CN102701722A - Method for producing yttrium aluminum garnet (YAG) nanopowder through fractional precipitation method - Google Patents
Method for producing yttrium aluminum garnet (YAG) nanopowder through fractional precipitation method Download PDFInfo
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Abstract
The invention provides a method for producing yttrium aluminum garnet (YAG) nanopowder through a fractional precipitation method. The method is characterized by comprising the steps: firstly, producing an alumina precursor by adopting a reverse dipping technology based on analytical pure Al (NO)3 and Y(NO3)3 as raw materials and NH4HCO3 as a precipitant; then, dispersing the produced alumina precursor in a Y(NO3)3 solution to form a suspension system; after the suspension system is uniformly dispersed, dropwise adding the NH4HCO3 solution; respectively carrying out washing and alcohol washing on the obtained precipitate for three times; and drying to obtain the YAG precursor; subsequently, calcining the precursor, so as to obtain the YAG nanopowder. Vice versa, a yttrium oxide precursor is firstly produced, then the YAG precursor is produced, and the YAG block material which is produced by YAG nanopowder which is obtained by calcinating the precursor at 1050 DEG C has good light transmission performance.
Description
Technical field
The present invention relates to a kind of preparation method of YAG nano-powder, the present invention adopts the method for fractional precipitation to prepare the YAG nano-powder or rather, and this powder can be used for the preparation of crystalline ceramics.The preparing technical field that belongs to crystalline ceramics.
Background technology
Nineteen ninety-five, Japanese scientist A.Ikesue [A.Ikesue, T.Kinoshita; And K.Kamata; Fabrication and optical properties of high-performance polycrystalline Nd:YAGceramics for solid-state lasers, J.Am.Ceramic.Soc., 1995; 78 (4); 1033.] prepare high-quality Nd:YAG crystalline ceramics, and realize the laser output of crystalline ceramics first, develop first Nd:YAG ceramic laser in the world simultaneously.With traditional laser gain dielectric crystal and glassy phase ratio, it is simple that crystalline ceramics has preparation, and the doping content height is prone to realize comprehensive advantages such as large size.The successful preparation of laser transparent ceramic has promoted the development of optical clear pottery greatly.1998, a day Benshen island chemical company successfully adopted nano-powder technology and vacuum sintering method to prepare YAG crystalline ceramics [T.Yanagitani, H.Yagi, and M.Ichikawa; Japanese patent, 1998,10-101333.; T.Yanagitani, H.Yagi, and Y Hiro; Japanese patent, 1998,10-101411.].2000, the Nd:YAG crystalline ceramics that rice is prepared with this method was successfully realized efficient laser output [J.Lu, the M.Prabhu of crystalline ceramics; And J.Xu; Highly efficient 2%Nd:yttrium aluminum garnet ceramic laser, Appl.Phys.Lett., 2000; 77 (23), 3707-3709.].After this; Based on this technology; The crystal institute of the refreshing island chemical company of Japan, NEC film, Russian Academy Of Sciences etc. develops jointly out the superpower and the high-level efficiency solid statelaser of a series of diode pumpings; Laser output power is brought up to 72W, 88W and 1.46KW from 31W, and light-phototranstormation efficiency brings up to 28.8%, 30% and 42% from 14.5%.
From present existing document and patent analyses, the nano-powder technology combines vacuum sintering method to possess than remarkable advantages.Wherein the preparation of nano-powder is the method that adopts co-precipitation; The result of study in early stage shows; The suitable preparation condition of alumina precursor and yttrium oxide presoma is different, and has bigger difference, so the present invention attempts adopting the method for fractional precipitation to prepare the YAG nano-powder.Compare with prior coprecipitation method, the nano-powder that this method makes possesses higher sintering activity, can prepare higher-quality crystalline ceramics.
Summary of the invention
The object of the present invention is to provide a kind of step-by-step precipitation method to prepare the method for YAG nano-powder, can make the nano-powder of higher sintering activity.
The present invention implements like this: adopt Al (NO)
3And Y (NO
3)
3Be raw material, with NH
4HCO
3As precipitation agent, the purity of raw material and precipitation agent is analytical pure.Elder generation takes by weighing raw material according to stoichiometric ratio and is diluted to the solution of desired concn; Its two, adopt step-by-step precipitation method, prepare the throw out of a kind of aluminum ion or ruthenium ion metals ion; After washing and ageing; The throw out that makes is dispersed in the another kind of metal ion solution fully stirs the back and add precipitant solution and form suspension-s, obtain mixed precipitation, again through ageing, washing, alcohol wash and drying after obtain the YAG presoma.At last this presoma is calcined, promptly obtained the YAG nano-powder.
The preparation technology of YAG crystalline ceramics provided by the invention, as shown in Figure 1, it is characterized in that:
(1) adopt the method for fractional precipitation, deposition one metal ion species earlier, after the throw out that obtains earlier is scattered in the another kind of metal ion solution, add precipitation agent again, obtain precipitation mixture, i.e. the YAG presoma.This presoma can obtain the YAG nano-powder behind drying and calcining.
(2) concentration of the metal ion solution of described Al or Y is 0.1-2.0M.
(3) concentration of described precipitation agent is 0.1-2.0M; Precipitation agent is NH
4HCO
3
The preparation technology's of YAG crystalline ceramics provided by the invention characteristics are:
(1) be different from coprecipitation method, the present invention adopts step-by-step precipitation method to prepare the YAG nano-powder.
(2) can obtain the component mixing uniformity suitable with coprecipitation technology.
(3) it is higher to make the sintering activity of YAG powder.
The invention provides the method that a kind of step-by-step precipitation method prepares the YAG nano-powder, it is characterized in that adopting analytical pure Al (NO)
3, Y (NO
3)
3For raw material with NH
4HCO
3Be precipitation agent, at first adopt the anti-technology of dripping, produce alumina precursor, then the alumina precursor that makes is dispersed in Y (NO
3)
3Form outstanding turbid system in the solution, after waiting to hang turbid system homodisperse, dropwise add NH
4HCO
3Solution is washed the throw out that obtains respectively, and alcohol is given a baby a bath on the third day after its birth inferior, after drying, promptly obtains the YAG presoma again.Calcine this presoma then, obtain the YAG nano-powder.Vice versa, produces the yttrium oxide presoma earlier, produces the YAG presoma then, becomes the YAG block materials to have good light transmittance by 1050 ℃ of prepared nanometer YAG powder preparing of calcining of presoma.
Description of drawings
The technical process of preparation YAG nano-powder among Fig. 1 embodiment 1;
The XRD phase transformation result of the YAG presoma of preparation among Fig. 2 embodiment 1;
The FESEM pattern of the YAG nano-powder of preparation among Fig. 3 embodiment 1;
The transmittance curve of the YAG of preparation pottery among Fig. 4 embodiment 1;
The photo in kind of the YAG of preparation pottery among Fig. 5 embodiment 1;
The technical process of preparation YAG nano-powder among Fig. 6 embodiment 2;
The XRD phase transformation result of the YAG presoma of preparation among Fig. 7 embodiment 2;
The FESEM pattern of the YAG nano-powder of preparation among Fig. 8 embodiment 2;
The photo in kind of the YAG of preparation pottery among Fig. 9 embodiment 2;
The technical process of preparation YAG nano-powder in Figure 10 Comparative Examples 1;
The XRD phase transformation result of the YAG presoma of preparation in Figure 11 Comparative Examples 1;
The FESEM pattern of the YAG nano-powder of preparation in Figure 12 Comparative Examples 1;
The photo in kind of the YAG of preparation pottery in Figure 13 Comparative Examples 1;
The technical process of preparation YAG nano-powder in Figure 14 Comparative Examples 2;
The XRD phase transformation result of the YAG presoma of preparation in Figure 15 Comparative Examples 2;
The FESEM pattern of the YAG nano-powder of preparation in Figure 16 Comparative Examples 2;
The transmittance curve of the YAG of preparation pottery in Figure 17 Comparative Examples 2;
The photo in kind of the YAG of preparation pottery in Figure 18 Comparative Examples 2.
Embodiment
Further specify embodiment and effect with following indefiniteness embodiment:
Embodiment 1
According to technical process shown in Figure 1, take 19.93g Y (NO respectively
3)
3Solution, 33.94gAl (NO
3)
3Solution, 66.92g and 348.52g NH
4HCO
3Solution is raw material.Diluting soln at first is to 33.94gAl (NO
3)
3Solution, 66.92g and 348.52g NH
4HCO
3Add deionized water in the solution respectively to 350mL, 400ml and 420mL.And then with Al (NO
3)
3Solution joins the NH of 400ml with the speed of 0.5-1.5mL/min
4HCO
3In the solution, form Al ionic throw out.The 3rd step was with the deposition ageing 24h that obtains, and washing for twice, the four step with deionized water again is with Y (NO
3)
3Solution joined for the 3rd step in the deposition of washed with de-ionized water, and back fully dispersed with stirring forms suspension-s, and the 5th step was that dilution is 420mlNH
4HCO
3Solution joins with the speed with 0.5-1.5mL/min and comprises throw out and Y (NO
3)
3In the suspension-s of solution composition, can make mixed precipitation,, and give a baby a bath on the third day after its birth time with deionized water and absolute ethyl alcohol respectively, can make the YAG presoma after ageing 24h.This presoma can make the YAG nano-powder through calcining after the drying.
To calcine the back powder and cross 200 mesh sieves, and in punching block, adopt the pressure precompressed of 100MPa to obtain biscuit, again biscuit carried out static pressure processing such as 200MPa.With the biscuit sintering under vacuum condition that waits after static pressure is handled, 1750 ℃ of temperature, soaking time 20h.Sample after the vacuum sintering is annealed 1450 ℃ of temperature, time 10h under air atmosphere.
Based on the result among Fig. 2, presoma can obtain the YAG powder through 1050 ℃ of calcinings.Fig. 3 is the transmission electron microscope pattern of the YAG powder that makes.As can be seen from Figure 3, powder dispersity is better, and particle size is 200nm-500nm.Fig. 4 is the transmittance curve of sample.As can be seen from Figure 4, the transmitance that makes sample can reach 66% at the 1100nm place, and the transmitance in the visible region is about 60%.Fig. 5 is the photo in kind that makes sample, and as can be seen from Figure 5, the sample that the powder sintering that adopts step-by-step precipitation method to make goes out possesses light transmission preferably.
Embodiment 2
According to technical process shown in Figure 6, take 19.93g Y (NO respectively
3)
3Solution, 33.94g Al (NO
3)
3Solution, 66.92g and 348.52g NH
4HCO
3Solution is raw material.Diluting soln at first is to 199.3gY (NO
3)
3Solution, Al (NO
3)
3Solution and 66.92g NH
4HCO
3Add deionized water in the solution respectively to 210mL, 350ml and 400mL.Then with the speed adding Y (NO of 400mL solution with 1mL/min
3)
3In the solution.After the deposition ageing 24h that will obtain, wash twice with deionized water again, then with NH
4HCO
3Solution adds in the deposition that makes, and the back is dispersed with stirring fully, then with 350ml Al (NO
3)
3Solution joins with the speed of 1mL/min and comprises deposition and NH
4HCO
3In the suspension liquid of solution, can make mixed precipitation, then through ageing 24h, and it is inferior to give a baby a bath on the third day after its birth with deionized water and absolute ethyl alcohol respectively, can make the YAG presoma.This presoma makes the YAG nano-powder through calcining after the drying.
To calcine the back powder and cross 200 mesh sieves, and in punching block, adopt the pressure precompressed of 100MPa to obtain biscuit, again biscuit carried out static pressure processing such as 200MPa.With the biscuit sintering under vacuum condition that waits after static pressure is handled, 1750 ℃ of temperature, soaking time 20h.Sample after the vacuum sintering is annealed 1450 ℃ of temperature, time 10h under air atmosphere.
Based on the result among Fig. 7, presoma can obtain the YAG powder through 1350 ℃ of calcinings.Fig. 8 is the transmission electron microscope pattern of the YAG powder that makes.As can be seen from Figure 8, particle size is 200nm-300nm.Fig. 9 is the photo in kind (not polishing) that makes sample, and as can be seen from Figure 9, the sample that the powder sintering that adopts step-by-step precipitation method to make goes out possesses light transmission preferably.
Embodiment 1 and 2 with the experimental result of the metals ion that only provides a kind of concentration and a kind of precipitation agent concentration, but as presses metal ionic concn 0.1-2.0M and precipitation agent concentration 0.1-2.0M all can obtain the similar result like embodiment 1 and 2.
For the effect of fractional precipitation provided by the invention more is described, intend the characteristic that provides Comparative Examples 1 (just dripping co-precipitation) and Comparative Examples 2 (counter drip co-precipitation) to prepare nanometer YAG powder, further to show effect of the present invention.
Comparative Examples 1
Figure 10 is for just dripping the technical process that coprecipitation method prepares the YAG nano-powder.According to technical process shown in Figure 10, get 36.22mL Y (NO respectively
3)
3Solution and 89.02ml Al (NO
3)
3Solution changes in the beaker, adds deionized water to 500mL, takes by weighing 118.58gNH
4HCO
3, be dissolved in the deionized water, and add deionized water to 1000mL.Then with NH
4HCO
3Solution adds in the metal ion solution with the speed of 1mL/min.Behind the deposition ageing 24h that obtains, it is inferior to give a baby a bath on the third day after its birth with deionized water and absolute ethyl alcohol respectively, can make the YAG presoma through drying again.Presoma can make the YAG powder through calcining.The moulding and the sintering condition of YAG pottery are identical with embodiment 1.
Based on the result among Figure 11, presoma can obtain the YAG powder through 900 ℃ of calcinings.Figure 12 is the transmission electron microscope pattern of the YAG powder that makes.As can be seen from Figure 12, powder dispersity is relatively poor, has serious agglomeration in the powder.There are two kinds of sizes in particle, and a kind of is about 500nm, and is another kind of less than 100nm.Figure 13 is the photo in kind that makes sample, as can be seen from Figure 13, adopts the sintering character just dripping the powder that coprecipitation method makes relatively poor.
Comparative Examples 2
The technical process that Figure 14 prepares the YAG nano-powder for an anti-coprecipitation method.According to technical process shown in Figure 14, get 36.22mLY (NO respectively
3)
3Solution and 89.02mlAl (NO
3)
3Solution changes in the beaker, adds deionized water to 500mL, takes by weighing 118.58gNH
4HCO
3, be dissolved in the deionized water, and add deionized water to 1000mL.Then with the speed adding NH of metal ion solution with 1mL/min
4HCO
3In the solution.Behind the deposition ageing 24h that obtains, it is inferior to give a baby a bath on the third day after its birth with deionized water and absolute ethyl alcohol respectively, can make the YAG presoma through drying again.Presoma can make the YAG powder through calcining.The moulding and the sintering condition of YAG pottery are identical with embodiment 1.
Based on the result among Figure 15, presoma can obtain the YAG powder through 1050 ℃ of calcinings.Figure 16 is the transmission electron microscope pattern of the YAG powder that makes.As can be seen from Figure 16, powder dispersity still can, particle size is about 100nm.Figure 17 is the transmittance curve of sample.As can be seen from Figure 17, the transmitance that makes sample has only about 15% at the 1100nm place, and the transmitance in the visible region is about 15-20%.Figure 18 is the photo in kind that makes sample, as can be seen from Figure 18, adopt anti-sintering character of dripping the powder that coprecipitation method makes still can, the YAG pottery of preparing possesses certain light transmission, but compares the bigger gap of existence with embodiment 1.
Claims (8)
1. the preparation method of a YAG nano-powder is characterized in that: adopt the method for fractional precipitation, earlier deposition one metal ion species; After the throw out that obtains earlier is scattered in the another kind of metal ion solution; Add precipitation agent again, obtain precipitation mixture, be i.e. the YAG presoma; The YAG presoma of gained can obtain the YAG nano-powder after calcining.
2. by the described method of claim 1, it is characterized in that adopting Al (NO
3)
3And Y (NO
3)
3Be raw material, with NH
4HCO
3As precipitation agent; Elder generation takes by weighing raw material according to stoichiometric ratio and is diluted to the solution of desired concn; It two adopts step-by-step precipitation method throw out of a kind of aluminum ion of preparation or ruthenium ion metals ion earlier, through after washing and the ageing, the throw out that makes is dispersed in fully stirs the back in the another kind of metal ion solution and add precipitant solution formation suspension-s; Obtain mixed precipitation, again through ageing, washing, alcohol wash and drying after obtain the YAG presoma; At last this presoma is calcined, promptly obtained the YAG nano-powder.
3. by the described method of claim 2, it is characterized in that described metal ion solution concentration is 0.1-2.0M.
4. by the described method of claim 1, it is characterized in that described precipitation agent concentration is 0.1-2.0M.
5. by claim 3 or 4 described methods, the purity that it is characterized in that described raw material and precipitation agent is analytical pure.
6. by the described method of claim 2, it is characterized in that adopting step-by-step precipitation method is with Al (NO
3)
3Or Y (NO
3)
3Solution joins NH with the speed of 0.5-1.5ml/min
4HCO
3In the solution.
7. by claim 1 or 2 described methods, it is characterized in that presoma incinerating temperature is 1050 ℃.
8. by the described method of claim 8, it is characterized in that calcining the YAG powder granule size 200-500nm of back gained.
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Cited By (3)
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| CN103351862A (en) * | 2013-06-25 | 2013-10-16 | 彩虹集团电子股份有限公司 | Yellow fluorescent powder for white LED (Light-Emitting Diode) with high photosynthetic efficiency white and preparation method of yellow fluorescent powder |
| RU2576271C1 (en) * | 2014-12-23 | 2016-02-27 | Федеральное Государственное Бюджетное Учреждение Науки Институт Химии И Химической Технологии Сибирского Отделения Российской Академии Наук (Иххт Со Ран) | Method for producing yttrium aluminum garnet nanopowders |
| CN106311268A (en) * | 2015-07-06 | 2017-01-11 | 中国石油化工股份有限公司 | Method for improving performance of methanol synthesis catalyst |
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| CN103351862A (en) * | 2013-06-25 | 2013-10-16 | 彩虹集团电子股份有限公司 | Yellow fluorescent powder for white LED (Light-Emitting Diode) with high photosynthetic efficiency white and preparation method of yellow fluorescent powder |
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| CN106311268A (en) * | 2015-07-06 | 2017-01-11 | 中国石油化工股份有限公司 | Method for improving performance of methanol synthesis catalyst |
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Application publication date: 20121003 |