CN113716961A - Rare earth tantalate RE prepared based on molten salt growth method3TaO7Spherical powder and preparation method thereof - Google Patents
Rare earth tantalate RE prepared based on molten salt growth method3TaO7Spherical powder and preparation method thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 137
- 150000003839 salts Chemical class 0.000 title claims abstract description 90
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 55
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 70
- 238000000034 method Methods 0.000 claims abstract description 59
- 238000001354 calcination Methods 0.000 claims abstract description 56
- 239000002994 raw material Substances 0.000 claims abstract description 51
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 45
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 43
- 238000000498 ball milling Methods 0.000 claims description 39
- 238000007873 sieving Methods 0.000 claims description 38
- 239000000047 product Substances 0.000 claims description 35
- 239000008367 deionised water Substances 0.000 claims description 34
- 229910021641 deionized water Inorganic materials 0.000 claims description 34
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 29
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 26
- 239000000706 filtrate Substances 0.000 claims description 22
- 150000003841 chloride salts Chemical class 0.000 claims description 18
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 16
- 239000011780 sodium chloride Substances 0.000 claims description 15
- 238000012360 testing method Methods 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 239000003153 chemical reaction reagent Substances 0.000 claims description 11
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- ZIKATJAYWZUJPY-UHFFFAOYSA-N thulium (III) oxide Inorganic materials [O-2].[O-2].[O-2].[Tm+3].[Tm+3] ZIKATJAYWZUJPY-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 3
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 claims description 3
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 3
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 claims description 3
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 3
- 229910003443 lutetium oxide Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 3
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 8
- 238000003786 synthesis reaction Methods 0.000 abstract description 8
- 239000000919 ceramic Substances 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 3
- 229910052715 tantalum Inorganic materials 0.000 abstract description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002002 slurry Substances 0.000 description 32
- 238000005303 weighing Methods 0.000 description 22
- 101710134784 Agnoprotein Proteins 0.000 description 9
- 239000013078 crystal Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical class [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000012720 thermal barrier coating Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000012798 spherical particle Substances 0.000 description 3
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical group [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000011805 ball Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- -1 rare earth ions Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
- 238000007751 thermal spraying Methods 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
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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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
- C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- 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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- 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
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Abstract
The invention belongs to the technical field of ceramic powder preparation, and particularly relates to a rare earth tantalate RE prepared based on a molten salt growth method3TaO7Spherical powder and a preparation method thereof. The scheme of the invention provides a rare earth tantalate RE prepared based on a molten salt growth method3TaO7Spherical powder, rare earth oxide RE2O3And Ta tantalum pentoxide2O5Two raw materials, corresponding preparation method, rare earth tantalate RE synthesized by molten salt method3TaO7The spherical powder has high purity and low synthesis temperature. In addition, the method can control the morphology and the particle size of the powder by controlling the proportion of the molten salt to the raw material, the molten salt components, the calcination temperature and the calcination time, and obtain the rare earth tantalum with high sphericity rate and good fluidityAcid salt RE3TaO7Spherical powder. In addition, the rare earth tantalate RE prepared by the invention3TaO7The spherical powder has the characteristics of uniform particle size, excellent performance, stable quality, strong controllability, suitability for industrial production and the like.
Description
Technical Field
The invention belongs to the technical field of ceramic powder preparation, and particularly relates to a rare earth tantalate RE prepared based on a molten salt growth method3TaO7Spherical powder and a preparation method thereof.
Background
RE3TaO7And RE2Zr2O7Having a similar crystal structure, in most cases RE3TaO7(RE = La-Dy, Y) is an orthorhombic phase (ordered), i.e. a cryo-magnesia type structure, with the remainder of the rare earth ions having a smaller radius RE3TaO7(RE = Ho-Lu) ceramic having a cubic fluorite structure (disorder), in RE3TaO7Wherein the cation vacancy of 2/3 and the rare earth atom of 1/3 form a rare earth atom position, the cation defect concentration at the rare earth atom position is 2/3, and a Ta atom coordinates with 6O atoms to form a TaO6Octahedron, structure formed therefrom and RE of orthorhombic phase3TaO7The crystal structure is similar.
Chinese patent CN109437927A discloses a rare earth tantalum/niobate (RE)3Ta/NbO7) The ceramic powder and the preparation method thereof have the problems of low powder purity, high synthesis temperature, loss in the centrifugal spray granulation process and the like in the calcination process.
Therefore, the rare earth tantalate RE prepared by the prior art is aimed at3TaO7The invention develops a rare earth tantalate RE prepared based on a molten salt method3TaO7The spherical powder and the preparation method have the advantages of low synthesis temperature, high sphericity rate, good fluidity and excellent thermal and mechanical properties.
Disclosure of Invention
The first purpose of the invention is to provide a rare earth tantalate RE prepared based on a molten salt method3TaO7Spherical powder;
the invention also aims to provide the rare earth tantalate RE prepared based on the molten salt method3TaO7A preparation method of spherical powder;
the first object of the present invention is achieved by the powdered rare earth oxide RE2O3And Ta tantalum pentoxide2O5Two kinds of raw materials.
Another object of the invention is achieved in that the method comprises the steps of:
the method specifically comprises the following steps:
(1) rare earth oxide RE2O3And Ta tantalum pentoxide2O5Mixing the raw materials, molten salt and deionized water in a ball milling tank, adding zirconia balls, and performing ball milling by a planetary ball mill until the raw materials are uniformly mixed; sequentially carrying out filter pressing, drying and sieving treatment on the mixed powder, and then calcining;
(2) cooling to room temperature with the furnace, taking out the powder, repeatedly cleaning the obtained product with heated deionized water to remove excessive chloride salt until the filtrate does not contain Cl-Until the end;
(3) filtering, drying and sieving the washed powder to obtain the rare earth tantalate RE with the required particle size3TaO7Spherical powder.
The scheme of the invention provides a rare earth tantalate RE prepared based on a molten salt growth method3TaO7Spherical powder and preparation method thereof, and rare earth oxide RE of powder2O3And Ta tantalum pentoxide2O5Two kinds of raw materials. Will be provided withRare earth oxide RE2O3And Ta tantalum pentoxide2O5Mixing the raw materials, molten salt and deionized water in a ball milling tank, adding zirconia balls, and performing ball milling by a planetary ball mill until the raw materials are uniformly mixed; sequentially carrying out filter pressing, drying and sieving treatment on the mixed powder, and then calcining; cooling to room temperature with the furnace, taking out the powder, repeatedly cleaning the obtained product with heated deionized water to remove excessive chloride salt until the filtrate does not contain Cl-Until the end; filtering, drying and sieving the washed powder to obtain the rare earth tantalate RE with the required particle size3TaO7Spherical powder. That is to say, the spherical powder with high spherical rate and good fluidity is prepared by changing the calcining temperature, the calcining time and the molten salt proportion so as to improve the thermal property and the mechanical property of the spherical powder used as the thermal barrier coating. The method has the advantages of low synthesis temperature, short reaction time, simple process, high purity of the synthesized product, controllable crystal form and shape of the powder particles, no agglomeration, easy dispersion and the like.
That is, the rare earth tantalate RE synthesized by the molten salt method according to the scheme of the invention3TaO7The spherical powder has high purity and low synthesis temperature. In addition, the method can control the morphology and the particle size of the powder by controlling the proportion of the molten salt to the raw material, the molten salt components, the calcination temperature and the calcination time, and obtain the rare earth tantalate RE with high sphericity rate and good fluidity3TaO7Spherical powder. In addition, the rare earth tantalate RE prepared by the invention3TaO7The spherical powder has the characteristics of uniform particle size, excellent performance, stable quality, strong controllability, suitability for industrial production and the like.
Drawings
FIG. 1 shows a rare earth tantalate RE prepared based on a molten salt growth method3TaO7Preparation of Y by molten salt method of preparation of spherical powder3TaO7Obtaining an XRD map schematic diagram;
FIG. 2 shows a rare earth tantalate RE prepared based on a molten salt growth method3TaO7Molten salt method for preparing Y from spherical powder3TaO7Obtaining an SEM map schematic diagram;
FIG. 3 shows a rare earth tantalate RE prepared based on a molten salt growth method3TaO7Calcination time and Y in the preparation of spherical powder3TaO7The relationship map of the particle size is shown.
Detailed Description
The invention will be further described with reference to the drawings and examples, but the invention is not limited thereto in any way, and any modification or improvement based on the teaching of the invention is within the scope of the invention.
As shown in figures 1-3, the invention provides a rare earth tantalate RE prepared based on a molten salt method3TaO7Spherical powder, the rare earth oxide RE of the powder2O3And Ta tantalum pentoxide2O5Two kinds of raw materials.
The rare earth oxide RE2O3And Ta tantalum pentoxide2O5In a molar ratio of 3: 1; the rare earth oxide RE2O3And Ta tantalum pentoxide2O5The particle size of (2) is 15-60 mu m.
The rare earth oxide RE2O3The method specifically comprises the following steps: y is2O3、La2O3、Nd2O3、Pm2O3、Sm2O3、Eu2O3、Gd2O3、Tb2O3、Dy2O3、Ho2O3、Er2O3、Tm2O3、Yb2O3、Lu2O3Any one or more of them in combination.
The invention also provides a rare earth tantalate RE prepared based on a molten salt growth method3TaO7The preparation method of the spherical powder comprises the following steps:
(1) rare earth oxide RE2O3And Ta tantalum pentoxide2O5Mixing the raw materials, molten salt and deionized water in a ball mill, adding zirconia balls and passing through planetary ballsBall milling is carried out by a mill until the mixture is uniform; sequentially carrying out filter pressing, drying and sieving treatment on the mixed powder, and then calcining;
(2) cooling to room temperature with the furnace, taking out the powder, repeatedly cleaning the obtained product with heated deionized water to remove excessive chloride salt until the filtrate does not contain Cl-Until the end;
(3) filtering, drying and sieving the washed powder to obtain the rare earth tantalate RE with the required particle size3TaO7Spherical powder.
The rare earth oxide RE in the step (1)2O3And Ta tantalum pentoxide2O5In a molar ratio of 3: 1, the mass ratio of the raw materials to the molten salt is 1-10: 1-5;
the ratio of the zirconia balls to the raw materials to the deionized water is 4-5: 1-2: 1-2, the ball milling time is 10-50 h, and the rotating speed of the ball mill is 200-600 r/min.
The particle size of the powder particles after ball milling in the step (1) is 0.1-10 μm.
The molten salt is KCl and NaCl; the mass ratio of KCl to NaCl is 1-10: 1 to 5.
The drying and sieving treatment tool in the step (1) is as follows:
drying the filter-pressed powder at 60-100 ℃ for 12-50 h, then sieving with a 100-200 mesh sieve, taking the undersize product, then sieving with a 400-1000 mesh sieve, taking the oversize product, and obtaining the powder with the particle size of 10-38 mu m to 75-100 mu m;
the calcination is specifically as follows: calcining the sieved powder at 600-1200 ℃ for 2-30 h, wherein the heating rate is 5-10 ℃/min.
In the step (2), the obtained product is repeatedly washed by heated deionized water to remove excessive chloride salt until the filtrate does not contain Cl-So far, specifically:
ultrasonically cleaning the calcined material with deionized water and alcohol for several times to remove excessive chloride salt, and using silver nitrate AgNO3When the filtrate is tested by the reagent, the washed filtrate can be recycled until no white precipitate is generated.
The filtering, drying and sieving treatment in the step (3) specifically comprises the following steps: drying the cleaned and filtered powder at 60-100 ℃ for 10-50 h, sequentially sieving the powder by 100-200 meshes and 400-1000 meshes, and testing the particle size of the powder by using a laser particle sizer, wherein the particle size range is 10-100 mu m.
That is to say, the scheme of the invention provides a method for preparing rare earth tantalate RE3TaO7 spherical powder by a molten salt growth method, which is characterized by comprising the following steps:
weighing raw materials and molten salt according to a certain proportion, pouring the raw materials and the molten salt into a ball milling tank, taking deionized water as a medium, carrying out ball milling in a planetary ball mill uniformly, removing water in a powder solution by using a filter press, drying, sieving, then placing in a resistance furnace, heating to a certain temperature, calcining for a plurality of hours, cooling along with the furnace after calcining is finished, taking out powder when the temperature is reduced to room temperature, repeatedly cleaning the obtained product by using the heated deionized water to remove redundant chloride salt until silver nitrate (AgNO) is used3) Reagent test filtrate does not contain Cl-Until the salt in the filtrate can be recycled, and the washed powder is filtered, dried and sieved to obtain the rare earth tantalate RE with required particle size3TaO7Spherical powder.
Specifically, the raw material is rare earth oxide RE2O3And Ta tantalum pentoxide2O5The molten salt is mixed salt of KCl and NaCl, wherein the rare earth oxide RE2O3Is Y2O3、La2O3、Nd2O3、Pm2O3、Sm2O3、Eu2O3、Gd2O3、Tb2O3、Dy2O3、Ho2O3、Er2O3、Tm2O3、Yb2O3、Lu2O3Purity of raw materials and molten salts>99.99 percent, and the particle size is 15-60 mu m.
Rare earth oxide RE2O3And Ta tantalum pentoxide2O5In a molar ratio of 3: KCl and Na in molten saltThe mass ratio of Cl is (1-10): (1-5), wherein the mass ratio of the raw materials to the molten salt is (1-10): (1-5), wherein the chemical reaction formula of the rare earth tantalate is 3RE2O3+Ta2O5=2RE3TaO7。
During ball milling, the proportion of zirconia balls, raw materials and deionized water is 4-5: 1-2: 1-2, the ball milling time is 10-50 h, the rotating speed of the ball mill is 200-600 r/min, the particle size of particles in the slurry is 0.1-10 mu m after ball milling by using a laser particle sizer, and after the ball milling is finished, the slurry after ball milling is subjected to pressure filtration by using a pressure filter to remove water in the slurry.
Drying the filter-pressed powder at 60-100 ℃ for 12-50 h, then sieving with a 100-200 mesh sieve (taking undersize products), and then sieving with a 400-1000 mesh sieve (taking oversize products), so as to obtain powder with the particle size of 10-38 mu m to 75-100 mu m.
Calcining the sieved powder at 600-1200 ℃ for 2-30 h, wherein the heating rate is 5-10 ℃/min.
Ultrasonically cleaning the calcined material with deionized water and alcohol for several times to remove excessive chloride salt, and treating with silver nitrate (AgNO)3) When the filtrate is tested by the reagent, the washed filtrate can be recycled until no white precipitate is generated.
Drying the washed and filtered powder for 10-50 h at 60-100 ℃, sequentially sieving the powder for 100-200 meshes and 400-1000 meshes, testing the particle size of the powder by using a laser particle sizer, wherein the particle size range is 10-100 mu m, testing the flowability by using a Hall flow meter, observing the morphology of the powder particles by using a scanning electron microscope, and calculating the sphericity ratio.
In the examples of the present invention, rare earth tantalate RE3TaO7(RE = La, Nd, Sm, Eu, Gd, Dy) has low thermal conductivity (1.1-2.1 W.m)-1·K-125-900 deg.C) and is significantly lower than YSZ (2.3-3.5 Wm)-1·K-1900 ℃ C.) to RE2Zr2O7（1.3-2.5W·m-1·K-1900 ℃ C.) approach, by doping to RE3TaO7The modification of Sm was investigated2YbTaO7And Sm2YTaO7All have a typical defect fluorite type structure, where Sm2YbTaO7Thermal conductivity ratio Sm2YTaO7Lower because of the greater difference in mass between the displaced and displaced atoms. Rare earth tantalate RE3TaO7Has a high thermal expansion coefficient of 8.8-10.6 x 10-6 K-1(100-1200℃)，RE3TaO7The hardness and Young modulus of the alloy are respectively between 5.0-10GPa and 131.0-260.0 GPa.
To ensure and improve rare earth tantalate RE3TaO7As the thermal and mechanical properties of the thermal barrier coating, it is highly desirable to improve the sphericity and fluidity of the powder during the thermal spraying process. And rare earth tantalate RE3TaO7The preparation of powders is a very critical step in the preparation of TBCs, the quality of which directly affects the properties of the coating.
The specific embodiment is as follows:
example 1
In this example, a molten salt method is used to prepare rare earth tantalate Y3TaO7The method for preparing the spherical powder comprises the following steps:
and (3) according to molar ratio: 1 weighing raw material rare earth oxide Y2O3(6.774 kg) and Ta tantalum pentoxide2O5(4.419 kg) 11.193kg in total, based on (1-6): (1-3) weighing a mixed salt of KCl and NaCl according to the proportion shown in Table 1, wherein the weight ratio of KCl to NaCl is 1: 5 weighing raw materials (11.193 kg) and molten salt (55.965 kg), pouring the raw materials and the molten salt into a ball milling tank, ball milling for 12h (500 r/min) in a planetary ball mill by using deionized water as a medium, removing water in slurry by using a filter press after finishing ball milling, drying the slurry for 24h at 90 ℃, sieving the slurry by a 400-mesh sieve, then placing the slurry into a resistance furnace for calcining, wherein the calcining temperature and the calcining time are respectively 800 ℃ and 5h, the heating rate is 5 ℃/min, cooling the slurry along with the furnace after the calcining is finished, taking out powder after the temperature is reduced to room temperature, repeatedly washing the obtained product by using heated deionized water for several times to remove redundant chloride salt until silver nitrate (AgNO) is used for removing the redundant chloride salt3) Reagent test filtrate does not contain Cl-Filtering the washed powder, drying at 90 deg.C for 24 hr, sieving with 100 mesh sieve, sieving with 400 mesh sieve, and testing with laser particle sizerThe powder has a particle diameter in the range of 40-90 μm, and a flowability of (45-53) s/50g as measured by a Hall flow meter. And observing the morphology of the powder particles by using a scanning electron microscope, and calculating the sphericity ratio.
As shown in FIG. 1, the synthesis of Y by molten salt method3TaO7XRD pattern of (A), XRD pattern and Y measured3TaO7(PDF: 38-1403) and the peaks of the XRD and the standard PDF card are completely coincided, which shows that the synthesized Y3TaO7High purity and less impurities. As shown in FIG. 2, Y was observed by a Scanning Electron Microscope (SEM)3TaO7The microscopic morphology and sphericity ratio of the spherical powder can be seen as Y3TaO7The particle diameter of the spherical powder is 40-70 mu m, and the sphericity ratio>99%, it can be seen from table 1 that the ratio of KCl to NaCl is (5-6): the powder has better sphericity ratio and fluidity when 1, the sphericity ratio is calculated by the ratio of spherical particles to total particles in fig. 2, and the powder particles are all in a nearly spherical shape as can be seen from a scanning electron microscope atlas. That is, the morphology of the powder is regulated and controlled through the proportion of the molten salt, the calcination temperature and the calcination time, and the standard of judgment is to observe the sphericity degree and the particle size range of the calcined powder under a scanning electron microscope.
TABLE 1 ratio of KCl and NaCl in molten salt to rare earth tantalate Y3TaO7Relationship between sphericity and fluidity
Example 2
In this example, the molten salt method for preparing rare earth tantalate Dy3TaO7The method for preparing the spherical powder comprises the following steps:
and (3) according to molar ratio: 1 weighing raw material rare earth oxide Dy2O3(11.19 kg) and Ta tantalum pentoxide2O5(4.419 kg) 15.609kg in total, as 6: weighing KCl and NaCl mixed molten salt according to the proportion of 1, and mixing according to the proportion of (1-2): (2-7) weighing raw materials and molten salt, pouring the raw materials and the molten salt into a ball milling tank, taking deionized water as a medium, and carrying out planetary ball millingBall milling 12h (500 r/min) in a machine, removing water in the slurry by using a filter press after ball milling is finished, drying the slurry for 24h at 90 ℃, firstly sieving the slurry by using a 100-mesh sieve (taking undersize products), then sieving the slurry by using a 400-mesh sieve (taking oversize products), then placing the slurry in a resistance furnace for calcining, wherein the calcining temperature and the calcining time are respectively 800 ℃ and 5h, the heating rate is 5 ℃/min, cooling the slurry along with the furnace after calcining is finished, taking out the powder after the temperature is reduced to the room temperature, repeatedly washing the obtained product by using heated deionized water for several times to remove redundant chloride salt until silver nitrate (AgNO) is used3) Reagent test filtrate does not contain Cl-The powder washed was filtered, dried at 90 ℃ for 24 hours, sieved through 100 mesh (undersize) and sieved through 400 mesh (oversize), the particle size of the powder was measured by a laser particle sizer, the particle size ranged from 40 μm to 90 μm, the flowability was measured by a hall flow meter, the morphology of the powder particles was observed by a scanning electron microscope, the sphericity was calculated, and as can be seen from table 2, the ratio of raw material to molten salt was 1: (5-6), the powder has a good sphericity ratio (97-99%) and a fluidity of (33-37 s)/50 g.
TABLE 2 raw materials and molten salt ratio and rare earth tantalate Dy3TaO7Relationship between sphericity and fluidity
Example 3
This example describes a molten salt method for preparing Yb of a rare earth tantalate3TaO7The method for preparing the spherical powder comprises the following steps:
and (3) according to molar ratio: 1 weighing raw material rare earth oxide Yb2O3(11.823 kg) and Ta tantalum pentoxide2O5(4.419 kg) 16.242kg in total, as 6: weighing mixed salt (97.452 kg) of KCl (83.53 kg) and NaCl (13.922 kg) according to the mass ratio of 1: 6 weighing raw materials (16.242 kg) and molten salt (97.452 kg), pouring into a ball milling tank, ball milling for 12h (500 r/min) in a planetary ball mill by using deionized water as a medium, removing water in the slurry by using a filter press after finishing ball milling, and drying for 24h at 90 DEG CSieving with a 100-mesh sieve (taking undersize products), sieving with a 400-mesh sieve (taking oversize products), calcining in a resistance furnace at 600-1200 ℃ for 5h, as shown in Table 3, at a temperature rise rate of 5 ℃/min, cooling with the furnace after calcining, taking out the powder after the temperature is reduced to room temperature, repeatedly washing the obtained product with heated deionized water for several times to remove excessive chloride salt until silver nitrate (AgNO) is used3) Reagent test filtrate does not contain Cl-Until now, the washed powder is filtered, dried for 24 hours at 90 ℃, sieved with 100 meshes and then sieved with 400 meshes, the particle size of the powder is tested by a laser particle sizer, the particle size range is 40-90 μm, the fluidity is tested by a Hall flow meter, the morphology of the powder particles is observed by a scanning electron microscope, and the sphericity ratio is calculated, as can be seen from Table 3, when the calcination temperature is 700-900 ℃, the powder has better sphericity ratio (97-99%) and fluidity (29-35 s)/50 g.
TABLE 3 calcination temperature and Yb of rare earth tantalate3TaO7Relationship between sphericity and fluidity
Example 4
In this example, a molten salt method is used to prepare a rare earth tantalate Tm3TaO7The method for preparing the spherical powder comprises the following steps:
and (3) according to molar ratio: 1 weighing raw material rare earth oxide Tm2O3(11.5758 kg) and Ta tantalum pentoxide2O5(4.419 kg) 15.9948kg in total, as 6: weighing KCl (82.26 kg) and NaCl (13.71 kg) mixed salt (55.965 kg) in a mass ratio of 1: 6 weighing raw materials (15.9948 kg) and molten salt (95.97 kg), pouring the raw materials and the molten salt into a ball milling tank, ball milling the raw materials for 12 hours (500 r/min) in a planetary ball mill by using deionized water as a medium, removing water in slurry by using a filter press after finishing ball milling, drying the slurry for 24 hours at 90 ℃, sieving the slurry for 100 meshes (taking undersize products), sieving the slurry for 400 meshes (taking oversize products), then placing the slurry in a resistance furnace for calcination, wherein the calcination temperature and the calcination time are respectively 800 ℃ and 2-10 hours,as shown in fig. 3, the temperature rise rate is 5 ℃/min, the furnace is cooled after the calcination is finished, the powder is taken out when the temperature is reduced to the room temperature, and the obtained product is repeatedly washed by heated deionized water for several times to remove the redundant chloride salt until silver nitrate (AgNO) is used3) Reagent test filtrate does not contain Cl-The washed powder is filtered, dried at 90 ℃ for 24 hours, sieved with 100 meshes and then sieved with 400 meshes, the particle size of the powder is tested by a laser particle sizer, the particle size range is 10-90 mu m, the flowability is tested by a Hall flow meter, the morphology of the powder particles is observed by a scanning electron microscope, the sphericity ratio is calculated, and the size of the crystal grains is increased along with the extension of the sintering time.
Example 5
This example describes a molten salt process for preparing a rare earth tantalate (Y)1/2Dy1/2) 3TaO7The method for preparing the spherical powder comprises the following steps:
according to molar ratio 3/2: 3/2: 1 weighing raw material rare earth oxide Y2O3（3.3872kg）、Dy2O3(5.595 kg) and Ta tantalum pentoxide2O5(4.419 kg) 13.4012kg in total, as 6: weighing mixed salt (55.965 kg) of KCl (68.9205 kg) and NaCl (11.4867 kg) according to the mass ratio of 1: 6 weighing raw materials (13.4012 kg) and molten salt (80.4072 kg), pouring the raw materials and the molten salt into a ball milling tank, ball milling for 12h (500 r/min) in a planetary ball mill by using deionized water as a medium, removing water in slurry by using a filter press after finishing ball milling, drying the slurry for 24h at 90 ℃, sieving the slurry for 100 meshes (taking undersize), sieving the slurry for 400 meshes (taking oversize), calcining the obtained product in a resistance furnace, wherein the calcining temperature and the calcining time are respectively 800 ℃ and 4h, the heating rate is 5 ℃/min, cooling the calcined product along with the furnace after the calcining is finished, taking out powder when the temperature is reduced to room temperature, repeatedly washing the obtained product by using heated deionized water for several times to remove redundant chloride salt until silver nitrate (AgNO) is used for removing the excessive chloride salt3) Reagent test filtrate does not contain Cl-The washed powder was filtered, dried at 90 ℃ for 24 hours, sieved through 100 mesh sieve and then 400 mesh sieve, and the particle size of the powder was measured by a laser particle sizer (Y)1/2Dy1/2) 3TaO7The particle size is in the range of 10-90 μm, and the chemical reaction formula is
。
Example 6
This example describes a molten salt process for preparing a rare earth tantalate (Y)1/3Dy1/3 Yb1/3) 3TaO7The method for preparing the spherical powder comprises the following steps:
according to the mol ratio of 1: 1: 1 weighing raw material rare earth oxide Y2O3（2.2581kg）、Dy2O3（3.73kg）、Yb2O3(3.941 kg) and Ta tantalum pentoxide2O5(4.419 kg) 14.3481kg in total, as 6: weighing mixed salt (56.088 kg) of KCl (73.7897 kg) and NaCl (12.2983 kg) according to the mass ratio of 1: 6 weighing raw materials (14.3481 kg) and molten salt (86.088 kg), pouring the raw materials and the molten salt into a ball milling tank, ball milling for 12h (500 r/min) in a planetary ball mill by using deionized water as a medium, removing water in slurry by using a filter press after finishing ball milling, drying the slurry for 24h at 90 ℃, sieving the slurry for 100 meshes (taking undersize), sieving the slurry for 400 meshes (taking oversize), calcining the obtained product in a resistance furnace, wherein the calcining temperature and the calcining time are respectively 800 ℃ and 4h, the heating rate is 5 ℃/min, cooling the calcined product along with the furnace after the calcining is finished, taking out powder when the temperature is reduced to room temperature, repeatedly washing the obtained product by using heated deionized water for several times to remove redundant chloride salt until silver nitrate (AgNO) is used for removing the excessive chloride salt3) Reagent test filtrate does not contain Cl-The washed powder was filtered, dried at 90 ℃ for 24 hours, sieved through 100 mesh sieve and then 400 mesh sieve, and the particle size of the powder was measured by a laser particle sizer (Y)1/3Dy1/3 Yb1/3) 3TaO7The particle size ranges from 10 μm to 90 μm, and the chemical reaction formula is as follows:
example 7
This example describesPreparation of rare earth tantalate (Y) by molten salt method1/4Dy1/4 Yb1/4 Tm1/4) 3TaO7The method for preparing the spherical powder comprises the following steps:
according to molar ratio 3/4: 3/4: 3/4: 1 weighing raw material rare earth oxide Y2O3（1.6936kg）、Dy2O3（2.7975kg）、Yb2O3（2.9558kg）、Tm2O3(2.8940 kg) and Ta tantalum pentoxide2O5(4.419 kg) 14.7599kg in total, as 6: weighing mixed salt (88.5591 kg) of KCl (75.9078 kg) and NaCl (12.6513 kg) according to the mass ratio of 1: 6 weighing raw materials (14.7599 kg) and molten salt (88.5591 kg), pouring the raw materials and the molten salt into a ball milling tank, ball milling for 12h (500 r/min) in a planetary ball mill by using deionized water as a medium, removing water in slurry by using a filter press after finishing ball milling, drying the slurry for 24h at 90 ℃, sieving the slurry for 100 meshes (taking undersize), sieving the slurry for 400 meshes (taking oversize), calcining the obtained product in a resistance furnace, wherein the calcining temperature and the calcining time are respectively 800 ℃ and 4h, the heating rate is 5 ℃/min, cooling the calcined product along with the furnace after the calcining is finished, taking out powder when the temperature is reduced to room temperature, repeatedly washing the obtained product by using heated deionized water for several times to remove redundant chloride salt until silver nitrate (AgNO) is used for removing the excessive chloride salt3) Reagent test filtrate does not contain Cl-The washed powder was filtered, dried at 90 ℃ for 24 hours, sieved through 100 mesh sieve and then 400 mesh sieve, and the particle size of the powder was measured by a laser particle sizer (Y)1/3Dy1/3 Yb1/3) 3TaO7The particle size ranges from 10 μm to 90 μm, and the chemical reaction formula is as follows:
。
the scheme of the invention provides a rare earth tantalate RE prepared based on a molten salt growth method3TaO7Spherical powder and preparation method thereof, and rare earth oxide RE of powder2O3And Ta tantalum pentoxide2O5Two kinds of raw materials. Rare earth oxide RE2O3And Ta tantalum pentoxide2O5Mixing the raw materials, molten salt and deionized water in a ball milling tank, adding zirconia balls, and performing ball milling by a planetary ball mill until the raw materials are uniformly mixed; sequentially carrying out filter pressing, drying and sieving treatment on the mixed powder, and then calcining; cooling to room temperature with the furnace, taking out the powder, repeatedly cleaning the obtained product with heated deionized water to remove excessive chloride salt until the filtrate does not contain Cl-Until the end; filtering, drying and sieving the washed powder to obtain the rare earth tantalate RE with the required particle size3TaO7Spherical powder. That is, spherical powder with high sphericity ratio and good fluidity is prepared by changing the calcination temperature, calcination time and molten salt ratio (the fluidity is tested by a Hall flow meter, the fluidity of the invention is 28-53s/50g, namely the time for 50g of powder to completely leak to a bottom plate from a funnel is 28-53 s), so that the thermal and mechanical properties of the powder as a thermal barrier coating are improved. The method has the advantages of low synthesis temperature, short reaction time, simple process, high purity of the synthesized product, controllable crystal form and shape of the powder particles, no agglomeration, easy dispersion and the like.
That is, the present invention scheme has not been previously reported in the related literature to prepare spherical RE by molten salt process3TaO7And the rare earth tantalate RE is prepared into the spherical powder by the molten salt method for the first time3TaO7The spherical powder has high purity and low synthesis temperature, and specifically, as shown in FIG. 1, the XRD pattern and Y are measured3TaO7(PDF: 38-1403) and the peaks of the XRD and the standard PDF card are completely coincided, which shows that the synthesized Y3TaO7High purity and less impurities. RE without addition of molten salt3TaO7The calcination temperature is 1500-1700 ℃, and after the molten salt is added, the calcination temperature is reduced to 600-1200 ℃. In addition, the method can control the shape and the particle size of the powder by controlling the proportion of the molten salt to the raw material, the components of the molten salt, the calcining temperature and the calcining time, and obtain the spherical particles with high sphericity rate (better sphericity rate, wherein the calculation method of the spherical rate is that the spherical particles and the total particles in the graph 2Ratio, as can be seen from the scanning electron microscope atlas, the powder particles are all in the shape of a nearly spherical) and rare earth tantalate RE with good fluidity3TaO7Spherical powder. In addition, the rare earth tantalate RE prepared by the invention3TaO7The spherical powder has the characteristics of uniform particle size, excellent performance (specifically, as shown in a Scanning Electron Microscope (SEM) spectrum shown in figure 2, the particle size range is 10-70 mu m, the distribution of the particle size of the powder in the interval can be observed), stable quality, strong controllability, suitability for industrial production and the like.
Claims (10)
1. Rare earth tantalate RE prepared based on molten salt growth method3TaO7Spherical powder, characterized in that the powder rare earth oxide RE2O3And Ta tantalum pentoxide2O5Two kinds of raw materials.
2. The RE tantalate prepared based on molten salt method as claimed in claim 13TaO7Spherical powder, characterized in that the rare earth oxide RE2O3And Ta tantalum pentoxide2O5In a molar ratio of 3: 1; the rare earth oxide RE2O3And Ta tantalum pentoxide2O5The particle size of (2) is 15-60 mu m.
3. The rare earth tantalate RE prepared based on the molten salt method according to claim 1 or 23TaO7Spherical powder, characterized in that the rare earth oxide RE2O3The method specifically comprises the following steps: y is2O3、La2O3、Nd2O3、Pm2O3、Sm2O3、Eu2O3、Gd2O3、Tb2O3、Dy2O3、Ho2O3、Er2O3、Tm2O3、Yb2O3、Lu2O3Any one or more of them in combination.
4. Rare earth tantalate RE prepared based on molten salt growth method3TaO7The preparation method of the spherical powder is characterized by comprising the following steps:
(1) rare earth oxide RE2O3And Ta tantalum pentoxide2O5Mixing the raw materials, molten salt and deionized water in a ball milling tank, adding zirconia balls, and performing ball milling by a planetary ball mill until the raw materials are uniformly mixed; sequentially carrying out filter pressing, drying and sieving treatment on the mixed powder, and then calcining;
(2) cooling to room temperature with the furnace, taking out the powder, repeatedly cleaning the obtained product with heated deionized water to remove excessive chloride salt until the filtrate does not contain Cl-Until the end;
(3) filtering, drying and sieving the washed powder to obtain the rare earth tantalate RE with the required particle size3TaO7Spherical powder.
5. The RE tantalate prepared according to claim 4 based on the molten salt method3TaO7The preparation method of the spherical powder is characterized in that the rare earth oxide RE in the step (1)2O3And Ta tantalum pentoxide2O5In a molar ratio of 3: 1, the mass ratio of the raw materials to the molten salt is 1-10: 1-5;
the ratio of the zirconia balls to the raw materials to the deionized water is 4-5: 1-2: 1-2, the ball milling time is 10-50 h, and the rotating speed of the ball mill is 200-600 r/min.
6. The RE tantalate prepared according to claim 4 based on the molten salt method3TaO7The preparation method of the spherical powder is characterized in that the particle size of the powder particles after ball milling in the step (1) is 0.1-10 μm.
7. The rare earth tantalate RE prepared based on the molten salt method according to claim 4 or 53TaO7Preparation of spherical powderThe method is characterized in that the molten salt is KCl and NaCl; the mass ratio of KCl to NaCl is 1-10: : 1 to 5.
8. The RE tantalate prepared according to claim 4 based on the molten salt method3TaO7The preparation method of the spherical powder is characterized in that the drying and sieving treatment tool in the step (1) is as follows:
drying the filter-pressed powder at 60-100 ℃ for 12-50 h, then sieving with a 100-200 mesh sieve, taking the undersize product, then sieving with a 400-1000 mesh sieve, taking the oversize product, and obtaining the powder with the particle size of 10-38 mu m to 75-100 mu m;
the calcination is specifically as follows: calcining the sieved powder at 600-1200 ℃ for 2-30 h, wherein the heating rate is 5-10 ℃/min.
9. The RE tantalate prepared according to claim 4 based on the molten salt method3TaO7The preparation method of the spherical powder is characterized in that in the step (2), the product obtained by repeatedly washing with heated deionized water is used for removing the redundant chloride salt until the filtrate does not contain Cl-So far, specifically:
ultrasonically cleaning the calcined material with deionized water and alcohol for several times to remove excessive chloride salt, and using silver nitrate AgNO3When the filtrate is tested by the reagent, the washed filtrate can be recycled until no white precipitate is generated.
10. The RE tantalate prepared according to claim 4 based on the molten salt method3TaO7The preparation method of the spherical powder is characterized in that the filtering, drying and sieving treatment in the step (3) specifically comprises the following steps: drying the cleaned and filtered powder at 60-100 ℃ for 10-50 h, sequentially sieving the powder by 100-200 meshes and 400-1000 meshes, and testing the particle size of the powder by using a laser particle sizer, wherein the particle size range is 10-100 mu m.
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