CN109081694A - Precursor liquid and high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder with and preparation method thereof - Google Patents
Precursor liquid and high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder with and preparation method thereof Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims abstract description 71
- 239000002243 precursor Substances 0.000 title claims abstract description 69
- 239000011858 nanopowder Substances 0.000 title claims abstract description 61
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 58
- 239000004411 aluminium Substances 0.000 title claims abstract description 58
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910052727 yttrium Inorganic materials 0.000 title claims abstract description 58
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000002131 composite material Substances 0.000 title claims abstract description 56
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 53
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000654 additive Substances 0.000 claims abstract description 40
- 230000000996 additive effect Effects 0.000 claims abstract description 40
- 150000003839 salts Chemical class 0.000 claims abstract description 30
- 239000003960 organic solvent Substances 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 15
- 230000009471 action Effects 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 30
- 229910021645 metal ion Inorganic materials 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 19
- 229910002651 NO3 Inorganic materials 0.000 claims description 18
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000009826 distribution Methods 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 claims description 8
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical compound CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 claims description 7
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 150000007942 carboxylates Chemical class 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- YPIFGDQKSSMYHQ-UHFFFAOYSA-N 7,7-dimethyloctanoic acid Chemical compound CC(C)(C)CCCCCC(O)=O YPIFGDQKSSMYHQ-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 150000007513 acids Chemical class 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- 125000002843 carboxylic acid group Chemical group 0.000 claims description 4
- 238000002485 combustion reaction Methods 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 4
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 4
- -1 villaumite Chemical compound 0.000 claims description 4
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 3
- 150000001768 cations Chemical class 0.000 claims description 2
- 239000007789 gas Substances 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 16
- 239000000843 powder Substances 0.000 description 16
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 13
- 239000012071 phase Substances 0.000 description 11
- 230000008569 process Effects 0.000 description 11
- 239000002105 nanoparticle Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000007791 liquid phase Substances 0.000 description 6
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 5
- 230000003760 hair shine Effects 0.000 description 5
- 238000005118 spray pyrolysis Methods 0.000 description 5
- 238000013459 approach Methods 0.000 description 4
- 238000000889 atomisation Methods 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 239000002223 garnet Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 229910017053 inorganic salt Inorganic materials 0.000 description 3
- 238000009688 liquid atomisation Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000011164 primary particle Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 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 description 3
- 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 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- 229910001051 Magnalium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 239000000039 congener Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 229910002106 crystalline ceramic Inorganic materials 0.000 description 1
- 239000011222 crystalline ceramic Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910001959 inorganic nitrate Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- KUBYTSCYMRPPAG-UHFFFAOYSA-N ytterbium(3+);trinitrate Chemical compound [Yb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O KUBYTSCYMRPPAG-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/505—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 based on yttrium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62665—Flame, plasma or melting treatment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/442—Carbonates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/443—Nitrates or nitrites
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
- C04B2235/445—Fluoride containing anions, e.g. fluosilicate
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- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention provides a kind of preparation method of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder, comprising: is atomized precursor liquid to form drop, the precursor liquid includes Y3+And Al3+Inorganic salts, additive and organic solvent；And the drop is passed through in flame and is reacted, generate yttrium aluminium composite oxide nano-powder, wherein the additive is used for and the Y3+And Al3+Inorganic salts under the action of the flame the precursor liquid formed the drop in generate volatilization temperature be lower than the Y3+And Al3+Inorganic salts substance, to improve the Y3+And Al3+Volatility of the inorganic salts in the flame.The present invention also provides a kind of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder and precursor liquids.
Description
Technical field
The invention belongs to structure and function ceramic material nano-powder synthesis field more particularly to a kind of precursor liquids, use
The high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder and preparation method of the precursor liquid preparation.
Background technique
Yttrium-aluminium-garnet (Y3Al5O12, YAG) and belong to cubic system, there are stable physics and chemical property, these characteristics
So that YAG is widely used in the fields such as structure and function material, YAG fluorescent material is such as prepared into crystalline ceramics as LED backlight
Source and encapsulating material；YAG down-conversion luminescent material can effectively improve the photoelectric conversion efficiency of solar battery；Polycrystalline YAG is expected to
Monocrystal material is replaced to become laser material of new generation.In addition, YAG become in the transparent characteristic of 0.2 to 5 mu m waveband it is novel
Infrared window and dome material.Currently, the synthesis of YAG ceramics or powder mainly uses solid-phase synthesis, coprecipitation, hydro-thermal
Method, sol-gel method, flame spray pyrolysis method and gas phase flame synthesis etc..
Comparative study shows solid reaction process preparation YAG ceramic material, and not only reaction temperature is high, the time is long, and is also easy to produce
Middle entry, this is one of the most important factor for influencing material property；Coprecipitation prepares powder excessive cycle, reacts not easily-controllable
System；Hydro-thermal method prepares the low efficiency of powder；The predecessor of sol-gel method preparation is difficult to wash and predecessor (metal organic salt)
It is expensive.The advantages that flame synthesis prepares nano-powder, has technical process simple, and the reaction time is short, is easy into phase.In addition,
In order to improve the physics, chemistry and mechanical performance of all kinds of metal oxide materials, element replaces and doping is common effective hand
Section.But element replaces and the percentage and its uniform doping of doping, is to be difficult accurately to control when using prior synthesizing method
System.Flame synthesis is reacted in flame using precursor solution, not only can be with rapid synthesis high-purity micro-/ nano metal oxygen
Compound material more can accurately realize that element replaces or adulterates.In addition, flame synthesis is because equipment is simple, can continuous production,
Yield is high and can obtain fine and close spheric granules and receive extensive attention.
In recent years, the industrial requirement of a large amount of Nano-function thin films drives flame synthetic technology continuous past 10 years
Obtain new breakthrough.Predecessor is liquid phase feeding by gas-phase feed development, and synthetic product is also developed to by single oxide polynary
Doping component.Currently, liquid phase forerunner article how to be used to realize that high-temperature atomizing flame vapor- phase synthesis particle is uniform, even size is controllable
Nano-powder, the especially nanometer multicomponent powder of two or more metal, it has also become have in the level of International Technology forward position
" seizing by the throat " problem for thering is major application to be worth.WJ applies patent document disclosed in Plutarch and " is produced with flame spray pyrolysis method
Metal oxide " article " the flame spray pyrolysis method synthesizing rare-earth delivered of (publication number CN1665743A) and the yellow east etc. that continues
Oxide ", " rare earth ", 2017 (6): the predecessor in 125-136 is metallo-organic compound, and not only production cost is higher, and
And combustion synthesis reaction process is lacked to regulate and control." flame spray pyrolysis method prepares nanocrystalline magnalium to the article that Zhang Chengan etc. is delivered
Spinel powder ", " refractory material ", 2007,41 (5): 369-372 uses inorganic nitrate as predecessor, and precursor liquid solvent
For the mixed solution of ethyl alcohol and distilled water, although reducing costs, the powder granule particle diameter distribution that it is synthesized is very wide.More than
Research is prepared for associated materials simply by the method for preliminary flame spray pyrolysis, exists for the YAG powder synthesized
The problem that particle is uneven, size is uncontrollable, it is difficult to obtain the nano-level sphere particle of size uniformity.
Summary of the invention
Based on this, it is necessory to provide a kind of precursor liquid, yttrium is synthesized using high-temperature atomizing flame prepared by the precursor liquid
Aluminium composite oxide nano-powder and preparation method.
A kind of preparation method of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder, comprising:
Precursor liquid is atomized to form drop, the precursor liquid includes Y3+And Al3+Inorganic salts, additive and organic solvent；
And
The drop is passed through in flame and is reacted, yttrium aluminium composite oxide nano-powder is generated,
Wherein, the additive is used for and the Y3+And Al3+Inorganic salts under the action of the flame in the forerunner
Volatilization temperature is generated in the drop that liquid is formed is lower than the Y3+And Al3+Inorganic salts substance, to improve the Y3+With
Al3+Volatility of the inorganic salts in the flame.
In one embodiment, under the action of the additive, the volatilization temperature is lower than the Y3+And Al3+'s
The substance of inorganic salts evaporating completely in flame is changed into gas phase, then by the gas phase forming core, grow up that it is compound to generate the yttrium aluminium
Nm-class oxide powder.
In one embodiment, the additive contains carboxylic acid group, can be with the Y3+And Al3+Inorganic salts exist
Y is generated in the drop that the precursor liquid is formed3+And Al3+Carboxylate.
In one embodiment, the additive include 2 ethyl hexanoic acid, citric acid, aphthenic acids, in neodecanoic acid extremely
Few one kind.
In one embodiment, mass fraction of the additive in the precursor liquid is 5% to 50%.
In one embodiment, mass fraction of the additive in the precursor liquid is 18% to 30%.
In one embodiment, the enthalpy of combustion of the organic solvent is greater than 20kJ/ml.
In one embodiment, the organic solvent includes at least one of methanol, ethyl alcohol, n-butanol, isopropanol.
In one embodiment, the precursor liquid further includes the water to dissolve each other with the organic solvent.
In one embodiment, the Y3+And Al3+Inorganic salts include Y3+And Al3+Nitrate, villiaumite, villaumite, bromine
At least one of salt, salt compounded of iodine, carbonate.
In one embodiment, the precursor liquid further includes the inorganic salts of doped metal ion, the doping metals from
Attached bag includes Yb3+、Nd3+、Ce3+And Eu3+At least one of.
In one embodiment, total concentration of the metal ion in the precursor liquid is 0.16~0.8mol/L.
In one embodiment, the temperature of the flame is 1200 DEG C to 1900 DEG C.
A kind of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder, average grain diameter are 20 nanometers to 30 nanometers.
In one embodiment, the material of the high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder includes
Y3Al5O12And M:Y3Al5O12At least one of, M is trivalent metal cation.
In one embodiment, M Yb3+、Nd3+、Ce3+And Eu3+At least one of.
In one embodiment, particle diameter distribution is 20 nanometers to 30 nanometers.
In one embodiment, particle diameter distribution meets D95-D5≤ 10 nanometers.
A kind of precursor liquid synthesizes yttrium aluminium composite oxide nano-powder for high-temperature atomizing flame, and the precursor liquid includes
Y3+And Al3+Inorganic salts, additive and organic solvent, the additive is for improving the Y3+And Al3+Inorganic salts in flame
In volatility.
In one embodiment, the additive include 2 ethyl hexanoic acid, citric acid, aphthenic acids, in neodecanoic acid extremely
Few one kind.
Provided by the present invention for being added in the precursor liquid of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder
It can be improved Y3+And Al3+Volatile additive of the inorganic salts in flame, it is right in combination with inorganic salts and organic solvent
Liquid phase feeding is atomized the evaporation process in flame synthesis process and carries out active control, is single by the synthesis path control in flame field
One " gas phase-particle " avoids " liquid phase-particle " and " gas phase-particle " two kinds of route of synthesis from coexisting, and synthesizes road by control
Diameter solves the problems, such as that particle size is non-uniform, and the chemical constituent of the yttrium aluminium composite oxide nano-powder of preparation is more accurate, and
With nano-level sphere granule-morphology, particle size is uniform.Also, the raw material and equipment that this method is related to are simple, aggregate velocity
Fastly, process safety is suitble to heavy industrialization to utilize.
Detailed description of the invention
Fig. 1 is that the high-temperature atomizing flame of the embodiment of the present invention synthesizes the preparation method of yttrium aluminium composite oxide nano-powder
Flow chart；
Fig. 2 is that primary particles form and gather simultaneously growing mechanism schematic diagram in flame synthesis process；
Fig. 3 is the transmission electricity for the yttrium aluminium composite oxide nano-powder that the high-temperature atomizing flame of the embodiment of the present invention 1 synthesizes
Mirror (TEM) photo；
Fig. 4 is that the TEM for the yttrium aluminium composite oxide nano-powder that the high-temperature atomizing flame of the embodiment of the present invention 2 synthesizes shines
Piece；
Fig. 5 is that the TEM for the yttrium aluminium composite oxide nano-powder that the high-temperature atomizing flame of comparative example 1 of the present invention synthesizes shines
Piece；
Fig. 6 is that the TEM for the yttrium aluminium composite oxide nano-powder that the high-temperature atomizing flame of comparative example 2 of the present invention synthesizes shines
Piece；
Fig. 7 is that the TEM for the yttrium aluminium composite oxide nano-powder that the high-temperature atomizing flame of comparative example 3 of the present invention synthesizes shines
Piece；
Fig. 8 is that the TEM for the yttrium aluminium composite oxide nano-powder that the high-temperature atomizing flame of comparative example 4 of the present invention synthesizes shines
Piece；
Fig. 9 is the power spectrum point for the yttrium aluminium composite oxide nano-powder that the high-temperature atomizing flame of the embodiment of the present invention 3 synthesizes
Analyse (EDS) distribution diagram of element.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, right with reference to the accompanying drawings and embodiments
The present invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, not
For limiting the present invention.
Referring to Fig. 1, the embodiment of the present invention provides a kind of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder
Preparation method, comprising:
Precursor liquid is atomized to form drop by S1, and the precursor liquid includes Y3+And Al3+Inorganic salts, additive and organic molten
Agent；And
The drop is passed through in flame and reacts by S2, generates yttrium aluminium composite oxide nano-powder.
The additive is used for and the Y3+And Al3+Inorganic salts under the action of the flame in the precursor liquid shape
At the drop in generate volatilization temperature be lower than the Y3+And Al3+Inorganic salts substance, to improve the Y3+And Al3+
Volatility of the inorganic salts in the flame.
Referring to Fig. 2, different types of predecessor decides synthesis and the growth crack of subsequent nano particle, in flame field
The synthesis and growth of nano particle experienced primary particles formation and primary particles are gathered by collision-and form the mistake of nano particle
Journey.Gas phase predecessor forms product vapor by physically or chemically reaction, then the mistake of nano particle is converted by nucleation approach
Journey, i.e. " gas phase-particle " conversion.Liquid phase forerunner article forms atomized drop by atomization, and atomized drop evaporates in flame field to be turned
Gas phase is turned to, nano particle is converted by gas phase approach；Or it is converted into after approach such as hydatogenesis, particles' interactions
Nano particle.This process is extremely complex, it is necessary to consider the variation inside liquid drop and grain and the direct conversion of " droplet-particle ".
Inventor is had found by numerous studies, ensures that the liquid phase feeding of " gas phase-particle " path for transformation is atomized flame gas-phase synthesizing method
It is the key that the nano-scale particle for obtaining size uniformity.Inventor is added in precursor liquid can be improved Y3+And Al3+Inorganic salts
Volatile additive in flame is atomized flame synthesis process to liquid phase feeding in combination with inorganic salts and organic solvent
In evaporation process carry out active control, the synthesis path in flame field is controlled as single " gas phase-particle ", " liquid is avoided
Phase-particle " and " gas phase-particle " two kinds of route of synthesis coexist, and by controlling synthesis path, it is non-uniform to solve particle size
The chemical constituent of problem, the yttrium aluminium composite oxide nano-powder of preparation is more accurate, and has nano-level sphere granule-morphology,
Particle size is uniform.Also, the raw material and equipment that this method is related to are simple, and aggregate velocity is fast, process safety, are suitble to large-scale industry
Change and utilizes.
Specifically, passing through Y in control precursor liquid3+And Al3+Stoichiometric ratio, yttrium aluminium composite oxygen can be accurately controlled
The chemical constituent of compound nano-powder.In one embodiment, yttrium aluminium composite oxide nano-powder is preferably doped or undoped
Yttrium-aluminium-garnet (Y3Al5O12, YAG) and nano-powder.
In the precursor liquid, the Y3+And Al3+Inorganic salts, additive be dispersed or dissolved in organic solvent, uniformly
Mixing.The Y3+And Al3+Inorganic salts be preferably at least one of nitrate, villiaumite, villaumite, bromide, salt compounded of iodine, carbonate.
Preferably nitrate, such as yttrium nitrate and aluminum nitrate.Nitrate raw material for configuring the precursor liquid for example can be for six water
Yttrium nitrate (Y (NO3)3·6H2) and nine water aluminum nitrate (Al (NO O3)3·9H2O)。
In some embodiments, the precursor liquid further includes the inorganic salts of doped metal ion, the doped metal ion
Including Yb3+、Nd3+、Ce3+And Eu3+At least one of.It is synthesized using the precursor liquid of the inorganic salts with doped metal ion
Product is the yttrium aluminium composite oxide nano-powder of doping, such as the yttrium-aluminium-garnet of doping, and doped chemical is in nano-powder
It is evenly distributed.The inorganic salts of the doped metal ion be preferably nitrate, villiaumite, villaumite, bromide, salt compounded of iodine, in carbonate
It is at least one.Preferably, the inorganic salts of the doped metal ion and the Y3+And Al3+Inorganic salts be it is congener inorganic
Salt, i.e. anion are identical.More preferably, the inorganic salts of the doped metal ion are the nitrate of doping metals.It is described to add
Add agent be also used for the inorganic salts of the doped metal ion under the action of flame the precursor liquid formed described in
Substance of the volatilization temperature lower than the inorganic salts of the doped metal ion is generated in drop, to improve the doped metal ion
Volatility of the inorganic salts in the flame.
The additive is for improving Y3+And Al3+Inorganic salts and/or doped metal ion inorganic salts in the flame
In volatility, specifically, the additive can be with the Y3+And Al3+Inorganic salts and/or doped metal ion it is inorganic
Salt reacts in the flame generates volatilization temperature lower than the Y3+And Al3+Inorganic salts substance.In one embodiment, institute
State Y3+And Al3+Inorganic salts be nitrate, the additive contains carboxylic acid group, can be with the Y3+And Al3+Inorganic salts exist
Y is generated in flame3+And Al3+Carboxylate.Y3+And Al3+Carboxylate volatilization temperature be lower than Y3+And Al3+Nitrate, thus
Y is improved in flame synthesis process3+And Al3+Nitrate volatility.In one embodiment, the doped metal ion
Inorganic salts be nitrate, the additive contains carboxylic acid group, can be with the inorganic salts of the doped metal ion in flame
The middle carboxylate for generating doped metal ion.The volatilization temperature of the carboxylate of doped metal ion is lower than the nitre of doped metal ion
Hydrochlorate, to improve the volatility of the nitrate of doped metal ion in flame synthesis process.
In one embodiment, the additive includes 2 ethyl hexanoic acid, citric acid, aphthenic acids, at least one in neodecanoic acid
Kind.Mass fraction of the additive in the precursor liquid is preferably 5% to 50%, and more preferably 18% to 30%.
The organic solvent is preferably capable dissolving the Y3+And Al3+Inorganic salts and/or doped metal ion it is inorganic
Salt and the additive, can be according to Y3+And Al3+Inorganic salts and/or doped metal ion inorganic salts and additive
Specific substance selection, preferably include at least one of methanol, ethyl alcohol, n-butanol, isopropanol.In one embodiment, described
Precursor liquid can also include water, and the organic solvent can be miscible with water.Metal ion, such as Y3+And Al3+Or Y3+And Al3+
With the combination of Doped ions, the total concentration in the precursor liquid is preferably 0.16~0.8mol/L.
In the precursor liquid, the organic solvent is used in flame synthesis process provide heat as incendiary agent, right
Flame temperature is adjusted.Preferably, the enthalpy of combustion of the organic solvent is greater than 20kJ/ml.To make to react way in flame synthesis
Diameter is easier to control, and in the precursor liquid, excludes other burning capacity sources substantially in addition to organic solvent, preferably only with
Inorganic salts are as Y3+And Al3+Source, to make synthesis path with being easy to control, on this basis using Y can be adjusted3+With
Al3+Boiling characteristics additive, make synthesis path control be single " gas phase-particle ".Preferably, in the additive
Under effect, the drop is completely transformed into gas phase in flame, then by the gas phase forming core, grow up, it is compound to generate the yttrium aluminium
Nm-class oxide powder.
In step s 2, the drop is passed through in flame the step of oxidation reaction occurs, including is by precursor liquid atomization
Drop, and the step of drop is passed through burner.The drop that precursor liquid is formed directly synthesizes yttrium in the flame of burner
Aluminium composite oxide nano-powder.The temperature of the flame is preferably controlled to 1200 DEG C to 1900 DEG C.In one embodiment, it burns
Flame burnt and formed in oxygen-enriched environment by methane, the volume ratio of methane and oxygen is preferably 1:3.
The embodiment of the present invention also provides a kind of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder.Preferably,
The material of yttrium aluminium composite oxide nano-powder includes Y3Al5O12And M:Y3Al5O12At least one of, M be trivalent metal sun from
Son.It is furthermore preferred that M is Yb3+、Nd3+、Ce3+And Eu3+At least one of.
The average grain diameter of the yttrium aluminium composite oxide nano-powder is 20 nanometers to 30 nanometers.Specifically, the yttrium aluminium
The particle diameter distribution of Composite Oxides Nanometric Powder body is 20 nanometers to 30 nanometers.Preferably, the yttrium aluminium composite oxide nano powder
The particle diameter distribution of body meets D95-D5≤ 10 nanometers, that is, there is relatively narrow particle diameter distribution.
Embodiment 1
With yttrium nitrate hexahydrate (Y (NO3)3·6H2) and nine water aluminum nitrate (Al (NO O3)3·9H2O it is) predecessor, is dissolved in pure
In ethyl alcohol, additive is 2 ethyl hexanoic acid, and the mass fraction in the precursor liquid is 50%.It stoichiometrically prepares molten
Liquid, Y in precursor liquid3+:Al3+=3:5, Y in precursor liquid3+And Al3+Total concentration be 0.4mol/L.After precursor liquid atomization, into combustion
In burner flame, YAG spherical nanoparticle powder can get.
Embodiment 2
Embodiment 2 is same as Example 1, distinguishes the only mass fraction in additive 2 ethyl hexanoic acid in the precursor liquid
It is 18%.
Please refer to Fig. 3 and Fig. 4, it can be seen that since synthesis path is controlled in " gas phase-atomization precursor liquid in flame
Grain ", the particle sphericity in the nano-powder that Examples 1 and 2 obtain is good, and has relatively narrow particle diameter distribution.
Comparative example 1
Comparative example 1 is same as Example 1, distinguishes only additive-free in precursor liquid.
Referring to Fig. 5, it can be seen that, the grain diameter of powder obtained in comparative example 1 is larger, is atomized precursor liquid in flame
Synthesis path still has " droplet-particle " approach in.
Comparative example 2
With yttrium nitrate hexahydrate (Y (NO3)3·6H2) and nine water aluminum nitrate (Al (NO O3)3·9H2O it is) predecessor, is dissolved in pure
It is additive-free in deionized water, stoichiometrically prepare solution, Y in precursor liquid3+:Al3+=3:5, Y in precursor liquid3+And Al3+
Total concentration be 0.16mol/L.After precursor liquid atomization, into burner flame, YAG spheric granules powder can get.
Comparative example 3
Comparative example 3 is identical as comparative example 2, distinguishes the only Y in precursor liquid3+And Al3+Total concentration be 0.4mol/L.
Comparative example 4
Comparative example 4 is identical as comparative example 2, distinguishes the only Y in precursor liquid3+And Al3+Total concentration be 0.8mol/L.
Fig. 6 to 8 is please referred to, synthesis path has " drop-in flame due to atomization precursor liquid in comparative example 2 to 4
The path of grain ", the grain diameter of obtained powder is larger, and size distribution is more uneven.
Embodiment 3
With yttrium nitrate hexahydrate (Y (NO3)3·6H2O), nine water aluminum nitrate (Al (NO3)3·9H2) and five water ytterbium nitrate Yb O
(NO3)3·5H2O is predecessor, and wherein Yb is doped chemical, is dissolved in the in the mixed solvent of deionized water and n-butanol, water: positive fourth
Alcohol=3:1 (volume ratio).Additive is citric acid, and the mass fraction in the precursor liquid is 5%.Stoichiometrically prepare
Solution, Yb in precursor liquid3+:(Y3++Al3+)=0.05, Y in precursor liquid3+And Al3+Total concentration be 0.4mol/L.Forerunner's liquid mist
After change, into burner flame, 5%Yb-YAG doping spherical nanoparticle powder can get.
Referring to Fig. 9, atomization precursor liquid is in flame it can be seen that each element is uniformly distributed in product nano granular powder
Middle synthesis path is " gas phase-particle ".
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (20)
1. a kind of preparation method of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder characterized by comprising
Precursor liquid is atomized to form drop, the precursor liquid includes Y3+And Al3+Inorganic salts, additive and organic solvent；And
The drop is passed through in flame and is reacted, yttrium aluminium composite oxide nano-powder is generated,
Wherein, the additive is used for and the Y3+And Al3+Inorganic salts under the action of the flame in the precursor liquid shape
At the drop in generate volatilization temperature be lower than the Y3+And Al3+Inorganic salts substance, to improve the Y3+And Al3+
Volatility of the inorganic salts in the flame.
2. the preparation method of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder according to claim 1,
It is characterized in that, under the action of the additive, the volatilization temperature is lower than the Y3+And Al3+Inorganic salts substance in fire
Evaporating completely is changed into gas phase in flame, then by the gas phase forming core, grow up, generate the yttrium aluminium composite oxide nano-powder.
3. the preparation method of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder according to claim 1,
It is characterized in that, the additive contains carboxylic acid group, can be with the Y3+And Al3+Inorganic salts formed in the precursor liquid
Y is generated in the drop3+And Al3+Carboxylate.
4. the preparation method of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder according to claim 1,
It is characterized in that, the additive includes at least one of 2 ethyl hexanoic acid, citric acid, aphthenic acids, neodecanoic acid.
5. the preparation method of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder according to claim 1,
It is characterized in that, mass fraction of the additive in the precursor liquid is 5% to 50%.
6. the preparation method of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder according to claim 1,
It is characterized in that, mass fraction of the additive in the precursor liquid is 18% to 30%.
7. the preparation method of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder according to claim 1,
It is characterized in that, the enthalpy of combustion of the organic solvent is greater than 20kJ/ml.
8. the preparation method of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder according to claim 1,
It is characterized in that, the organic solvent includes at least one of methanol, ethyl alcohol, n-butanol, isopropanol.
9. the preparation method of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder according to claim 1,
It is characterized in that, the precursor liquid further includes the water to dissolve each other with the organic solvent.
10. the preparation method of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder according to claim 1,
It is characterized in that, the Y3+And Al3+Inorganic salts include Y3+And Al3+Nitrate, villiaumite, villaumite, bromide, salt compounded of iodine, in carbonate
At least one.
11. the preparation method of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder according to claim 1,
It is characterized in that, the precursor liquid further includes the inorganic salts of doped metal ion, and the doped metal ion includes Yb3+、Nd3+、Ce3 +And Eu3+At least one of.
12. according to claim 1 or high-temperature atomizing flame described in 11 synthesis yttrium aluminium composite oxide nano-powder preparation side
Method, which is characterized in that total concentration of the metal ion in the precursor liquid is 0.16~0.8mol/L.
13. the preparation method of high-temperature atomizing flame synthesis yttrium aluminium composite oxide nano-powder according to claim 1,
It is characterized in that, the temperature of the flame is 1200 DEG C to 1900 DEG C.
14. a kind of high-temperature atomizing flame synthesizes yttrium aluminium composite oxide nano-powder, which is characterized in that average grain diameter is 20 nanometers
To 30 nanometers.
15. high-temperature atomizing flame according to claim 14 synthesizes yttrium aluminium composite oxide nano-powder, which is characterized in that
Material includes Y3Al5O12And M:Y3Al5O12At least one of, M is trivalent metal cation.
16. high-temperature atomizing flame according to claim 15 synthesizes yttrium aluminium composite oxide nano-powder, which is characterized in that
M is Yb3+、Nd3+、Ce3+And Eu3+At least one of.
17. high-temperature atomizing flame according to claim 15 synthesizes yttrium aluminium composite oxide nano-powder, which is characterized in that
Particle diameter distribution is 20 nanometers to 30 nanometers.
18. high-temperature atomizing flame according to claim 15 synthesizes yttrium aluminium composite oxide nano-powder, which is characterized in that
Particle diameter distribution meets D95-D5≤ 10 nanometers.
19. a kind of precursor liquid synthesizes yttrium aluminium composite oxide nano-powder for high-temperature atomizing flame, which is characterized in that described
Precursor liquid includes Y3+And Al3+Inorganic salts, additive and organic solvent, the additive is for improving the Y3+And Al3+Nothing
Volatility of the machine salt in flame.
20. high-temperature atomizing flame according to claim 19 synthesizes yttrium aluminium composite oxide nano-powder, which is characterized in that
The additive includes at least one of 2 ethyl hexanoic acid, citric acid, aphthenic acids, neodecanoic acid.
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| CN116514546A (en) * | 2023-07-04 | 2023-08-01 | 乌镇实验室 | Potassium sodium niobate-based leadless piezoelectric ceramic powder and preparation method of leadless piezoelectric ceramic |
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| CN115055067A (en) * | 2022-05-05 | 2022-09-16 | 清华大学 | Proton conduction medium-temperature fuel cell electrolyte based on flame synthesis and preparation method thereof |
| CN115055067B (en) * | 2022-05-05 | 2024-02-02 | 清华大学 | Proton conduction medium-temperature fuel cell electrolyte based on flame synthesis and preparation method thereof |
| CN116514546A (en) * | 2023-07-04 | 2023-08-01 | 乌镇实验室 | Potassium sodium niobate-based leadless piezoelectric ceramic powder and preparation method of leadless piezoelectric ceramic |
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