CN109019677A - Prepare Ti4O7Method - Google Patents
Prepare Ti4O7Method Download PDFInfo
- Publication number
- CN109019677A CN109019677A CN201811286928.5A CN201811286928A CN109019677A CN 109019677 A CN109019677 A CN 109019677A CN 201811286928 A CN201811286928 A CN 201811286928A CN 109019677 A CN109019677 A CN 109019677A
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- Prior art keywords
- sintering
- titanium valve
- tio
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- microwave
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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
-
- 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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention relates to preparation Ti4O7Method, belong to titanium field of material technology.The technical problem to be solved by the present invention is to existing Ti4O7Preparation method product quality is not high, and preparation condition requires high.The technical solution that the present invention solves technical problem, which is to provide, a kind of prepares Ti4O7Method, method includes the following steps: preparing titanium valve and TiO according to molar ratio 1:72, it is uniformly mixed, carries out microwave sintering, 600~1200 DEG C of sintering temperature, obtain Ti4O7.The method of the present invention, simple process is easily-controllable, and product quality is high, and industrialization prospect is good.
Description
Technical field
The invention belongs to titanium field of material technology, and in particular to a kind of to prepare Ti4O7Method.
Background technique
Ti4O7It is black to be commonly called as titanium, it is conductive it is good, visible light-responded ability is strong, electrochemical performance, environment-protecting and non-poisonous etc.
Many good characteristics, so Ti4O7It is widely used in electrochemistry related fields, for example, Ti4O7In TiO2Electric resistance transition memory
(RRMA) crucial effect, Ti are played in4O7It has been repaired in electrolysis water, electrolytic metallurgy, plating, electrochemical soil as inert electrode
There is a large amount of application in the fields such as multiple, wastewater treatment, cathodic protection, electrophoresis.
At present, Ti4O7Preparation method mainly passes through thermal reduction method, by using reducing agent (such as H2, C etc.) certain
Under conditions of (general 1200 DEG C or so) reduction TiO2Prepare Ti4O7.Use H2, C etc. as reducing agent when, due to reduction temperature
It is required that high, the Ti caused4O7Powder sintered phenomenon is serious.And H2As the entire reaction process of reducing agent to the airtight of equipment
Property require high, and H2Presence increase the risk of entire technical process；And that other are then readily incorporated as reducing agent is miscellaneous by C
Phase influences the Ti being prepared4O7Quality.
Summary of the invention
The technical problem to be solved by the present invention is to existing Ti4O7Preparation method product quality is not high, and preparation condition requires high.
The technical solution that the present invention solves technical problem, which is to provide, a kind of prepares Ti4O7Method.This method includes following step
It is rapid:
Titanium valve and TiO are prepared according to molar ratio 1:72, it is uniformly mixed, carries out microwave sintering, sintering temperature 600~1200
DEG C, obtain Ti4O7。
Wherein, titanium valve described in the above method is micron order titanium valve.
Wherein, above method titanium valve and TiO2After mixing, ball milling is carried out.Further, Ball-milling Time is 0.5~2h.
Wherein, the raw material after ball milling described in the above method is put into corundum crucible and carries out microwave sintering.
Wherein, the microwave sintering in the above method carries out under vacuum or inert gas shielding.
Wherein, the microwave sintering in the above method is carried out in industrial microwave oven.
Wherein, the sintering time of microwave sintering is 1~4h in the above method.
Wherein, sintered product is crushed in the above method, then carries out ball mill grinding, 1~2h of milling time.
The beneficial effects of the present invention are: the present invention has creatively used Ti and TiO2As raw material, in microwave heating
Under conditions of prepare Ti4O7, Ti and TiO can be improved moment using microwave heating2It is complete well to the temperature for the needs that react
At reaction.The method of the present invention is low to equipment and reaction condition requirement, and reaction temperature also decreases, and product obtained is sintered situation
Alleviated.And use titanium valve as raw material, it is not introduced into new impurity phase, the high-quality Ti of purity > 99% can be prepared4O7
Product, fineness have a good application prospect up to micron order.
Detailed description of the invention
Fig. 1 is the XRD diagram of 1 product of embodiment.
Fig. 2 is the particle size distribution figure of 1 product of embodiment.
Specific embodiment
The technical solution that the present invention solves technical problem, which is to provide, a kind of prepares Ti4O7Method.The method of the present invention uses
Ti and TiO2As raw material, Ti is prepared under conditions of microwave heating4O7, overcome the prior art and be easy excess agglomeration and appearance
The preferable micron order Ti of quality can be prepared in the disadvantages of being easily introduced impurity4O7。
The method of the present invention is the following steps are included: prepare titanium valve and TiO according to molar ratio 1:72, it is uniformly mixed, carries out microwave
Sintering, obtains Ti by 600~1200 DEG C of sintering temperature4O7.For the purity of product, titanium valve and TiO2Used in amounts to meet mole
Easily there is Ti in the excessive product of titanium valve in requirement than 1:73O5, easily there is Ti in the very few product of titanium valve5O9、Ti6O11Equal titanyls
Object.Sintering temperature is too low, and reaction can not carry out, and temperature is excessively high, Ti4O7Easily aoxidize at high temperature.
Wherein, titanium valve described in the above method is micron order titanium valve.Preferably, the titanium valve is -45 μm of titanium valves.And one
As TiO2Powder is all nanoscale, has been able to satisfy reaction and has required.
Wherein, above method titanium valve and TiO2After mixing, ball milling is carried out.The main function of ball milling is to try to make raw material herein
It is uniformly mixed.Further, Ball-milling Time is 0.5~2h.
Wherein, the raw material after ball milling described in the above method is put into corundum crucible and carries out microwave sintering.
Wherein, the microwave sintering in the above method carries out under vacuum or inert gas shielding.
Wherein, the microwave sintering in the above method carries out in industrial microwave oven.
Wherein, the sintering time of microwave sintering is 1~4h in the above method.Sintered product is crushed, then is carried out
Ball mill grinding, 1~2h of milling time, obtains Ti4O7Powder.
Specifically, the method for the present invention can be carried out by step in detail below:
A, with micron order titanium valve, TiO2For raw material, ingredient is carried out according to molar ratio 1:7, ball mill progress is put into after preparing
Ball milling, 0.5~2h of Ball-milling Time；
B, the raw material after ball milling is put into corundum crucible, then the corundum crucible after charging is put into microwave agglomerating furnace,
Heat-agglomerating is carried out under the protection of vacuum or inert atmosphere；
C, 600~1200 DEG C of sintering temperature, 1~4h of sintering time after sintering, naturally cool to room temperature, finally go out
Furnace is crushed, grinding, obtains Ti4O7Powder.
It is discussed in detail that the present invention will be described in more detail below by way of specific embodiment.
Embodiment 1 prepares micron order Ti using the method for the present invention4O7
With titanium valve (< 10 μm), TiO2For raw material, 608g (wherein titanium valve 48g, TiO is amounted to2560g), by the raw material after preparing
It is put into ball mill and carries out ball milling, Ball-milling Time 2h after ball milling, takes out raw material, is put into corundum crucible, then will be charged
Corundum crucible, which is put into micro-wave oven, carries out heat-agglomerating, and 1150 DEG C of sintering temperature, sintering time 1h, while using argon gas as protection
Gas.After sintering, micro-wave oven cooled to room temperature opens micro-wave oven, takes out product, and product is ground, is crushed,
And test and analyze, it is Ti that confirmation, which obtains final product,4O7, purity > 99%.
Embodiment 2 prepares micron order Ti using the method for the present invention4O7
With titanium valve (< 10 μm), TiO2For raw material, 304g (wherein titanium valve 24g, TiO is amounted to2280g), by the raw material after preparing
It is put into ball mill and carries out ball milling, Ball-milling Time 1h after ball milling, takes out raw material, is put into corundum crucible, then will be charged
Corundum crucible is put into micro-wave oven and carries out under vacuum conditions heat-agglomerating, and 750 DEG C of sintering temperature, sintering time 4h.Sintering
After, micro-wave oven cooled to room temperature opens micro-wave oven, takes out product, and product is ground, is crushed, and is detected
Analysis, it is Ti that confirmation, which obtains final product,4O7, purity > 99%.
Claims (9)
1. preparing Ti4O7Method, comprising the following steps: prepare titanium valve and TiO according to molar ratio 1:72, it is uniformly mixed, carries out micro-
Wave sintering, 600~1200 DEG C of sintering temperature obtain sintered product, then sintered product are crushed, is ground, and obtain Ti4O7Powder
End.
2. according to the method described in claim 1, it is characterized by: the titanium valve is micron order titanium valve.
3. method according to claim 1 or 2, it is characterised in that: the titanium valve and TiO2After mixing, ball milling is carried out.
4. described in any item methods according to claim 1~3, it is characterised in that: the Ball-milling Time is 0.5~2h.
5. method according to any one of claims 1 to 4, it is characterised in that: the raw material after ball milling be put into corundum crucible into
Row microwave sintering.
6. described in any item methods according to claim 1~5, it is characterised in that: microwave sintering is protected in vacuum or inert gas
Shield is lower to be carried out.
7. described in any item methods according to claim 1~6, it is characterised in that: microwave sintering is carried out in industrial microwave oven.
8. described in any item methods according to claim 1~6, it is characterised in that: the sintering time of microwave sintering is 1~4h.
9. described in any item methods according to claim 1~6, it is characterised in that: sintered product is crushed, then into
Row ball mill grinding, 1~2h of milling time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811286928.5A CN109019677A (en) | 2018-10-31 | 2018-10-31 | Prepare Ti4O7Method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811286928.5A CN109019677A (en) | 2018-10-31 | 2018-10-31 | Prepare Ti4O7Method |
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| Publication Number | Publication Date |
|---|---|
| CN109019677A true CN109019677A (en) | 2018-12-18 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811286928.5A Pending CN109019677A (en) | 2018-10-31 | 2018-10-31 | Prepare Ti4O7Method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112266014A (en) * | 2020-10-29 | 2021-01-26 | 重庆大学 | Preparation of high-purity phase Ti with higher than gram level from industrial metatitanic acid powder containing impurities4O7Method for preparing nano material |
| CN114192562A (en) * | 2021-11-19 | 2022-03-18 | 中国科学院南京土壤研究所 | Method for removing polycyclic aromatic hydrocarbons in soil by combining electric remediation with anodic oxidation |
| CN117776257A (en) * | 2023-12-26 | 2024-03-29 | 西南大学 | Ti (titanium) 4 O 7 Powder material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274456A (en) * | 2013-06-05 | 2013-09-04 | 四川大学 | Doped Ti4O7 powder and preparation methods thereof |
| CN104925857A (en) * | 2015-06-09 | 2015-09-23 | 四川大学 | Rotary dynamic continuous preparation method for titanium black powder |
-
2018
- 2018-10-31 CN CN201811286928.5A patent/CN109019677A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274456A (en) * | 2013-06-05 | 2013-09-04 | 四川大学 | Doped Ti4O7 powder and preparation methods thereof |
| CN104925857A (en) * | 2015-06-09 | 2015-09-23 | 四川大学 | Rotary dynamic continuous preparation method for titanium black powder |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112266014A (en) * | 2020-10-29 | 2021-01-26 | 重庆大学 | Preparation of high-purity phase Ti with higher than gram level from industrial metatitanic acid powder containing impurities4O7Method for preparing nano material |
| CN114192562A (en) * | 2021-11-19 | 2022-03-18 | 中国科学院南京土壤研究所 | Method for removing polycyclic aromatic hydrocarbons in soil by combining electric remediation with anodic oxidation |
| CN114192562B (en) * | 2021-11-19 | 2023-02-24 | 中国科学院南京土壤研究所 | Method for removing polycyclic aromatic hydrocarbons in soil by combining electric remediation with anodic oxidation |
| CN117776257A (en) * | 2023-12-26 | 2024-03-29 | 西南大学 | Ti (titanium) 4 O 7 Powder material and preparation method thereof |
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Application publication date: 20181218 |