CN1792805A - Preparation method of yttrium aluminum garnet nano powder - Google Patents
Preparation method of yttrium aluminum garnet nano powder Download PDFInfo
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- CN1792805A CN1792805A CN 200510110760 CN200510110760A CN1792805A CN 1792805 A CN1792805 A CN 1792805A CN 200510110760 CN200510110760 CN 200510110760 CN 200510110760 A CN200510110760 A CN 200510110760A CN 1792805 A CN1792805 A CN 1792805A
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- 239000011858 nanopowder Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 title description 2
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 title description 2
- 239000000843 powder Substances 0.000 claims abstract description 35
- 239000010431 corundum Substances 0.000 claims abstract description 13
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002425 crystallisation Methods 0.000 claims abstract description 9
- 230000008025 crystallization Effects 0.000 claims abstract description 9
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000032683 aging Effects 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 230000007704 transition Effects 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000000227 grinding Methods 0.000 abstract description 5
- 230000002776 aggregation Effects 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 7
- 238000010438 heat treatment Methods 0.000 abstract 3
- 238000005054 agglomeration Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 31
- 239000002243 precursor Substances 0.000 description 10
- 239000011222 crystalline ceramic Substances 0.000 description 4
- 229910002106 crystalline ceramic Inorganic materials 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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Abstract
A preparation method of YAG nano powder comprises the following steps: preparing a raw material solution; mixing Al 3)3Solution and Y (NO)3)3Dropping the mixed solution of the solution to NH4HCO3Fully stirring the solution at the same time, and then aging the solution to form a precipitation solution; carrying out vacuum filtration on the precipitation solution, and washing with deionized water and ethanol; after drying, grinding the mixture into powder in a corundum mortar; transferring the powder into a corundum crucible with a cover, placing the corundum crucible into a silicon-carbon rod electric furnace, and heating the corundum crucible to 850 ℃ from room temperature at the heating rate of 200-300 ℃/h in the air atmosphereRespectively preserving heat for 0.5-1 hour at the temperature of 130 ℃ and 200 ℃ corresponding to each endothermic peak, then increasing the temperature to the crystallization temperature at the heating rate of 50-100 ℃/hour, preserving heat for 1-2 hours at the initial temperature and the final temperature of 940 +/-50 ℃ of the crystallization reaction, and finally slowly reducing the temperature to the room temperature; and carefully grinding the sintered powder to obtain YAG nano powder. The examination shows that: the powder has uniform particle size, no agglomeration, a size of about 70nm and no transition phase.
Description
Technical field
The present invention relates to the preparation of yttrium aluminum garnet (hereinafter to be referred as YAG) nano powder, especially the sintering method of YAG precursor powder.
Background technology
The YAG crystalline ceramics is compared with the YAG monocrystalline, because the characteristics that have easy preparation, low cost, large size, can be mass-produced are widely used in solid laser medium material, high-temperature structural components and high-temperature infrared and survey with fields such as windows.Prepare high performance YAG crystalline ceramics, need the YAG powder of excellent performance, require powder that high phase purity is arranged, particle size is at nano level, and big or small homogeneous there is no reunion, and all these performances are all closely related with the sintering method of powder.
Traditional preparation process YAG nano powder often adopts solid reaction process, is with Al
2O
3And Y
2O
3Powder mixes by stoichiometric ratio, and long calcining obtains under 1600 ℃, and the formation of YAG phase will be passed through a series of following reaction: (1)
(YAM，900～1100℃)；
(2)
(YAP，1100～1250℃)；
(3)
(YAG，1400～1600℃)。
The YAG powder granule that finally makes is thick, and it is serious to reunite, and also has transition phase to exist, and is unfavorable for the YAG pottery that processability is good, thereby needs the new YAG powder preparation method of development.
Coprecipitation method is the common method of preparation ceramic powder, its advantage is that various compositions can uniform mixing, because the preparation condition of precursor and sintering method be to final particulate size, reunion situation and purity important influence mutually, so explore suitable preparation condition and sintering method has very practical meaning.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of YAG nano powder requires prepared YAG nano powder even particle size, does not have and reunites, and particle diameter is at 60～100nm, and no transition phase exists, the ceramic raw material of the YAG nano powder that obtained performance is good.
Technical solution of the present invention is as follows:
1. prepare the material solution of YAG nano powder: Al (NO
3)
3Solution, Y (NO
3)
3Solution and NH
4HCO
3Solution is pressed Y
3+, Al
3+The stoichiometric ratio of ion in YAG measured the Al (NO of respective volume
3)
3Solution and Y (NO
3)
3Solution mixes the formation mixing solutions, measure 〉=1.6 times to the NH of mixed liquor volume
4HCO
3Solution for standby;
2. described mixing solutions is added drop-wise to described NH with the speed of≤3 ml/min
4HCO
3In the solution, stir fully simultaneously, ageing forms precipitated liquid then;
3. the precipitated liquid of gained is carried out vacuum filtration, in suction filtration with deionized water rinsing at least 4 times, alcohol flushing at least 2 times;
4.: gained white precipitate behind the suction filtration is carried out long-time drying at low temperature 20-50 ℃, in the corundum mortar, grind the acquisition powder again;
5. the powder of gained is transferred in the corundum crucible with a lid, place then in the silicon carbon rod electric furnace, temperature rise rate with 200～300 ℃/hour rises to 850 ℃ from room temperature earlier in air atmosphere, and need respectively under 130 ℃ and 200 ℃ of each endotherm(ic)peak corresponding temperatures, respectively to be incubated 0.5～1 hour, rise to crystallization temperature with 50～100 ℃/hour temperature rise rate then, and respectively be incubated 1-2 hour for 940 ± 50 ℃ the initial of this crystallization and termination temperature, slowly reduce to room temperature at last;
6. sintering gained powder is transferred in the corundum mortar and carefully grinds, obtain required YAG nano-powder.
Described material solution and concentration are as follows:
The feed composition volumetric molar concentration
Al (NO
3)
3Solution 0.25～0.30
Y (NO
3)
3Solution is Al (NO
3)
30.6 times of strength of solution
NH
4HCO
3Solution 1.20～1.50
Measure Al (NO by 1: 1 volume ratio
3)
3And Y (NO
3)
3Solution mixes the formation mixing solutions, measure 〉=3.2 times to Al (NO
3)
3The NH of liquor capacity
4HCO
3Solution for standby.
Described mixing solutions is added drop-wise to described NH with the speed of≤3 ml/min
4HCO
3During solution, the pH of precipitation system should be greater than 7.8.
Technique effect of the present invention:
In the preparation process of precursor, owing to limit rate of addition≤3ml/min, the pH that makes precipitation system guarantees Y all the time greater than 7.8
3+, Al
3+Respectively with Y
2(CO
3)
3, NH
4Al (OH)
2CO
3Form precipitation, thereby reduced the sintering temperature of final powder;
In the drying process of precursor, adopt long-time at low temperatures exsiccant method, make in the washing process volatile matter such as moisture of remaining ethanol and trace can spontaneous evaporation, thereby weaken capillary force, suppress the intergranular soft-agglomerated hard aggregation that develops into of precursor, the dispersiveness of sintered powder is improved greatly;
In the sintering process of precursor, generate YAG polycrystalline phase transition temperature interval and be generally crystallization temperature ± 50 ℃, be incubated respectively by terminal temperature, and temperature rise rate is 50-100 ℃/h at crystallization, thereby make transition phase change the YAG phase into, guaranteed the purity of final powder phase.
The experiment proved that: the YAG nano-powder of gained of the present invention, even particle size does not have reunion, and no transition phase exists, and illustrates that this nano powder can be used as a kind of good ceramic raw material.
Description of drawings
Fig. 1 is the TG/DSC graphic representation of the YAG nano powder precursor of embodiment of the invention preparation;
Fig. 2 is the XRD figure of the YAG nano powder of embodiment of the invention preparation;
Embodiment
The invention will be further described below in conjunction with embodiment and comparative example, but should not limit protection scope of the present invention with this.
Embodiment 1:
The preparation method of YAG nano powder of the present invention comprises the following steps:
1. prepare the material solution of YAG nano powder by following concentration:
Feed composition volumetric molar concentration (mol/l)
Al (NO
3)
3Solution 0.25～0.30
Y (NO
3)
3Solution is Al (NO
3)
30.6 times of strength of solution
NH
4HCO
3Solution 1.20～1.50
As required, by 1: 1 volume ratio, measure Al (NO
3)
3And Y (NO
3)
3Solution mixes the formation mixing solutions, measure 〉=3.2 times to Al (NO
3)
3The NH of liquor capacity
4HCO
3Solution for standby;
2. described mixing solutions is added drop-wise to described NH with the speed of≤3ml/min
4HCO
3In the solution, stir fully simultaneously, be added dropwise to complete back 2 hours and stop to stir, ageing is 12 hours then, and the pH of precipitation system should form precipitated liquid greater than 7.8;
3. the precipitated liquid of gained is carried out vacuum filtration, in suction filtration, use deionized water rinsing 4 times, alcohol flushing 2 times;
4.: with gained white precipitate behind the suction filtration at low temperature 30 ℃ of dryings 48 hours, in the corundum mortar, grind the acquisition powder again;
5. the powder of gained is transferred in the corundum crucible with a lid, placed then in the silicon carbon rod electric furnace, the speed with 250 ℃/h in air atmosphere is warming up to 850 ℃, wherein respectively is incubated 0.5 hour at 130 ℃ and 200 ℃ respectively; Be warming up to 1000 ℃ with the speed of 100 ℃/h from 850 ℃ again, and respectively be incubated 1h at 900 ℃ and 1000 ℃ respectively; Reduce to room temperature with the speed of 100 ℃/h at last;
6. sintering gained powder is transferred in the corundum mortar and carefully grinds, obtain required YAG nano-powder.
Test result to the present embodiment nano powder is as follows:
The TG/DSC graphic representation of the YAG nano powder precursor of embodiment of the invention preparation as shown in Figure 1, XRD figure is as shown in Figure 2.The powder granule size does not evenly have reunion, and size is about 70nm, the approximate spheroid shape that is, and no transition phase exists.Illustrate that this nano powder can be used as a kind of raw material of good preparation crystalline ceramics.
The preparation technology of embodiment 2 to embodiment 8 is substantially the same manner as Example 1, and its processing parameter is as shown in table 1 below
The preparation condition of table 1.YAG nano powder
| The precursor drying conditions | The precursor sintering condition | Powder characteristics | ||||||
| Temperature (℃) | Soaking time (h) | Endotherm peak temperature insulation (h) | Crystallization terminal temperature insulation (h) | Particle diameter (nm) | Dispersed | |||
| 130 | 200℃ | 900 | 1000 | |||||
| Embodiment | ||||||||
| 2 | 20 | 72 | 0.5 | 0.5 | 1 | 1 | 60.4 | Excellent |
| Embodiment 3 | 25 | 60 | 0.5 | 0.5 | 1.5 | 1.5 | 78.1 | Excellent |
| Embodiment 4 | 30 | 48 | 0.5 | 0.5 | 2 | 2 | 92.6 | Excellent |
| Embodiment 5 | 35 | 36 | 0.75 | 0.75 | 1 | 1 | 66.3 | Very |
| Embodiment 6 | 40 | 24 | 0.75 | 0.75 | 1.5 | 1.5 | 80.5 | Very |
| Embodiment 7 | 45 | 12 | 1 | 1 | 1 | 1 | 67.9 | Very |
| Embodiment 8 | 50 | 6 | 1 | 1 | 1.5 | 1.5 | 81.7 | In |
The ☆ dispersiveness is observed by transmission electron microscope (TEM) and is determined
The ☆ particle diameter calculates definite by thanking to the Lay formula
Comparative example
Traditional preparation process YAG nano powder often adopts solid reaction process, specifically comprises the steps:
1. according to reaction formula
Determine the stoichiometry of each raw material, and strict weighing;
2. with the Y of weighing
2O
3, Al
2O
3Powder mixes, and adds analytically pure TEOS (tetraethyl silicate) as additive, and content is 0.5%, is that 95% ethanol is made grinding medium, high-purity ZrO with concentration
2Ball is made grinding element, carries out wet-milling;
3. wet-milling is good powder is dry 5h under 120 ℃;
4. dried powder is contained in the quartz boat 1600 ℃ of calcining 5h in the mobile oxygen atmosphere;
5. the powder that sinters is carried out careful grinding, obtain the YAG superfine powder.
Because solid state reaction can't be avoided the problem of powder raw material microcell lack of homogeneity and stoicheiometry mismatch, even in higher sintering temperature with under than long soaking time, the YAG powder still has a spot of transition phase to exist, and powder granule is thick, size also has significantly and reunites between 1～2 μ m.Illustrate that this powder is not suitable as the raw material of preparation crystalline ceramics.
Explanation is that above embodiment is only unrestricted in order to technical scheme of the present invention to be described at last.Although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (3)
1, a kind of preparation method of YAG nano powder is characterized in that this method comprises the following steps:
1. prepare the material solution of YAG nano powder: Al (NO
3)
3Solution, Y (NO
3)
3Solution and NH
4HCO
3Solution is pressed Y
3+, Al
3+The stoichiometric ratio of ion in YAG measured the Al (NO of respective volume
3)
3Solution and Y (NO
3)
3Solution mixes the formation mixing solutions, measure 〉=1.6 times to the NH of mixed liquor volume
4HCO
3Solution for standby;
2. described mixing solutions is added drop-wise to described NH with the speed of≤3 ml/min
4HCO
3In the solution, stir fully simultaneously, ageing forms precipitated liquid then;
3. the precipitated liquid of gained is carried out vacuum filtration, in suction filtration with deionized water rinsing at least 4 times, alcohol flushing at least 2 times;
4.: gained white precipitate behind the suction filtration is carried out long-time drying at low temperature 20-50 ℃, in the corundum mortar, grind the acquisition powder again;
5. the powder of gained is transferred in the corundum crucible with a lid, place then in the silicon carbon rod electric furnace, temperature rise rate with 200～300 ℃/hour rises to 850 ℃ from room temperature earlier in air atmosphere, and need respectively under 130 ℃ and 200 ℃ of each endotherm(ic)peak corresponding temperatures, respectively to be incubated 0.5～1 hour, rise to crystallization temperature with 50～100 ℃/hour temperature rise rate then, and respectively be incubated 1-2 hour for 940 ± 50 ℃ the initial of this crystallization and termination temperature, slowly reduce to room temperature at last;
6. sintering gained powder is transferred in the corundum mortar and carefully grinds, obtain required YAG nano-powder.
2, the preparation method of YAG nano powder according to claim 1 is characterized in that described material solution and concentration are as follows:
The feed composition volumetric molar concentration
Al (NO
3)
3Solution 0.25～0.30
Y (NO
3)
3Solution is Al (NO
3)
30.6 times of strength of solution
NH
4HCO
3Solution 1.20～1.50
Measure Al (NO by 1: 1 volume ratio
3)
3And Y (NO
3)
3Solution mixes the formation mixing solutions, measure 〉=3.2 times to Al (NO
3)
3The NH of liquor capacity
4HCO
3Solution for standby.
3, the preparation method of YAG nano powder according to claim 1 and 2 is characterized in that described mixing solutions is added drop-wise to described NH with the speed of≤3 ml/min
4HCO
3During solution, the pH of precipitation system should be greater than 7.8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510110760 CN1792805A (en) | 2005-11-25 | 2005-11-25 | Preparation method of yttrium aluminum garnet nano powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510110760 CN1792805A (en) | 2005-11-25 | 2005-11-25 | Preparation method of yttrium aluminum garnet nano powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1792805A true CN1792805A (en) | 2006-06-28 |
Family
ID=36804478
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510110760 Pending CN1792805A (en) | 2005-11-25 | 2005-11-25 | Preparation method of yttrium aluminum garnet nano powder |
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| Country | Link |
|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100441658C (en) * | 2007-02-06 | 2008-12-10 | 江苏苏博特新材料股份有限公司 | Method of preparing yttrium aluminium garnet fluorescent powder |
| CN102701722A (en) * | 2012-02-13 | 2012-10-03 | 中国科学院上海硅酸盐研究所 | Method for producing yttrium aluminum garnet (YAG) nanopowder through fractional precipitation method |
| CN102898148A (en) * | 2012-10-17 | 2013-01-30 | 西南科技大学 | Preparation method for yttrium aluminium garnet nano-powder |
| CN104341152A (en) * | 2013-07-25 | 2015-02-11 | 中国科学院宁波材料技术与工程研究所 | Preparation method for garnet phase nano-powder |
| CN115368144A (en) * | 2022-07-11 | 2022-11-22 | 苏州隐冠半导体技术有限公司 | Piezoelectric ceramic superfine powder, preparation method and piezoelectric ceramic diaphragm |
-
2005
- 2005-11-25 CN CN 200510110760 patent/CN1792805A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100441658C (en) * | 2007-02-06 | 2008-12-10 | 江苏苏博特新材料股份有限公司 | Method of preparing yttrium aluminium garnet fluorescent powder |
| CN102701722A (en) * | 2012-02-13 | 2012-10-03 | 中国科学院上海硅酸盐研究所 | Method for producing yttrium aluminum garnet (YAG) nanopowder through fractional precipitation method |
| CN102898148A (en) * | 2012-10-17 | 2013-01-30 | 西南科技大学 | Preparation method for yttrium aluminium garnet nano-powder |
| CN104341152A (en) * | 2013-07-25 | 2015-02-11 | 中国科学院宁波材料技术与工程研究所 | Preparation method for garnet phase nano-powder |
| CN115368144A (en) * | 2022-07-11 | 2022-11-22 | 苏州隐冠半导体技术有限公司 | Piezoelectric ceramic superfine powder, preparation method and piezoelectric ceramic diaphragm |
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