CN110156456A - A kind of titanium monoxide semiconductive ceramic and preparation method thereof - Google Patents
A kind of titanium monoxide semiconductive ceramic and preparation method thereof Download PDFInfo
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- CN110156456A CN110156456A CN201910452496.9A CN201910452496A CN110156456A CN 110156456 A CN110156456 A CN 110156456A CN 201910452496 A CN201910452496 A CN 201910452496A CN 110156456 A CN110156456 A CN 110156456A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
The present invention relates to a kind of titanium monoxide semiconductive ceramics and preparation method thereof.Mixed solution is obtained this method comprises: butyl titanate is dissolved in aqueous citric acid solution；The pH for adjusting mixed solution forms colloidal sol, and combustion adjuvant is added into colloidal sol, is aged at room temperature, aged colloidal sol is placed in water-bath and is chemically reacted, and obtains wet gel；Wet gel is placed in baking oven and is dried, xerogel is obtained, xerogel is ground, the first powder is obtained, the first powder is placed in Muffle furnace and is sintered, the first powder through being sintered is ground, the second powder is obtained, the second powder is pressed by disk by powder compressing machine；It is sintered using laser scanning disk, and during the scanning process, uses argon gas as reaction protective gas, obtain titanium monoxide semiconductive ceramic.Technical solution provided by the invention can reduce the production cost and energy consumption of titanium monoxide semiconductive ceramic.
Description
Technical field
The present invention relates to technical field of semiconductors more particularly to a kind of titanium monoxide semiconductive ceramic and preparation method thereof.
Background technique
Titanium monoxide (TiO) is a kind of non-stoichiometric compound, and generally oxygen-containing 52%-54% (atom) is contained
15% structural vacancy is equivalent to one kind with titanium dioxide (TiO2) be substrate extrinsic semiconductor, with it is stronger it is acidproof,
Caustic corrosion and higher hardness, and it is in the titanium dioxide of state of insulation at room temperature relatively, titanium monoxide has good
Electric conductivity.
Currently, the preparation of titanium monoxide is relatively difficult, and because reaction temperature is higher, when temperature is 700-800K,
Even if controlling partial pressure of oxygen, ingredient still can be highly unstable.In addition, traditional ceramics technique heating and cooling process is slower,
Therefore it is difficult to synthesize titanium monoxide.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of titanium monoxide semiconductive ceramic and preparation method thereof.
In a first aspect, the present invention provides a kind of titanium monoxide semiconductive ceramic preparation method, this method comprises the following steps:
Butyl titanate is dissolved in aqueous citric acid solution by S1, obtains mixed solution.
S2 is added ammonium hydroxide in the mixed solution and adjusts pH, forms colloidal sol, combustion adjuvant is added in Xiang Suoshu colloidal sol,
It is aged at room temperature, aged colloidal sol is placed in 100 DEG C of water-bath and is chemically reacted, obtain wet gel.
The wet gel is placed in 180 DEG C of baking oven and dries by S3, obtains xerogel, the xerogel is carried out
Grinding obtains the first powder, and it is to be sintered in 600 DEG C of Muffle furnace that first powder, which is placed in sintering temperature, when heat preservation
Between be 4h, the first powder through being sintered is ground, obtain the second powder, by powder compressing machine under 10MPa pressure will
Second powder is pressed into disk.
S4 is sintered using disk described in laser scanning, and during the scanning process, and argon gas is used to protect gas as reaction
Body obtains titanium monoxide semiconductive ceramic.
Specifically, pH is 5 to 6 in S2.
Specifically, combustion adjuvant described in S2 is ethylene glycol.
Specifically, a length of 1 to 3h when the reaction chemically reacted in S2.
Specifically, dried in S3 when a length of 2 to 4h.
Specifically, the diameter of disk described in S4 is 10mm, with a thickness of 0.5 to 1mm.
Specifically, the power of laser described in S4 is 83W, spot size 0.5mm2, by the continuous shape half of 980nm wavelength
Conductor laser issues.
Specifically, the power density of laser described in S4 is 166W/cm2。
Specifically, the room temperature is 15 to 25 DEG C.
Second aspect, the present invention also provides a kind of titanium monoxide semiconductive ceramic, the titanium monoxide semiconductive ceramic is adopted
It is made with above-mentioned preparation method.
Compared with prior art, the beneficial effects of the present invention are:
1) preparation method process is more simple compared to the prior art, and can realize at room temperature, equipment cost also compared with
It is low, the special reactor for making reaction betide environment in vacuum or water in the prior art is not needed, titanium monoxide can be greatly reduced
The production cost and energy consumption of semiconductive ceramic.
2) titanium monoxide semiconductor component made from is more stable, and purity is higher.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is this hair
Bright some embodiments for those of ordinary skill in the art without any creative labor, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the structural schematic diagram of the preparation facilities of the embodiment of the present invention；
Fig. 2 is the X-ray diffractogram of the titanium dioxide ceramic of the embodiment of the present invention；
Fig. 3 is the X-ray diffractogram of the titanium monoxide ceramics of the embodiment of the present invention.
Specific embodiment
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the invention.
Embodiment 1
The present embodiment provides a kind of titanium monoxide semiconductive ceramic preparation methods, and this method comprises the following steps:
S1 stoichiometrically takes 0.03mol butyl titanate and 0.03*1.5mol citric acid monohydrate, by citrate hydrate
Acid is dissolved in 20mL deionized water, obtains aqueous citric acid solution, then under ultrasonic wave dispersion, butyl titanate is dissolved in citric acid
Aqueous solution obtains mixed solution.
S2 is stirred continuously the mixed solution, and it is 5 that ammonium hydroxide, which is added, to adjust pH in the mixed solution, forms colloidal sol,
Ethylene glycol of the 10mL as combustion adjuvant is added into the colloidal sol, is aged at room temperature at 15 DEG C for 24 hours, by aged colloidal sol
It is placed in 100 DEG C of water-bath and is chemically reacted, reaction time 1h obtains wet gel.
The wet gel is placed in 180 DEG C of baking oven and carries out the drying of 2h by S3, so that organic solvent volatilization, is done
Gel grinds the xerogel in air, obtains the first powder, first powder, which is placed in sintering temperature, is
It is sintered in 600 DEG C of Muffle furnace, soaking time 4h, so that the organic matter in the xerogel is discharged, will be sintered
First powder is ground, and is obtained the second powder, is pressed into second powder directly under 10MPa pressure by powder compressing machine
Diameter is 10mm, the disk with a thickness of 0.5mm.
The disk is that rutile is main phase, and the titanium dioxide including a small amount of Anatase, as shown in Fig. 2, being the circle
Piece, that is, the X-ray diffractogram of titanium dioxide ceramic.
S4, issuing power by the continuous shape semiconductor laser 1 of 980nm wavelength is 83W, spot size 0.5mm2, function
Rate density is 166W/cm2Laser, as shown in Figure 1, being adjusted in laser irradiation direction perpendicular to the disk, and with
The speed of 0.8mm/s completes the laser scanning to the surface all areas of the disk, is sintered and completes in the laser scanning of one side
Afterwards, turn-over completes the laser scanning sintering of another side, meanwhile, during the scanning process, argon tanks outlet mouth of pipe 2 is opened, argon is used
As reaction protective gas, and after the completion of scanning, 30s closes argon tanks outlet mouth of pipe 2 to gas, and the final titanium monoxide that obtains partly is led
Body ceramics.
Embodiment 2
The present embodiment provides a kind of titanium monoxide semiconductive ceramic preparation methods, and this method comprises the following steps:
S1 stoichiometrically takes 0.03mol butyl titanate and 0.03*1.5mol citric acid monohydrate, by citrate hydrate
Acid is dissolved in 20mL deionized water, obtains aqueous citric acid solution, then under ultrasonic wave dispersion, butyl titanate is dissolved in citric acid
Aqueous solution obtains mixed solution.
S2 is stirred continuously the mixed solution, and it is 5.5 that ammonium hydroxide, which is added, to adjust pH in the mixed solution, is formed molten
Ethylene glycol of the 10mL as combustion adjuvant is added in Xiang Suoshu colloidal sol, is aged at room temperature at 20 DEG C for 24 hours for glue, will be aged
Colloidal sol is placed in 100 DEG C of water-bath and is chemically reacted, reaction time 1.5h, obtains wet gel.
The wet gel is placed in 180 DEG C of baking oven and carries out the drying of 3h by S3, so that organic solvent volatilization, is done
Gel grinds the xerogel in air, obtains the first powder, first powder, which is placed in sintering temperature, is
It is sintered in 600 DEG C of Muffle furnace, soaking time 4h, so that the organic matter in the xerogel is discharged, will be sintered
First powder is ground, and is obtained the second powder, is pressed into second powder directly under 10MPa pressure by powder compressing machine
Diameter is 10mm, the disk with a thickness of 0.75mm.
S4, issuing power by the continuous shape semiconductor laser of 980nm wavelength is 83W, spot size 0.5mm2, power
Density is 166W/cm2Laser, laser irradiation direction is adjusted to perpendicular to the disk, and with the speed of 0.8mm/s completion
Laser scanning to the surface all areas of the disk, after the completion of the laser scanning of one side sintering, turn-over completes another side
Laser scanning sintering, meanwhile, during the scanning process, open argon tanks outlet mouth of pipe, use argon gas as react protective gas,
And 30s closes argon tanks outlet mouth of pipe after the completion of scanning, it is final to obtain titanium monoxide semiconductive ceramic.
Embodiment 3
The present embodiment provides a kind of titanium monoxide semiconductive ceramic preparation methods, and this method comprises the following steps:
S1 stoichiometrically takes 0.03mol butyl titanate and 0.03*1.5mol citric acid monohydrate, by citrate hydrate
Acid is dissolved in 20mL deionized water, obtains aqueous citric acid solution, then under ultrasonic wave dispersion, butyl titanate is dissolved in citric acid
Aqueous solution obtains mixed solution.
S2 is stirred continuously the mixed solution, and it is 6 that ammonium hydroxide, which is added, to adjust pH in the mixed solution, forms colloidal sol,
Ethylene glycol of the 10mL as combustion adjuvant is added into the colloidal sol, is aged at room temperature at 25 DEG C for 24 hours, by aged colloidal sol
It is placed in 100 DEG C of water-bath and is chemically reacted, reaction time 2h obtains wet gel.
The wet gel is placed in 180 DEG C of baking oven and carries out the drying of 4h by S3, so that organic solvent volatilization, is done
Gel grinds the xerogel in air, obtains the first powder, first powder, which is placed in sintering temperature, is
It is sintered in 600 DEG C of Muffle furnace, soaking time 4h, so that the organic matter in the xerogel is discharged, will be sintered
First powder is ground, and is obtained the second powder, is pressed into second powder directly under 10MPa pressure by powder compressing machine
Diameter is 10mm, the disk with a thickness of 1mm.
S4, issuing power by the continuous shape semiconductor laser of 980nm wavelength is 83W, spot size 0.5mm2, power
Density is 166W/cm2Laser, laser irradiation direction is adjusted to perpendicular to the disk, and with the speed of 0.8mm/s completion
Laser scanning to the surface all areas of the disk, after the completion of the laser scanning of one side sintering, turn-over completes another side
Laser scanning sintering, meanwhile, during the scanning process, open argon tanks outlet mouth of pipe, use argon gas as react protective gas,
And 30s closes argon tanks outlet mouth of pipe after the completion of scanning, it is final to obtain titanium monoxide semiconductive ceramic.
As shown in figure 3, titanium monoxide semiconductive ceramic wide-angle in X ray diffracting spectrum made from through the foregoing embodiment
Partially (2-80 ° of θ=30 °) diffraction maximum is very clear, and occurs without the diffraction maximum of other miscellaneous phases, illustrates that gained one aoxidizes
Titanium semiconductive ceramic purity is higher.
Reader should be understood that in the description of this specification reference term " one embodiment ", " is shown " some embodiments "
The description of example ", specific examples or " some examples " etc. mean specific features described in conjunction with this embodiment or example, structure,
Material or feature are included at least one embodiment or example of the invention.In the present specification, above-mentioned term is shown
The statement of meaning property need not be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described
It may be combined in any suitable manner in any one or more of the embodiments or examples.In addition, without conflicting with each other, this
The technical staff in field can be by the spy of different embodiments or examples described in this specification and different embodiments or examples
Sign is combined.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of titanium monoxide semiconductive ceramic preparation method, which is characterized in that described method includes following steps:
Butyl titanate is dissolved in aqueous citric acid solution by S1, obtains mixed solution；
S2 is added ammonium hydroxide in the mixed solution and adjusts pH, forms colloidal sol, combustion adjuvant is added in Xiang Suoshu colloidal sol, in room temperature
Under be aged, aged colloidal sol is placed in 100 DEG C of water-bath and is chemically reacted, obtain wet gel；
The wet gel is placed in 180 DEG C of baking oven and dries by S3, obtains xerogel, the xerogel is ground,
The first powder is obtained, first powder is placed in the Muffle furnace that sintering temperature is 600 DEG C and is sintered, soaking time is
4h grinds the first powder through being sintered, and obtains the second powder, will be described under 10MPa pressure by powder compressing machine
Second powder is pressed into disk；
S4 is sintered using disk described in laser scanning, and during the scanning process, use argon gas as reaction protective gas,
Obtain titanium monoxide semiconductive ceramic.
2. titanium monoxide semiconductive ceramic preparation method according to claim 1, which is characterized in that pH is 5 to 6 in S2.
3. titanium monoxide semiconductive ceramic preparation method according to claim 1, which is characterized in that combustion adjuvant described in S2
For ethylene glycol.
4. titanium monoxide semiconductive ceramic preparation method according to claim 1, which is characterized in that chemically reacted in S2
A length of 1 to 3h when reaction.
5. titanium monoxide semiconductive ceramic preparation method according to claim 1, which is characterized in that the duration dried in S3
It is 2 to 4h.
6. titanium monoxide semiconductive ceramic preparation method according to claim 1, which is characterized in that disk described in S4
Diameter is 10mm, with a thickness of 0.5 to 1mm.
7. titanium monoxide semiconductive ceramic preparation method according to claim 1, which is characterized in that laser described in S4
Power is 83W, spot size 0.5mm2, issued by the continuous shape semiconductor laser of 980nm wavelength.
8. titanium monoxide semiconductive ceramic preparation method according to claim 1, which is characterized in that laser described in S4
Power density is 166W/cm2。
9. titanium monoxide semiconductive ceramic preparation method according to any one of claims 1 to 8, which is characterized in that described
Room temperature is 15 to 25 DEG C.
10. a kind of titanium monoxide semiconductive ceramic, which is characterized in that the titanium monoxide semiconductive ceramic uses such as claim
1 to 9 described in any item titanium monoxide semiconductive ceramic preparation methods are made.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2758402C1 (en) * | 2021-04-15 | 2021-10-28 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Method for producing a single crystal of titanium monoxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55140760A (en) * | 1979-04-20 | 1980-11-04 | Sumitomo Electric Industries | Titanium dioxide sintered body and its manufacture |
| CN106676543A (en) * | 2016-12-08 | 2017-05-17 | 苏州求是真空电子有限公司 | Method for reducing copper surface bivalent copper ions through lasers |
| CN109231263A (en) * | 2018-10-31 | 2019-01-18 | 攀钢集团攀枝花钢铁研究院有限公司 | The method for preparing TiO |
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- 2019-05-28 CN CN201910452496.9A patent/CN110156456B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55140760A (en) * | 1979-04-20 | 1980-11-04 | Sumitomo Electric Industries | Titanium dioxide sintered body and its manufacture |
| CN106676543A (en) * | 2016-12-08 | 2017-05-17 | 苏州求是真空电子有限公司 | Method for reducing copper surface bivalent copper ions through lasers |
| CN109231263A (en) * | 2018-10-31 | 2019-01-18 | 攀钢集团攀枝花钢铁研究院有限公司 | The method for preparing TiO |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2758402C1 (en) * | 2021-04-15 | 2021-10-28 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Method for producing a single crystal of titanium monoxide |
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