CN102485968A - Preparation method of zinc-doped titanium dioxide nano-tube array - Google Patents
Preparation method of zinc-doped titanium dioxide nano-tube array Download PDFInfo
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- CN102485968A CN102485968A CN2010105734200A CN201010573420A CN102485968A CN 102485968 A CN102485968 A CN 102485968A CN 2010105734200 A CN2010105734200 A CN 2010105734200A CN 201010573420 A CN201010573420 A CN 201010573420A CN 102485968 A CN102485968 A CN 102485968A
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Abstract
The invention belongs to the technical field of photoelectric materials and specially, relates to a preparation method of a zinc-doped titanium dioxide nano-tube array. The preparation method comprises the following steps that 1, an electrolyte of a HF aqueous solution having HF content of 0.3 to 1.0 wt%, an anode of pure titanium foil subjected to surface pretreatment and a cathode of a Pt sheet undergo an electrochemical anodization reaction under direct voltage of 10 to 50V to produce a titanium dioxide nano-tube array; and the titanium dioxide nano-tube array as a cathode, an anode of a platinum sheet and an electrolyte of a Zn(NO3) solution having concentration of 0.1 to 0.5mol/L undergo an electrochemical deposition reaction under direct voltage of 0.3 to 1.0V so that zinc is added into titanium dioxide nano-tube layers and the zinc-doped titanium dioxide nano-tube array is obtained. The preparation method provided by the invention has the advantages that ion implantation time is short; and doped ions Zn<2+> can enter into a titanium dioxide nano-tube under a electric field force and capillary action so that the zinc-doped titanium dioxide nano-tube array having good photoelectric properties and a light absorption range widen to a visible light range is prepared.
Description
Technical field
The invention belongs to the photovaltaic material technical field; Be specifically related to a kind of method of utilizing anonizing to prepare the zinc doping Nano tube array of titanium dioxide, particularly relate to a kind of method of preparing the good zinc doping Nano tube array of titanium dioxide of photoelectric properties through follow-up electrochemical deposition method.
Background technology
Titanium oxide is a kind of important inorganic functional material; Its aspect such as pollutent in the storage of sun power and utilization, opto-electronic conversion, the photochromic and big G&W of photocatalytic degradation has broad application prospects; Because of its raw material resources is abundant, low price; And toxicological harmless is the focus of studying in the world in recent years.Titanium oxide mainly contains anatase octahedrite, rutile and three kinds of crystal formations of unsettled brookite; Because crystal formation is different; The energy gap of titanium oxide is distributed in about 3.0～3.2, can only absorb to account in the solar spectral 3～5% ultraviolet portion, and visible light is not almost absorbed.The Nano tube array of titanium dioxide of ordered arrangement has tangible quantum confined effect, high-sequential oriented structure and big specific surface area; Can improve the interfacial separation in electronics-hole and the directional transmissions efficient of current carrier effectively, make it important application prospects arranged in technical fields such as dye-sensitized cell, light () catalyzing and degrading pollutant, transmitters.
The main method that present preparation doped titanium dioxide nanotube array is taked has electrolysis modification method, pickling process etc.In these methods, electrolytic solution modification method has changed charge migration speed in the electrolytic solution because of the adding of metals ion, and electric current is increased, and part ion and F
-Complex reaction takes place, and has reduced F in the electrolytic solution
-Concentration is unfavorable for reacting and carries out, and does not therefore possess ubiquity; In the pickling process modification, ion implantation main drive is a capillary action, this method length consuming time, and ion is difficult for entering into titania nanotube.Therefore the present invention proposes a kind of new ion injection method comes titania nanotube is carried out doping vario-property; It is follow-up electrochemical deposition method; Make ion under the dual function of kapillary and electrical forces, effectively be injected into titania nanotube inside; Can come the existing way of controlled doping amount and dopant ion through the regulation and control to dopant ion concentration and deposition voltage, be a kind of effective doping modification method.
Summary of the invention
The technical problem that the present invention will solve provides the preparation method of the good zinc doping Nano tube array of titanium dioxide of a kind of photoelectric properties; This method technical process is simple, clean environment firendly; Be fit to batch preparations, with low cost, the zinc doping titania nanotube size that makes and uniform diameter is controlled, thermostability and photoelectric properties are good, can be widely used in field of photovoltaic materials.
For solving the problems of the technologies described above, the invention provides the preparation method of the good zinc doping Nano tube array of titanium dioxide of a kind of photoelectric properties, comprise the steps:
(1) pure titanium foil is polished to surperficial no marking, clean up subsequent use;
(2) preparing electrolyte: electrolytic solution is the hydrofluoric acid hydrofluoric acid of 40wt% and the mixing solutions of deionized water preparation by HF content, and the content of HF is 0.3wt%-1.0wt% in the electrolytic solution;
(3) with surface treated pure titanium foil as anode; Platinized platinum connects D.C. regulated power supply as negative electrode, in HF electrolytic solution, carries out electrochemical anodic oxidation; Keeping the spacing between the two poles of the earth is 20-50mm; Anodic oxidation voltage is 10-50V, and oxidization time is 1-4h, makes unformed Nano tube array of titanium dioxide;
(4) preparation of zinc doping Nano tube array of titanium dioxide: unformed Nano tube array of titanium dioxide is done negative electrode, and platinized platinum is an anode, with the Zn (NO of 0.1-0.5mol/L
3)
2Solution is electrolytic solution, under the volts DS of 0.3-1.0V, carries out electrochemical deposition 20-60min, Zn
2+Electrical forces with wicking action under enter into titania nanotube;
(5) will put into retort furnace through the Nano tube array of titanium dioxide of electro-chemical deposition process, cycle annealing 2-4h under 450-600 ℃ of condition promptly gets the zinc doping Nano tube array of titanium dioxide.
Said anodised best volts DS is 20-40V.
The best volts DS of said electrochemical deposition is 0.4-0.7V, Zn (NO in the electrolytic solution
3)
2Optimum concn be 0.1-0.3mol/L.
The invention provides a kind of preparation method of zinc doping Nano tube array of titanium dioxide, when voltage is lower, oxidization time makes the nanotube marshalling, even aperture distribution more in short-term; When deposition voltage is low, depositing time can get the higher zinc doping titania nanotube of photoelectric activity more in short-term; Calcining temperature is low more, and the pore size distribution of the zinc doping titania nanotube of formation is even more, and has the surface of good pattern.
Major advantage of the present invention:
Compare with the method for the metal-doped Nano tube array of titanium dioxide of existing preparation, the present invention has adopted a kind of new doping way, promptly through follow-up electrochemical deposition method Nano tube array of titanium dioxide is carried out doping vario-property, can make Zn
2+Under capillary action and electrical forces dual function, enter into titania nanotube inside; Can make Zn through regulation and control to volts DS in the electrochemical deposition process
2+Incorporation and the existing way in nanotube thereof realize controlled; Prepared titania nanotube is evenly distributed, and marshalling directly links to each other with the metal titanium substrate, in conjunction with firm; Nano tube array of titanium dioxide has ordered structure and very high quantum effect; The sample of preparation is compared with the zinc doping Nano tube array of titanium dioxide for preparing through the electrolytic solution modification, have more excellent photoelectric performance, can be widely used in photoelectrocatalysis and field of dye-sensitized solar cells.
Description of drawings
Fig. 1 is the sem photograph of zinc doping Nano tube array of titanium dioxide
The sem photograph of zinc doping Nano tube array of titanium dioxide of the present invention is to adopt JEOL JSM-6700F sem, is 3.0KV at acceleration voltage, and magnification is to take under the condition of 30000 times (a) and 150000 times (b).
Fig. 2 is the X ray diffracting spectrum of Nano tube array of titanium dioxide
The X ray diffracting spectrum of zinc doping Nano tube array of titanium dioxide of the present invention is to adopt SEMENS D5000X x ray diffractometer x, and test condition: target is Cu; Tube voltage 35KV, tube current 30mA, sweep limit is 10 °～80 °; 0.02 ° of scanning step, integral time 0.2s.Fig. 2 (a) is the X ray diffracting spectrum of pure titinium dioxide nano-tube array, and Fig. 2 (b) is the X ray diffracting spectrum of zinc doping nano titania array pipe.
Embodiment
Through specific embodiment, further specify the preparation method of zinc doping Nano tube array of titanium dioxide below.
Embodiment 1:
(1) pure titanium foil is polished to surperficial no marking, clean up subsequent use;
(2) preparing electrolyte: electrolytic solution is to be the mixing solutions of hydrofluoric acid and the deionized water preparation of 40wt% by HF content, and the content of HF is 0.3wt% in the electrolytic solution;
(3) under the 20V volts DS, be anode with the pure titanium foil, platinized platinum is a negative electrode, and keeping the spacing between the two poles of the earth is 30mm, in electrolytic solution, carries out anodic oxidation, and oxidization time is 4h, makes unformed Nano tube array of titanium dioxide;
(4) preparation of zinc doping Nano tube array of titanium dioxide: the Nano tube array of titanium dioxide with above preparation is done negative electrode, and platinized platinum is an anode, with the Zn (NO of 0.1mol/L
3)
2Solution is electrolytic solution, under the volts DS of 0.4V, carries out electrochemical deposition 60min;
The Nano tube array of titanium dioxide that (5) will pass through electro-chemical deposition process is put into retort furnace, and cycle annealing 2h under 450 ℃ of conditions promptly gets the zinc doping Nano tube array of titanium dioxide.
Embodiment 2:
(1) pure titanium foil is polished to surperficial no marking, clean up subsequent use;
(2) preparing electrolyte: electrolytic solution is to be the mixing solutions of hydrofluoric acid and the deionized water preparation of 40wt% by HF content, and the content of HF is 0.5wt% in the electrolytic solution;
(3) under the 30V volts DS, be anode with the pure titanium foil, platinized platinum is a negative electrode, and keeping the spacing between the two poles of the earth is 40mm, in electrolytic solution, carries out anodic oxidation, and oxidization time is 3h, makes unformed Nano tube array of titanium dioxide;
(4) preparation of zinc doping Nano tube array of titanium dioxide: the Nano tube array of titanium dioxide with above preparation is done negative electrode, and platinized platinum is an anode, with the Zn (NO of 0.2mol/L
3)
2Solution is electrolytic solution, under the volts DS of 0.6V, carries out electrochemical deposition 30min;
The Nano tube array of titanium dioxide that (5) will pass through electro-chemical deposition process is put into retort furnace, and cycle annealing 2h under 450 ℃ of conditions promptly gets the zinc doping Nano tube array of titanium dioxide.
Embodiment 3:
(1) pure titanium foil is polished to surperficial no marking, clean up subsequent use;
(2) preparing electrolyte: electrolytic solution is to be the mixing solutions of hydrofluoric acid and the deionized water preparation of 40wt% by HF content, and the content of HF is 0.7wt% in the electrolytic solution;
(3) under the 40V volts DS, be anode with the pure titanium foil, platinized platinum is a negative electrode, and keeping the spacing between the two poles of the earth is 50mm, in electrolytic solution, carries out anodic oxidation, and oxidization time is 2h, makes unformed Nano tube array of titanium dioxide;
(4) preparation of zinc doping Nano tube array of titanium dioxide: the Nano tube array of titanium dioxide with above preparation is done negative electrode, and platinized platinum is an anode, with the Zn (NO of 0.3mol/L
3)
2Solution is electrolytic solution, under the volts DS of 0.5V, carries out electrochemical deposition 60min;
The Nano tube array of titanium dioxide that (5) will pass through electro-chemical deposition process is put into retort furnace, and cycle annealing 2h under 600 ℃ of conditions promptly gets the zinc doping Nano tube array of titanium dioxide.
Embodiment 4:
(1) pure titanium foil is polished to surperficial no marking, clean up subsequent use;
(2) preparing electrolyte: electrolytic solution is to be the mixing solutions of hydrofluoric acid and the deionized water preparation of 40wt% by HF content, and the content of HF is 1.0wt% in the electrolytic solution;
(3) under the 50V volts DS, be anode with the pure titanium foil, platinized platinum is a negative electrode, and keeping the spacing between the two poles of the earth is that 40mm carries out anodic oxidation in electrolytic solution, and oxidization time is 2h, makes unformed Nano tube array of titanium dioxide;
(4) preparation of zinc doping Nano tube array of titanium dioxide: the Nano tube array of titanium dioxide with above preparation is done negative electrode, and platinized platinum is an anode, with the Zn (NO of 0.5mol/L
3)
2Solution is electrolytic solution, under the volts DS of 0.7V, carries out electrochemical deposition 30min;
The Nano tube array of titanium dioxide that (5) will pass through electro-chemical deposition process is put into retort furnace, and cycle annealing 3h under 450 ℃ of conditions promptly gets the zinc doping Nano tube array of titanium dioxide.
Embodiment 5:
(1) pure titanium foil is polished to surperficial no marking, clean up subsequent use;
(2) preparing electrolyte: electrolytic solution is to be the mixing solutions of hydrofluoric acid and the deionized water preparation of 40wt% by HF content, and the content of HF is 0.5wt% in the electrolytic solution;
(3) under the 20V volts DS, be anode with the pure titanium foil, platinized platinum is a negative electrode, and keeping the spacing between the two poles of the earth is that 30mm carries out anodic oxidation in electrolytic solution, and oxidization time is 2h, makes unformed Nano tube array of titanium dioxide;
(4) preparation of zinc doping Nano tube array of titanium dioxide: the Nano tube array of titanium dioxide with above preparation is done negative electrode, and platinized platinum is an anode, with the Zn (NO of 0.3mol/L
3)
2Solution is electrolytic solution, under the volts DS of 0.6V, carries out electrochemical deposition 60min;
The Nano tube array of titanium dioxide that (5) will pass through electro-chemical deposition process is put into retort furnace, and cycle annealing 4h under 600 ℃ of conditions promptly gets the zinc doping Nano tube array of titanium dioxide.
Claims (3)
1. an anonizing prepares the method for zinc doping Nano tube array of titanium dioxide, it is characterized in that following step:
(1) pure titanium foil is polished to surperficial no marking, clean up subsequent use;
(2) preparing electrolyte: electrolytic solution is to be hydrofluoric acid and the formulated mixing solutions of deionized water of 40wt% by HF content, and the content of HF is 0.3wt%-1.0wt% in the electrolytic solution;
(3) under the 10-50V volts DS, be anode with the pure titanium foil, platinized platinum is a negative electrode, and keeping the spacing between the two poles of the earth is 20-50mm, in electrolytic solution, carries out anodic oxidation reactions, and reaction 1-4h makes unformed Nano tube array of titanium dioxide;
(4) preparation of zinc doping Nano tube array of titanium dioxide: the Nano tube array of titanium dioxide with above preparation is done negative electrode, and platinized platinum is an anode, with the Zn (NO of 0.1-0.5mol/L
3)
2Solution is electrolytic solution, under the volts DS of 0.3-1.0V, carries out electrochemical deposition 20-60min, Zn
2+Under electrical forces and wicking action, enter into the titania nanotube internal layer;
(5) in retort furnace with 450-600 ℃ of cycle annealing 2-4h, promptly get the zinc doping Nano tube array of titanium dioxide.
2. method according to claim 1 is characterized in that described anodic oxidation voltage is 10-50V.
3. method according to claim 1 is characterized in that being 0.3-1.0V with titania nanotube that makes and the exchange of titanium sheet anode and cathode at volts DS, and concentration is the Zn (NO of 0.1-0.5mol/L
3)
2Carry out electrochemical deposition in the solution.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102485969A (en) * | 2010-12-06 | 2012-06-06 | 长沙理工大学 | Method for preparing nitrogen and gadolinium co-doped titania nano-tube array |
| CN102826630A (en) * | 2012-09-09 | 2012-12-19 | 桂林理工大学 | Application of Bi/TiO2 nanotube array to photocatalytic degradation of sugar manufacturing wastewater |
| CN102980915A (en) * | 2012-11-08 | 2013-03-20 | 清华大学 | Preparation method of palladium-doped TiO2 nano-tube array Schottky junction hydrogen-sensitive sensor |
| CN103774198A (en) * | 2014-01-15 | 2014-05-07 | 浙江大学 | Method for preparing rare-soil Eu-doped CaF2 film on titanium dioxide nano tube by light-assisted electrodeposition method |
| CN103866370A (en) * | 2012-12-11 | 2014-06-18 | 中国科学院上海硅酸盐研究所 | Method for preparing low-oxygen titania nanotube array |
| CN107083151A (en) * | 2017-05-19 | 2017-08-22 | 重庆中鼎三正科技有限公司 | Method for preparing degraded catalysis material |
| CN107129734A (en) * | 2017-05-19 | 2017-09-05 | 重庆中鼎三正科技有限公司 | The preparation method of composite photocatalyst material |
| CN108620112A (en) * | 2018-04-02 | 2018-10-09 | 华南理工大学 | A kind of preparation method of the composite mixed film of Nano tube array of titanium dioxide of Zn-N with visible light activity |
| CN112162020A (en) * | 2020-10-09 | 2021-01-01 | 浙江科技学院 | Preparation method of high-performance hydrogen sulfide gas sensor free from humidity influence |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102485969A (en) * | 2010-12-06 | 2012-06-06 | 长沙理工大学 | Method for preparing nitrogen and gadolinium co-doped titania nano-tube array |
| CN102485969B (en) * | 2010-12-06 | 2016-03-23 | 长沙理工大学 | The preparation method of nitrogen, gadolinium codope titanium dioxide nanotube array |
| CN102826630A (en) * | 2012-09-09 | 2012-12-19 | 桂林理工大学 | Application of Bi/TiO2 nanotube array to photocatalytic degradation of sugar manufacturing wastewater |
| CN102980915A (en) * | 2012-11-08 | 2013-03-20 | 清华大学 | Preparation method of palladium-doped TiO2 nano-tube array Schottky junction hydrogen-sensitive sensor |
| CN103866370A (en) * | 2012-12-11 | 2014-06-18 | 中国科学院上海硅酸盐研究所 | Method for preparing low-oxygen titania nanotube array |
| CN103866370B (en) * | 2012-12-11 | 2016-05-18 | 中国科学院上海硅酸盐研究所 | A kind of method of preparing hypoxemia titania nanotube array |
| CN103774198A (en) * | 2014-01-15 | 2014-05-07 | 浙江大学 | Method for preparing rare-soil Eu-doped CaF2 film on titanium dioxide nano tube by light-assisted electrodeposition method |
| CN107083151A (en) * | 2017-05-19 | 2017-08-22 | 重庆中鼎三正科技有限公司 | Method for preparing degraded catalysis material |
| CN107129734A (en) * | 2017-05-19 | 2017-09-05 | 重庆中鼎三正科技有限公司 | The preparation method of composite photocatalyst material |
| CN108620112A (en) * | 2018-04-02 | 2018-10-09 | 华南理工大学 | A kind of preparation method of the composite mixed film of Nano tube array of titanium dioxide of Zn-N with visible light activity |
| CN112162020A (en) * | 2020-10-09 | 2021-01-01 | 浙江科技学院 | Preparation method of high-performance hydrogen sulfide gas sensor free from humidity influence |
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Application publication date: 20120606 |