CN109704753A - A kind of preparation method of β phase titanium pentoxide crystal wafer - Google Patents
A kind of preparation method of β phase titanium pentoxide crystal wafer Download PDFInfo
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- CN109704753A CN109704753A CN201910048307.1A CN201910048307A CN109704753A CN 109704753 A CN109704753 A CN 109704753A CN 201910048307 A CN201910048307 A CN 201910048307A CN 109704753 A CN109704753 A CN 109704753A
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Abstract
The invention discloses a kind of preparation methods of β phase titanium pentoxide crystal wafer, the steps include: phenolic resin in mass ratio: titanium dioxide=1:8.5~10 weigh raw material phenolic resin, titanium dioxide respectively, phenolic resin is first pre-dissolved in organic solvent, titanium dioxide is added after completely dissolution and carries out ball milling mixing, dry, grinding, sieving, then tabletting is sintered stage by stage under an inert atmosphere, finally cooling to obtain product.The titanium pentoxide crystal of sheet can be made in the present invention, crystal phase is β phase, and purity reaches 99.99%, and yield is 83~85%, the β phase titanium pentoxide crystal of sheet can be shortened the plated film fritting time, plating membrane efficiency is improved, and the present invention, using after physics ball milling mixing method, temperature range of the direct step near 1300 DEG C calcines to obtain, and it is not necessarily to vacuum environment, equipment requirement is low, and controllability and safety greatly improve, while also greatly reducing production cost.
Description
Technical field
The present invention relates to Coating Materials, catalytic chemistry material, data storage and new energy fields, and in particular to a kind of
The preparation method of shape titanium pentoxide crystal.
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 is between 1.66~1.70, and there are five types of crystal phase (ɑ, β, λ, γ, δ) for tool, has both semiconductor
And metallic character, acid-alkali-corrosive-resisting can replace noble metal to do electrode material.Because it hinders temperature, coefficient is small again, but resistance can be with gas
The change of atmosphere and change and a kind of potential 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 β phase titanium pentoxide, thicknesses of layers is uniform, and refractive index is steady
It is fixed.Currently, β phase titanium pentoxide has been widely used for optics and electronics as vacuum evaporation target vapor deposition titanium deoxid film
In the application of device.
In the prior art, being mainly obtained by for titanium pentoxide restores titanium dioxide to realize, commonly restores
Agent has 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 more 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.Industrialized production is mainly with Ti powder and TiO at present2Powder high vacuum after mixing
Lower high temperature sintering is realized, but the method severe reaction conditions, not only needs high vacuum environment, required temperature is also all higher than
It is 1800 DEG C, high to production equipment requirement, production cost is substantially increased, safety coefficient is also difficult to ensure.Guo-Hua Zhang
Et al. respectively in 2016 (Journal of Materials Science.2016,51 (14): 7008-7015.) and 2017
(Journal of Materials Science.2017,52 (12): 7546-7554.) does carbon source using phenolic resin and prepares carbon
Change titanium and titanium nitride.Experimental data shows wrapped good, reducing property stabilization after phenolic resin carbonized, but in its reaction
Between product be λ phase and γ phase Ti3O5, phase stability is poor, and it is obvious by temperature change, and lead to refractive index difference, it is unable to satisfy height
The requirement of precision Coating Materials.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of β phase titanium pentoxide crystal wafer, and reaction temperature is low, safety
Height, phase stability are good.
To achieve the above object, The technical solution adopted by the invention is as follows: a kind of preparation of β phase titanium pentoxide crystal wafer
Method, comprising the following steps:
Step 1: phenolic resin in mass ratio: titanium dioxide=1:9.5~10.5 weigh raw material phenolic resin, dioxy respectively
Change titanium, phenolic resin is first pre-dissolved in organic solvent, titanium dioxide is added after completely dissolution and carries out ball milling mixing, after ball milling feeding into
Row drying is then ground to powder, sieving, 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~1000 DEG C, 1~5 DEG C/min of heating rate；
B.1000 DEG C, 4~6h is kept the temperature；
DEG C C.1000~final sintering temperature, 1~5 DEG C/min of heating rate；
D. final sintering temperature keeps the temperature 4~6h；Final sintering temperature is 1250~1350 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 β phase titanium pentoxide piece.
Preferably, in step 1, the organic solvent and mixed powder mass ratio are 1.5~3.5:1, Ball-milling Time 24~
28h, rotational speed of ball-mill are 60~200r/min.
Preferably, in step 1, the organic solvent is alcoholic solvent.It is furthermore preferred that the organic solvent is dehydrated alcohol.
Preferably, in step 1, the temperature of the drying is 60~100 DEG C.
Preferably, in step 1, the step of the tabletting are as follows: using dry-pressing formed, pressure is in 1.5~4MPa, time 15
~60s.
Alternatively, in step 1, the step of the tabletting are as follows: first using dry-pressing formed, pressure is in 1.5~4MPa, time 15
~60s then carries out isostatic cool pressing, and for parameter in 150~300MPa, the time is 150~350s.
Preferably, the phenolic resin is the alcohol-soluble phenolic resin with high Residual carbon, and purity is 99.99% or more,
The titanium dioxide partial size is 30~40nm, and purity is 99.99% or more.
The present invention dissolves in the characteristic of organic solvent using phenolic resin, as carbon source, is used as ball after completely dissolution
Grinding media carrys out dispersed titanium dioxide.In subsequent drying process, the titanium dioxide of the fully wrapped around dispersion of phenolic resin energy of precipitation
Titanium, high Residual carbon can also make the carbon thermal reduction efficiency of subsequent progress reach highest.
Compared with prior art, the invention has the following beneficial effects:
(1) β phase titanium pentoxide crystal wafer can be made in the present invention, and phase stability is good, and purity reaches 99.99%, and yield exists
83~85%, increase by 10% or so compared with of the same trade；β phase titanium pentoxide crystal wafer can be shortened the plated film fritting time, improve
Membrane efficiency is plated, discharge quantity is low, complies fully with the requirement for doing Coating Materials.
(2) for the phenolic resin for using remaining carbon high for reducing agent, resin wraps up titanium dioxide raw material powder in organic solvent
Body, reduction effect is good, the later period become gas after directly exclude, carbon-free remnants, formed 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 equipment requirement is low, and controllability and safety mention significantly
Height, while also greatly reducing production cost.
Detailed description of the invention
Fig. 1 is the pictorial diagram of β phase titanium pentoxide product made from the embodiment of the present invention 1.
Fig. 2 is the XRD diagram of β phase titanium pentoxide product made from the embodiment of the present invention 1.
Fig. 3 is the SEM figure of β phase 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 special instruction, and the phenolic resin is with high residual
The alcohol-soluble phenolic resin of carbon rate, purity are 99.99% or more, and the titanium dioxide partial size is 30~40nm, and purity is
99.99% or more.
Embodiment 1
Step 1: phenolic resin in mass ratio: titanium dioxide=1:10.5 weighs raw material phenolic resin, titanium dioxide respectively,
Phenolic resin is first pre-dissolved in dehydrated alcohol, is added titanium dioxide after completely dissolution, ball milling mixing for 24 hours, rotational speed of ball-mill 200r/
Min, dehydrated alcohol and mixed powder mass ratio are 1.5:1；Feeding is dried in 60 DEG C of drying boxes after ball milling, is taken after drying completely
Mixing out sieves with 100 mesh sieve after mechanical lapping；Using dry-pressing formed, pressure obtains mixing tabletting in 1.5MPa, time 60s；
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~1000 DEG C, 2 DEG C/min of heating rate；
B.1000 DEG C, 4h is kept the temperature；
DEG C C.1000~1250 DEG C, 2 DEG C/min of heating rate；
D.1250 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 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 β phase titanium pentoxide crystal wafer, pictorial diagram are as shown in Figure 1.After tested, yield 84%.
According to GB/T 7962.12-1987 colouless optical glass test method, refraction of the product at wavelength 560nm
Rate is 2.309, can be used as high refractive index Coating Materials use.
Sample is subjected to XRD test, as shown in Fig. 2, after with β-titanium pentoxide standard card comparison, it is known that, sample is
Pure β phase titanium pentoxide belongs to monoclinic system 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: phenolic resin in mass ratio: titanium dioxide=1:9.5 weighs raw material phenolic resin, titanium dioxide respectively,
Phenolic resin is first pre-dissolved in dehydrated alcohol, and titanium dioxide, ball milling mixing 28h, rotational speed of ball-mill 60r/ are added after completely dissolution
Min, dehydrated alcohol and mixed powder mass ratio are 3.5:1；Feeding is dried in 60 DEG C of drying boxes after ball milling, is taken after drying completely
Mixing out sieves with 100 mesh sieve after mechanical lapping；Using dry-pressing formed, pressure obtains mixing tabletting in 4MPa, time 15s；
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~1000 DEG C, 1 DEG C/min of heating rate；
B.1000 DEG C, 6h is kept the temperature；
DEG C C.1000~1300 DEG C, 1 DEG C/min of heating rate；
D.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 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 β phase titanium pentoxide crystal wafer.After tested, yield 85%.
According to GB/T 7962.12-1987 colouless optical glass test method, refraction of the product at wavelength 560nm
Rate is 2.307, 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 β phase titanium pentoxide, without any miscellaneous phase.
Embodiment 3
Step 1: phenolic resin in mass ratio: titanium dioxide=1:10 weighs raw material phenolic resin, titanium dioxide, phenol respectively
Urea formaldehyde is first pre-dissolved in dehydrated alcohol, is added titanium dioxide after completely dissolution, ball milling mixing for 24 hours, rotational speed of ball-mill 200r/min,
Dehydrated alcohol and mixed powder mass ratio are 2:1；Feeding is dried in 100 DEG C of drying boxes after ball milling, and dry rear take out completely is mixed
Material, sieves with 100 mesh sieve after mechanical lapping；Using dry-pressing formed, pressure then carries out isostatic cool pressing in 2MPa, time 20s, ginseng
Number obtains mixing tabletting in 300MPa, time 150s；
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~1000 DEG C, 5 DEG C/min of heating rate；
B.1000 DEG C, 4h is kept the temperature；
DEG C C.1000~1350 DEG C, 5 DEG C/min of heating rate；
D.1350 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 β phase titanium pentoxide crystal wafer.After tested, yield 83%.
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 β phase titanium pentoxide, without any miscellaneous phase.
Embodiment 4
Step 1: phenolic resin in mass ratio: titanium dioxide=1:9.7 weighs raw material phenolic resin, titanium dioxide respectively,
Phenolic resin is first pre-dissolved in dehydrated alcohol, is added titanium dioxide after completely dissolution, ball milling mixing for 24 hours, rotational speed of ball-mill 150r/
Min, dehydrated alcohol and mixed powder mass ratio are 2:1；Feeding is dried in 80 DEG C of drying boxes after ball milling, dry completely rear taking-up
Mixing sieves with 100 mesh sieve after mechanical lapping；Using dry-pressing formed, pressure then carries out cold etc. quiet in 1.5MPa, time 60s
Pressure, parameter obtain mixing tabletting in 200MPa, time 240s；
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~1000 DEG C, 2 DEG C/min of heating rate；
B.1000 DEG C, 4h is kept the temperature；
DEG C C.1000~1300 DEG C, 2 DEG C/min of heating rate；
D.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 β phase titanium pentoxide crystal wafer.After tested, yield 84%.
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 β phase titanium pentoxide, without any miscellaneous phase.
Claims (8)
1. a kind of preparation method of β phase titanium pentoxide crystal wafer, which comprises the following steps:
Step 1: phenolic resin in mass ratio: titanium dioxide=1:9.5 ~ 10.5 weigh raw material phenolic resin, titanium dioxide respectively,
Phenolic resin is pre-dissolved in organic solvent, titanium dioxide is added after completely dissolution and carries out ball milling mixing, feeding is done after ball milling
It is dry, it 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 ~ 1000 DEG C, 1 ~ 5 DEG C/min of heating rate；
B.1000 DEG C, 4 ~ 6h is kept the temperature；
DEG C C.1000 ~ final sintering temperature, 1 ~ 5 DEG C/min of heating rate；
D. final sintering temperature keeps the temperature 4 ~ 6h；Final sintering temperature is 1250 ~ 1350 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 β phase titanium pentoxide piece.
2. the preparation method of β phase titanium pentoxide crystal wafer according to claim 1, which is characterized in that in step 1, have
Solvent and mixed powder mass ratio are 1.5 ~ 3.5:1,24 ~ 28 h of Ball-milling Time, 60 ~ 200 r/min of rotational speed of ball-mill.
3. the preparation method of β phase titanium pentoxide crystal wafer according to claim 1 or 2, which is characterized in that in step 1,
The organic solvent is alcoholic solvent.
4. the preparation method of β phase titanium pentoxide crystal wafer according to claim 3, which is characterized in that in step 1, institute
Stating organic solvent is dehydrated alcohol.
5. the preparation method of β phase titanium pentoxide crystal wafer according to claim 1 or 2, which is characterized in that in step 1,
The temperature of the drying is 60 ~ 100 DEG C.
6. the preparation method of β phase titanium pentoxide crystal wafer according to claim 1 or 2, 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 ~ 4MPa, the time is 15 ~ 60s.
7. the preparation method of β phase titanium pentoxide crystal wafer according to claim 1 or 2, 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 ~ 4MPa, time, then carries out isostatic cool pressing,
For parameter in 150 ~ 300MPa, the time is 150 ~ 350s.
8. the preparation method of β phase titanium pentoxide crystal wafer according to claim 1 or 2, which is characterized in that the phenolic aldehyde
Resin is the alcohol-soluble phenolic resin with high Residual carbon, and purity is 99.99% or more, and the titanium dioxide partial size is 30 ~ 40
Nm, purity are 99.99% or more.
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Citations (8)
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|---|---|---|---|---|
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| 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 |
| CN101648821A (en) * | 2009-08-25 | 2010-02-17 | 山东理工大学 | Preparing method of denitration nanometer titanium dioxide honeycomb ceramics |
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| EP2371767A4 (en) * | 2008-12-25 | 2012-05-30 | Univ Tokyo | Fine structural body, method for manufacturing fine structural body, magnetic memory, charge storage memory and optical information recording medium |
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| CN104973622A (en) * | 2015-02-12 | 2015-10-14 | 四川大学 | Preparation method of light-induced phase transition storage powdery material lamda-Ti3O5 |
| CN109863381A (en) * | 2016-10-25 | 2019-06-07 | 松下知识产权经营株式会社 | Pressure sensor |
-
2019
- 2019-01-18 CN CN201910048307.1A patent/CN109704753A/en active Pending
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|---|---|---|---|---|
| EP0932059A2 (en) * | 1998-01-21 | 1999-07-28 | Sumitomo Chemical Company, Limited | Phase retarder film |
| 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 |
| WO2010064575A1 (en) * | 2008-12-04 | 2010-06-10 | 国立大学法人東京大学 | Titanium oxide particles, manufacturing method thereof, magnetic memory, and charge storage type memory |
| EP2371767A4 (en) * | 2008-12-25 | 2012-05-30 | Univ Tokyo | Fine structural body, method for manufacturing fine structural body, magnetic memory, charge storage memory and optical information recording medium |
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| CN104973622A (en) * | 2015-02-12 | 2015-10-14 | 四川大学 | Preparation method of light-induced phase transition storage powdery material lamda-Ti3O5 |
| CN109863381A (en) * | 2016-10-25 | 2019-06-07 | 松下知识产权经营株式会社 | Pressure sensor |
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| KEHAN WU等: "Formation of submicrometer titanium nitride from a titanium dioxide/phenolic resin composite", 《JOURNAL OF MATERIALS SCIENCE》 * |
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