CN111574215B - Method for preparing yttrium aluminum garnet powder - Google Patents
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- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 title claims abstract description 37
- 239000000843 powder Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 32
- 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 claims abstract description 30
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 69
- 239000000243 solution Substances 0.000 claims description 51
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 34
- 239000002243 precursor Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 238000006243 chemical reaction Methods 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 239000002244 precipitate Substances 0.000 claims description 24
- 229910052751 metal Inorganic materials 0.000 claims description 19
- 239000002184 metal Substances 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 17
- DEXZEPDUSNRVTN-UHFFFAOYSA-K yttrium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Y+3] DEXZEPDUSNRVTN-UHFFFAOYSA-K 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 16
- 229910052727 yttrium Inorganic materials 0.000 claims description 15
- 239000000725 suspension Substances 0.000 claims description 14
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 14
- 239000006228 supernatant Substances 0.000 claims description 10
- QBAZWXKSCUESGU-UHFFFAOYSA-N yttrium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QBAZWXKSCUESGU-UHFFFAOYSA-N 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 229910021645 metal ion Inorganic materials 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 claims description 5
- 239000012266 salt solution Substances 0.000 claims description 5
- 238000004448 titration Methods 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 abstract description 13
- 238000001914 filtration Methods 0.000 abstract description 9
- 238000001556 precipitation Methods 0.000 abstract description 9
- 239000006185 dispersion Substances 0.000 abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- 230000007062 hydrolysis Effects 0.000 abstract 1
- 238000006460 hydrolysis reaction Methods 0.000 abstract 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 16
- 239000002994 raw material Substances 0.000 description 7
- 239000012535 impurity Substances 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 239000001099 ammonium carbonate Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 2
- 235000012501 ammonium carbonate Nutrition 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 235000013877 carbamide Nutrition 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 229910009523 YCl3 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- PSNPEOOEWZZFPJ-UHFFFAOYSA-N alumane;yttrium Chemical compound [AlH3].[Y] PSNPEOOEWZZFPJ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 1
- -1 yttrium ions Chemical class 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
- C01F17/32—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 oxide or hydroxide being the only anion, e.g. NaCeO2 or MgxCayEuO
- C01F17/34—Aluminates, e.g. YAlO3 or Y3-xGdxAl5O12
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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Abstract
The invention discloses a method for preparing yttrium aluminum garnet powder,the chemical formula of the yttrium aluminum garnet is Y3Al5O12(ii) a The preparation method comprises the processes of solution preparation, precipitation, washing, mixing, hydrolysis, hydrothermal reaction, filtration, drying and calcination. The yttrium aluminum garnet polycrystalline powder prepared by the method has the advantages of high purity, accurate stoichiometric ratio, uniform components and uniform dispersion.
Description
Technical Field
The invention belongs to the technical field of polycrystalline ceramic powder preparation, and particularly relates to a method for preparing yttrium aluminum garnet powder.
Background
Yttrium aluminum garnet (Y)3Al5O12YAG) belongs to a cubic system, and the lattice parameter is 1.2 nm. YAG crystals are important laser host materials, and Nd-doped YAG (Nd: YAG) crystals are widely used in high power lasers.
At present, the YAG synthesis method is mainly a high-temperature solid-phase method, namely, a polycrystalline material of YAG is prepared by utilizing a component oxide solid-phase reaction method. The YAG polycrystalline material synthesized by the solid phase reaction method needs higher reaction temperature and longer reaction time, and the ball milling mixing is difficult to achieve uniform chemical composition, so that impurity phases are easy to introduce. Further, it has been reported that YAG powder is produced by a sol-gel method, a combustion method, etc. (CN 201410073804.4 is a method of producing nano-sized yttrium aluminum garnet powder by adding ammonium citrate; CN03129583.5 is a method of producing yttrium aluminum garnet nano-powder). The YAG powder can be obtained at a relatively low temperature by the methods, but the methods have some disadvantages, such as addition of complexing agents such as citric acid and triethanolamine is often required, so that impurity elements such as N or C are inevitably introduced, the purity of the final YAG product is influenced, particle agglomeration is possibly caused in the drying and roasting processes, and the YAG powder with uniform dispersion is difficult to form. There is also a document (CN 201110005422.4 a method for preparing yttrium aluminum garnet powder and a reaction device thereof) that a metal nitrate is prepared into mixed solutions with different concentrations, and the mixed solutions are added into a plasma arc, and a final product is obtained by high-frequency induction thermal plasma instant high-temperature gasification. Although the method avoids introducing impurity elements such as N or C, the method has high requirements on equipment, relatively complex process and difficult operation.
In recent years, a liquid-phase coprecipitation method has been widely used for synthesizing YAG powder. However, the coprecipitation method is also used for preparing the polycrystalline YAG powderThere are some significant disadvantages: (1) the precursor powder with accurate stoichiometric ratio and uniform components is difficult to form due to the difference of solubility product and sedimentation rate; (2) it is difficult to control the pH to an appropriate value for Y+3、Al+3Complete precipitation is carried out at the same time; (3) the drying and roasting process may cause particle agglomeration, and the YAG powder with uniform dispersion is difficult to obtain; (4) the use of precipitants such as ammonia water, urea, ammonium carbonate and ammonium bicarbonate inevitably causes impurity elements such as N or C to be mixed in the final product, and the purity of the obtained YAG product is influenced; (5) the filtering and washing processes of the precipitation precursor inevitably cause the loss of metal ions, and the yttrium aluminum garnet polycrystalline powder with high purity and accurate stoichiometric ratio is difficult to obtain.
Disclosure of Invention
The invention aims to provide yttrium aluminum garnet powder (chemical formula is Y) with high purity, accurate stoichiometric ratio, uniform components and uniform dispersion3Al5O12) The yttrium aluminum garnet polycrystalline powder prepared by the method has the advantages of high purity, accurate stoichiometric ratio, uniform components and uniform dispersion.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing yttrium aluminum garnet powder comprises the following steps:
(1) according to the formula Y of yttrium aluminum garnet3Al5O12Respectively weighing yttrium metal salt and aluminum isopropoxide according to a molar ratio of Y to Al =3 to 5;
(2) respectively dissolving yttrium metal salt and NaOH in deionized water to respectively obtain yttrium metal salt solution and NaOH solution; dissolving aluminum isopropoxide in absolute ethyl alcohol or isopropanol to obtain an alcoholic solution of aluminum isopropoxide;
(3) slowly dropwise adding NaOH solution into yttrium metal salt solution at room temperature under continuous stirring until the pH value of the solution reaches 11-12, and stopping titration to obtain yttrium hydroxide precipitate precursor suspension;
(4) centrifuging the obtained suspension at high speed, separating supernatant (the supernatant is slowly sucked out with a syringe or a suction tube without usingTouching the lower filter cake), then adding a proper amount of deionized water to clean the lower filter cake, after cleaning, performing centrifugal separation on the suspension of the precipitation precursor again, and repeating the process for 2-3 times until the redundant Na in the solution is removed+Is thoroughly washed away to finally obtain a yttrium hydroxide precipitate precursor;
(5) transferring the obtained yttrium hydroxide precipitate precursor into an alcohol solution of aluminum isopropoxide, and continuously stirring to obtain a metal ion mixed solution;
(6) putting the metal mixed solution into a high-pressure reaction kettle with a stainless steel lining, adding a proper amount of deionized water, and fully stirring to uniformly mix the metal mixed solution;
(7) sealing the high-pressure reaction kettle, putting the sealed high-pressure reaction kettle into a muffle furnace or an oven, taking out the high-pressure reaction kettle after high-temperature reaction, and naturally cooling the high-pressure reaction kettle to room temperature;
(8) centrifuging or filtering and separating the cooled product to obtain yttrium aluminum garnet powder with high purity, accurate stoichiometric ratio, uniform components and uniform dispersion;
in the step (1), the salt of the metal yttrium is anhydrous yttrium chloride or yttrium nitrate hexahydrate Y (NO)3)3·6H2O。
In the step (1), the yttrium metal salt and aluminum isopropoxide are dried in an oven at 110-160 ℃ for 24-36 h, and then weighed.
In the step (2), the concentration of the salt solution of the metal yttrium is 0.5-1.0 mol/L; the concentration of the NaOH solution is 0.5-1.0 mol/L; the concentration of the alcoholic solution of the aluminum isopropoxide is 2.0-3.0 mol/L;
in the step (6), the addition amount of water is 50-70% of the volume of the stainless steel lining.
In the step (7), the reaction temperature is 310-350 ℃, and the reaction time is 5-24 h.
The invention has the following advantages: (1) for reaction raw material Y (NO) before experiment3)3·6H2Fully drying O and aluminum isopropoxide at 120-160 ℃, and avoiding weighing errors of the sample caused by water absorption; (2) precipitating agents such as ammonia water, urea, ammonium carbonate, ammonium bicarbonate and the like are not used, so that impurity elements such as N or C and the like are prevented from being introduced; (3) addingThe excessive NaOH solution can ensure that the metal yttrium ions are completely precipitated; (4) the method adopts the mode of 'centrifugal separation → sucking out supernatant liquid → directly transferring to aluminum isopropoxide solution', so as to avoid the loss of metal yttrium in the yttrium hydroxide precipitate precursor caused by the conventional modes of filtering, washing and the like; (5) the aluminum isopropoxide hydrolysate is directly fed into a high-temperature furnace for hydrothermal reaction without being filtered, washed and dried, so that the consumption of raw materials is low, the pollution is less, and the purity of the obtained product is high; (6) the low-temperature hydrothermal reaction is adopted, particle agglomeration possibly caused in the high-temperature roasting process is avoided, and the YAG powder which is fluffy, uniformly dispersed and free of agglomeration is easily formed, so that the yttrium aluminum garnet powder with high purity, accurate stoichiometric ratio, uniform components and uniform dispersion can be prepared, and the method is an ideal method for preparing the multi-element oxide.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) photograph of the yttrium aluminum garnet powder prepared in example 1.
Fig. 2 is an X-ray diffraction (XRD) pattern of the yttrium aluminum garnet powder prepared in example 1.
Detailed Description
The following examples are intended to further illustrate the process features of the present invention and are not intended to limit the invention.
Example l
(1) Reaction raw material Y (NO)3)3·6H2O and aluminum isopropoxide were thoroughly dried at 160 ℃. According to the formula Y3Al5O1210.814g of yttrium nitrate hexahydrate, 9.600g of aluminum isopropoxide and 0.6g of NaOH were weighed out separately.
(2) Dissolving weighed yttrium nitrate hexahydrate in 30ml of deionized water, dissolving NaOH in 30ml of deionized water, and dissolving aluminum isopropoxide in 20ml of absolute ethyl alcohol to prepare corresponding solution.
(3) Slowly dripping NaOH solution into yttrium nitrate solution while stirring at room temperature until the pH value of the solution is 12, and stopping titration to obtain yttrium hydroxide precipitate precursor suspension.
(4) And (3) centrifugally separating the obtained suspension of the precipitate precursor at a high speed, slowly sucking out supernatant by using an injector or a suction pipe, adding deionized water to wash the lower filter cake, centrifugally separating and washing again, and repeating the steps for 3 times to obtain the yttrium hydroxide precipitate precursor.
(5) And transferring the precipitation precursor into an ethanol solution of aluminum isopropoxide, and uniformly stirring to obtain a mixed solution of metal ions.
(6) And (3) putting the mixed solution into a 50mL high-pressure reaction kettle with a stainless steel lining, adding deionized water to enable the volume of the solution to reach 35mL, and fully stirring to enable the solution to be uniformly mixed.
(7) And sealing the high-pressure reaction kettle, putting the high-pressure reaction kettle into a muffle furnace, reacting for 24 hours at 320 ℃, taking out, and naturally cooling to room temperature.
(8) And then filtering and washing the cooled product, and placing the product in a 60 ℃ oven for vacuum drying for 24 hours to obtain loose yttrium aluminum garnet powder.
And observing the single particle size and morphology of the obtained yttrium aluminum garnet powder by using a HITACHI S-4300 Scanning Electron Microscope (SEM). The obtained powder was subjected to phase analysis using Bruker D8 advanced Rigaku D/Max-rA X-ray diffractometer (XRD). The results are shown in FIGS. 1 and 2, respectively.
Example 2
(1) Reaction raw material Y (NO)3)3·6H2O and aluminum isopropoxide were thoroughly dried at 140 ℃. According to the formula Y3Al5O125.632g of yttrium nitrate hexahydrate, 5g of aluminum isopropoxide and 0.3g of NaOH were weighed out separately.
(2) Dissolving weighed yttrium nitrate hexahydrate in 15ml of deionized water, dissolving NaOH in 30ml of deionized water, and dissolving aluminum isopropoxide in 25ml of absolute ethyl alcohol to prepare corresponding solution.
(3) Slowly dripping NaOH solution into yttrium nitrate solution while stirring at room temperature until the pH value of the solution is 12, and stopping titration to obtain yttrium hydroxide precipitate precursor suspension.
(4) And (3) centrifugally separating the obtained suspension of the precipitate precursor at a high speed, slowly sucking out supernatant by using an injector or a suction pipe, adding deionized water to wash the lower filter cake, centrifugally separating and washing again, and repeating the steps for 3 times to obtain the yttrium hydroxide precipitate precursor.
(5) And transferring the precipitation precursor into an ethanol solution of aluminum isopropoxide, and uniformly stirring to obtain a mixed solution of metal ions.
(6) The mixed solution is placed in a 50mL stainless steel liner, deionized water is added to enable the volume of the solution to reach 35mL, and the solution is fully stirred to be uniformly mixed.
(7) And sealing the high-pressure reaction kettle, putting the high-pressure reaction kettle into a muffle furnace, reacting for 24 hours at 330 ℃, taking out, and naturally cooling to room temperature.
(8) And then filtering and washing the cooled product, and placing the product in a 60 ℃ oven for vacuum drying for 24 hours to obtain loose yttrium aluminum garnet powder.
Example 3
(1) Reaction raw material Y (NO)3)3·6H2O and aluminum isopropoxide were thoroughly dried at 120 ℃. According to the formula Y3Al5O124.055g of yttrium nitrate hexahydrate, 3.600g of aluminum isopropoxide and 0.6g of NaOH were weighed out separately.
(2) Dissolving weighed yttrium nitrate hexahydrate in 20ml of deionized water, dissolving NaOH in 30ml of deionized water, and dissolving aluminum isopropoxide in 20ml of absolute ethyl alcohol to prepare corresponding solution.
(3) Slowly dripping NaOH solution into yttrium nitrate solution while stirring at room temperature until the pH value of the solution is 12, and stopping titration to obtain yttrium hydroxide precipitate precursor suspension.
(4) And (3) centrifugally separating the obtained precipitate precursor suspension at a high speed, slowly sucking out supernatant by using an injector or a suction pipe, adding deionized water to wash the lower filter cake, centrifugally separating and washing again, and repeating the steps for 3 times to obtain the yttrium hydroxide precipitate precursor.
(5) And transferring the precipitation precursor into an ethanol solution of aluminum isopropoxide, and uniformly stirring to obtain a mixed solution of metal ions.
(6) The mixed solution is placed in a 50mL stainless steel liner, deionized water is added to enable the volume of the solution to reach 35mL, and the solution is fully stirred to be uniformly mixed.
(7) And sealing the high-pressure reaction kettle, putting the high-pressure reaction kettle into a muffle furnace, reacting for 24 hours at 320 ℃, taking out, and naturally cooling to room temperature.
(8) And filtering and washing the cooled product, and placing the product in a 60 ℃ oven for vacuum drying for 24 hours to obtain loose yttrium aluminum garnet powder.
Example 4
(1) Reaction raw material Y (NO)3)3·6H2And fully drying the O and the aluminum isopropoxide at 120-160 ℃. According to the formula Y3Al5O123.380g of yttrium nitrate hexahydrate, 3.000g of aluminum isopropoxide and 0.6g of NaOH were weighed out separately.
(2) Dissolving weighed yttrium nitrate hexahydrate in 18ml of deionized water, dissolving NaOH in 30ml of deionized water, and dissolving aluminum isopropoxide in 20ml of absolute ethyl alcohol to prepare corresponding solution.
(3) Slowly dripping NaOH solution into yttrium nitrate solution at room temperature while stirring for one year, and stopping dripping until the pH value of the solution is 12 to obtain yttrium hydroxide precipitate precursor suspension.
(4) And (3) centrifugally separating the obtained precipitate precursor suspension at a high speed, slowly sucking out supernatant by using an injector or a suction pipe, adding deionized water to wash the lower filter cake, centrifugally separating and washing again, and repeating the steps for 3 times to obtain the yttrium hydroxide precipitate precursor.
(5) And transferring the precipitation precursor into an ethanol solution of aluminum isopropoxide, and uniformly stirring to obtain a mixed solution of metal ions.
(6) The mixed solution is placed in a 50mL stainless steel liner, deionized water is added to enable the volume of the solution to reach 35mL, and the solution is fully stirred to be uniformly mixed.
(7) And sealing the high-pressure reaction kettle, putting the high-pressure reaction kettle into a muffle furnace, reacting for 24 hours at 320 ℃, taking out, and naturally cooling to room temperature.
(8) And filtering and washing the cooled product, and placing the product in a 60 ℃ oven for vacuum drying for 24 hours to obtain loose yttrium aluminum garnet powder.
Example 5
(1) Reaction raw material YCl3And fully drying the mixture and aluminum isopropoxide at 120-160 ℃. According to the formula Y3Al5O124.350g of yttrium chloride and 3.000g of aluminum isopropoxide and 0.6g of NaOH were weighed out separately.
(2) Dissolving weighed yttrium chloride in 18ml of deionized water, dissolving NaOH in 30ml of deionized water, and dissolving aluminum isopropoxide in 20ml of absolute ethyl alcohol to prepare corresponding solution.
(3) Slowly dripping NaOH solution into yttrium chloride solution at room temperature while stirring for one year, and stopping dripping until the pH value of the solution is 12 to obtain yttrium hydroxide precipitate precursor suspension.
(4) And (3) centrifugally separating the obtained precipitate precursor suspension at a high speed, slowly sucking out supernatant by using an injector or a suction pipe, adding deionized water to wash the lower filter cake, centrifugally separating and washing again, and repeating the steps for 3 times to obtain the yttrium hydroxide precipitate precursor.
(5) And transferring the precipitation precursor into an ethanol solution of aluminum isopropoxide, and uniformly stirring to obtain a mixed solution of metal ions.
(6) The mixed solution is placed in a 50mL stainless steel liner, deionized water is added to enable the volume of the solution to reach 35mL, and the solution is fully stirred to be uniformly mixed.
(7) And sealing the high-pressure reaction kettle, putting the high-pressure reaction kettle into a muffle furnace, reacting for 24 hours at 320 ℃, taking out, and naturally cooling to room temperature.
(8) And filtering and washing the cooled product, and placing the product in a 60 ℃ oven for vacuum drying for 24 hours to obtain loose yttrium aluminum garnet powder.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (4)
1. A method for preparing yttrium aluminum garnet powder is characterized by comprising the following steps: which comprises the following steps:
(1) putting the yttrium metal salt and aluminum isopropoxide into a drying oven at 110-160 ℃ for dryingDrying for 24-36 h, and then obtaining the yttrium aluminum garnet with the chemical formula Y3Al5O12Respectively weighing yttrium metal salt and aluminum isopropoxide according to a molar ratio of Y to Al =3 to 5;
(2) respectively dissolving yttrium metal salt and NaOH in water to respectively obtain 0.5-1.0 mol/L yttrium metal salt solution and 0.5-1.0 mol/L NaOH solution; dissolving aluminum isopropoxide in absolute ethyl alcohol or isopropanol to obtain 2.0-3.0 mol/L of an alcohol solution of the aluminum isopropoxide;
(3) slowly dropwise adding NaOH solution into yttrium metal salt solution at room temperature under continuous stirring until the pH value of the solution reaches 11-12, and stopping titration to obtain yttrium hydroxide precipitate precursor suspension;
(4) centrifuging the obtained precipitate precursor turbid liquid at a high speed, separating out supernatant, slowly sucking out the supernatant by using a syringe or a suction pipe without touching a lower filter cake, adding water to clean the lower filter cake, centrifuging the precipitate precursor turbid liquid again after cleaning, repeating the steps for 2-3 times until redundant Na in the solution is removed+Is thoroughly washed away to finally obtain a yttrium hydroxide precipitate precursor;
(5) transferring the obtained yttrium hydroxide precipitate precursor into an alcohol solution of aluminum isopropoxide, and continuously stirring to obtain a metal ion mixed solution;
(6) putting the metal mixed solution into a high-pressure reaction kettle with a stainless steel lining, adding water, and fully stirring to uniformly mix the metal mixed solution;
(7) sealing the high-pressure reaction kettle, putting the sealed high-pressure reaction kettle into a muffle furnace or an oven, reacting at the high temperature of 310-350 ℃ for 5-24 h, taking out, and naturally cooling to room temperature;
(8) and (4) centrifuging or performing suction filtration separation on the cooled product to obtain yttrium aluminum garnet powder.
2. The method of claim 1, wherein the yttrium aluminum garnet powder comprises: in the step (1), the salt of the metal yttrium is anhydrous yttrium chloride or yttrium nitrate hexahydrate.
3. The method of claim 1, wherein the yttrium aluminum garnet powder comprises: in the step (6), the addition amount of water is 50-70% of the volume of the stainless steel lining.
4. The method of claim 1, wherein the yttrium aluminum garnet powder comprises: the water used in each step was deionized water.
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