CN109437928A - Zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder and preparation method thereof - Google Patents
Zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder and preparation method thereof Download PDFInfo
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- CN109437928A CN109437928A CN201811647695.7A CN201811647695A CN109437928A CN 109437928 A CN109437928 A CN 109437928A CN 201811647695 A CN201811647695 A CN 201811647695A CN 109437928 A CN109437928 A CN 109437928A
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- 239000000843 powder Substances 0.000 title claims abstract description 134
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 42
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 41
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 35
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 35
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910001928 zirconium oxide Inorganic materials 0.000 title claims abstract description 32
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 30
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000919 ceramic Substances 0.000 claims abstract description 50
- 239000010936 titanium Substances 0.000 claims abstract description 15
- 239000002002 slurry Substances 0.000 claims abstract description 14
- 239000000853 adhesive Substances 0.000 claims abstract description 10
- 230000001070 adhesive effect Effects 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 8
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 6
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002019 doping agent Substances 0.000 claims abstract description 4
- 238000003746 solid phase reaction Methods 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract 2
- 238000001035 drying Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 15
- 238000005507 spraying Methods 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 8
- 238000005336 cracking Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910052727 yttrium Inorganic materials 0.000 claims description 4
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 3
- 229910052691 Erbium Inorganic materials 0.000 claims description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims description 3
- 229910052772 Samarium Inorganic materials 0.000 claims description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000010671 solid-state reaction Methods 0.000 claims description 3
- 229910052765 Lutetium Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910052573 porcelain Inorganic materials 0.000 claims 1
- 238000002390 rotary evaporation Methods 0.000 claims 1
- 239000012071 phase Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 7
- 239000007921 spray Substances 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 4
- 229910000420 cerium oxide Inorganic materials 0.000 abstract description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 abstract description 3
- 239000008187 granular material Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 9
- 239000010955 niobium Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 5
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 239000012720 thermal barrier coating Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 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 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229920000084 Gum arabic Polymers 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 241000978776 Senegalia senegal Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000000205 acacia gum Substances 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 1
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 1
- 229910003443 lutetium oxide Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 1
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium(III) oxide Inorganic materials O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- 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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Abstract
The present invention relates to ceramic powder preparation technical fields, specifically disclose zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder, using dopant (zirconium oxide/titanium oxide/cerium oxide), RE2O3Powder, Ta2O5Powder or Nb2O5After powder ball milling, target phase is obtained through solid phase reaction, is mixed to form slurry with organic adhesive afterwards, is dried using the method that high-temperature spray cracks, the powder granule of near-spherical is obtained, rear sintering obtains zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobate ceramics powder；The chemical general formula of the ceramic powder is RE3‑x(Ta/Nb)1‑x(Zr/Ce/Ti)2xO7, 0 < x < 1, crystal structure is orthorhombic phase, and lattice vacancy group is C2221, partial size is 10-50 μm, and the ceramic powder is spherical in shape.Obtain can satisfy zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobate ceramics powder of APS technical requirements using technical solution of the present invention.
Description
Technical field
The present invention relates to ceramic powder preparation technical fields, in particular to rare earth tantalum/niobate ceramics powder and its preparation
Method.
Background technique
Heat barrier coat material is mainly used in aero-engine industry, has lower thermal conductivity, high thermal expansion coefficient, anti-burning
Knot, the advantages that high-temperature stability is good, primarily serve it is heat-insulated, anti-oxidation, be effective against particle impacting to protect aeroplane engine
The effect of machine high-temperature area piece-part substrates.
Air plasma spraying (APS) and electro beam physics vapor phase deposition (EBPVD) technology are industrial preparations at present
The general technology of preparing of heat barrier coat material, EBPVD is chiefly used in preparing the thermal barrier coating of columnar crystal morphology, and APS technology is more
It is used to prepare laminar structured thermal barrier coating, and coating is close, the porosity is few.But APS technology has many requirements to powder,
The density for needing to have certain including powder, organic adhesive is appropriate, the shape of powder, and with certain particle size range
Deng, and usually will be in 10~200 μ ms for particle size range, and the shape of powder wants spherical in shape or subsphaeroidal.
YSZ (yttria-stabilized zirconia) is current research and the thermal barrier coating being most widely used, but due to
At 1200 DEG C or more, YSZ can undergo phase transition and lead to coating failure, and researcher is promoted to look for substitute the thermal boundary of YSZ
Coating, Harvard University Clarke professor seminar in 2007 propose tantalum with professor Levi etc. of University of California--Santa Barbara
Sour yttrium (YTaO4) ferroelastics is expected to as novel heat barrier coat material, but the research about rare earth tantalate is concentrated mainly on it
The theoretical calculation of crystal structure and luminescent properties etc.；The dilute of densification has been made by solid reaction process in Wang in 2016 et al.
Native tantalates block materials have shown that thermal conductivity is much smaller than the conclusion of YSZ material, and in addition there are also studies have shown that in 317 phases
RE3Ta/NbO7Compound in doping quadrivalent ion can further decrease the thermal conductivity of base material, promote base material
Thermal expansion coefficient etc., the application that numerous studies and the experiment conclusion of researcher is rare earth tantalate on thermal barrier coating provide
Theoretical basis.
But the rare earth doped tantalum/niobate ceramics powder for meeting APS technique can be prepared there is presently no a kind of technique
Body.
Summary of the invention
The present invention provides zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder and
Preparation method, to meet requirement of the APS technology to ceramic powder partial size and shape, and by rare earth tantalum/niobate ceramics
After powder is sprayed on alloy substrate, it can play the role of reducing heat transfer.
In order to achieve the above object, base case of the invention are as follows:
Zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder, the change of the ceramic powder
General formula is RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7, 0 < x < 1, which is orthorhombic phase, and lattice is empty
Between group be C2221, partial size is 10-50 μm, and the ceramic powder is spherical in shape.
The technical principle and effect of this base case are:
1, zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobates RE in this base case3Ta/NbO7Ceramic powder
Particle size range in 10-50 μ m, on the one hand, such particle size range meets the powder requirement of APS spraying technology, will not
The problem of spray nozzle clogging of spray gun is lived because diameter of particle is too big, is failed so as to cause spraying；It on the other hand, will not be because of powder
Partial size it is too small so that powder quality is too small, cause powder in the outer surface of the plasma firewire of spray gun, and do not enter its heart
Portion, such powder directly vapors away under long-time heating effect, and spraying is caused to fail.
2, zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobates RE in this base case3Ta/NbO7Ceramic powder
Spherical in shape, such powder surface is relatively smooth, and the mobility that this allows for powder is preferable, has both met APS spraying technology in this way
Requirement, while zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobates coating of high quality is also obtained.
3, in RE in this base case3Ta/NbO7Compound in adulterate quadrivalent ion (Zr4+Or Ce4+Or Ti4+) can be into
One step reduces the thermal conductivity of substrate, promotes the thermal expansion coefficient of substrate.
Further, the mixing of one or more of RE Sc, Y, La, Nd, Sm, Eu, Gd, Dy, Er, Yb, Lu.
The utility model has the advantages that verifying of the inventor by experiment is obtained using these types or several mixed rare earth elements
Rare earth tantalum/niobates (RE3Ta/NbO7) ceramic powder particle size range is more uniform.
Further, zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobates (RE3TaO7/RE3NbO7) ceramic powder
Preparation method, comprising the following steps:
Step (1): RE:(Ta/Nb is weighed): the molar ratio of (Zr/Ce/Ti) is (3-x): the Ta of (1-x): 2x2O5Powder or
Nb2O5Powder, dopant (ZrO2Powder or CeO2Powder or TiO2Powder), RE2O3Powder is added in solvent, and it is molten to form mixing
Liquid carries out ball milling to mixed solution using ball mill, and time of ball milling is not less than 10h, the revolving speed of ball mill not less than 300 turns/
Point, dry powders A is obtained after drying；
Step (2): the powders A that step (1) is obtained carries out high temperature solid state reaction, and reaction temperature is 1600-1800 DEG C, instead
It is 6-20h between seasonable, obtaining ingredient is RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7Powder B；
Step (3): powder B and solvent, organic adhesive that step (2) obtains are mixed to get slurry C, the slurry C
The mass percent of middle powder B is 10%~40%, and the mass percent of organic adhesive is 0.1%~3%, remaining is molten
Agent, carries out spraying cracking drying to slurry C at 1000-1200 DEG C of temperature, and drying time 30-60min obtains dry material
Grain D；
Step (4): the material grain D that step (3) obtains is sintered at 1400-1600 DEG C of temperature, and sintering time 2-4h is obtained
Zirconium oxide/the titanium oxide arrived/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder.
The utility model has the advantages that the oxidation of the partial size that used what step (1)~step (4) technique was prepared for 10~50 μm
Zirconium/titanium oxide/cerium oxide-doped rare earth tantalum/niobates (RE3TaO7/RE3NbO7) ceramic powder.
Target phase RE is obtained using step (1) and step (2)3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7Ceramic powders.
Step (3) using high-temperature spray cracking by the way of slurry C obtained is dried, wherein organic adhesive be for
By target phase RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7Tiny powder particle is reunited together in ceramic powders, and is sprayed
Crack dry principle are as follows: by slurry C obtained, it is atomized by high pressure gas, so that slurry C forms tiny drop,
Under 1000-1200 DEG C of high temperature, fast liquid evaporation in drop, and then obtain subsphaeroidal powder.
The sintering of step (4) is material grain D-shaped in order to obtain step (3) into certain bond strength, is had certain
Density, and then the glomerate pattern of shape.
Further, the drying in the step (1) is dried using Rotary Evaporators, and drying temperature is 40-60 DEG C, rotation
Turning evaporation time is 2-4h.
The utility model has the advantages that being dried using Rotary Evaporators, the dry time is shorter, and powder can be in rotary course
It obtains more adequately drying.
Further, the oxidation that the powder B and step (4) that the step (1) obtains powders A, step (2) obtain are obtained
Zirconium/titanium oxide/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder is all made of the sieve of 200-500 mesh.
The utility model has the advantages that the powder that each step is obtained is sieved, the biggish powder of particle is avoided the occurrence of, is with sintering step
Example, due to that in sintering process, may generate block, therefore sieving can dispose these blocks.
Further, the spraying cracking temperature in the step (3) is 1200 DEG C, time 60min.
The utility model has the advantages that inventor show that the particle size range that powder is obtained under the parameter is more uniform by the verifying tested,
It and is in spherical pattern.
Further, the step (1) carries out predrying to powder before weighing powder, and predrying temperature is 600-800
DEG C, drying time 8-10h.
The utility model has the advantages that predrying can reduce the water content in precursor powder, to reduce influence of the moisture to precise.
Further, ZrO in the step (1)2Powder or CeO2Powder or TiO2Powder, RE2O3Powder, Ta2O5Powder or
Nb2O5The purity of powder is not less than 99.9%.
The utility model has the advantages that reducing the impurity element of introducing using the higher precursor powder of purity, reduces impurity and is is prepared by powder
Adverse effect.
Detailed description of the invention
Fig. 1 is cerium oxide-doped rare earth tantalate (Y made from the embodiment of the present invention 22.8Ta0.8Ce0.4O7) XRD diagram；
Fig. 2 is cerium oxide-doped rare earth tantalate (Y made from the embodiment of the present invention 22.8Ta0.8Ce0.4O7) SEM figure.
Specific embodiment
It is further described below by specific embodiment:
Zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder, the change of the ceramic powder
General formula is RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7, 0 < x < 1, RE Sc, Y, La, Nd, Sm, Eu, Gd, Dy, Er, Yb,
The mixing of one or more of Lu, the ceramic powder crystal structure are orthorhombic phase, and lattice vacancy group is C2221, partial size 10-
50 μm, the ceramic powder is spherical in shape.
Zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7The preparation method of ceramic powder, including
Following steps:
Step (1): by dopant (zirconium oxide (ZrO2) powder or cerium oxide (CeO2) powder or titanium oxide (TiO2) powder
One of), RE oxide powder (rare earth oxide Sc2O3、Y2O3、La2O3、Nd2O3、Sm2O3、Eu2O3、Gd2O3、
Dy2O3、Er2O3、Yb2O3、Lu2O3One or more of), tantalum pentoxide (Ta2O5) powder or niobium pentaoxide (Nb2O5) powder
End carries out predrying, and pre-dried temperature is 600-800 DEG C, and the pre-dried time is 8-10h, according to RE3-x(Ta/Nb)1-x
(Zr/Ce/Ti)2xO7The stoichiometric ratio of corresponding element weighs the powder after predrying respectively, is added to deionized water or ethyl alcohol
In solvent, mixed solution is obtained, so that RE:(Ta/Nb in mixed solution): the molar ratio of (Zr/Ce/Ti) is (3-x): (1-x):
2x carries out ball milling to mixed solution using ball mill, and time of ball milling is not less than 10h, the revolving speed of ball mill not less than 300 turns/
Point.
The slurry obtained after ball milling is dried using Rotary Evaporators (model: N-1200B), drying temperature 40-
60 DEG C, the dry time is 2-4h, obtains powders A, and powders A is used to the sieve of 200-500 mesh.
Step (2): the powders A after being sieved in step (1) carries out high temperature solid state reaction, reaction temperature 1600-
1800 DEG C, reaction time 6-20h, obtaining ingredient is RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7Powder B, powder B is adopted
With the sieve of 200-500 mesh.
Step (3): the powder B after step (2) is sieved is mixed with deionized water or alcohol solvent, organic adhesive
Slurry C is obtained, wherein the mass percent of powder B is 10%~40% in slurry C, and the mass percent of organic adhesive is
0.1%~3%, remaining is solvent, and organic adhesive uses polyvinyl alcohol or gum arabic, at 1000-1200 DEG C of temperature
Under spraying cracking drying is carried out to slurry C, drying time 30-60min obtains dry material grain D；
Step (4): the material grain D that step (3) obtains is sintered at 1400-1600 DEG C of temperature, and sintering time 2-4h is obtained
Zirconium oxide/the titanium oxide arrived/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder, the zirconium oxide/oxygen that will be obtained
Change titanium/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder uses the sieve of 200-500 mesh.
The above method is used to obtain partial size as 10~50 μm of zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobic acid
Salt RE3Ta/NbO7Ceramic powder, and the pattern that ceramic powder detects is spherical in shape.
Table one be 1-6 of the embodiment of the present invention design parameter (in table slash indicate in the embodiment without containing this at
Point):
Table two be 7-12 of the embodiment of the present invention design parameter (in table slash indicate in the embodiment without containing this at
Point):
Embodiment 1-12 is detected using scanning electron microscope, and the particle size range for obtaining powder is in 10-50 μ m, and
It is spherical.
By taking embodiment 2 as an example, to obtained cerium oxide-doped rare earth tantalate (Y2.8Ta0.8Ce0.4O7) ceramic powder material
It is characterized:
1, XRD characterization:
X ray diffracting spectrum is as shown in Figure 1, it is known that the cerium oxide-doped rare earth tantalate that embodiment 2 obtains
(Y2.8Ta0.8Ce0.4O7) ceramic powder be orthorhombic phase, no miscellaneous phase, lattice vacancy group be C2221。
2, SEM is characterized:
Cerium oxide-doped rare earth tantalate (Y prepared by embodiment 22.8Ta0.8Ce0.4O7) ceramic powder SEM spectrum as scheme
Shown in 2, the particle size range of powder is at 10-50 μm as can be seen from Figure 2, and pattern spherical in shape.
3 groups of comparative example are enumerated to compare with the obtained ceramic powder of embodiment 1-12:
Comparative example 1: the difference from embodiment 1 is that, it is not dried by the way of cracking by spraying, dry temperature is
800 DEG C, drying time 1.5h, the diameter of particle range finally obtained is 180 μm -220 μm, and powder is in irregular shape
Looks.
Comparative example 2: the difference with embodiment 1 is only that the time of ball milling is 7h, and the powder average grain diameter finally obtained is big
In 200 μm.
Comparative example 3: the difference with embodiment 1 is only that, does not carry out sieving processing after sintering, is contained in the powder finally obtained
There is partial size to be greater than 220 μm of block.
To sum up, zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobates RE of the present embodiment 1-12 preparation3Ta/NbO7
Ceramic powder, particle size range is 10-50 μm, and is in spherical pattern, meets requirement of the APS spraying technology to powder, and is compared
Example 1-3 does not obtain the ceramic powder for meeting APS spraying technology requirement.
What has been described above is only an embodiment of the present invention, and the common sense such as well known specific structure and characteristic are not made herein in scheme
Excessive description.It, without departing from the structure of the invention, can be with it should be pointed out that for those skilled in the art
Several modifications and improvements are made, these also should be considered as protection scope of the present invention, these all will not influence what the present invention was implemented
Effect and patent practicability.The scope of protection required by this application should be based on the content of the claims, in specification
The records such as specific embodiment can be used for explaining the content of claim.
Claims (8)
1. zirconium oxide/titanium oxide/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder, it is characterised in that: the pottery
The chemical general formula of porcelain powder is RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7, 0 < x < 1, which is orthogonal
Phase, lattice vacancy group are C2221, particle size range is 10-50 μm, and the ceramic powder is spherical in shape.
2. zirconium oxide/titanium oxide according to claim 1/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder
Body, it is characterised in that: the mixing of one or more of RE Sc, Y, La, Nd, Sm, Eu, Gd, Dy, Er, Yb, Lu.
3. zirconium oxide/titanium oxide according to claim 2/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder
The preparation method of body, it is characterised in that: the following steps are included:
Step (1): RE:(Ta/Nb is weighed): the molar ratio of (Zr/Ce/Ti) is (3-x): the Ta of (1-x): 2x2O5Powder or Nb2O5
Powder, dopant (ZrO2Powder or CeO2Powder or TiO2Powder), RE2O3Powder is added in solvent, forms mixed solution, uses
Ball mill carries out ball milling to mixed solution, and the time of ball milling is not less than 10h, and the revolving speed of ball mill is not less than 300 revs/min, through dry
Dry powders A is obtained after dry；
Step (2): the powders A that step (1) is obtained carries out high temperature solid state reaction, and reaction temperature is 1600-1800 DEG C, when reaction
Between be 6-20h, obtain ingredient be RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7Powder B；
Step (3): powder B and solvent, organic adhesive that step (2) obtains are mixed to get slurry C, powder in the slurry C
The mass percent of last B is 10%~40%, and the mass percent of organic adhesive is 0.1%~3%, remaining is solvent,
Spraying cracking drying is carried out to slurry C at 1000-1200 DEG C of temperature, drying time 30-60min obtains dry material grain D；
Step (4): the material grain D that step (3) obtains is sintered at 1400-1600 DEG C of temperature, and sintering time 2-4h obtains oxygen
Change zirconium/titanium oxide/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder.
4. zirconium oxide/titanium oxide according to claim 3/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder
The preparation method of body, it is characterised in that: the drying in the step (1) is dried using Rotary Evaporators, and drying temperature is
40-60 DEG C, the rotary evaporation time is 2-4h.
5. zirconium oxide/titanium oxide according to claim 4/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder
The preparation method of body, it is characterised in that: powder B that powders A that the step (1) obtains, step (2) obtain and step (4)
Zirconium oxide/the titanium oxide arrived/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder is all made of the sieve of 200-500 mesh
Son sieving.
6. zirconium oxide/titanium oxide according to claim 5/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder
The preparation method of body, it is characterised in that: the spraying cracking temperature in the step (3) is 1200 DEG C, time 60min.
7. zirconium oxide/titanium oxide according to claim 6/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder
The preparation method of body, it is characterised in that: the step (1) carries out predrying, predrying temperature to powder before weighing powder
It is 600-800 DEG C, drying time 8-10h.
8. zirconium oxide/titanium oxide according to claim 7/cerium oxide-doped rare earth tantalum/niobates RE3Ta/NbO7Ceramic powder
The preparation method of body, it is characterised in that: ZrO in the step (1)2Powder or CeO2Powder or TiO2Powder, RE2O3Powder,
Ta2O5Powder or Nb2O5The purity of powder is not less than 99.9%.
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| CN111394099A (en) * | 2020-04-22 | 2020-07-10 | 吉林大学 | Preparation and application of novel single-matrix double-light near-infrared tantalum-based pyrochlore material |
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| CN114105672A (en) * | 2020-08-31 | 2022-03-01 | 厦门稀土材料研究所 | Zirconium-tantalum composite rare earth-based porous high-entropy ceramic and preparation method thereof |
| CN113264769A (en) * | 2021-07-08 | 2021-08-17 | 昆明理工大学 | High-entropy stable rare earth tantalate/niobate ceramic and preparation method thereof |
| CN113264769B (en) * | 2021-07-08 | 2022-07-22 | 昆明理工大学 | High-entropy stable rare earth tantalate/niobate ceramic and preparation method thereof |
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Application publication date: 20190308 |