CN109485408A - A kind of technique of TiC reduction preparation sheet titanium pentoxide - Google Patents
A kind of technique of TiC reduction preparation sheet titanium pentoxide Download PDFInfo
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Abstract
The invention discloses the techniques that a kind of TiC restores preparation sheet titanium pentoxide, the steps include: titanium carbide in mass ratio: titanium dioxide=1:8.5~10 weigh raw material titanium carbide, titanium dioxide respectively, water for ball milling is added to mix, it is dry, grinding, sieving, tabletting, then it is sintered stage by stage under an inert atmosphere, it is finally cooling to obtain product.The titanium pentoxide crystal of sheet can be made in the present invention, purity reaches 99.99%, yield is 86~88%, the titanium pentoxide crystal of sheet can be shortened the plated film fritting time, improve plating membrane efficiency, and the present invention is using after physics ball milling mixing method, temperature range of the direct step near 1300 DEG C calcines to obtain, temperature is lower than 500 DEG C of traditional industry temperature or more, and is not necessarily to vacuum environment, and equipment requirement is low.
Description
Technical field
The present invention relates to Coating Materials, catalytic chemistry material, data storage and new energy fields, are related to one kind five and aoxidize
A kind of preparation process of Tritanium/Trititanium, and in particular to technique of TiC reduction preparation sheet titanium pentoxide.
Background technique
Titanium pentoxide is a kind of black-and-blue non-stoichiometric compound with metallic luster.Its density is about 4.29g/
cm3, 2180 DEG C of fusing point, oxygen titanium atom ratio has both semiconductor and metallic character, acid-alkali-corrosive-resisting can between 1.66~1.70
Electrode material is done instead of noble metal.Because it hinders temperature, coefficient is small again, but resistance can change with the change of atmosphere, and a kind of latent
Oxygen-sensitive material.
Titanium deoxid film has excellent machinery, chemistry, optically and electrically performance, is most heavy in optics and electronic application
The dielectric thin-film material wanted.Early period, mainly it is deposited titanium deoxid film in plated film industry using titanium dioxide coating materials, but
Can decompose oxygen loss during vapor deposition, release a large amount of oxygen while generating high-selenium corn titanium suboxide, inevitably
Sputtering phenomenon occurs.Therefore hardly result in that thickness is uniform, the film layer of stable refractive index.With going deep into for research, it has been found that one
The titanium suboxide of series can be oxidized to titanium dioxide, so the material as evaporation reaction is selected, wherein people
It was found that evaporation clout composition transfer is little when only original material is titanium pentoxide, thicknesses of layers is uniform, stable refractive index.Mesh
Before, titanium pentoxide has been widely used for answering for optics and electronic device as vacuum evaporation target vapor deposition titanium deoxid film
In.
In the prior art, being mainly obtained for titanium pentoxide restores titanium dioxide to realize, common reducing agent
There are C, Ti, Si, H2,Zr.But Si (Vacuum.2017,143:380-385), Zr (J.Am.Chem.Soc.2012,134,
Generated impurity not can be removed when 10894-10898) making reducing agent；H2(Crystal Growth&Design.2015,15
(2): 653-657.Nature Communications.2015,6 (1) restoring method) is difficult to control, and safety coefficient
It is not high；As for carbon dust, although reaction temperature is relatively low and cheap, because can not be mixed with titanium dioxide sufficiently, also
Excessively high unstable (Journal of Alloys and Compounds G21 (2015) 404- for leading to reaction temperature of originality
649 (2015) 939-948 of 410.Journal of Alloys and Compounds) and be easy to produce seven oxidations, four titanium etc.
Low oxide impurity (Applied Catalysis B:Environmental.2009,88 (1-2): 160-164.)；Therefore
Above method is difficult to apply to industrial production.It has to take the second best, industrialized production is mainly with Ti powder and TiO at present2Powder mixing
High temperature sintering is realized under high vacuum after uniformly.But the method severe reaction conditions, not only need high vacuum environment, required temperature
Degree is high to production equipment requirement all also above 1800 DEG C, substantially increases production cost, safety coefficient is also difficult to ensure.
Therefore be highly desirable to a kind of easy to operate, cost is relatively low, and can temperature production guarantee the method for safety, to promote
Industrial production.
Summary of the invention
The object of the present invention is to provide the techniques that a kind of TiC restores preparation sheet titanium pentoxide, and reaction temperature is low, safety
Property it is high.
To achieve the above object, The technical solution adopted by the invention is as follows: a kind of TiC reduction preparation sheet titanium pentoxide
Technique, comprising the following steps:
Step 1: titanium carbide in mass ratio: titanium dioxide=1:8.5~10 weigh raw material titanium carbide, titanium dioxide respectively,
Water for ball milling is added to mix, feeding is dried after ball milling, is then ground to powder, it is sieved, tabletting；
Step 2: the mixing tabletting that step 1 obtains being placed in Muffle furnace in crucible, inertia is passed through into furnace chamber
Gas is to empty furnace chamber air；
Step 3: it is sintered stage by stage, and is continually fed into inert gas in entire sintering process, steps are as follows:
A. room temperature~1100 DEG C, 1~5 DEG C/min of heating rate；
B.1100 DEG C, 4~6h is kept the temperature；
DEG C C.1100~1200 DEG C, 1~5 DEG C/min of heating rate；
D.1200 DEG C, 4~6h is kept the temperature；
DEG C E.1200~final sintering temperature, 1~5 DEG C/min of heating rate；
F. final sintering temperature keeps the temperature 4~6h；Final sintering temperature is 1250~1330 DEG C；
Step 4: the Muffle furnace is slowly decreased to 400 DEG C with the rate of temperature fall of 1~5 DEG C/min, then is down to room temperature with furnace, will
Burnt product is come out of the stove, i.e. acquisition titanium pentoxide piece.
Preferably, in step 1, water and mixed powder mass ratio are 2.5~5:1,24~28h of Ball-milling Time, rotational speed of ball-mill
For 80~250r/min.
Preferably, in step 1, the temperature of the drying is 60~80 DEG C.
Preferably, in step 1, the step of the tabletting are as follows: using dry-pressing formed, pressure is in 1.5~3MPa, time 15
~60s.
Alternatively, in step 1, the step of the tabletting are as follows: first using dry-pressing formed, pressure is in 1.5~3MPa, time 15
~60s then carries out isostatic cool pressing, and for parameter in 100~250MPa, the time is 200~400s.
Preferably, the titanium carbide partial size be 2~4 μm, purity be 99.99% or more, the titanium dioxide partial size be 2~
5 μm, purity is 99.99% or more.
The chemical reaction occurred in production process has:
TiC+8TiO2=3Ti3O5+C
3TiO2+ C=Ti3O5+CO
Compared with prior art, the invention has the following beneficial effects:
(1) present invention can be made the titanium pentoxide crystal of sheet, and purity reaches 99.99, and yield is and same 86~88%
Industry is compared to increase by 10% or so；Sheet titanium pentoxide crystal can shorten the fritting time when being used as Coating Materials；Discharge quantity is low；
Comply fully with the requirement for doing Coating Materials.
(2) reactant TiC is both reaction raw materials and reducing agent, and the C and CO of generation can play the role of reduction, and
Later period directly excludes after becoming gas, carbon-free remnants, forms mutually purity is high.
(3) using after physics ball milling mixing method, temperature range of the direct step near 1300 DEG C calcines to obtain for this reaction,
Temperature is lower than 500 DEG C of traditional industry temperature or more, and is not necessarily to vacuum environment, and reducing atmosphere is from a wealth of sources, and production cost drops significantly
It is low.
Detailed description of the invention
Fig. 1 is the pictorial diagram of titanium pentoxide product made from the embodiment of the present invention 1.
Fig. 2 is the XRD diagram of titanium pentoxide product made from the embodiment of the present invention 1.
Fig. 3 is the SEM figure of titanium pentoxide product made from the embodiment of the present invention 1.
Specific embodiment
Invention is further described in detail in the following with reference to the drawings and specific embodiments.
Raw material used in following embodiment is commercial goods without specified otherwise, and titanium carbide partial size is 2~4 μm, purity
It is 99.99% or more, titanium dioxide partial size is 2~5 μm, and purity is 99.99% or more.
Embodiment 1
Step 1: titanium carbide in mass ratio: titanium dioxide=1:8.5 weighs raw material titanium carbide, titanium dioxide respectively, adds water
For 24 hours, rotational speed of ball-mill 150r/min, water and mixed powder mass ratio are 2.5:1 to ball milling；Feeding is in 60 DEG C of drying boxes after ball milling
Drying, dry completely rear taking-up mixing, sieves with 100 mesh sieve after mechanical lapping；Using dry-pressing formed, pressure is in 1.5MPa, time
60s obtains mixing tabletting；
Step 2: the mixing tabletting that step 1 obtains being placed in Muffle furnace in crucible, argon gas is passed through into furnace chamber
20min is to empty furnace chamber air；
Step 3: it is sintered stage by stage, and is continually fed into argon gas in entire sintering process, steps are as follows:
A. room temperature~1100 DEG C, 1 DEG C/min of heating rate；
B.1100 DEG C, 4h is kept the temperature；
DEG C C.1100~1200 DEG C, 1 DEG C/min of heating rate；
D.1200 DEG C, 4h is kept the temperature；
DEG C E.1200~1330 DEG C, 1 DEG C/min of heating rate；
F.1330 DEG C, 4h is kept the temperature；
Step 4: the Muffle furnace is slowly decreased to 400 DEG C with the rate of temperature fall of 1 DEG C/min, then is down to room temperature with furnace, by institute
It burns product to come out of the stove, i.e., acquisition titanium pentoxide piece, pictorial diagram are as shown in Figure 1.After tested, yield 86.0%.
According to GB/T 7962.12-1987 colouless optical glass test method, refraction of the product at wavelength 560nm
Rate is 2.310, can be used as high refractive index Coating Materials use.
Sample is subjected to XRD test, as shown in Fig. 2, comparing with PDF 82-1138 titanium pentoxide standard card serial number
Afterwards, it is known that, sample is pure phase titanium pentoxide, without any miscellaneous phase.
Sample grind up is placed under scanning electron microscope and is observed, as shown in figure 3, it is found that sample is pure phase.
Embodiment 2
Step 1: titanium carbide in mass ratio: titanium dioxide=1:10 weighs raw material titanium carbide, titanium dioxide respectively, adds water polo
28h is ground, rotational speed of ball-mill 250r/min, water and mixed powder mass ratio are 3:1；Feeding is dried in 80 DEG C of drying boxes after ball milling
Dry, dry completely rear taking-up mixing sieves with 100 mesh sieve after mechanical lapping；Using dry-pressing formed, pressure in 3MPa, time 15s,
Obtain mixing tabletting；
Step 2: the mixing tabletting that step 1 obtains being placed in Muffle furnace in crucible, argon gas is passed through into furnace chamber
20min is to empty furnace chamber air；
Step 3: it is sintered stage by stage, and is continually fed into argon gas in entire sintering process, steps are as follows:
A. room temperature~1100 DEG C, 2 DEG C/min of heating rate；
B.1100 DEG C, 6h is kept the temperature；
DEG C C.1100~1200 DEG C, 2 DEG C/min of heating rate；
D.1200 DEG C, 6h is kept the temperature；
DEG C E.1200~1250 DEG C, 2 DEG C/min of heating rate；
F.1250 DEG C, 6h is kept the temperature；
Step 4: the Muffle furnace is slowly decreased to 400 DEG C with the rate of temperature fall of 2 DEG C/min, then is down to room temperature with furnace, by institute
It burns product to come out of the stove, i.e. acquisition titanium pentoxide piece.After tested, yield 87.6%.
According to GB/T 7962.12-1987 colouless optical glass test method, refraction of the product at wavelength 560nm
Rate is 2.308, can be used as high refractive index Coating Materials use.
Sample is subjected to XRD and SEM characterization, it is known that, sample is pure phase titanium pentoxide, without any miscellaneous phase.
Embodiment 3
Step 1: titanium carbide in mass ratio: titanium dioxide=1:9.5 weighs raw material titanium carbide, titanium dioxide respectively, adds water
Ball milling 28h, rotational speed of ball-mill 200r/min, water and mixed powder mass ratio are 5:1；Feeding is dried in 60 DEG C of drying boxes after ball milling
Dry, dry completely rear taking-up mixing sieves with 100 mesh sieve after mechanical lapping；Using dry-pressing formed, pressure in 3MPa, time 15s,
Isostatic cool pressing is then carried out, parameter obtains mixing tabletting in 250MPa, time 400s；
Step 2: the mixing tabletting that step 1 obtains being placed in Muffle furnace in crucible, nitrogen is passed through into furnace chamber
20min is to empty furnace chamber air；
Step 3: it is sintered stage by stage, and is continually fed into nitrogen in entire sintering process, steps are as follows:
A. room temperature~1100 DEG C, 5 DEG C/min of heating rate；
B.1100 DEG C, 6h is kept the temperature；
DEG C C.1100~1200 DEG C, 5 DEG C/min of heating rate；
D.1200 DEG C, 6h is kept the temperature；
DEG C E.1200~1300 DEG C, 5 DEG C/min of heating rate；
F.1300 DEG C, 6h is kept the temperature；
Step 4: the Muffle furnace is slowly decreased to 400 DEG C with the rate of temperature fall of 5 DEG C/min, then is down to room temperature with furnace, by institute
It burns product to come out of the stove, i.e. acquisition titanium pentoxide piece.After tested, yield 88.0%.
According to GB/T 7962.12-1987 colouless optical glass test method, refraction of the product at wavelength 560nm
Rate is 2.303, can be used as high refractive index Coating Materials use.
Sample is subjected to XRD and SEM characterization, it is known that, sample is pure phase titanium pentoxide, without any miscellaneous phase.
Embodiment 4
Step 1: titanium carbide in mass ratio: titanium dioxide=1:9.5 weighs raw material titanium carbide, titanium dioxide respectively, adds water
For 24 hours, rotational speed of ball-mill 300r/min, water and mixed powder mass ratio are 3:1 to ball milling；Feeding is dried in 60 DEG C of drying boxes after ball milling
Dry, dry completely rear taking-up mixing sieves with 100 mesh sieve after mechanical lapping；Using dry-pressing formed, pressure in 2MPa, time 20s,
Isostatic cool pressing is then carried out, parameter obtains mixing tabletting in 100MPa, time 200s；
Step 2: the mixing tabletting that step 1 obtains being placed in Muffle furnace in crucible, nitrogen is passed through into furnace chamber
20min is to empty furnace chamber air；
Step 3: it is sintered stage by stage, and is continually fed into nitrogen in entire sintering process, steps are as follows:
A. room temperature~1100 DEG C, 2 DEG C/min of heating rate；
B.1100 DEG C, 6h is kept the temperature；
DEG C C.1100~1200 DEG C, 2 DEG C/min of heating rate；
D.1200 DEG C, 6h is kept the temperature；
DEG C E.1200~1300 DEG C, 2 DEG C/min of heating rate；
F.1300 DEG C, 6h is kept the temperature；
Step 4: the Muffle furnace is slowly decreased to 400 DEG C with the rate of temperature fall of 2 DEG C/min, then is down to room temperature with furnace, by institute
It burns product to come out of the stove, i.e. acquisition titanium pentoxide piece.After tested, yield 87.9%.
According to GB/T 7962.12-1987 colouless optical glass test method, refraction of the product at wavelength 560nm
Rate is 2.306, can be used as high refractive index Coating Materials use.
Sample is subjected to XRD and SEM characterization, it is known that, sample is pure phase titanium pentoxide, without any miscellaneous phase.
Claims (6)
1. a kind of technique of TiC reduction preparation sheet titanium pentoxide, which comprises the following steps:
Step 1: titanium carbide in mass ratio: titanium dioxide=1:8.5~10 weigh raw material titanium carbide, titanium dioxide respectively, add water
Ball milling mixing, feeding is dried after ball milling, is then ground to powder, is sieved, tabletting；
Step 2: the mixing tabletting that step 1 obtains being placed in Muffle furnace in crucible, inert gas is passed through into furnace chamber
To empty furnace chamber air；
Step 3: it is sintered stage by stage, and is continually fed into inert gas in entire sintering process, steps are as follows:
A. room temperature~1100 DEG C, 1~5 DEG C/min of heating rate；
B.1100 DEG C, 4~6h is kept the temperature；
DEG C C.1100~1200 DEG C, 1~5 DEG C/min of heating rate；
D.1200 DEG C, 4~6h is kept the temperature；
DEG C E.1200~final sintering temperature, 1~5 DEG C/min of heating rate；
F. final sintering temperature keeps the temperature 4~6h；Final sintering temperature is 1250~1330 DEG C；
Step 4: the Muffle furnace is slowly decreased to 400 DEG C with the rate of temperature fall of 1~5 DEG C/min, then is down to room temperature with furnace, will be burnt
Product is come out of the stove, i.e. acquisition titanium pentoxide piece.
2. the technique of TiC reduction preparation sheet titanium pentoxide according to claim 1, which is characterized in that in step 1,
Water and mixed powder mass ratio are 2.5~5:1,24~28h of Ball-milling Time, 80~250r/min of rotational speed of ball-mill.
3. the technique of TiC reduction preparation sheet titanium pentoxide according to claim 1, which is characterized in that in step 1,
The temperature of the drying is 60~80 DEG C.
4. the technique of TiC reduction preparation sheet titanium pentoxide according to claim 1, which is characterized in that in step 1,
The step of tabletting are as follows: use is dry-pressing formed, and for pressure in 1.5~3MPa, the time is 15~60s.
5. the technique of TiC reduction preparation sheet titanium pentoxide according to claim 1, which is characterized in that in step 1,
The step of tabletting are as follows: first using dry-pressing formed, pressure is 15~60s in 1.5~3MPa, time, is then carried out cold etc. quiet
Pressure, for parameter in 100~250MPa, the time is 200~400s.
6. the technique of TiC reduction preparation sheet titanium pentoxide according to claim 1, which is characterized in that the carbonization
Titanium partial size is 2~4 μm, and purity is 99.99% or more, and the titanium dioxide partial size is 2~5 μm, and purity is 99.99% or more.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111217390A (en) * | 2020-03-04 | 2020-06-02 | 四川大学 | Lambda-Ti3O5Powder preparation method |
| CN113213915A (en) * | 2021-04-15 | 2021-08-06 | 有研资源环境技术研究院(北京)有限公司 | Preparation method of low-temperature trititanium pentoxide crystal coating material |
| CN117776257A (en) * | 2023-12-26 | 2024-03-29 | 西南大学 | Ti (titanium) 4 O 7 Powder material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101333003A (en) * | 2008-08-01 | 2008-12-31 | 上海特旺光电材料有限公司 | Method for preparing Ti3O5 filming material |
| CN103787409A (en) * | 2014-01-10 | 2014-05-14 | 四川大学 | Preparation methods of Ti3O5 powder |
| CN103806099A (en) * | 2014-01-20 | 2014-05-21 | 福州阿石创光电子材料有限公司 | Method for preparing titanium oxide crystal |
| CN203846137U (en) * | 2014-01-20 | 2014-09-24 | 福州阿石创光电子材料有限公司 | Trititanium pentoxide crystal |
-
2019
- 2019-01-18 CN CN201910048945.3A patent/CN109485408A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101333003A (en) * | 2008-08-01 | 2008-12-31 | 上海特旺光电材料有限公司 | Method for preparing Ti3O5 filming material |
| CN103787409A (en) * | 2014-01-10 | 2014-05-14 | 四川大学 | Preparation methods of Ti3O5 powder |
| CN103806099A (en) * | 2014-01-20 | 2014-05-21 | 福州阿石创光电子材料有限公司 | Method for preparing titanium oxide crystal |
| CN203846137U (en) * | 2014-01-20 | 2014-09-24 | 福州阿石创光电子材料有限公司 | Trititanium pentoxide crystal |
Non-Patent Citations (1)
| Title |
|---|
| F. REJASSE: "Study of the TiC1-x -TiO2 reactive interface", 《ACTA MATERIALIA》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111217390A (en) * | 2020-03-04 | 2020-06-02 | 四川大学 | Lambda-Ti3O5Powder preparation method |
| CN113213915A (en) * | 2021-04-15 | 2021-08-06 | 有研资源环境技术研究院(北京)有限公司 | Preparation method of low-temperature trititanium pentoxide crystal coating material |
| 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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