies in the prior art, the invention provides a kind of Er ions potassium tantalate-niobate lithium pottery and preparation method thereof.
Technical scheme: for solving the problems of the technologies described above, the technical solution used in the present invention is:
A preparation method for Er ions potassium tantalate-niobate lithium pottery, is characterized in that, utilize solid reaction process, comprise the following steps:
Step 1), batching: salt of wormwood (K
2cO
3), Quilonum Retard (Li
2cO
3), tantalum oxide (Ta
2o
5), niobium oxides (Nb
2o
5) powder according to the molar ratio weigh batching of 0.6:0.4:0.5:0.5, and is respectively Er according to doping content
3+singly mix 0.1mol%-1.0mol% and add Erbium trioxide (Er
2o
3) powder; The K wherein used
2cO
3, Li
2cO
3, Ta
2o
5and Nb
2o
5the molar ratio of powder is the primary condition of Er ions potassium tantalate-niobate lithium ceramic preparation success or failure.
Step 2), grinding, obtain powder;
Step 3), compressing tablet: use hydropress that powder is pressed into material piece;
Pre-burning: material piece is loaded corundum crucible, and on material piece, cover the identical powder of proportioning, put into retort 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 burn-in process; This process makes raw material carry out sufficient chemical reaction.
Step 4), regrind: the material piece after pre-burning is placed in agate mortar, smashs to pieces, grind; Add dehydrated alcohol, be ground to absolute ethanol volatilizes clean, repeatedly repetitive operation; Instill certain polyvinyl alcohol (PVA) solution, be ground to polyvinyl alcohol solution volatilization clean; Add dehydrated alcohol again, 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, obtain granularity between the feed particles of 75 μm ~ 106 μm; To obtain evengranular crystal grain.
Step 6), sintering: take feed particles 0.8g/ part that step 5) process obtains, compressing tablet, diameter is 13.5mm; Load corundum crucible, put into retort 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 2-4h, carry out the binder removal process of discharging PVA; Be warming up to 850 DEG C with 150 DEG C/h, be warming up to 1170-1175 DEG C with 60 DEG C/h, keep 4-6h; Be cooled to 800 DEG C with 40 DEG C/h, with 120 DEG C/h to room temperature, complete sintering process, obtain Er ions potassium tantalate-niobate lithium pottery.
In step 1), the purity of salt of wormwood, Quilonum Retard, tantalum oxide, niobium oxides and Erbium trioxide is not less than 99.9%.
Preferably, in step 1), the doping content of Erbium trioxide is Er
3+singly mix 0.1mol%, 0.2mol%, 0.5mol% or 1.0mol%.
Step 2) in, grinding specifically refers to: mixed powder is put into agate mortar, grinding; Add dehydrated alcohol grinding, until absolute ethanol volatilizes is clean, repeat to add dehydrated alcohol grinding operation three times, to ensure that powder can grind and mix, powder after grinding is put into corundum crucible, puts into drying baker and dry, obtain dry pottery growth mixed powder.This step in triplicate object makes raw material fully grind and mix.
In step 3), hydropress pressure is 20Pa, keeps one minute.
In step 4), regrind specifically refers to: be placed in agate mortar by the material piece after pre-burning, smash to pieces, be ground to without macrobead; Add 10ml dehydrated alcohol, grind more than one hour, until absolute ethanol volatilizes is clean, repeat to add 10ml dehydrated alcohol grinding operation twice; Instillation concentration is polyvinyl alcohol (PVA) solution 20 of 5%, is ground to solution evaporation clean; Add 10ml dehydrated alcohol, be ground to absolute ethanol volatilizes clean, put into drying baker and dry.
Regrind process is carried out to the material piece after pre-burning, and adds polyvinyl alcohol (PVA) solution 20 wherein and play adhesive effect, object be the raw material making to sinter obtain in follow-up sintering process larger evenly crystal grain.
Er ions potassium tantalate-niobate lithium pottery provided by the invention, adopt the preparation method of above-mentioned Er ions potassium tantalate-niobate lithium pottery to obtain, crystalline structure is Tetragonal tungsten bronze type.
Beneficial effect: in the present invention, what utilize solid reaction process initiative prepares Er ions potassium tantalate-niobate lithium pottery, has filled up the blank both at home and abroad in this research; Can realize the controlled sintering of Er ions pottery, and ceramic sintered compact degree is very high, becomes porcelain effect fine.The relative technique of the method is simple in addition, does not use specific equipment, does not need special atmosphere to grow, the features such as environmentally safe.The method serves important pushing effect for the extensive Synthesis and applications of rear-earth-doped potassium tantalate-niobate lithium pottery.Utilize ripe solid reacting method can carry out the preparation of potassium tantalate-niobate lithium pottery, and technique is simple, cost is lower, sample physical and chemical performance is stablized, in addition, can be adulterated the rare earth ion of higher concentration in pottery, conveniently carries out structure and the luminescent properties research of high concentration rare earth ion doping pottery.Therefore the present invention utilizes solid phase reaction method to carry out rare earth Er
3+the potassium tantalate-niobate lithium ceramic preparation technique of doping, and obtain good achievement.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure of Er ions potassium tantalate-niobate lithium pottery;
Fig. 2 is the powder X-ray RD mode chart of Er ions potassium tantalate-niobate lithium ceramics sample;
Fig. 3 is scanning electronic microscope surface and cross-section morphology figure: (a) (b) 0.1mol%Er of Er ions potassium tantalate-niobate lithium ceramics sample
3+: KLTN; (c) (d) 0.2mol%Er
3+: KLTN; (e) (f) 0.5mol%Er
3+: KLTN pottery;
Fig. 4 is the up-conversion fluorescence spectrogram of Er ions potassium tantalate-niobate lithium ceramics sample under 975nm laser excitation.
Embodiment
Below in conjunction with example, the present invention is illustrated:
embodiment 1:
As shown in Figure 1, Er ions potassium tantalate-niobate lithium pottery is prepared by following steps:
One, prepare burden: purity is the salt of wormwood (K of 99.9%
2cO
3), Quilonum Retard (Li
2cO
3), tantalum oxide (Ta
2o
5) and niobium oxides (Nb
2o
5) powder weighs 10g according to the molar ratio of 0.6:0.4:0.5:0.5 and prepare burden four parts, and adds Erbium trioxide (Er according to molar ratio 0.1mol%, 0.2mol%, 0.5mol% and 1.0mol% respectively in every part
2o
3) powder is mixed with ceramic preparation raw material;
Two, grind: mixed powder is put into agate mortar, is ground to without large particle.Add 10ml dehydrated alcohol, grind more than one hour, until absolute ethanol volatilizes is clean.This operation will in triplicate, to ensure that powder can grind and mix.Powder after grinding is put into corundum crucible, puts into drying baker and dry, obtain dry mixed powder raw material;
Three, compressing tablet: use hydropress powder to be pressed into the material piece that diameter is 30mm, hydropress pressure is 20Pa, keeps a minute.Pre-burning: material piece is loaded corundum crucible, and on material piece, cover the identical powder of proportioning, put into retort 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 burn-in process;
Four, regrind: the material piece after pre-burning is placed in agate mortar, smashs to pieces, be ground to without macrobead.Add 10ml dehydrated alcohol, grind more than one hour, until absolute ethanol volatilizes is clean, this operation repetition twice.Instillation concentration is polyvinyl alcohol (PVA) solution 20 of 5%, is ground to solution evaporation clean.Add 10ml dehydrated alcohol, be ground to absolute ethanol volatilizes clean, put into drying baker and dry;
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 granularity between the feed particles of 75 μm ~ 106 μm.Excessive again the sieving through grinding again of particle.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 meets granularity requirements;
Six, sinter: the powder handled well is taken 0.8g/ part, compressing tablet, diameter is 13.5mm.Load corundum crucible, put into retort 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 2-4h, carry out the binder removal process of discharging PVA; Be warming up to 850 DEG C with 150 DEG C/h, be warming up to 1170 DEG C with 60 DEG C/h, keep 4-6h; Be cooled to 800 DEG C with 40 DEG C/h, with 120 DEG C/h to room temperature, complete sintering process, obtain pottery.
Seven, pottery is characterized, comprise X-ray diffraction (XRD), scanning electronic microscope (SEM) and 975nm and excite up-conversion fluorescence spectrum.
Embodiment 2: present embodiment and embodiment 1 difference are in step one, changes Er
3+concentration is 0.2mol%.
Embodiment 3: present embodiment and embodiment 1 difference are in step one, changes Er
3+concentration is 0.5mol%.
Embodiment 4: present embodiment and embodiment 1 difference are in step one, changes Er
3+concentration is 1.0mol%.
Embodiment 5: present embodiment and embodiment 1 difference are in step one, and along with the increase of rare earth concentration, sintering temperature rises to 1175 DEG C by 1170 DEG C.
Fig. 2 is the powder X-ray RD mode chart of obtained sample, shows that pottery has tungsten bronze crystalline structure, and ceramic structure cell belongs to 4mm point group, P4/mbm spacer.
Fig. 3 is Er
3+: the scanning electronic microscope surface of KLTN ceramics sample and cross-section morphology figure, sample Er
3+concentration is respectively 0.1mol%, 0.2mol% and 0.5mol%.As can be seen from left-hand face photo, sample grain shape is still rectangular parallelepiped, but the mean size of crystal grain is obviously than singly mixing Er
3+kLTN sample little.As can be seen from the section photograph on right side, the transgranular fracture phenomenon of sample is more obvious, illustrates that the rising of doping with rare-earth ions concentration have impact on the crystalline condition of pottery.Experimental result shows, along with the rising of doping with rare-earth ions concentration, the desirable sintering temperature of pottery reduces.The low power SEM photo display of pottery, the rear-earth-doped concentration of sample is higher, and void content is also higher.This is mainly because actual sintered temperature drift, and when making to sinter, the component volatilization of sample is comparatively serious, causes pore to increase.
Fig. 4 is the up-conversion fluorescence spectrogram utilizing 975nm semiconductor laser to excite, and crystal has very strong green emitting at 548nm place, has emitting red light at 665nm place, has weak infraluminescence at 850nm place.Further, four increment product at this point, along with doping Er
3+the increase of concentration, up-conversion fluorescence intensity increases thereupon.
Below disclose the present invention with preferred embodiment, so it is not intended to limiting the invention, and all employings are equal to replacement or the technical scheme that obtains of equivalent transformation mode, all drop within protection scope of the present invention.
Claims (7)
1. a preparation method for Er ions potassium tantalate-niobate lithium pottery, is characterized in that, utilize solid reaction process, comprise the following steps:
Step 1), batching: salt of wormwood, Quilonum Retard, tantalum oxide, niobium oxide powder according to the molar ratio weigh batching of 0.6:0.4:0.5:0.5, and are respectively Er according to doping content
3+singly mix 0.1mol%-1.0mol% and add Erbium trioxide powder;
Step 2), grinding, obtain powder;
Step 3), compressing tablet: use hydropress that powder is pressed into material piece;
Pre-burning: material piece is loaded corundum crucible, puts into retort furnace, is warming up to 100 DEG C, and keeps 30min with 150 DEG C/h; 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 burn-in process;
Step 4), regrind: the material piece after pre-burning is placed in agate mortar, smashs to pieces, grind; Add dehydrated alcohol, be ground to absolute ethanol volatilizes clean, repeatedly repetitive operation; Instill certain polyvinyl alcohol solution, be ground to polyvinyl alcohol solution volatilization clean; Add dehydrated alcohol again, 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, obtain granularity between the feed particles of 75 μm ~ 106 μm;
Step 6), sintering: take the feed particles that step 5) process obtains, compressing tablet; Load corundum crucible, put into retort 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 2-4h; Be warming up to 850 DEG C with 150 DEG C/h, be warming up to 1170-1175 DEG C with 60 DEG C/h, keep 4-6h; Be cooled to 800 DEG C with 40 DEG C/h, with 120 DEG C/h to room temperature, complete sintering process, obtain Er ions potassium tantalate-niobate lithium pottery.
2. the preparation method of Er ions potassium tantalate-niobate lithium pottery according to claim 1, it is characterized in that: in step 1), the purity of salt of wormwood, Quilonum Retard, tantalum oxide, niobium oxides and Erbium trioxide is not less than 99.9%.
3. the preparation method of Er ions potassium tantalate-niobate lithium pottery according to claim 1, is characterized in that: step 2) in, grinding specifically refers to: mixed powder is put into agate mortar, grinding; Add dehydrated alcohol grinding, until absolute ethanol volatilizes is clean, repeat to add dehydrated alcohol grinding operation three times, to ensure that powder can grind and mix, powder after grinding is put into corundum crucible, puts into drying baker and dry, obtain dry pottery growth mixed powder.
4. the preparation method of Er ions potassium tantalate-niobate lithium pottery according to claim 1, it is characterized in that: in step 3), hydropress pressure is 20Pa, keeps one minute.
5. the preparation method of Er ions potassium tantalate-niobate lithium pottery according to claim 1, it is characterized in that: in step 4), regrind specifically refers to: be placed in agate mortar by the material piece after pre-burning, smash to pieces, be ground to without macrobead; Add 10ml dehydrated alcohol, grind more than one hour, until absolute ethanol volatilizes is clean, repeat to add 10ml dehydrated alcohol grinding operation twice; Instillation concentration is the polyvinyl alcohol solution 20 of 5%, is ground to solution evaporation clean; Add 10ml dehydrated alcohol, be ground to absolute ethanol volatilizes clean, put into drying baker and dry.
6. an Er ions potassium tantalate-niobate lithium pottery, adopts the preparation method of the Er ions potassium tantalate-niobate lithium pottery described in any one of claim 1-5 to obtain.
7. Er ions potassium tantalate-niobate lithium pottery according to claim 1, is characterized in that: described Er ions potassium tantalate-niobate lithium pottery is Tetragonal tungsten bronze crystal structure.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105789600A (en) * | 2016-04-27 | 2016-07-20 | 宁德时代新能源科技股份有限公司 | Lithium battery positive electrode material, preparation method thereof and lithium ion battery containing material |
| CN109485417A (en) * | 2018-11-19 | 2019-03-19 | 福州大学 | A kind of erbium/lanthanum relied on fluorescence temperature is co-doped with the preparation method of potassium-sodium niobate crystalline 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 |
| CN114605151A (en) * | 2022-04-24 | 2022-06-10 | 西安理工大学 | Gd-Ta co-doped tungsten bronze structure ferroelectric energy storage ceramic material and preparation method thereof |
-
2015
- 2015-11-27 CN CN201510848616.9A patent/CN105347796A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 李磊: "Er3+及Er3+/Yb3+掺杂钽铌酸钾锂晶体生长和光谱性能", 《中国博士学位论文全文数据库 基础科学辑》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105789600A (en) * | 2016-04-27 | 2016-07-20 | 宁德时代新能源科技股份有限公司 | Lithium battery positive electrode material, preparation method thereof and lithium ion battery containing material |
| CN105789600B (en) * | 2016-04-27 | 2019-05-07 | 宁德时代新能源科技股份有限公司 | Lithium battery positive electrode material, preparation method thereof and lithium ion battery containing material |
| CN109485417A (en) * | 2018-11-19 | 2019-03-19 | 福州大学 | A kind of erbium/lanthanum relied on fluorescence temperature is co-doped with the preparation method of potassium-sodium niobate crystalline 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 |
| CN114605151A (en) * | 2022-04-24 | 2022-06-10 | 西安理工大学 | Gd-Ta co-doped tungsten bronze structure ferroelectric energy storage ceramic material and preparation method thereof |
| CN114605151B (en) * | 2022-04-24 | 2022-12-09 | 西安理工大学 | Gd-Ta co-doped tungsten bronze structure ferroelectric energy storage ceramic material and preparation method thereof |
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Application publication date: 20160224 |