CN108455651A - Y2O3Nano-powder and preparation method thereof - Google Patents
Y2O3Nano-powder and preparation method thereof Download PDFInfo
- Publication number
- CN108455651A CN108455651A CN201810482397.0A CN201810482397A CN108455651A CN 108455651 A CN108455651 A CN 108455651A CN 201810482397 A CN201810482397 A CN 201810482397A CN 108455651 A CN108455651 A CN 108455651A
- Authority
- CN
- China
- Prior art keywords
- powder
- nano
- preparation
- mixed solution
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000000843 powder Substances 0.000 title claims description 21
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000011858 nanopowder Substances 0.000 claims abstract description 41
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000243 solution Substances 0.000 claims abstract description 29
- 238000001354 calcination Methods 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 8
- 239000002270 dispersing agent Substances 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 4
- 239000008236 heating water Substances 0.000 claims abstract description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 18
- 229910017604 nitric acid Inorganic materials 0.000 claims description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 11
- 239000000908 ammonium hydroxide Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 235000005979 Citrus limon Nutrition 0.000 claims description 4
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 claims description 2
- 244000248349 Citrus limon Species 0.000 claims 3
- 238000005352 clarification Methods 0.000 claims 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 18
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 238000009826 distribution Methods 0.000 abstract description 5
- 235000015165 citric acid Nutrition 0.000 description 16
- 235000013339 cereals Nutrition 0.000 description 14
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 13
- 239000002243 precursor Substances 0.000 description 11
- 238000013019 agitation Methods 0.000 description 7
- 239000012452 mother liquor Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- 229910002651 NO3 Inorganic materials 0.000 description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 5
- 150000001768 cations Chemical class 0.000 description 4
- 239000011222 crystalline ceramic Substances 0.000 description 4
- 229910002106 crystalline ceramic Inorganic materials 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000009841 combustion method Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000005118 spray pyrolysis Methods 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- -1 europium ions Chemical class 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- RJOJUSXNYCILHH-UHFFFAOYSA-N gadolinium(3+) Chemical compound [Gd+3] RJOJUSXNYCILHH-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention provides a kind of Y2O3Nano-powder and preparation method thereof, including：Prepare Y (NO3)3Clear solution, and a concentration of 0.15~0.3mol/L of clear solution；It weighs citric acid and dispersant and is added sequentially to above-mentioned Y (NO3)3In clear solution, and control a concentration of 0.1~0.9mol/L of citric acid in mixed solution；The pH value for adjusting above-mentioned mixed solution, it is 2.5~4 to make its pH value, and then carrying out heating water bath to acid mixed solution obtains predecessor colloidal sol；Calcining is dried to get Y to above-mentioned predecessor colloidal sol2O3Nano-powder.The present invention can solve the obtained Y of existing preparation method2O3Nano-powder purity is low, chemical uniformity is bad, particle is big, includes present in the wide technical problem low with chemism of particle diameter distribution and existing preparation method itself：Required severe reaction conditions (high temperature, high pressure etc.) are not easy to mass produce, the problems such as preparation process is easily reunited, efficiency is low.
Description
Technical field
The invention belongs to rare earth nano Preparation Technique of Powders fields, and in particular to a kind of Y2O3Nano-powder and its preparation side
Method.
Background technology
The characteristics such as high temperature resistant, corrosion-resistant, high insulation, the high intensity that crystalline ceramics has ceramics intrinsic, and with glass
Optical property, many researchs and production unit are dedicated to the research and development of novel transparent ceramics at present.And yttrium oxide Y2O3Make
For a kind of excellent high-temperature infrared material and electronic material, have the good transparency, heat-and corrosion-resistant, high-temperature stability and dielectric normal
The features such as number is high, and its crystalline ceramics obtained, especially in infrared region, has very high light transmission in wider frequency range
Rate is widely used.
Y at present2O3Prepared by the vacuum hotpressing of crystalline ceramics generally use or in reducing atmosphere sintering, wherein reproducibility gas
Be sintered to the common method for preparing crystalline ceramics in atmosphere, but it is there is also certain defect, example sintering temperature as required generally compared with
Height, and need in sintering process that a large amount of sinter additives are added.Based on the defect, currently, researching and producing good dispersion, work
Property high, easy-sintering nanometer Ultrafine Yttrium Oxides Powders have become the effective ways for reducing sintering temperature.
Y2O3The preparation of related nano-powder has more research report, and preparation method has heterogeneous precipitation method, homogeneously sinks
Shallow lake method, combustion method, hydro-thermal method, spray pyrolysis, solid phase method etc..However, existing preparation method itself there are problems that,
In, heterogeneous precipitation method has the shortcomings that preparation process easily reunites, post-processes trouble in the presence of pollution；Homogeneous precipitation method prepares yield
It is low, and need to centrifuge；Combustion method reaction process is acutely difficult to control, is not easy industrial mass production；Hydro-thermal method and spraying heat
Solution needs expensive high-temperature high-pressure apparatus, and investment is larger, and operation is dangerous, and spray pyrolysis also there is powder to be not easy to receive in addition
The shortcomings of collection；Reaction temperature needed for solid phase method is high, and reunion behavior is more serious, and mechanical milling process is easily introduced impurity, causes powder
Purity is not high, these all seriously affect the performance of nano yttrium oxide powder, results in what existing preparation method was prepared
Y2O3Or nano-powder grain size is bigger or grain size is uneven, particle diameter distribution is wide or purity and activity it is not high.
It is another to there is patent application (CN201410488790.2) to report Y2O3The preparation of the nano-powder compounded with other components,
Such as citric acid sol-gel method combustion method is used to prepare nanometer Gd/Eu-Y2O3Why powder, the above method can prepare nanometer
Gd/Eu-Y2O3Powder, reason may is that：When carrying out pre-burning to lemon acid precursor, hydrogen and carbon and air reaction generate water and
Carbon dioxide is excluded, and metal cation is close to each other, due to distributing very evenly for metal cation, in any subrange
Metal cation ratio meet chemical constituent than therefore directly foring the uniform crystal phase structure of component；Meanwhile multiphase
Nano material can occur between ruthenium ion phase crystal grain and other europium ions, gadolinium ion phase grain structure during the reaction mutually
Staggeredly, pinning effect, and three kinds of crystal grain have different growth rates, can mutually inhibit, therefore this method is only suitable only for
It prepares multicomponent system, and single ruthenium ion is only used only and then lacks working in coordination between above-mentioned multiphase, be not easy to form grain size
Uniform nano yttrium oxide.
Invention content
The present invention provides a kind of Y2O3It is obtained can to solve existing preparation method for nano-powder and preparation method thereof
Y2O3Nano-powder purity is low, chemical uniformity is bad, particle is big, the wide technical problem low with chemism of particle diameter distribution and
Existing preparation method itself it is existing include：Required severe reaction conditions (high temperature, high pressure etc.) are not easy to mass produce, make
The standby technical problems such as process is easily reunited, efficiency is low.
Technical solution of the invention is：
A kind of Y is provided according to an aspect of the present invention2O3The preparation method of nano-powder, is realized by following steps：
Prepare Y (NO3)3Clear solution, and a concentration of 0.15~0.3mol/L of clear solution；
It weighs citric acid and dispersant and is added sequentially to above-mentioned Y (NO3)3In clear solution, and control mixed solution
A concentration of 0.1~0.9mol/L of middle citric acid；
The pH value for adjusting above-mentioned mixed solution, it is 2.5~4 to make its pH value, then to acid mixed solution
It carries out heating water bath and obtains predecessor colloidal sol；
Calcining is dried to get Y to above-mentioned predecessor colloidal sol2O3Nano-powder.
Further, in the present invention, the Y (NO3)3Clear solution can be used micron order Y2O3Powder heating is complete
It is dissolved in nitric acid and obtains, wherein micron order Y2O3Proportioning dosage with nitric acid is molar ratio 1：6.05~1：6.1, nitric acid matter
It is 65%~70% to measure score.
Further, in the present invention, the concentration of the citric acid is preferably 0.5~0.9mol/L；It is described mixed
The pH value of solution is preferably 3~4.
Further, in some embodiments, the dispersant in ethylene glycol, glycerine, PEG400 extremely
Few one kind, and the addition total amount of dispersant is theoretical nanometer Y2O3The 5~10% of quality.
When further, in the present invention, to mixed solution tune pH value, first its pH value can be tested, usually
In the case of the value be less than the range of above-mentioned restriction, therefore the pH value of the mixed solution is adjusted using alkaline matter
Section.
Further, the alkaline matter is preferably ammonium hydroxide.
Further, in the present invention, the water bath heating temperature is 60~90 DEG C, and heating time is 2~3h.
Further, in the present invention, the precursor colloidal sol drying temperature be 160~240 DEG C, drying time be 2~
4h。
Further, in the present invention, the calcination temperature be 500~800 DEG C, calcination time be (0,1h].
On the other hand, the present invention also provides a kind of Y2O3Nano-powder, the nano-powder are prepared using above-mentioned preparation method
It obtains.
It applies the technical scheme of the present invention, provides a kind of Y2O3Nano-powder and preparation method thereof, the present invention is in list
On the basis of one raw material micron order yttrium oxide powder, by selecting chelating agent (citric acid) type, regulation and control reactant pH and each group
Proportioning and concentration for dividing etc., which are realized, accurately controls forerunner's precursor reactant nucleation and granular grows.
On the one hand, as an important point of the invention, so that the pH value of reaction solution is in acidity under the action of ammonium hydroxide,
Especially under conditions of pH value is 2.5~4, is conducive to metal cation and is fixed on complex compound citric acid generation polymerisation
Among organic three-dimensional grid so that metal ion is evenly distributed in gel, and the addition of a small amount of ammonium hydroxide can be with yttrium
Ion forms alkali formula chelate so that crystal grain has different growth rates, can mutually inhibit；On the other hand, in the present invention
Under the acidic environment of setting, citric acid is used as reducing agent in redox, after nitrate and citric acid reactions, the gel of formation
When heated, redox reaction, wherein NO occurs3 -Oxidizing atmosphere, COO are provided-As fuel, in gel structure
NO3 -And COO-" original position " oxidation-reduction reaction occurs at a certain temperature and forms loose powder to which self-propagating combustion occur
End, reaction process are not required to filter, and shorten the reaction time, improve sample efficiencies.In addition, citric acid is lower as molecular weight
Carboxylic acid, the abundant hydroxyl in part carboxyl energy substitute particles surface, is combined to form mono layer adsorption with metal ion, makes particle table
Face takes negative electrical charge and mutually exclusive, plays peptizaiton, has stronger inhibiting effect to the growth of crystal grain, before reducing
The reunion and crystal grain for driving body particle are grown up.
To sum up, of the invention preparation method is simple, is suitable for large-scale production and the higher and prepared nanometer of yield
Powder has many advantages, such as that purity high (organic impurities high temperature easily decomposes), grain size is small, particle diameter distribution is narrow, uniformity is good, have compared with
Good prospects for commercial application.
Description of the drawings
Fig. 1 is the X-ray diffractogram according to prepared nano yttrium oxide provided in an embodiment of the present invention.
Specific implementation mode
Specific embodiments of the present invention are described in detail below.In the following description, unrestricted for explanation
Property purpose, elaborate detail, with help be apparent from the present invention.It will be apparent however, to one skilled in the art that it is aobvious and
It is clear to, the present invention can also be put into practice in the other embodiments departing from these details.
It should be noted that in order to avoid having obscured the present invention because of unnecessary details, only show in the accompanying drawings
The device structure closely related with scheme according to the present invention and/or processing step are gone out, and have been omitted with relationship of the present invention not
Big other details.
Embodiment 1
By micron order (4N) Y of certain mass2O3Powder (purity 99.99%) heating is dissolved completely in excessive nitric acid
(mass fraction 65%) is diluted with water the Y (NO for being made into 0.25mol/L3)3Clear solution, and micron order (4N) Y2O3With nitric acid
The proportioning dosage of (mass fraction 65%) dissolving is stoichiometric ratio 2：3；Under agitation successively by 9g citric acids,
Above-mentioned Y (NO are added in 0.806g ethylene glycol3)3Clear solution in, ammonium hydroxide (mass fraction is added to after fully transparent in stirring
25%) it adjusts pH to 3 and obtains mother liquor, 80 DEG C of water-bath 2.5h obtain faint yellow thick predecessor colloidal sol；By precursor sol 180
DEG C dry 2h, 600 DEG C of calcining 1h obtain Y2O3Nano-powder.The X-ray diffractogram of 1 gained nano yttrium oxide of the present embodiment is such as
Shown in Fig. 1, Fig. 1 illustrates that precursor obtains the pure crystalline phase of nano yttrium oxide through 600 DEG C of calcining 1h, and purity is very high；Using laser
Particle size analyzer is tested, the yttrium oxide nano-powder average grain diameter about 40nm that the present embodiment 1 obtains.
Embodiment 2
By micron order (4N) Y of certain mass2O3Powder (purity 99.99%) heating is dissolved completely in excessive nitric acid
(mass fraction 65%) is diluted with water the Y (NO for being made into 0.25mol/L3)3Clear solution, and micron order (4N) Y2O3With nitric acid
The proportioning dosage of (mass fraction 65%) dissolving is stoichiometric ratio 2：3；Under agitation successively by 12g citric acids,
Above-mentioned Y (NO are added in 0.906g glycerine3)3Clear solution in, ammonium hydroxide (mass fraction is added to after fully transparent in stirring
25%) it adjusts pH to 3 and obtains mother liquor, 90 DEG C of water-bath 2h obtain faint yellow thick predecessor colloidal sol；By 180 DEG C of precursor sol
Dry 2h, 800 DEG C of calcining 0.5h, obtains Y2O3Nano-powder.It is tested using laser particle analyzer, the yttrium oxide that the present embodiment 2 obtains
Nano-powder average grain diameter about 45nm.
Embodiment 3
By micron order (4N) Y of certain mass2O3Powder (purity 99.99%) heating is dissolved completely in excessive nitric acid
(mass fraction 65%) is diluted with water the Y (NO for being made into 0.2mol/L3)3Clear solution, and micron order (4N) Y2O3With nitric acid
The proportioning dosage of (mass fraction 65%) dissolving is stoichiometric ratio 2：3；Under agitation successively by 7.2g citric acids,
Above-mentioned Y (NO are added in 0.580g PEG 4003)3Clear solution in, ammonium hydroxide (mass fraction is added to after fully transparent in stirring
25%) it adjusts pH to 2.5 and obtains mother liquor, 80 DEG C of water-bath 2.5h obtain faint yellow thick predecessor colloidal sol；By precursor sol
240 DEG C of dry 1.5h, 600 DEG C of calcining 1h, obtain Y2O3Nano-powder.It is tested using laser particle analyzer, what the present embodiment 3 obtained
Yttrium oxide nano-powder average grain diameter about 48nm.
Embodiment 4
By micron order (4N) Y of certain mass2O3Powder (purity 99.99%) heating is dissolved completely in excessive nitric acid
(mass fraction 65%) is diluted with water the Y (NO for being made into 0.25mol/L3)3Clear solution, and micron order (4N) Y2O3With nitric acid
The proportioning dosage of (mass fraction 65%) dissolving is stoichiometric ratio 2：3；Under agitation successively by 9g citric acids,
Above-mentioned Y (NO are added in 0.806g ethylene glycol3)3Clear solution in, ammonium hydroxide (mass fraction is added to after fully transparent in stirring
25%) it adjusts pH to 3 and obtains mother liquor, 80 DEG C of water-bath 2.5h obtain faint yellow thick predecessor colloidal sol；By precursor sol 180
DEG C dry 2h, 800 DEG C of calcining 1h obtain Y2O3Nano-powder.It is tested using laser particle analyzer, the yttrium oxide that the present embodiment 4 obtains
Nano-powder average grain diameter about 45nm.
Embodiment 5
By micron order (4N) Y of certain mass2O3Powder (purity 99.99%) heating is dissolved completely in excessive nitric acid
(mass fraction 65%) is diluted with water the Y (NO for being made into 0.25mol/L3)3Clear solution, and micron order (4N) Y2O3With nitric acid
The proportioning dosage of (mass fraction 65%) dissolving is stoichiometric ratio 2：3；Under agitation successively by 12g citric acids,
Above-mentioned Y (NO are added in 0.806g ethylene glycol3)3Clear solution in, ammonium hydroxide (mass fraction is added to after fully transparent in stirring
25%) it adjusts pH to 3 and obtains mother liquor, 80 DEG C of water-bath 2.5h obtain faint yellow thick predecessor colloidal sol；By precursor sol 180
DEG C dry 2h, 800 DEG C of calcining 1h obtain Y2O3Nano-powder.It is tested using laser particle analyzer, the yttrium oxide that the present embodiment 5 obtains
Nano-powder average grain diameter about 45nm.
Embodiment 6
By micron order (4N) Y of certain mass2O3Powder (purity 99.99%) heating is dissolved completely in excessive nitric acid
(mass fraction 65%) is diluted with water the Y (NO for being made into 0.25mol/L3)3Clear solution, and micron order (4N) Y2O3With nitric acid
The proportioning dosage of (mass fraction 65%) dissolving is stoichiometric ratio 2：3；Under agitation successively by 12g citric acids,
Above-mentioned Y (NO are added in 0.806g ethylene glycol3)3Clear solution in, ammonium hydroxide (mass fraction is added to after fully transparent in stirring
25%) it adjusts pH to 4 and obtains mother liquor, 90 DEG C of water-bath 2h obtain faint yellow thick predecessor colloidal sol；By 240 DEG C of precursor sol
Dry 1.5h, 800 DEG C of calcining 0.5h, obtains Y2O3Nano-powder.It is tested using laser particle analyzer, the oxidation that the present embodiment 6 obtains
Yttrium nano-powder average grain diameter about 48nm.
Comparative example 1
By micron order (4N) Y of certain mass2O3Powder (purity 99.99%) heating is dissolved completely in excessive nitric acid
(mass fraction 65%) is diluted with water the Y (NO for being made into 0.25mol/L3)3Clear solution, and micron order (4N) Y2O3With nitric acid
The proportioning dosage of (mass fraction 65%) dissolving is stoichiometric ratio 2：3；Under agitation successively by 12g citric acids,
0.806g ethylene glycol is added in the clear solution of above-mentioned Y (NO3) 3, and ammonium hydroxide (mass fraction is added to after fully transparent in stirring
25%) it adjusts pH to 8 and obtains mother liquor, 90 DEG C of water-bath 2h obtain thick predecessor colloidal sol；By 240 DEG C of dryings of precursor sol
1.5h, 800 DEG C of calcining 0.5h, obtains Y2O3 nano-powders.It is tested using laser particle analyzer, the yttrium oxide that the present embodiment 6 obtains
Nano-powder average grain diameter about 65nm.
1 Y of table2O3Nano-powder laser particle analyzer test result
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative example 1 |
| 40nm | 45nm | 48nm | 45nm | 45nm | 48nm | 65nm |
From table 1 it follows that within the scope of the acid mother liquid defined by the method for the present invention, preparation-obtained Y2O3It receives
The grain size of rice flour body is smaller, and particle diameter distribution is also narrow, and limits range beyond the present invention, then grain size becomes larger.
As above it is directed to that a kind of embodiment describes and/or the feature that shows can be in a manner of same or similar at one or more
It is used in a number of other embodiments, and/or the feature in other embodiments is combined or substitutes with the feature in other embodiments
It uses.
It should be emphasized that term "comprises/comprising" refers to the presence of feature, one integral piece, step or component when being used herein, but simultaneously
It is not excluded for the presence or additional of one or more other features, one integral piece, step, component or combinations thereof.
The many features and advantage of these embodiments are clear according to the detailed description, therefore appended claims are intended to
Cover all these feature and advantage of these embodiments fallen into its true spirit and range.Further, since this field
Technical staff is readily apparent that many modifications and changes, therefore is not meant to the embodiment of the present invention being limited to illustrated and description essence
Really structurally and operationally, but all suitable modifications and the equivalent fallen within the scope of its can be covered.
Unspecified part of the present invention is known to the skilled person technology.
Claims (10)
1. a kind of Y2O3The preparation method of nano-powder, which is characterized in that the method is realized by following steps：
Prepare Y (NO3)3Clear solution, and a concentration of 0.15~0.3mol/L of clear solution；
It weighs citric acid and dispersant and is added sequentially to above-mentioned Y (NO3)3In clear solution, and control lemon in mixed solution
A concentration of 0.1~0.9mol/L of lemon acid；
The pH value for adjusting above-mentioned mixed solution, it is 2.5~4 to make its pH value, is then carried out to acid mixed solution
Heating water bath obtains predecessor colloidal sol；
Calcining is dried to get Y to above-mentioned predecessor colloidal sol2O3Nano-powder.
2. a kind of Y according to claim 12O3The preparation method of nano-powder, which is characterized in that the Y (NO3)3Clarification
Solution can be used micron order Y2O3Powder heating, which is dissolved completely in nitric acid, to be obtained, wherein the micron order Y2O3With the nitre
The proportioning dosage of acid is molar ratio 1：6.05~1：6.1.
3. a kind of Y according to claim 1 or 22O3The preparation method of nano-powder, which is characterized in that the lemon
The concentration of acid is preferably 0.5~0.9mol/L；The pH value of the mixed solution is preferably 3~4.
4. according to a kind of Y of claim 1-3 any one of them2O3The preparation method of nano-powder, which is characterized in that described
Dispersant is selected from least one of ethylene glycol, glycerine, PEG400, and the addition total amount of the dispersant is theoretical nanometer
Y2O3The 5~10% of quality.
5. according to a kind of Y of claim 1-4 any one of them2O3The preparation method of nano-powder, which is characterized in that use alkali
The pH value of the mixed solution is adjusted in property substance.
6. a kind of Y according to claim 52O3The preparation method of nano-powder, which is characterized in that the alkaline matter
Preferably ammonium hydroxide.
7. according to a kind of Y of claim 1-6 any one of them2O3The preparation method of nano-powder, which is characterized in that described
Water bath heating temperature is 60~90 DEG C, and heating time is 2~3h.
8. according to a kind of Y of claim 1-7 any one of them2O3The preparation method of nano-powder, which is characterized in that before described
Body colloidal sol drying temperature is 160~240 DEG C, and drying time is 2~4h.
9. according to a kind of Y of claim 1-8 any one of them2O3The preparation method of nano-powder, it is characterised in that：Described
Calcination temperature be 500~800 DEG C, calcination time be (0,1h].
10. a kind of Y2O3Nano-powder, which is characterized in that the Y2O3Nano-powder uses claim 1-9 any one of them
Preparation method is prepared.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810482397.0A CN108455651A (en) | 2018-05-18 | 2018-05-18 | Y2O3Nano-powder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810482397.0A CN108455651A (en) | 2018-05-18 | 2018-05-18 | Y2O3Nano-powder and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108455651A true CN108455651A (en) | 2018-08-28 |
Family
ID=63215511
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810482397.0A Pending CN108455651A (en) | 2018-05-18 | 2018-05-18 | Y2O3Nano-powder and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108455651A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1523077A (en) * | 2003-09-05 | 2004-08-25 | �й���ѧԺ�����о��� | Method for preparing rare earth oxide group nanometer luminescent powder |
| CN1686817A (en) * | 2005-04-29 | 2005-10-26 | 中国科学院上海光学精密机械研究所 | Method for synthesizing Y2O3 nano material directly from combustion method of citric acid |
| KR100792279B1 (en) * | 2006-06-28 | 2008-01-08 | 한국지질자원연구원 | Preparation Method of Nano Size Red Phosphor by Milling and Calcination of Gel Powder obtained by Sol-Gel Method and Heat Treatment |
| CN101462869A (en) * | 2009-01-09 | 2009-06-24 | 中国科学院上海硅酸盐研究所 | Far infrared radiation nano material and preparation thereof |
| CN105622131A (en) * | 2015-12-25 | 2016-06-01 | 浙江大学 | Preparation method for yttria-stabilized zirconia porous bulks |
-
2018
- 2018-05-18 CN CN201810482397.0A patent/CN108455651A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1523077A (en) * | 2003-09-05 | 2004-08-25 | �й���ѧԺ�����о��� | Method for preparing rare earth oxide group nanometer luminescent powder |
| CN1686817A (en) * | 2005-04-29 | 2005-10-26 | 中国科学院上海光学精密机械研究所 | Method for synthesizing Y2O3 nano material directly from combustion method of citric acid |
| KR100792279B1 (en) * | 2006-06-28 | 2008-01-08 | 한국지질자원연구원 | Preparation Method of Nano Size Red Phosphor by Milling and Calcination of Gel Powder obtained by Sol-Gel Method and Heat Treatment |
| CN101462869A (en) * | 2009-01-09 | 2009-06-24 | 中国科学院上海硅酸盐研究所 | Far infrared radiation nano material and preparation thereof |
| CN105622131A (en) * | 2015-12-25 | 2016-06-01 | 浙江大学 | Preparation method for yttria-stabilized zirconia porous bulks |
Non-Patent Citations (1)
| Title |
|---|
| 贾全利 等: "柠檬酸溶胶-凝胶法制备纳米Y2O3:Eu3+粉体", 《中国粉体技术》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP4289794A1 (en) | Layered cobalt-free positive electrode material and preparation method therefor, and lithium-ion battery | |
| CN106784817B (en) | Ferric phosphate/graphene composite material preparation method | |
| CN101113010A (en) | Method for preparing cerium oxide nano particle by auxiliary microwave | |
| CN112342605A (en) | Low-cost low-cobalt single crystal ternary cathode material and preparation method thereof | |
| CN108689422B (en) | Preparation method of large-specific-surface-area nano gadolinium oxide powder | |
| CN112875755B (en) | Preparation method of bismuth tungstate nano powder | |
| CN104387059A (en) | Scandium-cerium co-doped zirconium oxide powder and preparation method thereof | |
| CN102241516A (en) | Method for preparing Li4SiO4 ceramic powder by water-based sol-gel process | |
| CN115465904B (en) | Process for preparing nano iridium dioxide by strong dispersion | |
| CN107857300B (en) | A kind of preparation method of β type bismuth oxide | |
| WO2023134113A1 (en) | Preparation method for lithium bis(oxalato)borate | |
| CN114133240A (en) | Method for preparing scandium-cerium-ytterbium-doped zirconia superfine powder by hydrolysis-hydrothermal method | |
| CN109399709A (en) | A kind of reduction VO2The method of powder heat treatment temperature and phase transition temperature | |
| CN103482679A (en) | Aluminum zinc oxide (AZO) nano powder and preparation method of AZO sintered bodies | |
| CN107777718B (en) | A kind of Y2O3Nano-powder and preparation method thereof | |
| CN113292097A (en) | Method for preparing high-tetragonality barium titanate powder | |
| CN102167403B (en) | Preparation method of composite metallic oxide powder | |
| CN108455651A (en) | Y2O3Nano-powder and preparation method thereof | |
| CN105970323B (en) | A kind of antistatic powder and preparation method thereof | |
| CN102259909B (en) | Preparation method of lead carbonate combustion catalyst for solid propellant | |
| CN112573569B (en) | Rare earth composite oxide with high heat resistance and preparation method thereof | |
| CN104326467B (en) | A kind of preparation method of flower-shaped lithium manganese phosphate nano particle and product | |
| CN109019667B (en) | ZnO/Sm2O3Composite film and preparation method and application thereof | |
| CN106365192A (en) | Preparation method of ultra-small scale rare-earth oxide nano-powder | |
| CN108574094B (en) | Negative electrode material for lithium ion battery and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180828 |
|
| RJ01 | Rejection of invention patent application after publication |