CN105887182A - Preparation technology of trititanium pentoxide crystal - Google Patents
Preparation technology of trititanium pentoxide crystal Download PDFInfo
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- CN105887182A CN105887182A CN201410767346.4A CN201410767346A CN105887182A CN 105887182 A CN105887182 A CN 105887182A CN 201410767346 A CN201410767346 A CN 201410767346A CN 105887182 A CN105887182 A CN 105887182A
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Abstract
The invention discloses a preparation technology of trititanium pentoxide crystal. A stage heating sintering method is adopted and comprises the following steps of: in the first stage, heating to 1,200 DEG C from normal temperature, wherein the heating rate is 5-7 DEG C/min, and the vacuum degree is kept below 10<-3>-10<-4>pa; in the second stage, heating to 1,500 DEG C from 1,200 DEG C, wherein the heating rate is 2-4 DEG C/min; and when the temperature reaches 1,400 DEG C, introducing an inert protective gas; and in the third stage, heating from 1,500 DEG C to 1,750-1,850 DEG C, wherein the heating rate is 1.0-2.0 DEG C/min; impurities are not introduced into the preparation process, the formation of a large quantity of pores is effectively avoided, and the prepared trititanium pentoxide has relatively high purity and quality; meanwhile, stage heating sintering of the whole system is realized through an electromagnetic induction heating way, a low-voltage strong-current transformer essential to a resistance heating method is saved, and the device is simple, safe and reliable in operation and convenient to operate while the energy is saved by over 30%.
Description
Technical field
The present invention relates to Coating Materials field, the processing technology of a kind of five oxidation three titanium crystals.
Background technology
Five oxidation Tritanium/Trititaniums, are a kind of black blue powders, have metallic luster.Oxygen content is at 62.3%～64.3% (atom).Five oxidation three titanium crystals, belong to orthorhombic structure, are produced, lattice paprmeter α=0.3747nm by high temperature distillation crystallization.Density 4.29g/cm3, fusing point 2180 DEG C.For vacuum coating material, its advantage is that discharge quantity is little, purity is high, nothing collapses point, do not jumps medicine, stable refractive index, reaches top standard in the production technology same industry at home.
Five aoxidize metastable compound in the low price Series oxides that Tritanium/Trititaniums are titaniums, there is metalloid characteristic, there is the highest electric conductivity at normal temperatures, compared with noble metal electrode material, it is cheap, acid-alkali-corrosive-resisting strong, therefore can serve as electrode material to substitute noble metal.Five oxidation Tritanium/Trititaniums are a kind of non-stoichiometric compounds, and O/Ti can change between 1.66～1.70, and it is internal containing substantial amounts of Lacking oxygen, and quasi-free electron concentration is higher, and its resistance can change with the change of atmosphere, is therefore a kind of potential oxygen-sensitive material.
At present, five oxidation Tritanium/Trititaniums are widely used in the manufacture of opto-electronic device as the evaporation target of coating of titanium dioxide, device etc. as integrated in Display Technique, imaging technique, light output and light.Titanium oxide film layer has the highest refractive index, good stability and fastness in visible ray and near infrared spectral range.Early stage, people are mainly deposited with coating of titanium dioxide with titanium dioxide coating materials, but titanium dioxide coating materials can discharge substantial amounts of oxygen, even if sufficiently preheating during heating and fritting, sputtering or inevitably, and hardly result in that thickness is homogeneous, the film layer of stable refractive index.Along with going deep into of research, it has been found that after titanium dioxide coating materials fritting, its chemical composition is about five oxidation Tritanium/Trititaniums, thus can cause the releasing of a large amount of oxygen；Further, if titanium dioxide coating materials fritting is insufficient, the discordance of its melt composition then can cause the film layer hardly resulting in stable optical feature.If with five oxidation Tritanium/Trititaniums as deposition material, the shortcoming that titanium dioxide coating materials can be avoided, reduce discharge quantity, it is to avoid sputtering, obtain thickness homogeneous,
The high performance membrane layer of stable refractive index.Now, five oxidation Tritanium/Trititanium coating materials oneself progressively replace titanium dioxide coating materials and in high index film material, occupy main status.
In prior art, granular five oxidation Tritanium/Trititaniums are all readily incorporated impurity in preparation process, form a large amount of pore, there is the material that oxygen content relative different is bigger, thus affect purity and the quality of the film plating layer prepared.And play existing Ti 3 O 5 filming material of preparing and generally adopt the method being heated by resistive, insulation technology is required strict by electrical resistance heating, complex process, simultaneously need to high-power low pressure, high current power transformation device, power consumption is big, and production cost is high.
Summary of the invention
The technical problem to be solved in the present invention is the defect overcoming prior art, it is provided that the processing technology of a kind of five new oxidation three titanium crystals.
In order to solve above-mentioned technical problem, the invention provides following technical scheme:
The processing technology of a kind of five oxidation three titanium crystals, comprises the following steps:
1) it is, titanium in mass ratio by raw material titanium valve and titania powder: titanium dioxide=1: 9～12, mix homogeneously, pelletize, at 100～300 DEG C, drying, becomes sintering feed；Preferably, titanium: titanium dioxide=1: 10.
2), putting in crucible by sintering feed, crucible is transferred to high temperature and declines in stove, and being evacuated to vacuum in stove is 10-3～10-4Below pa；
3), to whole system heat up sintering stage by stage, and the parameter in each stage sets as follows:
First stage: room temperature rises to 1200 DEG C, heating rate is 5～7 DEG C/min, and vacuum is maintained at 10-3～10-4Below pa；
Second stage: 1200 rise to 1500 DEG C, heating rate is 2～4 DEG C/min, is filled with inert protective gas when temperature reaches 1400 DEG C；
Phase III: C.1500 DEG C rising to 1750～1850 DEG C, heating rate is 1.0～2.0 DEG C/min；
4), at 1750～1850 DEG C, being incubated 3～6 hours, melting sources is abundant, the temperature gradient of solid-liquid interface of crystal growth in the range of 30～48 DEG C/cm, crucible fall off rate between 1.5～3.5mm/h,
5), after crystal growth terminates, in growth furnace, appropriate location is incubated 10～24 hours, is the most at the uniform velocity down to room temperature.
Further, described step 3) in be electromagnetic induction heating to the mode of heating of whole system.
Further, described step 4) in, the temperature gradient of solid-liquid interface of crystal growth is in the range of 35～40 DEG C/cm, and crucible fall off rate is between 2mm/h.
Preferably, described step 5) in be down to room temperature with the speed of 25～80 DEG C/h, the crystal grown is made annealing treatment.
Preferably, described step 5) in be down to room temperature with the speed of 40～45 DEG C/h, the crystal grown is made annealing treatment.
Preferably, the particle diameter of described titanium valve is 10～12 μm, and purity is more than 99.9%；The particle diameter of described titanium dioxide is 3～5 μm, and purity is more than 99.99%.
Preferably, described step 3) in the inert protective gas that is filled with of second stage be Ar, He, H2In any one.
The technique of the present invention uses the method for the sintering that heats up stage by stage, and first will be evacuated to vacuum in stove is 10-3～10-4Pa, is filled with inert protective gas when temperature reaches 1400 DEG C；Preparation process is not the most easily introduced impurity, also effectively prevent the formation of a large amount of pore, the five oxidation Tritanium/Trititanium purity prepared and quality are higher, use the mode of electromagnetic induction heating to sintering that whole system is heated up stage by stage simultaneously, eliminating requisite low-voltage heavy current power transformation device in electrical resistance heating, device is simple, safe and reliable to operation, easy to operate, energy-conservation more than 30%.
Detailed description of the invention
Hereinafter the preferred embodiments of the present invention are illustrated, it will be appreciated that preferred embodiment described herein is merely to illustrate and explains the present invention, is not intended to limit the present invention.
Embodiment 1
The processing technology of a kind of five oxidation three titanium crystals, comprises the following steps:
1) it is, titanium in mass ratio by raw material titanium valve and titania powder: titanium dioxide=1: 9, mix homogeneously, pelletize, at 100～300 DEG C, drying, becomes sintering feed；The particle diameter of titanium valve is 10 μm, and purity is more than 99.9%；The particle diameter of described titanium dioxide is 3 μm, and purity is more than 99.99%.
2), putting in crucible by sintering feed, crucible is transferred to high temperature and declines in stove, and being evacuated to vacuum in stove is 10-3～10-4Below pa；
3), using electromagnetic induction heating to heat up whole system stage by stage sintering, the parameter setting in each stage is as follows:
First stage: room temperature rises to 1200 DEG C, heating rate is 5 DEG C/min, and vacuum is maintained at 10-3～10-4Below pa；
Second stage: 1200 rise to 1500 DEG C, heating rate is 2 DEG C/min, is filled with inert protective gas Ar when temperature reaches 1400 DEG C；
Phase III: C.1500 DEG C rising to 1750 DEG C, heating rate is 2.0 DEG C/min；
4), at 1750 DEG C, being incubated 6 hours, melting sources is abundant, the temperature gradient of solid-liquid interface of crystal growth in the range of 30 DEG C/cm, crucible fall off rate between 1.5mm/h,
5), after crystal growth terminates, in growth furnace, appropriate location is incubated 24 hours, and 85 DEG C/h is at the uniform velocity down to room temperature.
Embodiment 2
The processing technology of a kind of five oxidation three titanium crystals, comprises the following steps:
1) it is, titanium in mass ratio by raw material titanium valve and titania powder: titanium dioxide=1: 12, mix homogeneously, pelletize, at 100～300 DEG C, drying, becomes sintering feed；The particle diameter of titanium valve is 12 μm, and purity is more than 99.9%；The particle diameter of described titanium dioxide is 5 μm, and purity is more than 99.99%.
2), putting in crucible by sintering feed, crucible is transferred to high temperature and declines in stove, and being evacuated to vacuum in stove is 10-3～10-4Below pa；
3), using electromagnetic induction heating to heat up whole system stage by stage sintering, the parameter setting in each stage is as follows:
First stage: room temperature rises to 1200 DEG C, heating rate is 7 DEG C/min, and vacuum is maintained at 10-3～10-4Below pa；
Second stage: 1200 rise to 1500 DEG C, heating rate is 4 DEG C/min, is filled with inert protective gas He when temperature reaches 1400 DEG C；
Phase III: C.1500 DEG C rising to 1850 DEG C, heating rate is 1.0 DEG C/min；
4), at 1850 DEG C, being incubated 3 hours, melting sources is abundant, the temperature gradient of solid-liquid interface of crystal growth in the range of 48 DEG C/cm, crucible fall off rate between 3.5mm/h,
5), after crystal growth terminates, in growth furnace, appropriate location is incubated 10 hours, and then 25 DEG C/h is at the uniform velocity down to room temperature.
Embodiment 3
The processing technology of a kind of five oxidation three titanium crystals, comprises the following steps:
1) it is, titanium in mass ratio by raw material titanium valve and titania powder: titanium dioxide=1: 10, mix homogeneously, pelletize, at 100～300 DEG C, drying, becomes sintering feed；The particle diameter of described titanium valve is 11 μm, and purity is more than 99.9%；The particle diameter of described titanium dioxide is 4 μm, and purity is more than 99.99%.
2), putting in crucible by sintering feed, crucible is transferred to high temperature and declines in stove, and being evacuated to vacuum in stove is 10-3～10-4Below pa；
3), using electromagnetic induction heating to heat up whole system stage by stage sintering, the parameter setting in each stage is as follows:
First stage: room temperature rises to 1200 DEG C, heating rate is 6 DEG C/min, and vacuum is maintained at 10-3～10-4Below pa；
Second stage: 1200 rise to 1500 DEG C, heating rate is 3 DEG C/min, is filled with inert protective gas H when temperature reaches 1400 DEG C2；
Phase III: C.1500 DEG C rising to 1800 DEG C, heating rate is 1.5 DEG C/min；
4), at 1800 DEG C, being incubated 4.5 hours, melting sources is abundant, the temperature gradient of solid-liquid interface of crystal growth in the range of 35 DEG C/cm, crucible fall off rate between 2mm/h,
5), after crystal growth terminates, in growth furnace, appropriate location is incubated 20 hours, and then 40 DEG C/h is at the uniform velocity down to room temperature.
Embodiment 4
The processing technology of a kind of five oxidation three titanium crystals, comprises the following steps:
1) it is, titanium in mass ratio by raw material titanium valve and titania powder: titanium dioxide=1: 10, mix homogeneously, pelletize, at 100～300 DEG C, drying, becomes sintering feed；The particle diameter of described titanium valve is 10 μm, and purity is more than 99.9%；The particle diameter of described titanium dioxide is 4 μm, and purity is more than 99.99%.
2), putting in crucible by sintering feed, crucible is transferred to high temperature and declines in stove, and being evacuated to vacuum in stove is 10-3～10-4Below pa；
3), using electromagnetic induction heating to heat up whole system stage by stage sintering, the parameter setting in each stage is as follows:
First stage: room temperature rises to 1200 DEG C, heating rate is 7 DEG C/min, and vacuum is maintained at 10-3～10-4Below pa；
Second stage: 1200 rise to 1500 DEG C, heating rate is 3 DEG C/min, is filled with inert protective gas H when temperature reaches 1400 DEG C2；
Phase III: C.1500 DEG C rising to 1850 DEG C, heating rate is 1.6 DEG C/min；
4), at 1850 DEG C, being incubated 4 hours, melting sources is abundant, the temperature gradient of solid-liquid interface of crystal growth in the range of 40 DEG C/cm, crucible fall off rate between 2mm/h,
5), after crystal growth terminates, in growth furnace, appropriate location is incubated 18 hours, and then 45 DEG C/h is at the uniform velocity down to room temperature.
The specification of five oxidation three titanium crystals that embodiment of the present invention 1-4 is produced is 1.0～4.0mm, refractive index is 2.35/500nm, transparency range is 400-12000nm, evaporating temperature is 1800-2000 DEG C, it is higher that the discharge quantity of five oxidation three titanium crystals is little, purity is high, nothing collapses point, purity and quality, can be widely used for various anti-reflection film, multilayer film
Last it is noted that the foregoing is only the preferred embodiments of the present invention, it is not limited to the present invention, although the present invention being described in detail with reference to previous embodiment, for a person skilled in the art, technical scheme described in foregoing embodiments still can be modified by it, or wherein portion of techniques feature is carried out equivalent.All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (8)
1. the processing technology of oxidation three titanium crystals, it is characterised in that comprise the following steps:
1), be titanium in mass ratio by raw material titanium valve and titanium dioxide powder: titanium dioxide=1: 9～12, mix homogeneously, pelletize,
Dry at 100～300 DEG C, become sintering feed；
2), putting in crucible by sintering feed, crucible is transferred to high temperature and declines in stove, and being evacuated to vacuum in stove is 10-3~
10-4Below pa；
3), to whole system heat up sintering stage by stage, and the parameter in each stage sets as follows:
First stage: room temperature rises to 1200 DEG C, heating rate is 5～7 DEG C/min, and vacuum is maintained at 10-3～10-4pa
Below；
Second stage: 1200 rise to 1500 DEG C, heating rate is 2～4 DEG C/min, is filled with when temperature reaches 1400 DEG C
Inert protective gas；
Phase III: C.1500 DEG C rising to 1750～1850 DEG C, heating rate is 1.0～2.0 DEG C/min；
4), at 1750～1850 DEG C, being incubated 3～6 hours, melting sources is abundant, the solid liquid interface temperature of crystal growth
Gradient in the range of 30～48 DEG C/cm, crucible fall off rate between 1.5～3.5mm/h,
5), after crystal growth terminates, in growth furnace, appropriate location is incubated 10～24 hours, is then passed through at the uniform velocity being down to
Room temperature.
The processing technology of a kind of five oxidation three titanium crystals, it is characterised in that described step 3)
In be electromagnetic induction heating to the mode of heating of whole system.
The processing technology of a kind of five oxidation three titanium crystals, it is characterised in that described step 4)
In, the temperature gradient of solid-liquid interface of crystal growth in the range of 35～40 DEG C/cm, crucible fall off rate 2mm/h it
Between.
The processing technology of a kind of five oxidation three titanium crystals, it is characterised in that described step 5)
In be down to room temperature with the speed of 25～80 DEG C/h, the crystal grown is made annealing treatment.
The processing technology of a kind of five oxidation three titanium crystals, it is characterised in that described step 5)
In be down to room temperature with the speed of 40～45 DEG C/h, the crystal grown is made annealing treatment.
The processing technology of a kind of five oxidation three titanium crystals, it is characterised in that described titanium valve
Particle diameter is 10～12 μm, and purity is more than 99.9%；The particle diameter of described titanium dioxide is 3～5 μm, and purity is 99.99%
Above.
The processing technology of a kind of five oxidation three titanium crystals, it is characterised in that described step 1)
The quality of middle titanium valve and titanium dioxide powder is than titanium: titanium dioxide=1: 10.
The processing technology of a kind of five oxidation three titanium crystals, it is characterised in that described step 3)
The inert protective gas that middle second stage is filled with is Ar, He, H2In any one.
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| CN201410767346.4A CN105887182A (en) | 2014-12-15 | 2014-12-15 | Preparation technology of trititanium pentoxide crystal |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111217390A (en) * | 2020-03-04 | 2020-06-02 | 四川大学 | Lambda-Ti3O5Powder preparation method |
| CN114197041A (en) * | 2021-12-14 | 2022-03-18 | 苏州科睿浦光电科技有限公司 | Preparation method of trititanium pentoxide polycrystal material and trititanium pentoxide polycrystal material |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH054818A (en) * | 1991-06-26 | 1993-01-14 | Toho Titanium Co Ltd | Production of titanium suboxide |
| JPH059028A (en) * | 1991-06-27 | 1993-01-19 | Toho Titanium Co Ltd | Production of titanium suboxide |
| CN1952204A (en) * | 2005-10-20 | 2007-04-25 | 北京有色金属研究总院 | Preprocessed optical coating materials and preprocessed method thereof |
| CN101280456A (en) * | 2007-12-28 | 2008-10-08 | 上海晶生实业有限公司 | Growing method by Ti3O5 by bridgman method |
| 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 |
| CN103806100A (en) * | 2014-02-12 | 2014-05-21 | 常州瞻驰光电科技有限公司 | Vertical temperature gradient growing method of trititanium pentoxide polycrystal |
-
2014
- 2014-12-15 CN CN201410767346.4A patent/CN105887182A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH054818A (en) * | 1991-06-26 | 1993-01-14 | Toho Titanium Co Ltd | Production of titanium suboxide |
| JPH059028A (en) * | 1991-06-27 | 1993-01-19 | Toho Titanium Co Ltd | Production of titanium suboxide |
| CN1952204A (en) * | 2005-10-20 | 2007-04-25 | 北京有色金属研究总院 | Preprocessed optical coating materials and preprocessed method thereof |
| CN101280456A (en) * | 2007-12-28 | 2008-10-08 | 上海晶生实业有限公司 | Growing method by Ti3O5 by bridgman method |
| 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 |
| CN103806100A (en) * | 2014-02-12 | 2014-05-21 | 常州瞻驰光电科技有限公司 | Vertical temperature gradient growing method of trititanium pentoxide polycrystal |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111217390A (en) * | 2020-03-04 | 2020-06-02 | 四川大学 | Lambda-Ti3O5Powder preparation method |
| CN114197041A (en) * | 2021-12-14 | 2022-03-18 | 苏州科睿浦光电科技有限公司 | Preparation method of trititanium pentoxide polycrystal material and trititanium pentoxide polycrystal material |
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