CN115140760A - Preparation method of indium tin oxide nano powder based on microfluid rapid precipitation - Google Patents
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- 238000001556 precipitation Methods 0.000 title claims abstract description 31
- LNNWKAUHKIHCKO-UHFFFAOYSA-N dioxotin;oxo(oxoindiganyloxy)indigane Chemical compound O=[Sn]=O.O=[In]O[In]=O LNNWKAUHKIHCKO-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 26
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000005086 pumping Methods 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000012670 alkaline solution Substances 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 239000011858 nanopowder Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000012266 salt solution Substances 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 229910052738 indium Inorganic materials 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 4
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 4
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- PEVRKKOYEFPFMN-UHFFFAOYSA-N 1,1,2,3,3,3-hexafluoroprop-1-ene;1,1,2,2-tetrafluoroethene Chemical compound FC(F)=C(F)F.FC(F)=C(F)C(F)(F)F PEVRKKOYEFPFMN-UHFFFAOYSA-N 0.000 claims description 2
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 2
- 239000005350 fused silica glass Substances 0.000 claims description 2
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims description 2
- 229920002530 polyetherether ketone Polymers 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 2
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 16
- 238000009826 distribution Methods 0.000 abstract description 15
- 238000005054 agglomeration Methods 0.000 abstract description 6
- 230000002776 aggregation Effects 0.000 abstract description 6
- 239000002245 particle Substances 0.000 description 14
- 239000012071 phase Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 9
- 230000001965 increasing effect Effects 0.000 description 5
- 238000010899 nucleation Methods 0.000 description 5
- 230000006911 nucleation Effects 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 150000002500 ions Chemical group 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000003321 amplification Effects 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 3
- 238000009388 chemical precipitation Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 238000003199 nucleic acid amplification method Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 239000013077 target material Substances 0.000 description 3
- 150000004703 alkoxides Chemical class 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 229910003437 indium oxide Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- 238000010900 secondary nucleation Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910021617 Indium monochloride Inorganic materials 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- APHGZSBLRQFRCA-UHFFFAOYSA-M indium(1+);chloride Chemical group [In]Cl APHGZSBLRQFRCA-UHFFFAOYSA-M 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000016507 interphase Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002090 nanochannel Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- Nanotechnology (AREA)
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- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The invention relates to the preparation field of indium tin oxide nano powder, in particular to a method for preparing indium tin oxide nano powder based on microfluid rapid precipitation, which comprises the steps of preparing metal salt of indium tin into a reaction water phase according to a proportion, using an alkaline solution as a precipitation phase, pumping the reaction phase and the precipitation phase into a microreactor by using a flow pump to mix and react, carrying out solid-liquid separation, washing and drying a precursor, and calcining at high temperature to prepare ellipsoidal indium tin oxide nano powder. The average grain diameter of the prepared ITO powder is about 15nm, the distribution is uniform, and the agglomeration is not easy to occur.
Description
Technical Field
The invention relates to the field of preparation of indium tin oxide nano powder, in particular to a method for preparing indium tin oxide nano powder based on microfluid rapid precipitation.
Background
Indium Tin Oxide (ITO) is a mixture of 90wt% In 2 O 3 And 10wt% SnO 2 Mixing the components. The ITO powder as a highly degenerate N-type semiconductor material has excellent properties such as high light transmittance optical properties, low resistivity, electrode characteristics and the like after film formation, and thus has wide applications in high-tech fields such as liquid crystal displays, buildings, electronics, automotive industry, laser radiation protection, solar cells and the like. The industry mainly manufactures ITO powder into a target material, and then manufactures the ITO target material into an ITO film by using methods such as magnetron sputtering and the like. Therefore, the preparation of the monodisperse ITO nano powder with small particle size, narrow distribution and high purity is the key for preparing the high-density target material, so that the ITO film with excellent photoelectric performance can be sputtered and deposited.
At present, the production method of the ITO nano powder mainly comprises a mechanical ball milling method, a hydrothermal method, a sol-gel method, a micro-emulsion method, a chemical precipitation method and the like. Although the mechanical ball milling method is easy to realize production in industrial production, the prepared ITO nano powder is easy to be irradiated into harsh conditions of poor size controllability of the nano powder, more impurities, high temperature, high pressure and the like, so that the energy consumption and the equipment cost are high. The ITO nano powder produced by the hydrothermal method has the advantages of uniform particle size, good dispersibility and controllable crystal form, but has the same defects as the mechanical ball milling method. Although the sol-gel method can prepare high-purity ITO powder, the particle size distribution is narrow, the reaction process is easy to control, the metal alkoxide of the precursor has high toxicity and is easy to cause accidents, the metal alkoxide of the indium tin is expensive, and the obtained product has large shrinkage after being dried, thereby influencing the later application. The ITO nano powder prepared by the microemulsion method has the advantages of narrow particle size, uniform distribution, regular shape and good dispersibility, but a large amount of surfactant is required to be used in the preparation process and is difficult to remove, so that the product has low purity and high cost. The chemical precipitation method is simple and convenient to operate, mature in technology and mild in experimental conditions, so that the chemical precipitation method is the most ideal preparation method of the ITO nano powder at present. However, in the conventional stirred tank reactor, because the mass transfer distance of reactants is long and the specific surface area is small, the characteristic time of micromixing in the reactor is longer than the time of inducing nucleation, so that the nucleation growth process is in an uneven environment on a molecular scale, and the prepared ITO powder has the defects of large particle size, uneven distribution, easy agglomeration and the like. The microfluid precipitation method is to utilize single-phase or multi-phase fluid to make precipitation reaction in the microreactor whose size is millimeter or even nano channel. Microchannel reactors are also often abbreviated as microreactors and are widely used in the field of existing material preparation due to their high controllability and simplicity of operation. The channel size of the micro-reactor is generally in the range of micron to millimeter, the micro-structure in the micro-reactor ensures that the micro-reactor has short mass transfer distance of interaction on molecular scale, the specific surface area of reaction substances is extremely large (can reach hundreds of times or thousands of times of the traditional kettle reactor), physical fields such as a temperature field, a concentration field, a pressure field and the like in the micro-channel are uniformly distributed, instant uniform mixing and efficient heat and mass transfer of materials can be realized, the micro-mixing time is extremely short, and the nucleation rate is faster than that of the traditional kettle reactor, so that the prepared powder has the advantages of difficult agglomeration, narrow particle size distribution and the like, and the defects of the traditional kettle reactor are greatly overcome. Meanwhile, the micro-reactor has no amplification effect, the number of the micro-channels is increased only by a number increasing mode without changing the size of the micro-channels, and the reaction conditions and the physical field distribution are not changed, so that the product prepared after amplification has good repeatability and the controllability of the particle size distribution is better. Therefore, in the preparation of ITO nano powder, the microfluid precipitation technology implemented in the microreactor is easier to realize industrial production.
Disclosure of Invention
The invention aims to provide a method for preparing Indium Tin Oxide (ITO) nano powder, which has the advantages of simple process, easy amplification, good dispersibility and narrow particle size distribution.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a method for preparing indium tin oxide nano powder based on microfluid rapid precipitation comprises the steps of preparing metal salts of indium tin into a reaction water phase according to a proportion, using an alkaline solution as a precipitation phase, pumping the reaction phase and the precipitation phase into a microreactor accurately by using a flow pump for mixing and reacting, performing solid-liquid separation, washing and drying a precursor, and calcining at high temperature to prepare ellipsoidal indium tin oxide nano powder, and is characterized by comprising the following steps:
s1: preparing indium-containing salt solution and tin-containing salt solution into indium tin metal salt mixed solution with the concentration of In3+ of 0.1-2 mol/L according to the mass ratio of In2O3 to SnO2 of 9:1 In the ITO product;
s2: preparing an alkali liquor used as a precipitation phase, wherein the molar ratio of In & lt 3+ & gt In the indium-tin metal salt mixed solution to OH & lt- & gt In the alkali liquor is 1.2-1;
s3: accurately pumping the indium tin metal salt mixed solution and alkali liquor into the microreactor through a flow pump to quickly mix and react to generate indium tin compound precursor precipitate, wherein the total flow of the pumped two phases is 0.1-20 mL/min.
S4: washing and drying the generated indium tin compound precursor;
s5: and calcining the treated indium tin compound precursor at high temperature to prepare the ellipsoidal indium tin oxide nano powder.
Preferably, the mixing reaction time in the micro-reactor is 1-60 s, and the micro-channel reaction temperature of the micro-reactor is 20-80 ℃.
Preferably, the microreactor is any one of a capillary microreactor, a chip microreactor and a droplet flow microreactor.
Preferably, the material of the micro-reactor is any one or a combination of several of a stainless steel pipeline, a polytetrafluoroethylene pipeline, a polyether ether ketone pipeline, a perfluoroethylene propylene copolymer pipeline, a tetrafluoroethylene pipeline and a fused quartz pipeline.
Preferably, the micro-channel size of the micro-reactor is 0.1-3 mm.
Preferably, the indium-containing salt solution is any one or a combination of several of indium chloride solution, sulfate solution and nitrate solution; the tin-containing salt solution is any one or a combination of a plurality of tin chloride solution, sulfate solution and nitrate solution.
Preferably, the calcination temperature of the indium tin compound precursor is 300-500 ℃, and the calcination time is 0.5-2 h.
The invention has the beneficial effects that: the prior method for preparing ITO has a plurality of articles and patents related to the ITO, but the ITO is mostly prepared by a conventional stirring type liquid phase precipitation method. In the stirring process of a conventional large reactor, the phenomena of overlong material mixing time, slow mass transfer and heat transfer rates, overlong time of induced nucleation of precursor crystals and secondary nucleation exist. Meanwhile, in the stirring process, the materials are difficult to be ensured to be in a completely and uniformly distributed state, so that the local concentration is too high, and the agglomeration phenomenon of the powder is serious. Therefore, the ITO powder prepared by the conventional stirring type liquid phase precipitation method has the defects of wider particle size distribution and easy agglomeration, and the ITO powder with the average particle size of less than 20nm cannot be prepared.
The micro-reactor adopted in the micro-fluid precipitation method of the invention cuts the liquid-liquid phase into fluid with micron or even nano scale, the physical gradient of concentration, temperature, pressure and the like among the fluids is sharply increased, the inter-phase mass transfer distance is shortened, the mass transfer interfacial area and the mass transfer driving force are obviously enhanced, the mixing of materials has higher nucleation rate and high-efficiency mass transfer, and the phenomenon of secondary nucleation is greatly reduced. Therefore, the method for preparing the ITO nano powder by the microfluid precipitation method has the outstanding advantages of high mass transfer efficiency, short reaction time, small equipment size, uniform and rapid liquid-liquid phase mixing, uniform residence time distribution and the like through the structurization of the micro-channel without mechanical external force. The average grain diameter of the prepared ITO powder is about 15nm, the distribution is uniform, and the agglomeration is not easy to occur. In addition, in the industrial production, the number of the microreactors is modularly increased only by a 'number increasing mode' without amplifying the channel size, and the amplifying effect of a conventional large reactor does not exist, so that the prepared nano powder has good repeatability and excellent performance.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings may be obtained according to the drawings without creative efforts.
FIG. 1 is a TEM and particle size distribution chart of ITO powder prepared under the conditions of example 1 of the present invention;
FIG. 2 is a TEM and particle size distribution chart of ITO powder prepared under the conditions of example 2 of the present invention;
fig. 3 is an XRD pattern of a sample prepared according to an embodiment of the present invention, where a is the powder prepared in example 1 and B is the powder prepared in example 2.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The aqueous phase of the reactant is InCl 3 And SnCl 4 The mixed solution of (1), wherein In 3+ Ammonium bicarbonate solution with concentration of 0.1mol/L and precipitation phase of 0.4mol/L, reaction water phase and precipitation phase staying in microreactor at 20 deg.C for 20s, subjecting the obtained indium tin compound precursor to liquid-solid separation, and calcining at 500 deg.C for 1h to obtain the final productThe average particle size of the ITO nano powder is 14.5nm, the particle size distribution is between 5 and 40nm, wherein the powder accounting for 5 to 20nm is 86.5 percent, the energy spectrogram of the ITO nano powder prepared by XRD analysis is consistent with that of a standard indium oxide card (JCPDS.71-2194), and no other miscellaneous peaks and Sn are generated 4+ Ion substitution of In 3+ The position of the ion is completely doped In 2 O 3 In the unit cell of (1), in having a cubic structure is produced 2 O 3 A solid solution of (2).
Example 2
The aqueous phase of the reactant is In 2 (SO 4 ) 3 And SnSO 4 The mixed solution of (1), wherein In 3+ Ammonia water solution with concentration of 0.5mol/L and precipitation phase of 1mol/L, the reaction water phase and the precipitation phase stay for 60s in a microreactor with the temperature of 80 ℃, the obtained indium tin compound precursor is subjected to liquid-solid separation and is calcined for 0.5h at the temperature of 300 ℃, the average grain diameter of the prepared ITO nano powder is 14.8nm, the grain diameter distribution is between 5 and 40nm, the powder ratio between 5 and 20nm is 90 percent, the energy spectrogram of the ITO nano powder prepared by XRD analysis is consistent with the standard card of indium oxide (JCPDS.71-2194), other miscellaneous peaks are avoided, and Sn is in the ITO nano powder 4+ Ion substitution of In 3+ The position of the ion is completely doped In 2 O 3 In the unit cell of (1), in having a cubic structure is produced 2 O 3 A solid solution of (2).
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (7)
1. A method for preparing Indium Tin Oxide nano powder based on microfluid rapid precipitation comprises the steps of preparing metal salts of Indium Tin into a reaction water phase according to a proportion, using an alkaline solution as a precipitation phase, pumping the reaction phase and the precipitation phase into a microreactor accurately by using a flow pump for mixing and reacting, performing solid-liquid separation, washing and drying a precursor, and calcining at a high temperature to prepare ellipsoidal Indium Tin Oxide (ITO) nano powder, and is characterized by comprising the following steps:
s1: mixing indium-containing salt solution and tin-containing salt solution according to In ITO product 2 O 3 :SnO 2 Preparing indium tin metal salt mixed solution with In3+ concentration of 0.1-2 mol/L with the mass ratio of 9:1;
s2: preparing In mixed solution of alkali liquor and indium tin metal salt as precipitation phase 3+ With OH in the lye - 1.2 to 1;
s3: accurately pumping the indium tin metal salt mixed solution and alkali liquor into the microreactor through a flow pump to quickly mix and react to generate indium tin compound precursor precipitate, wherein the total flow of the pumped two phases is 0.1-20 mL/min.
S4: washing and drying the generated indium tin compound precursor;
s5: and calcining the treated indium tin compound precursor at high temperature to prepare the ellipsoidal indium tin oxide nano powder.
2. The preparation method of the indium tin oxide nano powder based on the microfluidic rapid precipitation as claimed in claim 1, wherein the mixing reaction time in the micro-reactor is 1-60 s, and the micro-channel reaction temperature of the micro-reactor is 20-80 ℃.
3. The method for preparing indium tin oxide nanopowder based on microfluidic rapid precipitation according to claim 1, wherein the microreactor is any one of a capillary microreactor, a chip microreactor and a droplet flow microreactor.
4. The method for preparing indium tin oxide nano-powder based on microfluid rapid precipitation according to claim 3, wherein the micro-reactor is made of any one or a combination of several of a stainless steel pipeline, a polytetrafluoroethylene pipeline, a polyether ether ketone pipeline, a perfluoroethylene propylene copolymer pipeline, a tetrafluoroethylene pipeline and a fused silica pipeline.
5. The method for preparing indium tin oxide nano powder based on microfluid rapid precipitation according to claim 3, wherein the micro-channel size of the micro-reactor is 0.1-3 mm.
6. The preparation method of indium tin oxide nano powder based on microfluidic rapid precipitation according to claim 1, wherein the indium-containing salt solution is any one or a combination of several of indium chloride solution, sulfate solution and nitrate solution; the tin-containing salt solution is any one or a combination of a plurality of tin chloride solution, sulfate solution and nitrate solution.
7. The preparation method of the indium tin oxide nano powder based on the microfluid rapid precipitation according to claim 1, wherein the calcination temperature of the indium tin compound precursor is 300-500 ℃ and the calcination time is 0.5-2 h.
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| JP2012051762A (en) * | 2010-09-01 | 2012-03-15 | Nano Cube Japan Co Ltd | Method for producing tin oxide ultrafine particle |
| CN105523579A (en) * | 2015-12-03 | 2016-04-27 | 清华大学 | Preparation method for indium tin oxide powder |
| CN109205659A (en) * | 2018-11-01 | 2019-01-15 | 清华大学 | A kind of preparation method for the indium oxide that crystal form is controllable |
| CN113548688A (en) * | 2021-07-02 | 2021-10-26 | 江西理工大学 | Micron-grade rosette SnO2Preparation method |
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2022
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2012051762A (en) * | 2010-09-01 | 2012-03-15 | Nano Cube Japan Co Ltd | Method for producing tin oxide ultrafine particle |
| CN105523579A (en) * | 2015-12-03 | 2016-04-27 | 清华大学 | Preparation method for indium tin oxide powder |
| CN109205659A (en) * | 2018-11-01 | 2019-01-15 | 清华大学 | A kind of preparation method for the indium oxide that crystal form is controllable |
| CN113548688A (en) * | 2021-07-02 | 2021-10-26 | 江西理工大学 | Micron-grade rosette SnO2Preparation method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115784297A (en) * | 2022-11-21 | 2023-03-14 | 西安近代化学研究所 | Spindle-shaped In 2 O 3 Preparation method and application of nano material |
| CN115784297B (en) * | 2022-11-21 | 2024-03-29 | 西安近代化学研究所 | Spindle-shaped In 2 O 3 Preparation method and application of nano material |
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