CN103214016A - 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 combine method of prepared YAG nano-powder of sol-gel and lyophilize of utilizing belongs to the crystalline ceramics preparing technical field.
Background technology
YAG has advantages such as good optical property and stable chemical properties, is widely used as window material and functional materials.Rare earth ion doped YAG monocrystalline is a kind of ideal laserable material, now has been widely used in laser technology field, is the important matrix of all solid state laser.Compare with monocrystalline, the YAG crystalline ceramics has that preparation technology is simple, cost is low, can realize high-concentration dopant, can make large size and can realize advantage such as multi-layer multi composite structure, becomes a research focus in recent years.Wherein, prepare the purity height, granularity is little, sintering activity is high YAG powder is the prerequisite of high optical quality YAG crystalline ceramics preparation.
At present, the method for preparing the YAG powder of report mainly contains both at home and abroad: solid reaction process, coprecipitation method, hydrothermal method and sol-gel method etc.
The preparation method of early stage YAG powder is a solid reaction process, promptly adopts high-purity Y
2O
3And Al
2O
3Powder through repeatedly ball milling and high-temperature calcination more than 1600 ℃, relies on Y
2O
3And Al
2O
3Powder at high temperature spreads to react and generates the YAG powder.The shortcoming that solid reaction process exists is: introduce impurity and raw material in the mechanical milling process easily and be not easy mixing, simultaneously, high-temperature calcination reduces the sintering activity of powder, and can't obtain nano level powder.In addition, in the calcinate except principal crystalline phase YAG mutually, often contain a spot 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 among the Japanese Patent JP2001270714, be configured to contain the solution of carbonate and sulfonium ion, form precipitation by the pH value of adjusting solution, throw out obtains the YAG powder of particle diameter 40～400nm through 800～1300 ℃ of calcinings.The shortcoming of the existence of this method is: because the difference of sedimentation speed between the different components makes different ions elder generation postprecipitation easily, thereby causes the microcosmic composition homogeneity to be difficult to control, and sedimentary washing and suction filtration difficulty relatively, powder is easily reunited.
People [Yukiya Hakuta et al such as Yukiya Hakuta, Production of phosphor (YAG:Tb) fine particles by hydrothermal synthesis in supercritical water, 1999,9 (10): 2671-2674] utilize Hydrothermal Preparation YAG:Tb powder.The shortcoming of this technology is: the equipment requirements height.
People (Michael Veith, et al, Low temperature synthesis of nanocrystalline Y such as Michael Veith
3Al
5O
12(YAG) and Ce-doped Y
3Al
5O
12Via different sol-gel methods.J.Mater.Chem., 1999 (12) 3069-3079) utilize sol-gel method to prepare the YAG nano-powder, the shortcoming that this method exists is: raw materials cost is higher, the major cause that cost is high is the synthesis condition of Y and other rare earth ion alkoxide harsh especially (wanting strict control moisture), complex technical process, and synthetic yield is lower; In addition, in the Drying of gels process,, cause powder to be reunited easily, if do not solve immediately, develop into hard aggregation the most at last, thereby reduce the sintering activity of powder if dry improper.
Summary of the invention
It is simple relatively that technical problem to be solved by this invention provides 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, have proposed a kind of combine method of prepared YAG nano-powder of sol-gel and lyophilize of utilizing.
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 may further comprise the steps:
1) aluminium salt is dissolved in the 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 the 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 3:5, 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 intense stirring condition, aluminum solutions dropwise is added drop-wise in the solution A, under 30～50 ℃ condition, stirred 1～3 hour, obtain colloidal sol; Under 60～80 ℃ condition, continue to stir 1～3 hour then, obtain gel;
3) with step 2) in the gel that obtains be transferred in the freeze drier, carry out pre-freeze, and then carry out drying, the presoma that obtains loosening;
4) presoma that obtains in the step 3) is calcined, promptly obtained described nanometer yttrium aluminium garnet powder.
The invention has the beneficial effects as follows: utilize preparation method of the present invention, can be with relatively low cost, under the temperature of lower (900～1100 ℃), prepare granularity little (30～100nm), the YAG nano-powder of sintering activity height, uniform doping.
In addition, the present invention adopts sol-gel and the lyophilize technology of combining to prepare the YAG nano powder, and lyophilize replaces conventional drying, has avoided powder because of the dry reunion that causes, thus can prepare lowly reunite, 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 the acetic acid yttrium; The acetate of described other rare earth ion comprises any one in acetic acid neodymium, acetic acid ytterbium, cerous acetate, acetic acid erbium, acetic acid europium, acetic acid holmium, acetic acid samarium, the praseodymium acetate etc.
Adopt the beneficial effect of above-mentioned further scheme to be, it is raw material that Al salt adopts aluminum isopropylate, and it is raw material that the salt of Y and other rare earth ion adopts corresponding acetate, and the preparation technology of acetate is simple relatively, and productive rate is higher, thereby can significantly 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 a doped with rare-earth elements, and described x represents doping, and common 0≤x≤0.1 is pure Y when x=0
3Al
5O
12
Further, in step 3), described processing condition of carrying out pre-freeze are: under-50～-70 ℃ condition, and pre-freeze 8～24 hours.
Further, in step 3), the described exsiccant processing condition of carrying out are: at-50～-70 ℃, and under the vacuum tightness of 1～15Pa, dry 20～50 hours.
Further, in step 4), the described incinerating processing condition of carrying out are: under 900～1100 ℃ condition, calcined 2～4 hours.
Description of drawings
Fig. 1 presses X-ray diffraction (X-ray Diffraction the is called for short XRD) spectrogram of embodiment 1 preparation YAG nanopowder for the present invention.
Fig. 2 presses projection electron micro-(Transmission Electron Micro-scope the is called for short TEM) figure of embodiment 1 preparation YAG nano powder for the present invention.
Embodiment
Below in conjunction with accompanying drawing principle of the present invention and feature are described, institute gives an actual example and only is used to explain the present invention, is not to be used to limit scope of the present invention.
A kind of preparation method of nanometer yttrium aluminium garnet powder may further comprise the steps:
1) aluminium salt is dissolved in the 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 the 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 3:5, 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 intense stirring condition, aluminum solutions dropwise is added drop-wise in the solution A, under 30～50 ℃ condition, stirred 1～3 hour, obtain colloidal sol; Under 60～80 ℃ condition, continue to stir 1～3 hour then, obtain gel;
3) with step 2) in the gel that obtains be transferred in the freeze drier, under-50～-70 ℃ condition, pre-freeze 8～24 hours, and then at-50～-70 ℃, under the vacuum tightness of 1～15Pa, dry 20～50 hours, the presoma that obtains loosening;
4) with the presoma that obtains in the step 3) under 900～1100 ℃ condition, calcined 2～4 hours, promptly 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 a doped with rare-earth elements, and described x represents doping, and common 0≤x≤0.1 is pure Y when x=0
3Al
5O
12
Below by several specific embodiments so that the present invention is specifically described.
Embodiment 1
Take by weighing aluminum isopropylate 102.12 grams and be dissolved in the 300ml Virahol, form aluminum solutions, take by weighing acetic acid yttrium (molecular formula: Y (CH
3COO)
34H
2O) 101.43 grams are dissolved in the 600ml deionized water, form the solution of yttrium.Under vigorous stirring, above-mentioned aluminum solutions dropwise is added drop-wise in the solution of yttrium, under 40 ℃, stir 2h, form colloidal sol, be warming up to 60 ℃ and continuation stirring 3h, form gel.Above-mentioned gel is transferred in the freeze drier, at-60 ℃ of pre-freeze 12h, under-60 ℃, 10Pa, dry 30h, the precursor powder that obtains loosening.Precursor powder obtains final product through 900 ℃ of high-temperature calcination 2h.Its XRD spectrum contrasts with standard card JCPDS33-40 as shown in Figure 1, and the position and the relative intensity of diffraction peak are in full accord, show that product is pure YAG phase.The TEM photo as shown in Figure 2, average grain size is about 30nm.
Embodiment 2
Take by weighing aluminum isopropylate 102.12 grams and be dissolved in the 600ml Virahol, form aluminum solutions, take by weighing acetic acid yttrium (molecular formula :) 100.4157 grams, acetic acid neodymium (molecular formula: Nd (CH with embodiment 1
3COO)
3H
2O) 1.0181 grams are dissolved in the 400ml deionized water, form the mixing solutions of yttrium and neodymium.Under vigorous stirring, above-mentioned aluminum solutions dropwise is added drop-wise in the mixing solutions of yttrium and neodymium, under 45 ℃, stir 2h, form colloidal sol, be warming up to 70 ℃ and continuation stirring 2h, form gel.Above-mentioned gel is transferred in the freeze drier, at-65 ℃ of pre-freeze 8h, under-65 ℃, 8Pa, dry 36h, the precursor powder that obtains loosening.Precursor powder obtains the Nd:YAG powder of Nd content 1.0at% at last through 1000 ℃ of high-temperature calcination 2h.Its XRD figure spectrum and TEM photo feature are with embodiment 1.The key technical indexes sees Table 1.
Embodiment 3
Take by weighing aluminum isopropylate 102.12 grams and be dissolved in the 400ml Virahol, form aluminum solutions, take by weighing acetic acid yttrium (molecular formula :) 96.3585 grams, acetic acid ytterbium (molecular formula: Yb (CH with embodiment 1
3COO)
34H
2O) 6.332 grams are dissolved in the 500ml deionized water, form the mixing solutions of yttrium and ytterbium.Under vigorous stirring, above-mentioned aluminum solutions dropwise is added drop-wise in the mixing solutions of yttrium and ytterbium, under 30 ℃, stir 3h, form colloidal sol, be warming up to 80 ℃ and continuation stirring 1h, form gel.Above-mentioned gel is transferred in the freeze drier, at-60 ℃ of pre-freeze 24h, under-60 ℃, 7Pa, dry 48h, the precursor powder that obtains loosening.Precursor powder obtains the Yb:YAG powder of Yb content 5.0at% at last through 1100 ℃ of high-temperature calcination 3h, and its XRD figure spectrum and TEM photo feature are with embodiment 1.The key technical indexes sees Table 1.
Embodiment 4
Take by weighing aluminum isopropylate 102.12 grams and be dissolved in the 500ml Virahol, form aluminum solutions, take by weighing acetic acid yttrium (molecular formula :) 101.3286 grams, cerous acetate (molecular formula: Ce (CH with embodiment 1
3COO)
35H
2O) 0.1222 gram is dissolved in the 300ml deionized water, forms the mixing solutions of yttrium and cerium.Under vigorous stirring, above-mentioned aluminum solutions dropwise is added drop-wise in the mixing solutions of yttrium and cerium, under 50 ℃, stir 2h, form colloidal sol, be warming up to 80 ℃ and continuation stirring 1h, form gel.Above-mentioned gel is transferred in the freeze drier, at-70 ℃ of pre-freeze 10h, under-60 ℃, 10Pa, dry 40h, the precursor powder that obtains loosening.Precursor powder obtains the Ce:YAG powder of Ce content 0.1at% at last through 900 ℃ of high-temperature calcination 2h, and its XRD figure spectrum and TEM photo feature are with embodiment 1.The key technical indexes sees Table 1.
Embodiment 5
Take by weighing aluminum isopropylate 102.12 grams and be dissolved in the 500ml Virahol, form aluminum solutions, take by weighing acetic acid yttrium (molecular formula :) 91.287 grams, acetic acid erbium (molecular formula: Er (CH with embodiment 1
3COO)
34H
2O) 12.4935 grams are dissolved in the 400ml deionized water, form the mixing solutions of yttrium and erbium.Under vigorous stirring, above-mentioned aluminum solutions dropwise is added drop-wise in the mixing solutions of yttrium and erbium, under 40 ℃, stir 2h, form colloidal sol, be warming up to 75 ℃ and continuation stirring 1h, form gel.Above-mentioned gel is transferred in the freeze drier, at-70 ℃ of pre-freeze 16h, under-65 ℃, 15Pa, dry 50h, the precursor powder that obtains loosening.Precursor powder obtains the Er:YAG powder of Er content 10at% at last through 1000 ℃ of high-temperature calcination 2h, and its XRD figure spectrum and TEM photo feature are with embodiment 1.The key technical indexes sees 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 as seen, utilize preparation method of the present invention, can be with relatively low cost, under the temperature of lower (900～1100 ℃), prepare granularity little (30～100nm), the YAG nano-powder of sintering activity height, uniform doping.
The above only is preferred embodiment of the present invention, and is in order to restriction the present invention, within the spirit and principles in the present invention not all, any modification of being done, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. the preparation method of a nanometer yttrium aluminium garnet powder is characterized in that, may further comprise the steps:
1) aluminium salt is dissolved in the 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 the 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 3:5, and the ratio of weight and number of described aluminium salt and Virahol is 1:2～1:6; 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 intense stirring condition, aluminum solutions dropwise is added drop-wise in the solution A, under 30～50 ℃ condition, stirred 1～3 hour, obtain colloidal sol; Under 60～80 ℃ condition, continue to stir 1～3 hour then, obtain gel;
3) with step 2) in the gel that obtains be transferred in the freeze drier, carry out pre-freeze, and then carry out drying, obtain presoma;
4) presoma that obtains in the step 3) is calcined, promptly obtained described nanometer yttrium aluminium garnet powder.
2. the preparation method of nanometer yttrium aluminium garnet powder according to claim 1, it is characterized in that: described aluminium salt is aluminum isopropylate.
3. the preparation method of nanometer yttrium aluminium garnet powder according to claim 1, it is characterized in that: described yttrium salt is the acetic acid yttrium; The acetate of described other rare earth ion comprises any one in acetic acid neodymium, acetic acid ytterbium, cerous acetate, acetic acid erbium, acetic acid europium, thick sour holmium, acetic acid samarium, the praseodymium acetate.
4. the preparation method of nanometer yttrium aluminium garnet powder according to claim 1, it is characterized in that: the granularity of described nanometer yttrium aluminium garnet powder is 30～100nm.
5. the preparation method of nanometer yttrium aluminium garnet powder according to claim 1, it 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 a doped with rare-earth elements, and described x represents doping, and common 0≤x≤0.1 is pure Y when x=0
3Al
5O
12
6. according to the preparation method of each described nanometer yttrium aluminium garnet powder of claim 1 to 5, it is characterized in that: in step 3), described processing condition of carrying out pre-freeze are: under-50～-70 ℃ condition, and pre-freeze 8～24 hours.
7. according to the preparation method of each described nanometer yttrium aluminium garnet powder of claim 1 to 5, it is characterized in that: in step 3), the described exsiccant processing condition of carrying out are: at-50～-70 ℃, and under the vacuum tightness of 1～15Pa, dry 20～50 hours.
8. according to the preparation method of each described nanometer yttrium aluminium garnet powder of claim 1 to 5, it is characterized in that: in step 4), the described incinerating processing condition of carrying out are: under 900～1100 ℃ condition, calcined 2～4 hours.
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| CN104326501A (en) * | 2014-10-21 | 2015-02-04 | 李金平 | Method for synthesizing yttrium aluminum garnet nano powder |
| CN105254295A (en) * | 2015-10-20 | 2016-01-20 | 南京航空航天大学 | Preparation method of neodymium doped barium titanate ceramic nano-powder |
| CN106518044A (en) * | 2016-11-28 | 2017-03-22 | 航天特种材料及工艺技术研究所 | Yttrium-scandium-aluminum garnet-based (>YSAG-based) nano-powder and preparation method thereof |
| CN106518046A (en) * | 2016-10-26 | 2017-03-22 | 中国地质大学（武汉） | Method for preparing magnesium-based lanthanum hexaaluminate powder through co-ion complexing |
| 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 |
| CN111574215A (en) * | 2020-05-26 | 2020-08-25 | 莆田学院 | Method for preparing yttrium aluminum garnet powder |
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| CN104326501A (en) * | 2014-10-21 | 2015-02-04 | 李金平 | Method for synthesizing yttrium aluminum garnet nano powder |
| CN104326501B (en) * | 2014-10-21 | 2016-01-20 | 李金平 | A kind of synthetic method of nanometer yttrium aluminium garnet powder |
| CN105254295A (en) * | 2015-10-20 | 2016-01-20 | 南京航空航天大学 | Preparation method of neodymium doped barium titanate ceramic nano-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 |
| CN106518046A (en) * | 2016-10-26 | 2017-03-22 | 中国地质大学（武汉） | Method for preparing magnesium-based lanthanum hexaaluminate powder through co-ion complexing |
| 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 |
| CN106518044A (en) * | 2016-11-28 | 2017-03-22 | 航天特种材料及工艺技术研究所 | Yttrium-scandium-aluminum garnet-based (>YSAG-based) nano-powder and preparation method thereof |
| 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 |
| CN111574215A (en) * | 2020-05-26 | 2020-08-25 | 莆田学院 | Method for preparing yttrium aluminum garnet powder |
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