CN103214016B - Preparation method of yttrium aluminum garnet (YAG) nano-powder - Google Patents
Preparation method of yttrium aluminum garnet (YAG) nano-powder Download PDFInfo
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Abstract
The invention relates to a preparation method of yttrium aluminum garnet (YAG) nano-powder. The preparation method comprises the steps of dissolving aluminum salt in isopropanol to prepare an aluminum solution, dissolving acetate of yttrium ions and/or other rare earth ions in deionized water to prepare a solution A, dropwise adding the aluminum solution to the solution A under the condition of vigorous stirring, executing the stages of collosol, gel, freeze drying and the like to form a precursor, and calcinating the precursor at a high temperature to form the YAG nano-powder. With the adoption of the preparation method, the YAG nano-powder which is small in particle size (30-110nm), high in sintering activity and uniform in doping can be prepared at lower cost and lower temperature (900-1100 DEG C).
Description
Technical field
The present invention relates to a kind of yttrium aluminum garnet (Y
3al
5o
12, be called for short YAG) and the preparation method of nano-powder, particularly a kind of sol-gel and lyophilize technique that combines that utilizes prepares the method for YAG nano powder, belongs to crystalline ceramics preparing technical field.
Background technology
YAG has the advantage such as excellent optical property and stable chemical property, is widely used as window material and functional materials.Rare earth ion doped YAG monocrystalline is a kind of desirable laserable material, is now widely used in laser technology field, is the important matrix of all solid state laser.Compared with monocrystalline, YAG crystalline ceramics has that preparation technology is simple, cost is low, can realize high-concentration dopant, can make large size and can realize the advantages such as multi-layer multi composite structure, becomes a study hotspot in recent years.Wherein, preparing the YAG powder that purity is high, granularity is little, sintering activity is high is prerequisite prepared by high optical quality YAG crystalline ceramics.
At present, the method preparing YAG powder of report mainly contains both at home and abroad: solid reaction process, coprecipitation method, hydrothermal method and sol-gel method etc.
Early stage YAG raw powder's production technology is solid reaction process, namely adopts high-purity Y
2o
3and Al
2o
3powder, through repeatedly ball milling and more than 1600 DEG C high-temperature calcinations, relies on Y
2o
3and Al
2o
3powder at high temperature spreads to react and generates YAG powder.The shortcoming that solid reaction process exists is: easily introduce impurity in mechanical milling process and raw material is not easy mixing, and meanwhile, high-temperature calcination makes the sintering activity of powder reduce, and cannot obtain nano level powder.In addition, in calcinate except principal crystalline phase YAG phase, often containing a small amount of YAlO
3(being called for short YAP) and Y
4al
2o
9(being called for short YAM) phase.
Adopt yttrium carbonate and dawsonite to make raw material in Japanese Patent JP2001270714, be configured to the solution containing carbonate and sulfonium ion, form precipitation by the pH value adjusting solution, throw out, through 800 ~ 1300 DEG C of calcinings, obtains the YAG powder of particle diameter 40 ~ 400nm.The shortcoming of the existence of the method is: due to the difference of sedimentation speed between different components, easily makes the first postprecipitation of different ions, thus causes microcosmic composition homogeneity to be difficult to control, and the washing of precipitation and suction filtration more difficult, powder is easily reunited.
People [the Yukiya Hakuta et al such as Yukiya Hakuta, Production of phosphor (YAG:Tb) fine particles by hydrothermal synthesis in supercriticalwater, 1999,9 (10): 2671-2674] hydrothermal method is utilized to prepare YAG:Tb powder.The shortcoming of this technology is: equipment requirements is high.
People (Michael Veith, et al, the Low temperaturesynthesis of nanocrystalline Y such as Michael Veith
3al
5o
12(YAG) and Ce-doped Y
3al
5o
12viadifferent sol-gel methods.J.Mater.Chem., 1999 (12) 3069-3079) utilize sol-gel method to prepare YAG nano powder, the shortcoming that the method exists is: raw materials cost is higher, the major cause that cost is high is the synthesis condition harsh especially (strictly will control moisture) of Y and other rare earth ion alkoxide, complex technical process, and synthetic yield is lower; In addition, in the drying process of gel, if dry improper, easily cause powder to be reunited, if immediately do not solved, develop into hard aggregation the most at last, thus reduce the sintering activity of powder.
Summary of the invention
It is relatively simple that technical problem to be solved by this invention is to provide a kind of preparation technology, and the preparation method of the higher nanometer yttrium aluminium garnet powder of productive rate.
Sol-gel method and Freeze Drying Technique have been merged in the present invention, propose a kind of sol-gel and lyophilize technique that combines that utilizes and prepare the method for YAG nano powder.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of preparation method of nanometer yttrium aluminium garnet powder, comprises the following steps:
1) aluminium salt is dissolved in Virahol, obtains the aluminum solutions that mass concentration is 15 ~ 35wt%; The acetate of yttrium salt and/or other rare earth ion is dissolved in deionized water, is made into the solution A that mass concentration is 15 ~ 25wt%; Wherein,
The mol ratio of the acetate of described aluminium salt and yttrium salt and/or other rare earth ion is 5:3, and the ratio of weight and number of described aluminium salt and Virahol is 1:2 ~ 1:6, and the acetate of described yttrium salt and/or other rare earth ion and the ratio of weight and number of deionized water are 1:3 ~ 1:6;
2) under the condition of vigorous stirring, aluminum solutions is dropwise added drop-wise in solution A, under the condition of 30 ~ 50 DEG C, stirs 1 ~ 3 hour, obtain colloidal sol; Then, under the condition of 60 ~ 80 DEG C, continue stirring 1 ~ 3 hour, obtain gel;
3) by step 2) in the gel that obtains be transferred in freeze drier, carry out pre-freeze, and then carry out drying, obtain the presoma loosened;
4) by step 3) in the presoma that obtains calcine, namely obtain described nanometer yttrium aluminium garnet powder.
The invention has the beneficial effects as follows: utilize preparation method of the present invention, can with relatively low cost, at the temperature of lower (900 ~ 1100 DEG C), prepare that granularity little (30 ~ 100nm), sintering activity are high, the YAG nano powder of uniform doping.
In addition, the present invention adopts sol-gel and lyophilize combined technology to prepare YAG nano powder, and lyophilize replaces conventional drying, avoids the reunion that powder causes because of dry, thus can prepare low reunion, YAG nanopowder that sintering activity is high.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described aluminium salt is aluminum isopropylate.
Further, described yttrium salt is acetic acid yttrium; The acetate of other rare earth ion described comprise in acetic acid neodymium, acetic acid ytterbium, cerous acetate, acetic acid erbium, acetic acid europium, acetic acid holmium, acetic acid samarium, praseodymium acetate etc. any one.
The beneficial effect of above-mentioned further scheme is adopted to be, Al salt adopts aluminum isopropylate to be raw material, and the salt of Y and other rare earth ion adopts corresponding acetate to be raw material, and the preparation technology of acetate is relatively simple, and productive rate is higher, thus significantly can reduce the cost of raw material.
Further, the granularity of described nanometer yttrium aluminium garnet powder is 30 ~ 100nm.
Further, described nanometer yttrium aluminium garnet powder is nanometer yttrium aluminium garnet powder or the rare earth ion doped nanometer yttrium aluminium garnet powder of undoping, and it consists of: Y
3-3xre
3xal
5o
12, wherein, described Re is doped with rare-earth elements, and described x represents doping, usual 0≤x≤0.1, is pure Y as x=0
3al
5o
12.
Further, in step 3) in, described in carry out pre-freeze processing condition be: under the condition of-50 ~-70 DEG C, pre-freeze 8 ~ 24 hours.
Further, in step 3) in, described in carry out dry processing condition and be: at-50 ~-70 DEG C, under the vacuum tightness of 1 ~ 15Pa, dry 20 ~ 50 hours.
Further, in step 4) in, described in the processing condition of carrying out calcining be: under the condition of 900 ~ 1100 DEG C, calcine 2 ~ 4 hours.
Accompanying drawing explanation
Fig. 1 is that the present invention prepares X-ray diffraction (X-rayDiffraction the is called for short XRD) spectrogram of YAG nanopowder by embodiment 1.
Fig. 2 is the projection electron that the present invention prepares YAG nano powder by embodiment 1 micro-(TransmissionElectron Micro-scope is called for short TEM) figure.
Embodiment
Be described principle of the present invention and feature below in conjunction with accompanying drawing, example, only for explaining the present invention, is not intended to limit scope of the present invention.
A preparation method for nanometer yttrium aluminium garnet powder, comprises the following steps:
1) aluminium salt is dissolved in Virahol, obtains the aluminum solutions that mass concentration is 15 ~ 35wt%; The acetate of yttrium salt and/or other rare earth ion is dissolved in deionized water, is made into the solution A that mass concentration is 15 ~ 25wt%; Wherein,
The mol ratio of the acetate of described aluminium salt and yttrium salt and/or other rare earth ion is 5:3, and the ratio of weight and number of described aluminium salt and Virahol is 1:2 ~ 1:6, and the acetate of described yttrium salt and/or other rare earth ion and the ratio of weight and number of deionized water are 1:3 ~ 1:6;
2) under the condition of vigorous stirring, aluminum solutions is dropwise added drop-wise in solution A, under the condition of 30 ~ 50 DEG C, stirs 1 ~ 3 hour, obtain colloidal sol; Then, under the condition of 60 ~ 80 DEG C, continue stirring 1 ~ 3 hour, obtain gel;
3) by step 2) in the gel that obtains be transferred in freeze drier, under the condition of-50 ~-70 DEG C, pre-freeze 8 ~ 24 hours, and then at-50 ~-70 DEG C, under the vacuum tightness of 1 ~ 15Pa, dry 20 ~ 50 hours, obtain the presoma loosened;
4) by step 3) in the presoma that obtains under the condition of 900 ~ 1100 DEG C, calcine 2 ~ 4 hours, namely obtaining granularity is 30 ~ 100nm nanometer yttrium aluminium garnet powder.
Described nanometer yttrium aluminium garnet powder is nanometer yttrium aluminium garnet powder or the rare earth ion doped nanometer yttrium aluminium garnet powder of undoping, and it consists of: Y
3-3xre
3xal
5o
12, wherein, described Re is doped with rare-earth elements, and described x represents doping, usual 0≤x≤0.1, is pure Y as x=0
3al
5o
12.
Below by way of several specific embodiment to be specifically described the present invention.
Embodiment 1
Taking aluminum isopropylate 102.12 grams is dissolved in 300ml Virahol, forms aluminum solutions, takes acetic acid yttrium (molecular formula: Y (CH
3cOO)
34H
2o) 101.43 grams are dissolved in 600ml deionized water, form the solution of yttrium.With vigorous stirring, above-mentioned aluminum solutions is dropwise added drop-wise in the solution of yttrium, at 40 DEG C, stirs 2h, form colloidal sol, be warming up to 60 DEG C and continue to stir 3h, forming gel.Above-mentioned gel is transferred in freeze drier, at-60 DEG C of pre-freeze 12h ,-60 DEG C, under 10Pa, dry 30h, obtains the precursor powder loosened.Precursor powder obtains final product through 900 DEG C of high-temperature calcination 2h.Its XRD composes as shown in Figure 1, and contrast with standard card JCPDS33-40, position and the relative intensity of diffraction peak are completely the same, show that product is pure YAG phase.As shown in Figure 2, average grain size is about 30nm to TEM photo.
Embodiment 2
Taking aluminum isopropylate 102.12 grams is dissolved in 600ml Virahol, forms aluminum solutions, takes acetic acid yttrium (molecular formula: with embodiment 1) 100.4157 grams, acetic acid neodymium (molecular formula: Nd (CH
3cOO)
3h
2o) 1.0181 grams are dissolved in 400ml deionized water, form the mixing solutions of yttrium and neodymium.With vigorous stirring, above-mentioned aluminum solutions is dropwise added drop-wise in the mixing solutions of yttrium and neodymium, at 45 DEG C, stirs 2h, form colloidal sol, be warming up to 70 DEG C and continue to stir 2h, forming gel.Above-mentioned gel is transferred in freeze drier, at-65 DEG C of pre-freeze 8h ,-65 DEG C, under 8Pa, dry 36h, obtains the precursor powder loosened.Precursor powder, through 1000 DEG C of high-temperature calcination 2h, finally obtains the Nd:YAG powder of Nd content 1.0at%.Its XRD figure spectrum and TEM photo eigen are with embodiment 1.The key technical indexes is in table 1.
Embodiment 3
Taking aluminum isopropylate 102.12 grams is dissolved in 400ml Virahol, forms aluminum solutions, takes acetic acid yttrium (molecular formula: with embodiment 1) 96.3585 grams, acetic acid ytterbium (molecular formula: Yb (CH
3cOO)
34H
2o) 6.332 grams are dissolved in 500ml deionized water, form the mixing solutions of yttrium and ytterbium.With vigorous stirring, above-mentioned aluminum solutions is dropwise added drop-wise in the mixing solutions of yttrium and ytterbium, at 30 DEG C, stirs 3h, form colloidal sol, be warming up to 80 DEG C and continue to stir 1h, forming gel.Above-mentioned gel is transferred in freeze drier, at-60 DEG C of pre-freeze 24h ,-60 DEG C, under 7Pa, dry 48h, obtains the precursor powder loosened.Precursor powder, through 1100 DEG C of high-temperature calcination 3h, finally obtains the Yb:YAG powder of Yb content 5.0at%, and its XRD figure spectrum and TEM photo eigen are with embodiment 1.The key technical indexes is in table 1.
Embodiment 4
Taking aluminum isopropylate 102.12 grams is dissolved in 500ml Virahol, forms aluminum solutions, takes acetic acid yttrium (molecular formula: with embodiment 1) 101.3286 grams, cerous acetate (molecular formula: Ce (CH
3cOO)
35H
2o) 0.1222 gram is dissolved in 300ml deionized water, forms the mixing solutions of yttrium and cerium.With vigorous stirring, above-mentioned aluminum solutions is dropwise added drop-wise in the mixing solutions of yttrium and cerium, at 50 DEG C, stirs 2h, form colloidal sol, be warming up to 80 DEG C and continue to stir 1h, forming gel.Above-mentioned gel is transferred in freeze drier, at-70 DEG C of pre-freeze 10h ,-60 DEG C, under 10Pa, dry 40h, obtains the precursor powder loosened.Precursor powder, through 900 DEG C of high-temperature calcination 2h, finally obtains the Ce:YAG powder of Ce content 0.1at%, and its XRD figure spectrum and TEM photo eigen are with embodiment 1.The key technical indexes is in table 1.
Embodiment 5
Taking aluminum isopropylate 102.12 grams is dissolved in 500ml Virahol, forms aluminum solutions, takes acetic acid yttrium (molecular formula: with embodiment 1) 91.287 grams, acetic acid erbium (molecular formula: Er (CH
3cOO)
34H
2o) 12.4935 grams are dissolved in 400ml deionized water, form the mixing solutions of yttrium and erbium.With vigorous stirring, above-mentioned aluminum solutions is dropwise added drop-wise in the mixing solutions of yttrium and erbium, at 40 DEG C, stirs 2h, form colloidal sol, be warming up to 75 DEG C and continue to stir 1h, forming gel.Above-mentioned gel is transferred in freeze drier, at-70 DEG C of pre-freeze 16h ,-65 DEG C, under 15Pa, dry 50h, obtains the precursor powder loosened.Precursor powder, through 1000 DEG C of high-temperature calcination 2h, finally obtains the Er:YAG powder of Er content 10at%, and its XRD figure spectrum and TEM photo eigen are with embodiment 1.The key technical indexes is in table 1.
Table 1
| Embodiment | Product | Color | Particle diameter (nm) |
| 1 | Y 3Al 5O 12 | White | 30 |
| 2 | Y 2.97Nd 0.03Al 5O 12 | Purple | 50 |
| 3 | Y 2.85Yb 0.15Al 5O 12 | White | 60 |
| 4 | Y 2.997Ce 0.003Al 5O 12 | Light yellow | 40 |
| 5 | Y 2.7Er 0.3Al 5O 12 | Pink | 50 |
By above embodiment and table 1 visible, utilize preparation method of the present invention, can with relatively low cost, at the temperature of lower (900 ~ 1100 DEG C), prepare that granularity little (30 ~ 100nm), sintering activity are high, the YAG nano powder of uniform doping.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. a preparation method for nanometer yttrium aluminium garnet powder, is characterized in that, comprises the following steps:
1) aluminium salt is dissolved in Virahol, obtains the aluminum solutions that mass concentration is 15 ~ 35wt%; The acetate of yttrium salt and other rare earth ion is dissolved in deionized water, is made into the solution A that mass concentration is 15 ~ 25wt%; Wherein,
The mol ratio of the acetate of described aluminium salt and yttrium salt and other rare earth ion is 5:3, and the ratio of weight and number of described aluminium salt and Virahol is 1:2 ~ 1:6; Described yttrium salt is 1:3 ~ 1:6 with the acetate of other rare earth ion and the ratio of weight and number of deionized water;
2) under the condition of vigorous stirring, aluminum solutions is dropwise added drop-wise in solution A, under the condition of 30 ~ 50 DEG C, stirs 1 ~ 3 hour, obtain colloidal sol; Then, under the condition of 60 ~ 80 DEG C, continue stirring 1 ~ 3 hour, obtain gel;
3) by step 2) in the gel that obtains be transferred in freeze drier, carry out pre-freeze, and then carry out drying, obtain presoma;
4) by step 3) in the presoma that obtains calcine, namely obtain described nanometer yttrium aluminium garnet powder; The granularity of described nanometer yttrium aluminium garnet powder is 30 ~ 100nm.
2. the preparation method of nanometer yttrium aluminium garnet powder according to claim 1, is characterized in that: described aluminium salt is aluminum isopropylate.
3. the preparation method of nanometer yttrium aluminium garnet powder according to claim 1, is characterized in that: described yttrium salt is acetic acid yttrium; The acetate of other rare earth ion described comprise in acetic acid neodymium, acetic acid ytterbium, cerous acetate, acetic acid erbium, acetic acid europium, acetic acid holmium, acetic acid samarium, praseodymium acetate any one.
4. the preparation method of nanometer yttrium aluminium garnet powder according to claim 1, is characterized in that: described nanometer yttrium aluminium garnet powder is nanometer yttrium aluminium garnet powder or the rare earth ion doped nanometer yttrium aluminium garnet powder of undoping, and it consists of: Y
3-3xre
3xal
5o
12, wherein, described Re is doped with rare-earth elements, and described x represents doping, usual 0≤x≤0.1, is pure Y as x=0
3al
5o
12.
5. the preparation method of the nanometer yttrium aluminium garnet powder according to any one of Claims 1-4, is characterized in that: in step 3) in, described in carry out pre-freeze processing condition be: under the condition of-50 ~-70 DEG C, pre-freeze 8 ~ 24 hours.
6. the preparation method of the nanometer yttrium aluminium garnet powder according to any one of Claims 1-4, is characterized in that: in step 3) in, described in carry out dry processing condition and be: at-50 ~-70 DEG C, under the vacuum tightness of 1 ~ 15Pa, dry 20 ~ 50 hours.
7. the preparation method of the nanometer yttrium aluminium garnet powder according to any one of Claims 1-4, is characterized in that: in step 4) in, described in the processing condition of carrying out calcining be: under the condition of 900 ~ 1100 DEG C, calcine 2 ~ 4 hours.
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| CN104326501B (en) * | 2014-10-21 | 2016-01-20 | 李金平 | A kind of synthetic method of nanometer yttrium aluminium garnet powder |
| CN105254295B (en) * | 2015-10-20 | 2017-06-27 | 南京航空航天大学 | A kind of preparation method of neodymium-doped titanium acid barium nano-ceramic powder |
| CN106518046B (en) * | 2016-10-26 | 2019-07-09 | 中国地质大学（武汉） | A kind of method of the method preparation magnesium-based lanthanum hexaaluminate powder using coion complexing |
| CN106518044B (en) * | 2016-11-28 | 2019-07-16 | 航天特种材料及工艺技术研究所 | YSAG base nano-powder and preparation method thereof |
| CN107541212A (en) * | 2016-12-01 | 2018-01-05 | 漳州旗滨玻璃有限公司 | It is a kind of that there is the YAG that luminescent properties are changed under high efficiency and broad band:Yb2+/3+Light-converting material and preparation method thereof |
| CN108002421A (en) * | 2017-12-25 | 2018-05-08 | 河南工业大学 | A kind of preparation method with fluorite type structure nano-powder |
| CN111574215B (en) * | 2020-05-26 | 2022-02-08 | 莆田学院 | Method for preparing yttrium aluminum garnet powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173775A (en) * | 2011-02-23 | 2011-09-07 | 山东大学 | Method for preparing neodymium-doped yttrium aluminum garnet micro/nano powder by spray freeze-drying |
| CN102807239A (en) * | 2011-05-31 | 2012-12-05 | 北京化工大学 | Method for preparing lanthanide-series rare-earth-doped nanometer YAG (Yttrium Aluminum Garnet) compound powder |
-
2013
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173775A (en) * | 2011-02-23 | 2011-09-07 | 山东大学 | Method for preparing neodymium-doped yttrium aluminum garnet micro/nano powder by spray freeze-drying |
| CN102807239A (en) * | 2011-05-31 | 2012-12-05 | 北京化工大学 | Method for preparing lanthanide-series rare-earth-doped nanometer YAG (Yttrium Aluminum Garnet) compound powder |
Non-Patent Citations (1)
| Title |
|---|
| Synthesis of yttrium aluminum garnet (YAG) by a new sol–gel method;Zhihong Sun等;《Journal of Alloys and Compounds》;20041231;第379卷(第1-2期);第L1页第二栏7-20行 * |
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