CN103539202A - Method for preparing titanium dioxide nanowire through self-reaction of single reagent - Google Patents
Method for preparing titanium dioxide nanowire through self-reaction of single reagent Download PDFInfo
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- CN103539202A CN103539202A CN201310373400.2A CN201310373400A CN103539202A CN 103539202 A CN103539202 A CN 103539202A CN 201310373400 A CN201310373400 A CN 201310373400A CN 103539202 A CN103539202 A CN 103539202A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 30
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title abstract description 10
- 239000003153 chemical reaction reagent Substances 0.000 title abstract description 5
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims abstract description 20
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- 230000035484 reaction time Effects 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 63
- 239000004408 titanium dioxide Substances 0.000 claims description 31
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000004033 plastic Substances 0.000 claims description 6
- 229920003023 plastic Polymers 0.000 claims description 6
- 230000007797 corrosion Effects 0.000 claims description 5
- 238000005260 corrosion Methods 0.000 claims description 5
- 239000004642 Polyimide Substances 0.000 claims description 3
- 150000001408 amides Chemical class 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 3
- 230000001186 cumulative effect Effects 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 15
- 239000000243 solution Substances 0.000 description 15
- 239000002070 nanowire Substances 0.000 description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- 239000011521 glass Substances 0.000 description 10
- 239000002253 acid Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 241000370738 Chlorion Species 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 230000032050 esterification Effects 0.000 description 3
- 238000005886 esterification reaction Methods 0.000 description 3
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 3
- 238000006068 polycondensation reaction Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 238000003491 array Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000010494 dissociation reaction Methods 0.000 description 2
- 230000005593 dissociations Effects 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 208000013201 Stress fracture Diseases 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 235000012149 noodles Nutrition 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing a titanium dioxide nanowire through self-reaction of a single reagent. The method comprises the following steps: (1) taking a titanium trichloride solution as an initial raw material, placing the titanium trichloride solution in a hydrothermal reaction kettle, placing in a thermostat, adjusting the reaction temperature to be 90-230 DEG C, and cooling to room temperature after reaction, wherein the reaction time is 1-100 hours; and (2) taking a sample out of the reaction kettle, cleaning and drying to obtain the titanium dioxide nanowire. The method has the advantages of simple process, easiness in operation and control, low cost, safety and environmental friendliness.
Description
Technical field
The present invention is specifically related to a kind of method that single agents autoreaction is prepared titanium dioxide nano thread.
Background technology
As the N-shaped semiconductor material of broad-band gap (3.1eV), titanium dioxide has obtained further investigation and widespread use in fields such as lithium cell, photochemical catalysis, dye-sensitized solar cells.Titanium dioxide one dimension Nano structure is if nano wire, nanotube and nanometer sheet etc. are because its special optical, electrical, magnetic, chemistry and mechanical characteristics etc. have attracted great concern.For example nano wire, in above-mentioned application, can provide the passage of the electric transmission of one dimension, thus fast transport electronics and the recombination losses that reduces electron-hole.
The method of the synthesis of titanium dioxide nano wire of having reported has electron beam evaporation [Yang T S, et al.Surf Sci, 2004, 548:75], tensio-active agent is assisted synthesis method [Adachi M, et al., J Am Chem Soc, 2004, 126:14943], electricity spraying method [Song M Y, et al., Appl Phys Lett, 2005, 87:113113], electrodip process [Natarajan C, et al.J Electrochem Soc, 1996, 143:1547], highly basic hydrothermal method [Enache-Pommer E, et al., Appl.Phys.Lett.2007, 91:123116.] and hydrochloric acid hydrothermal method [Liu B.et al., J.Am.Chem.Soc.2009, 131:3985].In aforesaid method, hydrothermal method is because cost is relatively low, and productive rate height is a kind of method of broad research.Wherein highly basic hydrothermal method is first by titanium source and highly basic (NaOH or KOH), to generate sodium titanate, then carries out ion-exchange generation metatitanic acid with hydrochloric acid, and final high temperature calcining generates titanium dioxide nano thread, the poly-complexity of step.In addition, hydrochloric acid hydrothermal method is to add titanium source and hydrochloric acid water thermal response in synthetic, hydrochloric acid suppresses the fast hydrolyzing in titanium source on the one hand, and what provide on the other hand that chlorion is adsorbed on titanium dioxide nucleus { on 110} face, makes it preferential along the reaction of [001] direction generation crystallographic orientation chemistry.Above-mentioned process using strong acid and highly basic, simultaneously also step is complicated relatively for highly basic hydrothermal method.Therefore be necessary to develop a kind of new technique simple, with low cost and be easy to realize the preparation technology of suitability for industrialized production.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method that single agents autoreaction is prepared titanium dioxide nano thread, and the method technique is simple, easy handling is controlled, cost is low, safety and environmental protection.
Above-mentioned technical problem of the present invention is achieved by the following technical solution: a kind of single agents autoreaction is prepared the method for titanium dioxide nano thread, contains following steps:
(1) get Titanium Trichloride Solution as starting raw material, Titanium Trichloride Solution is put into hydrothermal reaction kettle, then put into thermostat container, regulating temperature of reaction is 90～230 ℃, and the reaction times is 1～100 hour, is cooled to room temperature after reaction;
(2) take out the sample in reactor, after cleaning, drying, obtain titanium dioxide nano thread.
In step of the present invention (1), the quality percentage composition of Titanium Trichloride Solution is preferably 8%～30%, and Titanium Trichloride Solution volume preferably accounts for 5%～80% of reactor cumulative volume.
Described in step of the present invention (1), hydrothermal reaction kettle is preferably airtight high-temperature high-pressure reaction kettle, and described high-temperature high-pressure reaction kettle has metal shell, is preferably provided with heat-resisting and corrosion-resistant plastic or glass-lined in metal shell.
Heat-resisting and corrosion-resistant plastic of the present invention is preferably tetrafluoroethylene, polyimide, polybenzoate or PI polymeric amide.
In order better to generate titanium dioxide nanowire array, in step of the present invention (1), can supine conductive glass be set in Polycondensation Reactor and Esterification Reactor.Wherein conductive glass can be FTO conductive glass (SnO
2mix F) etc.
In step of the present invention (2), cleaning to be preferably adopts deionized water and dehydrated alcohol successively to wash for several times.
Temperature while drying in step of the present invention (2) is preferably 50～70 ℃, and drying time is preferably 5～48h.
The preparation method's of titanium dioxide nano thread of the present invention core is to occur to generate titanium dioxide nano thread after hydro-thermal reaction by means of titanous chloride single agents self, the Titanium Trichloride Solution that Yi Yuan factory produces (not making any dilution or concentration) is as starting raw material, Titanium Trichloride Solution is put into hydrothermal reaction kettle, hydrothermal reaction kettle is put into isothermal reaction case to react, after reaction finishes, hydrothermal reaction kettle is naturally cooled to room temperature, will after obtain sample cleaning, drying, can obtain titanium dioxide nano thread sample.
In the preparation method of titanium dioxide nano thread of the present invention, core reagent Titanium Trichloride Solution used, can there is hydrolysis generation titanium dioxide nucleus in titanous chloride under hydrothermal condition, there are hydrogen ion and chlorion product to generate simultaneously, thereby avoid the hydrochloric acid adding in traditional technology, the fast hydrolyzing that the hydrogen ion of dissociation suppresses titanous chloride generates unbodied titanium dioxide, and the chlorion of dissociation is adsorbed onto titanium dioxide nucleus and { on 110} face, makes it preferential along the reaction of [001] direction generation crystallographic orientation chemistry.Therefore the preparation method of titanium dioxide nano thread of the present invention can be realized by the Titanium Trichloride Solution of single agents the generation of nano wire.
Tool of the present invention has the following advantages:
(1) preparation method of the present invention, adopts Titanium Trichloride Solution as single agents, and the hydrogen ion and the chlorion that by titanous chloride self hydrolysis, generate replace the hydrochloric acid adding in traditional technology, thereby realize single agents autoreaction, generate titanium dioxide nano thread;
(2) preparation method of the present invention generates titanium dioxide nano thread by single agents autoreaction, avoided the proportioning of reagent in operating process to weigh, so the method technique is simple, easy handling is controlled, cost is low;
(3) preparation method of the present invention compares with the technique of the strong acid used of traditional technology in document and highly basic, avoided strong acid with highly basic, staff to be contacted in operating process potentially dangerous and the healthy effect that strong acid and highly basic cause the person, simultaneously relatively easy to reacted liquid waste disposal, so preparation method of the present invention is a kind of safety and environmental protection synthesis technique;
(4) preparation method of the present invention with respect to tradition the method with highly basic or strong acid Hydrothermal Synthesis titanium dioxide nano thread, avoid strong acid and highly basic to leak the damage to stove to the stainless corrosion damage of reactor shell and in reaction process, be conducive to reduce the cost depletions of equipment.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the titanium dioxide nano thread of preparation in the embodiment of the present invention 1;
Fig. 2 is the scanning electron microscope picture of the titanium dioxide nano thread of preparation in the embodiment of the present invention 1;
Fig. 3 is the scanning electron microscope picture of the titanium dioxide nano thread of preparation in the embodiment of the present invention 2, (a) is corresponding low range picture, is (b) corresponding high magnification picture;
Fig. 4 is the scanning electron microscope picture of the titanium dioxide nano thread of preparation in the embodiment of the present invention 3, and wherein (a) is corresponding low range picture, is (b) corresponding high magnification picture;
Fig. 5 is the scanning electron microscope picture of the titanium dioxide nano thread of preparation in the embodiment of the present invention 4, and wherein (a) is corresponding low range picture, is (b) corresponding high magnification picture;
Fig. 6 is the scanning electron microscope picture of the titanium dioxide nano thread of preparation in the embodiment of the present invention 5, and wherein (a) is corresponding low range picture, is (b) corresponding high magnification picture.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is further illustrated, but the scope of protection of present invention is lifted as the volume of reaction unit and temperature of reaction, reaction times and reaction liquid is not limited to embodiment.
(1) (manufacturer is Chemical Reagent Co., Ltd., Sinopharm Group to measure 5mL Titanium Trichloride Solution, quality percentage composition is 15～20%) without any dilution or concentrated being placed in 100mL reactor, conductive glass conducting surface is placed on to Polycondensation Reactor and Esterification Reactor induced nano line oriented growth upward, reactor is airtight high-temperature high-pressure reaction kettle, high-temperature high-pressure reaction kettle has metal shell, in metal shell, be provided with plastics or glass-lined, wherein plastics are tetrafluoroethylene, polyimide, the materials such as polybenzoate or PI polymeric amide, following examples are same, then after reactor being tightened, put in thermostat container, setting temperature of reaction is 150 ℃, reaction times is 12 hours, naturally cool to after completion of the reaction room temperature,
(2) after walking poly-(2) reactor and opening, the film that taking-up is deposited on conductive glass cleans for several times with deionized water and dehydrated alcohol, and be placed in thermostat container and dry 24 hours under 60 ℃ of conditions, the diffraction peak that synthetic sample is marked by Fig. 1 is all corresponding with titanium dioxide Rutile Type, and synthetic sample can see that by Fig. 2 the thickness forming for the nano wire by diameter 7～20 nanometers is about 2.8 microns of titanium dioxide nanowire arrays.
Embodiment 2
(1) (manufacturer is Chemical Reagent Co., Ltd., Sinopharm Group to measure 15mL Titanium Trichloride Solution, quality percentage composition is 15～20%) be placed in 100mL reactor, conductive glass conducting surface is placed on to Polycondensation Reactor and Esterification Reactor induction admittance rice noodles oriented growth upward, then after reactor being tightened, put in thermostat container, setting temperature of reaction is 150 ℃, reaction times is 12 hours, naturally cools to after completion of the reaction room temperature;
(2) after step (1) reactor is opened, the film that taking-up is deposited on conductive glass cleans for several times with deionized water and dehydrated alcohol, and be placed in thermostat container and dry 12 hours under 70 ℃ of conditions, synthetic sample can see that by Fig. 3 (a) thickness forming for nano wire is about 4 microns of titanium dioxide nanowire arrays, by Fig. 3 (b), can see the nanometer bundle that the nano wire by diameter 6～10nm forms.
Embodiment 3
(1) (manufacturer is Aladdin reagent (Shanghai) Co., Ltd. to measure 15mL Titanium Trichloride Solution, quality percentage composition is 15～20%) be placed in 100mL reactor, not putting as different from Example 1 conductive glass makes nano wire be orientated induced growth without array, then after reactor being tightened, put in thermostat container, setting temperature of reaction is 150 ℃, reaction times is 12 hours, naturally cools to after completion of the reaction room temperature;
(2) after step (1) reactor is opened, taking out sample cleans for several times with deionized water and dehydrated alcohol, and be placed in thermostat container and dry 24 hours under 60 ℃ of conditions, by Fig. 4 (a) with (b), low power and high power picture can find out that it is the micron ball of 5～10 microns that sample is about by diameter diameter that the nano wire of 6～10nm forms.
Embodiment 4
(1) (manufacturer is Chemical Reagent Co., Ltd., Sinopharm Group to measure 30mL Titanium Trichloride Solution, quality percentage composition is 15～20%) be placed in 100mL reactor, not putting as different from Example 1 conductive glass makes nano wire be orientated induced growth without array, then after reactor being tightened, put in thermostat container, setting temperature of reaction is 150 ℃, reaction times is 12 hours, naturally cools to after completion of the reaction room temperature;
(2) after step (1) reactor is opened, taking out sample cleans for several times with deionized water and dehydrated alcohol, and be placed in thermostat container and dry 24 hours under 50 ℃ of conditions, by Fig. 5 (a) with (b), low power and high power picture can find out that sample is about the micron ball of 1～10 micron of diameter that the nano wire of 6～10nm forms by diameter.
Embodiment 5
(1) (manufacturer is SIGMA-ALDRICH to measure 40mL Titanium Trichloride Solution, quality percentage composition is 12%) be placed in 100mL reactor, not putting as different from Example 1 conductive glass makes nano wire be orientated induced growth without array, then after reactor being tightened, put in thermostat container, setting temperature of reaction is 200 ℃, reaction times is 12 hours, naturally cools to after completion of the reaction room temperature;
(2) after step (1) reactor is opened, taking out sample cleans for several times with deionized water and dehydrated alcohol, and be placed in thermostat container and dry 24 hours under 60 ℃ of conditions, synthetic sample can see by Fig. 6 (a) micron ball that titanium dioxide nano thread forms, and because stress fracture becomes the aggregate of nano wire, by Fig. 6 (b), can see that the diameter of nano wire is about 10～20nm.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, be included in protection scope of the present invention.
Claims (6)
1. single agents autoreaction is prepared a method for titanium dioxide nano thread, it is characterized in that containing following steps:
(1) get Titanium Trichloride Solution as starting raw material, Titanium Trichloride Solution is put into hydrothermal reaction kettle, then put into thermostat container, regulating temperature of reaction is 90～230 ℃, and the reaction times is 1～100 hour, is cooled to room temperature after reaction;
(2) take out the sample in reactor, after cleaning, drying, obtain titanium dioxide nano thread.
2. single agents autoreaction according to claim 1 is prepared the method for titanium dioxide nano thread, it is characterized in that: in step (1), the quality percentage composition of Titanium Trichloride Solution is 8%～30%, and Titanium Trichloride Solution volume accounts for 5%～80% of reactor cumulative volume.
3. single agents autoreaction according to claim 1 is prepared the method for titanium dioxide nano thread, it is characterized in that: described in step (1), hydrothermal reaction kettle is airtight high-temperature high-pressure reaction kettle, described high-temperature high-pressure reaction kettle has metal shell, is provided with heat-resisting and corrosion-resistant plastic or glass-lined in metal shell.
4. single agents autoreaction according to claim 3 is prepared the method for titanium dioxide nano thread, it is characterized in that: described heat-resisting and corrosion-resistant plastic is tetrafluoroethylene, polyimide, polybenzoate or PI polymeric amide.
5. single agents autoreaction according to claim 1 is prepared the method for titanium dioxide nano thread, it is characterized in that: in step (2), clean as adopting deionized water and dehydrated alcohol successively to wash for several times.
6. single agents autoreaction according to claim 1 is prepared the method for titanium dioxide nano thread, it is characterized in that: the temperature while drying in step (2) is 50～70 ℃, and drying time is 5～48h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104229879A (en) * | 2014-09-02 | 2014-12-24 | 陈立晓 | Preparation method of rutile titanium dioxide nano powder |
| CN104528754A (en) * | 2014-11-17 | 2015-04-22 | 山东玉皇新能源科技有限公司 | Synthesis method of nanorod-shaped AlPO4-15 |
| CN105006370A (en) * | 2015-06-23 | 2015-10-28 | 南京航空航天大学 | Method for in-situ preparing CZTS counter electrode by means of solvent thermal and application of CZTS counter electrode |
| CN108264087A (en) * | 2018-03-16 | 2018-07-10 | 中国科学院广州地球化学研究所 | A kind of single agents autoreaction, which prepares to have, aligns Nb2O5The method of nanometer rods |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701277A (en) * | 2012-06-18 | 2012-10-03 | 山东轻工业学院 | Method for preparing rutile titanium dioxide |
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2013
- 2013-08-23 CN CN201310373400.2A patent/CN103539202B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701277A (en) * | 2012-06-18 | 2012-10-03 | 山东轻工业学院 | Method for preparing rutile titanium dioxide |
Non-Patent Citations (1)
| Title |
|---|
| EIJI HOSONO ET AL.: "Growth of Submicrometer-Scale Rectangular Parallelepiped Rutile TiO2 Films in Aqueous TiCl3 Solutions under Hydrothermal Conditions", 《J. AM. CHEM. SOC.》, vol. 126, no. 25, 8 June 2004 (2004-06-08), pages 7790 - 7791 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104229879A (en) * | 2014-09-02 | 2014-12-24 | 陈立晓 | Preparation method of rutile titanium dioxide nano powder |
| CN104528754A (en) * | 2014-11-17 | 2015-04-22 | 山东玉皇新能源科技有限公司 | Synthesis method of nanorod-shaped AlPO4-15 |
| CN104528754B (en) * | 2014-11-17 | 2016-08-24 | 山东玉皇新能源科技有限公司 | A kind of nano bar-shape AlPO4the synthetic method of-15 |
| CN105006370A (en) * | 2015-06-23 | 2015-10-28 | 南京航空航天大学 | Method for in-situ preparing CZTS counter electrode by means of solvent thermal and application of CZTS counter electrode |
| CN108264087A (en) * | 2018-03-16 | 2018-07-10 | 中国科学院广州地球化学研究所 | A kind of single agents autoreaction, which prepares to have, aligns Nb2O5The method of nanometer rods |
| CN108264087B (en) * | 2018-03-16 | 2020-05-05 | 中国科学院广州地球化学研究所 | Single reagent self-reaction preparation of Nb with directional arrangement2O5Method for producing nano-rod |
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