CN117088405A - Carbon-coated nano titanium oxide nano powder and method for rapidly preparing carbon-coated nano titanium oxide nano powder - Google Patents
Carbon-coated nano titanium oxide nano powder and method for rapidly preparing carbon-coated nano titanium oxide nano powder Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 29
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 95
- 239000000843 powder Substances 0.000 claims abstract description 41
- 239000010936 titanium Substances 0.000 claims abstract description 41
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 27
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 25
- 229910052786 argon Inorganic materials 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 13
- 239000012159 carrier gas Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims description 15
- 239000011858 nanopowder Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 7
- 238000011049 filling Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 230000001681 protective effect Effects 0.000 claims description 7
- 238000007669 thermal treatment Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 31
- 239000002253 acid Substances 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 9
- 229910052719 titanium Inorganic materials 0.000 abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 238000007557 optical granulometry Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- -1 titanium metal oxide Chemical class 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/043—Titanium sub-oxides
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
-
- 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
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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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
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
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- General Life Sciences & Earth Sciences (AREA)
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Abstract
The application discloses carbon-coated nano titanium oxide nano powder and a method for rapidly preparing the carbon-coated nano titanium oxide nano powder, and belongs to the technical field of powder material preparation. The method of the application uses the mixture of metatitanic acid or titanium dioxide and polyvinyl alcohol as raw material, uses argon or nitrogen as carrier gas and uses the air flow of 1L/min to be transferred into a rapid heat treatment reactor, and the material is reacted in a high-temperature zone during the falling process of the furnace and then is condensed in a collecting zone to obtain carbon-coated nano titanium oxide (Ti) n O 2n‑1 @c, n=4 or 8) powder, the morphology is spherical or ellipsoidal; the method can realize the rapid preparation of the carbon-coated titanium oxideThe process is short.
Description
The application relates to a divisional application of a method for rapidly preparing carbon-coated nano titanium oxide nano powder, which has the application date of 2019, 6-month and 28-day, the application number of 201910574789.4 and the application name of.
Technical Field
The application provides carbon-coated nano titanium oxide nano powder and a method for rapidly preparing the carbon-coated nano titanium oxide nano powder, belonging to the field of powder material preparation.
Background
The titanium oxide powder material is the first black titanium metal oxide in the world, magneli phase titanium oxide (Ti n O 2n-1 3 < n < 10) is a type of titanium oxide in which more studies are made. Although Magneli phase titanium oxide has been widely focused and studied as early as 60 years ago, researchers have only increased enthusiasm for the preparation and application of this material. The Magneli phase titanium oxide has super conductivity, excellent stability and excellent corrosion resistance and excellent photocatalytic activity. So that Magneli-phase titanium oxide has wide application in various fields, such as fuel cell field, lithium sulfur cell, lithium air cell, anodic oxidation treatment of waste water, photocatalytic degradation of organic matters, etc.
Numerous studies have shown that Magneli-phase titanium oxide has a strong photocatalytic activity. Under the irradiation of visible light, the Magneli phase titanium oxide can be used for photocatalytic decomposition and other organic pollutants such as methyl blue, methyl orange, rhodamine b and the like in a certain time.
Titanium element in titanium oxide is mainly Ti 3+ 、Ti 4+ Presence of Ti 3+ The introduction of the lithium ion battery can effectively improve the migration efficiency of lithium ions in the lithium ion battery, shorten the diffusion path of the lithium ions, remarkably improve the cycle performance, high-rate performance and specific capacity of the battery. It was found that Ti obtained by hydrogen reduction of nano-sized titania nanotubes 6 O 11 And Ti is 4 O 7 A matrix combined with sulfur species to produce a lithium battery cathode. Ti (Ti) 4 O 7 S exhibits a higher reversible capacity and a high cycle performance, capacityThe amounts are 1342, 1044 and 623mAhg -1 At 0.02,0.1 and 0.5C, respectively, and has a significant capacity retention of 99% (100 cycles at 0.1C).
At present, the titanium oxide powder is mainly prepared by a titanium dioxide reduction method, the titanium oxide powder is heated to a certain temperature and kept at a certain temperature for a certain time in vacuum or inert gas atmosphere, and reducing agents such as hydrogen, carbon black, active metals or carbon monoxide are used for reducing the titanium oxide to prepare a required powder sample.
CN106241861a discloses a method for preparing rod-like titanium oxide. The method is characterized in that the raw materials are Ti and O compound powder, a reducing agent and chloride, and the molar ratio of the raw materials for preparing the titanium dioxide powder is calculated according to the chemical formula of the titanium dioxide powder and the chemical reaction between the raw materials. And then the materials are mixed, dried, sintered, washed and dried to finally obtain the rod-shaped titanium oxide. The method can obtain purer single-phase titanium oxide, the photo-reduction time is 2-8 hours, and the process flow is long.
The rotary dynamic continuous preparation method of the CN104925857A titanium dioxide powder comprises the following process steps: (1) Proportioning, wherein the raw materials are compound powder of Ti and O and a reducing agent; (2) mixing and drying; (3) Sintering, heating the furnace tube under an open system or a closed system or under negative pressure, wherein the furnace tube is in an inclined state and a rotating state that the discharge port is lower than the feed port, continuously feeding the mixed powder obtained in the step (2) into the furnace tube when the temperature in the furnace tube reaches the reaction temperature, and completing the reaction in a spiral movement mode through the furnace tube heating zone after the mixed powder enters the furnace tube to form a reaction product which falls into the collecting chamber. The particle size of the titanium oxide powder prepared by the method is larger, and the carbon-coated titanium oxide powder cannot be prepared.
《Preparation ofcarbon-coatedMagneli phases TinO 2n- 1 andtheirphotocatalytic activityundervisible light although carbon-coated titanium oxide powder was obtained, titanium oxide was mostlyIs multiphase titanium oxide.
Disclosure of Invention
The application provides a method for rapidly preparing carbon-coated nano titanium oxide (Ti) by adopting a heat treatment furnace n O 2n-1 A method of @ C) powder; the method can obtain nano-scale carbon coated titanium oxide (Ti) n O 2n-1 And @ C) powder, the flow is simple, the efficiency is high, and the carbon-coated titanium oxide with titanium oxide as a single phase is prepared.
The application is realized by the following technical scheme:
a method for rapidly preparing carbon-coated nano titanium oxide nano powder comprises the following steps:
uniformly mixing rutile meta-titanic acid powder and polyvinyl alcohol powder according to the mass ratio of 9:1 or 1:9, and drying the obtained mixed material in a drying oven at 80 ℃ for overnight use;
vacuumizing the rapid thermal treatment furnace, filling argon as a protective gas, raising the furnace temperature to 1250 ℃, and then feeding the mixed material obtained by drying overnight into a high-temperature heating zone of the rapid thermal treatment furnace by taking the argon as a carrier gas and the air flow of 1L/min;
the mixed material obtained by drying overnight is driven by argon to react rapidly and fall into a powder cooling and collecting device, so that carbon-coated titanium dioxide nano powder is obtained;
when the mass ratio is 9:1 and the target temperature of the furnace temperature is 1250 ℃, the phase of the titanium dioxide is Ti 8 O 15 ;
When the mass ratio is 1:9 and the target temperature of the furnace temperature is 1265 ℃, the phase of the titanium dioxide is Ti 4 O 7 。
The application also provides the carbon-coated nano titanium oxide nano powder prepared by the method in the scheme, when the phase of the titanium oxide is Ti 8 O 15 When the carbon-coated titanium dioxide nano powder is used, the thickness of a carbon shell of the carbon-coated titanium dioxide nano powder is 2nm;
when the phase of the titanium dioxide is Ti 4 O 7 When in use, the carbon shell thickness of the carbon-coated titanium oxide nano powderThe degree was 16nm.
The application has the beneficial effects that:
(1) The method can realize continuous preparation of the carbon-coated titanium oxide powder, has extremely short preparation period and is easy to realize industrialization.
(2) The titanium oxide prepared by the method has the protection of the carbon shell, so that sintering agglomeration among powder in the traditional method is effectively inhibited.
(3) The particle size of the carbon-coated titanium oxide prepared by the method is smaller than that of the carbon-coated titanium oxide prepared by the traditional method, and the product is nano-scale powder.
(4) The titanium suboxide in the carbon-coated titanium suboxide prepared by the method is single-phase titanium suboxide.
Drawings
FIG. 1 is a graph of sample phases obtained for a mixture and under different temperature conditions;
FIG. 2 is a view of Ti n O 2n-1 TEM image of microstructure of carbon coated samples of microkernels.
Detailed Description
The application is described in further detail below with reference to the drawings and the specific embodiments, but the scope of the application is not limited to the description.
Example 1
Mixing commercial P25 powder and polyvinyl alcohol powder uniformly according to the mass ratio of 2:1, and drying the mixed material (P25+PVA) in a drying oven at 80 ℃ for standby.
Vacuumizing the rapid heat treatment furnace, filling argon as a protective gas, raising the furnace temperature to 1300 ℃, and feeding the mixed material into a high-temperature heating zone of the rapid heat treatment furnace by using the argon as a carrier gas and using the air flow of 0.5L/min; the materials react rapidly under the drive of argon and fall into a powder cooling and collecting device, thus obtaining carbon-coated titanium dioxide nano powder (Ti) n O 2n-1 @C)。
The product phase obtained in this example is Ti 4 O 7 ,Ti 3 O 5 ,Ti 2 O 3 And is made of Ti 4 O 7 Mainly, the particle size was about 100nm as analyzed by TEM photograph, and the thickness of the carbon shell was 4nm.The results of the product phases are shown in S1300 of FIG. 1 and summarized in Table 1, and TEM photographs are shown in FIG. 2 (A, E).
Example 2
The rutile type metatitanic acid powder and the polyvinyl alcohol powder are uniformly mixed according to the mass ratio of 1:1, and the mixed material (rutile type metatitanic acid+PVA) is dried in a drying oven at 80 ℃ for overnight use.
Vacuumizing the rapid thermal treatment furnace, filling nitrogen as a protective gas, and after the furnace temperature is raised to 1400 ℃ which is the target temperature, feeding the mixed material into a high-temperature heating zone of the rapid thermal treatment furnace by using nitrogen as a carrier gas and using the air flow of 2L/min; the materials react rapidly under the drive of argon and fall into a powder cooling and collecting device, thus obtaining carbon-coated titanium dioxide nano powder (Ti) n O 2n-1 @C)。
The product phase obtained in this example is Ti 3 O 5 ,Ti 2 O 3 The particle size is about 100nm as analyzed by TEM photograph, and the thickness of the carbon shell is 6nm; the results of the product phases are shown in FIG. 1S1400 and summarized in Table 1, and TEM photographs are shown in FIG. 2 (B, F).
Example 3
The rutile metatitanic acid powder and the polyvinyl alcohol powder are uniformly mixed according to the mass ratio of 1:2, and the mixed material (rutile metatitanic acid+PVA) is dried in a drying oven at 80 ℃ for overnight use.
Vacuumizing the rapid heat treatment furnace, filling argon as a protective gas, raising the furnace temperature to 1500 ℃, and feeding the mixed material into a high-temperature heating zone of the rapid heat treatment furnace by using the argon as a carrier gas and using the air flow of 5L/min; the materials react rapidly under the drive of argon and fall into a powder cooling and collecting device, thus obtaining carbon-coated titanium dioxide nano powder (Ti) n O 2n-1 @C)。
The product obtained in this example was analyzed by XRD and had the phase Ti 2 O 3 The particle size of the carbon shell is about 110nm and the thickness of the carbon shell is 11nm by TEM photo analysis; the results of the product phases are shown in FIG. 1S1500 and summarized in Table 1, and TEM photographs are shown in FIG. 2 (C, G).
Example 4
The rutile metatitanic acid powder and the polyvinyl alcohol powder are uniformly mixed according to the mass ratio of 9:1, and the mixed material (rutile metatitanic acid+PVA) is dried in a drying oven at 80 ℃ for overnight use.
Vacuumizing the rapid heat treatment furnace, filling argon as a protective gas, raising the furnace temperature to 1250 ℃, and feeding the mixed material into a high-temperature heating zone of the rapid heat treatment furnace by taking the argon as a carrier gas and the air flow of 1L/min;
the materials react rapidly under the drive of argon and fall into a powder cooling and collecting device, thus obtaining carbon-coated titanium dioxide nano powder (Ti) n O 2n-1 @C)。
The product obtained in this example was analyzed by XRD and had the phase Ti 8 O 15 The phase results are summarized in Table 1, and the particle size was about 105nm and the carbon shell thickness was 2nm as analyzed by TEM photograph.
Example 5
The rutile metatitanic acid powder and the polyvinyl alcohol powder are uniformly mixed according to the mass ratio of 1:9, and the mixed material (rutile metatitanic acid+PVA) is dried in a drying oven at 80 ℃ for overnight use.
Vacuumizing the rapid heat treatment furnace, filling argon as a protective gas, raising the furnace temperature to 1265 ℃, and feeding the mixed material into a high-temperature heating zone of the rapid heat treatment furnace by using the argon as a carrier gas and using the air flow of 1L/min; the materials react rapidly under the drive of argon and fall into a powder cooling and collecting device, thus obtaining carbon-coated titanium dioxide nano powder (Ti) n O 2n-1 @C)。
The product obtained in this example was analyzed by XRD and had the phase Ti 4 O 7 The phase results are summarized in Table 1, and the particle size was about 90nm and the carbon shell thickness was 16nm as analyzed by TEM photograph.
Table 1 shows experimental conditions and phases of samples for rapid preparation of carbon-coated titanium dioxide
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the application.
Claims (2)
1. A method for rapidly preparing carbon-coated nano titanium oxide nano powder is characterized by comprising the following steps:
uniformly mixing rutile meta-titanic acid powder and polyvinyl alcohol powder according to the mass ratio of 9:1 or 1:9, and drying the obtained mixed material in a drying oven at 80 ℃ for overnight use;
vacuumizing the rapid thermal treatment furnace, filling argon as a protective gas, raising the furnace temperature to 1250 ℃, and then feeding the mixed material obtained by drying overnight into a high-temperature heating zone of the rapid thermal treatment furnace by taking the argon as a carrier gas and the air flow of 1L/min;
the mixed material obtained by drying overnight is driven by argon to react rapidly and fall into a powder cooling and collecting device, so that carbon-coated titanium dioxide nano powder is obtained;
when the mass ratio is 9:1 and the target temperature of the furnace temperature is 1250 ℃, the phase of the titanium dioxide is Ti 8 O 15 ;
When the mass ratio is 1:9 and the target temperature of the furnace temperature is 1265 ℃, the phase of the titanium dioxide is Ti 4 O 7 。
2. The carbon-coated nano-titania nano-powder prepared by the method of claim 1, wherein the carbon-coated nano-titania nano-powder is characterized by: when the phase of the titanium dioxide is Ti 8 O 15 When the carbon-coated titanium dioxide nano powder is used, the thickness of a carbon shell of the carbon-coated titanium dioxide nano powder is 2nm;
when the phase of the titanium dioxide is Ti 4 O 7 And when the carbon shell thickness of the carbon-coated titanium dioxide nano powder is 16nm.
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CN104925857A (en) * | 2015-06-09 | 2015-09-23 | 四川大学 | Rotary dynamic continuous preparation method for titanium black powder |
CN107473264B (en) * | 2017-08-23 | 2019-04-09 | 昆明理工大学 | A kind of method of high-temperature plasma preparation nanometer Asia titanium oxide |
CN107522226B (en) * | 2017-08-30 | 2019-12-03 | 昆明理工大学 | A kind of method of the spherical sub- titanium oxide of plasma preparation |
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2019
- 2019-06-28 CN CN201910574789.4A patent/CN110182842A/en active Pending
- 2019-06-28 CN CN202311064768.0A patent/CN117088405A/en active Pending
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