CN106086991B - A kind of controlling type metal ion doping TiO in situ2The preparation method of nano-tube array - Google Patents

A kind of controlling type metal ion doping TiO in situ2The preparation method of nano-tube array Download PDF

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CN106086991B
CN106086991B CN201610693640.4A CN201610693640A CN106086991B CN 106086991 B CN106086991 B CN 106086991B CN 201610693640 A CN201610693640 A CN 201610693640A CN 106086991 B CN106086991 B CN 106086991B
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tube array
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CN106086991A (en
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汤丁丁
史德亮
李亚龙
刘凤丽
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Changjiang River Scientific Research Institute Changjiang Water Resources Commission
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/26—Anodisation of refractory metals or alloys based thereon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Abstract

The present invention relates to controlling type metal ion doping TiO in situ2The preparation method of nano-tube array, comprises the following steps：1) using titanium alloy piece or titanium alloy bar as anode, Pt pieces or Pt rods are negative electrode, and metal ion doping TiO in situ is prepared in fluorine-containing solution Anodic Oxidation2Nano-tube array, cleaning sample；2) by choosing appropriate acid or aqueous slkali, using ultrasonic wave added selectivity acid or alkali soluble solution leaching section metal ion, the quantitatively regulating and controlling of metal ion content in nano-tube array is realized；3) cleaned after the completion of regulating and controlling, drying to obtain controlling type metal ion original position doping TiO2Nano-tube array.The advantages of the present invention are：Using titanium alloy as base material, not only simplify metal ion mixing TiO2The preparation technology of nano-tube array, also make Doped ions scattered evenly；Metal ion mixing amount convenient can controllably be adjusted using ultrasonic wave added Selective dissolution method, reliable method is provided for the excellent catalyst of processability.

Description

A kind of controlling type metal ion doping TiO in situ2The preparation method of nano-tube array
Technical field
The invention belongs to field of nano material preparation, is related to a kind of controlling type metal ion doping TiO in situ2Nanotube battle array The preparation method of row.
Background technology
TiO2Nano-tube array has excellent light (electricity) catalytic activity and chemical stability, is widely used in light (electricity) and urges Change the fields such as production hydrogen, light (electricity) catalysis treatment environmental contaminants and solar cell.It is relatively low that energy is formed after metal ion mixing Doped energy-band to absorb visible ray, widen spectral response range, while can also be in TiO2Surface forms Lacking oxygen, promotes Ti3 +The formation of oxidation center, is advantageous to electric charge capture and to suppress electron-hole compound, lifts photo-quantum efficiency.At present, metal from Son doping TiO2Nano-tube array mainly using conventional later stage incorporation way, i.e., first prepares TiO2Nano-tube array, then passing through Metal ion is introduced to TiO by the methods of or electrochemistry2Nano-tube array surface.But it is difficult following two aspect to be present in which Topic：
1.TiO2Nano-tube array ttom of pipe is enclosed construction, and metal ion enters from the mouth of pipe, by diffusion into pipe Input, because solution lacks mobility in pipe, metal ion easily forms concentration difference during diffusing to ttom of pipe, makes orifice region Metal ion solubility is higher, and deposition is also more, and the metal ion solubility close to ttom of pipe region is relatively low, deposits also less, metal Ion concentration difference, which causes, adulterates uneven phenomenon；
2.TiO2Nano-tube array structure is fine and close, and space is very small between Guan Yuguan, and pipe outer wall is difficult to effective adhesion metal Oxide.
These two aspects problem causes most of metal oxide to concentrate at tube opening, and degree of scatter is poor, at tube opening It is preferable to adulterate effect, but is gradually reduced with effect is adulterated in the extension of pipe range, and pipe outer wall is difficult to adulterate.In recent years, Researchers are using introducing method in advance to TiO2Nano-tube array carries out metal ion mixing, achieves good effect.The party Method makees electrolytic anode with titanium alloy instead of pure titanium, introduces doping metals in advance, is prepared for the TiO of metal ion doping in situ2Receive Mitron array.But the metal-doped amount introduced in advance is mainly determined by titanium alloy component, therefore there is metal ion and mix in this method Miscellaneous ratio is difficult to the problem of regulation and control.Numerous researchs show that doping ratio is metal ion-modified TiO2Photocatalysis performance it is decisive One of factor.21 metal ion species of the different doping ratios (0.1-3at%) of such as Choi system researches are to TiO2Photocatalysis The influence of activity, finds in addition to the metal ion without modified effect, nano-TiO2Photocatalysis performance with metal ion mixing ratio The increase of example, shows first to rise the parabolic type changing rule declined afterwards, and research thinks that doping needs to control suitable Ratio (about 0.5at%), the very few effect that can not give full play to doping of ratio, substantial amounts of fault of construction, shape can at most be caused by crossing Into the complex centre of electron-hole.The examens such as L ó pez different proportion (0.1-5wt%) Cu dopen Nanos TiO2Property Can, finding 0.5wt% doping ratio has the doping ratio effect phase of optimal photocatalysis performance, 1wt% and 0.1wt% When more excessive doping can cause the degeneration of performance.Universal higher, the nanotube prepared therefrom of alloying component content in titanium alloy Array may there is also the problem of metal ion mixing excess.Therefore, doping TiO in situ to metal ion2Nano-tube array enters Row reprocessing, to optimize the doping ratio of metal ion, the optimization of photocatalysis performance can be achieved.
The content of the invention
The technical problems to be solved by the invention are to provide that a kind of cost is low, the simple controlling type metal ion of technique is in situ Adulterate TiO2The preparation method of nano-tube array.
Technical scheme is used by the present invention solves above-mentioned technical problem：A kind of doping in situ of controlling type metal ion TiO2The preparation method of nano-tube array, comprises the following steps：
1) using titanium alloy piece or titanium alloy bar as anode, Pt pieces or Pt rods are negative electrode, in fluorine-containing solution Anodic Oxidation system Standby metal ion doping TiO in situ2Nano-tube array, cleaning sample；
2) using the chemical property difference of doping metals and Ti, by choosing appropriate acid or aqueous slkali, and accurately control Leaching condition, using ultrasonic wave added selectivity acid or alkali soluble solution leaching section metal ion, realize metal in nano-tube array The quantitatively regulating and controlling of ion concentration；
3) cleaned after the completion of regulating and controlling, drying to obtain controlling type metal ion original position doping TiO2Nano-tube array.
By such scheme, the voltage of the anodic oxidation described in step 1) is 5-50V, and temperature is 20-50 DEG C, the time 30 min-4h。
By such scheme, the ultrasonic frequency that the ultrasonic wave added described in step 2) uses is 30-60KHz.
By such scheme, the solution temperature described in step 2) is 20-60 DEG C, dissolution time 20min-4h.
By such scheme, described titanium alloy be TA5, TA6, TA7, TA10, TA11, TA12, TA13, TA14, TA15, TA16、TA17、TA18、TA19、TA20、TA21、TA22、TA23、TA24、TA25、TA26、 TA28、TB2、TB3、TB4、TB5、 TB6、TB7、TB8、TB9、TB10、TB11、TC1、TC2、 TC3、TC4、TC6、TC8、TC9、TC10、TC11、TC15、TC16、 TC17, TC18, TC19, TC20, TC21, TC22, TC23, TC24, TC25 or TC26.
By such scheme, described fluorine-containing solution is organic solution or the inorganic solution of hydrofluoric acid containing containing ammonium fluoride.
By such scheme, described fluorine-containing solution is the water of the ethylene glycol containing ammonium fluoride, glycerin solution or hydrofluoric acid containing Solution.
By such scheme, described metal ion original position be doped to Al, Cu, Fe, Sn, V, Cr, Mo, Nb, Mn, Ni, Zr, Single ionic doping or different kinds of ions codope in Ta, W, Nd, Ru and Pd ion.
By such scheme, described acid solution is HCl, H2SO4、HNO3Or H3PO4Solution, described aqueous slkali be NaOH, KOH、Ca(OH)2Or Mg (OH)2Solution.
By such scheme, the acid solution pH added is 1-4, and it is 10-13 that the aqueous slkali added, which controls pH,.
The present invention uses titanium alloy to realize more excellent metal ion mixing effect for base material shell, to realize metal ion Regulation and control, while keep the structure of nano-tube array not to be destroyed, gentle ultrasonic wave added Selective dissolution method is developed first to be adjusted Metal ion content is controlled, under the ultrasonic assistant of lower frequency, suitable acid or aqueous slkali can go deep into inside nanotube, can The dissolution metal ion of control, realize controlling type metal ion doping TiO in situ2The preparation of nano-tube array.
The advantages of the present invention are：
1. using titanium alloy as base material, not only simplify metal ion mixing TiO2The preparation technology of nano-tube array, also make to mix Heteroion is scattered evenly；
It is that processability is excellent 2. convenient can controllably adjust metal ion mixing amount using ultrasonic wave added Selective dissolution method Good catalyst provides reliable method.
Embodiment
With reference to embodiment, the present invention will be further described in detail, and this explanation will not form the limit for the present invention System.
Embodiment 1
The TA5 alloy sheets that thickness is 2mm are cut to 2 × 8cm2Strip, polished by sand paper and made after being cleaned by ultrasonic Stand-by anode, using identical size Pt pieces as negative electrode and prepare water containing 2wt%, 0.3wt% ammonium fluorides ethylene glycol solution be electrolysed Matter.Electrolytic process uses two electrode DC electrolysis systems, voltage 50V, and temperature is 20 DEG C, time 30min.After the completion of electrolysis With the residual liquid of deionized water rinsing anode surface, then it is 30KHz frequencies in 1 HCl solution to be impregnated in the pH of 20 DEG C of constant temperature Take out after ultrasonic 2h under rate and rinsed well with deionized water, obtain the TiO of 1.5wt%Al ion dopings2Nano-tube array.Will The nano-tube array and conventional TiO2Nano-tube array is 10mg/L methyl blue solutions applied to the initial solubility of ultraviolet degradation, by In 1.5wt% Al ion dopings, contrast finds the Methyl blueness efficiency of the nano-tube array better than routine TiO2Nano-tube array, the remaining solubility of methyl blue solution is respectively 1.0mg/L and 1.3mg/L after 2h degradeds.
Embodiment 2
A diameter of 2cm TA6 alloy bars are cut to long 8cm corynebacterium, is polished by sand paper and treated after being cleaned by ultrasonic With anode, with 2 × 8cm2Pt pieces for negative electrode and prepare water containing 2wt%, the glycerin solution of 0.3wt% ammonium fluorides and be electrolysed Matter.Electrolytic process uses two electrode DC electrolysis systems, voltage 40V, and temperature is 30 DEG C, time 1h.Used after the completion of electrolysis The residual liquid of deionized water rinsing anode surface, then be impregnated in 30 DEG C of constant temperature pH be 3 H3PO4In solution, 30KHz frequencies Take out after lower ultrasonic 4h and rinsed well with deionized water, obtain 2wt%Al ions and the ion co-doped TiO of 1wt%Sn2Nanometer Pipe array.By the nano-tube array and conventional TiO2Nano-tube array is 10mg/L first applied to the initial solubility of ultraviolet degradation Base indigo plant solution, because 2wt% Al ions and 1wt% Sn are ion co-doped, contrast finds the photocatalysis of the nano-tube array Methyl blue efficiency degrade better than conventional TiO2Nano-tube array, the remaining solubility of methyl blue solution is respectively after 2h degradeds 0.9mg/L and 1.3mg/L.
Embodiment 3
The TA10 alloy sheets that thickness is 2mm are cut to 2 × 8cm2Strip, polished by sand paper and made after being cleaned by ultrasonic Stand-by anode, using identical size Pt pieces as negative electrode and prepare water containing 2wt%, 0.3wt% ammonium fluorides ethylene glycol solution be electrolysed Matter.Electrolytic process uses two electrode DC electrolysis systems, voltage 30V, and temperature is 40 DEG C, time 2h.Used after the completion of electrolysis The residual liquid of deionized water rinsing anode surface, then be impregnated in 40 DEG C of constant temperature pH be 4 H2SO4In solution, 40KHz frequencies Take out after lower ultrasonic 20min and rinsed well with deionized water, obtain 0.2wt%Mo ions and 0.5wt%Ni is ion co-doped TiO2Nano-tube array.By the nano-tube array and conventional TiO2Nano-tube array is applied to the initial solubility of ultraviolet degradation 10mg/L methyl blue solutions, because 0.2wt% Mo ions and 0.5wt% Ni are ion co-doped, contrast finds the nanotube The Methyl blueness efficiency of array is better than conventional TiO2Nano-tube array, methyl blue solution is remaining molten after 2h degradeds Degree is respectively 0.5mg/L and 1.3mg/L.
Embodiment 4
The TA11 alloy sheets that thickness is 2mm are cut to 2 × 8cm2Strip, polished by sand paper and made after being cleaned by ultrasonic Stand-by anode, using identical size Pt pieces as negative electrode and prepare water containing 2wt%, 0.3wt% ammonium fluorides ethylene glycol solution be electrolysed Matter.Electrolytic process uses two electrode DC electrolysis systems, voltage 20V, and temperature is 50 DEG C, time 3h.Used after the completion of electrolysis The residual liquid of deionized water rinsing anode surface, then the pH of 50 DEG C of constant temperature is impregnated in as in 12 NaOH solution, 50KHz is frequently Under rate after ultrasonic 2h take out and rinsed well with deionized water, obtain 1.5wt%Al ions, 0.4wt%Mo and 0.3wt%V from Sub- codope TiO2Nano-tube array.
Embodiment 5
The TA13 alloy sheets that thickness is 2mm are cut to 2 × 8cm2Strip, polished by sand paper and made after being cleaned by ultrasonic Stand-by anode, electrolyte is made using the aqueous solution of identical size Pt pieces ammonium fluoride containing 0.3wt% as negative electrode and preparation.Electrolytic process is adopted With two electrode DC electrolysis systems, voltage 10V, temperature is 30 DEG C, time 1h.With deionized water rinsing sun after the completion of electrolysis The residual liquid on pole surface, then be impregnated in 60 DEG C of constant temperature pH be 4 HCl solution in, taken out under 60KHz frequencies after ultrasonic 3h And rinsed well with deionized water, obtain the TiO of 0.5wt Cu ion dopings2Nano-tube array.
Embodiment 6
The TA23 alloy sheets that thickness is 2mm are cut to 2 × 8cm2Strip, polished by sand paper and made after being cleaned by ultrasonic Stand-by anode, electrolyte is made using the aqueous solution of identical size Pt pieces ammonium fluoride containing 0.3wt% as negative electrode and preparation.Electrolytic process is adopted With two electrode DC electrolysis systems, voltage 5V, temperature is 30 DEG C, time 1h.With deionized water rinsing sun after the completion of electrolysis The residual liquid on pole surface, then be impregnated in 30 DEG C of constant temperature pH be 13 KOH solution in, under 50KHz frequencies after ultrasonic 40min Take out and rinsed well with deionized water, obtain the ion co-doped TiO of 0.8wt%Al, 1.1wt%Zr and 0.3wt%Fe2Nanometer Pipe array.
Embodiment 7
The TC2 alloy sheets that thickness is 2mm are cut to 2 × 8cm2Strip, polished by sand paper and made after being cleaned by ultrasonic Stand-by anode, using identical size Pt pieces as negative electrode and prepare water containing 2wt%, 0.3wt% ammonium fluorides ethylene glycol solution be electrolysed Matter.Electrolytic process uses two electrode DC electrolysis systems, voltage 50V, and temperature is 30 DEG C, time 4h.Used after the completion of electrolysis The residual liquid of deionized water rinsing anode surface, then be impregnated in 30 DEG C of constant temperature pH be 10 Mg (OH)2In solution, 50 KHz Take out after ultrasonic 4h under frequency and rinsed well with deionized water, obtain the ion co-doped TiO of 2.1wt%Al and 0.5wt%Mn2 Nano-tube array.
Embodiment 8
The TB7 alloy sheets that thickness is 2mm are cut to 2 × 8cm2Strip, polished by sand paper and made after being cleaned by ultrasonic Stand-by anode, using identical size Pt pieces as negative electrode and prepare water containing 2wt%, 0.3wt% ammonium fluorides ethylene glycol solution be electrolysed Matter.Electrolytic process uses two electrode DC electrolysis systems, voltage 50V, and temperature is 30 DEG C, time 4h.Used after the completion of electrolysis The residual liquid of deionized water rinsing anode surface, then be impregnated in 30 DEG C of constant temperature pH be 11 Ca (OH)2In solution, 50 KHz Take out after ultrasonic 4h under frequency and rinsed well with deionized water, obtain the TiO of 4.8wt%Mo ion dopings2Nano-tube array.

Claims (10)

  1. A kind of 1. controlling type metal ion doping TiO in situ2The preparation method of nano-tube array, comprises the following steps：
    1) using titanium alloy piece or titanium alloy bar as anode, Pt pieces or Pt rods are negative electrode, and gold is prepared in fluorine-containing solution Anodic Oxidation Belong to ion doping TiO in situ2Nano-tube array, cleaning sample；
    2) using the chemical property difference of doping metals and Ti, by choosing appropriate acid or aqueous slkali, and accurately control is leached Condition, using ultrasonic wave added selectivity acid or alkali soluble solution leaching section metal ion, realize metal ion in nano-tube array The quantitatively regulating and controlling of content；
    3) cleaned after the completion of regulating and controlling, drying to obtain controlling type metal ion doping TiO in situ2Nano-tube array.
  2. 2. the controlling type metal ion doping TiO in situ as described in claim 12The preparation method of nano-tube array, its feature exist In：The voltage of anodic oxidation described in step 1) is 5-50V, and temperature is 20-50 DEG C, time 30min-4h.
  3. 3. the controlling type metal ion doping TiO in situ as described in claim 12The preparation method of nano-tube array, its feature exist In：The ultrasonic frequency that ultrasonic wave added described in step 2) uses is 30-60KHz.
  4. 4. the controlling type metal ion doping TiO in situ as described in claim 12The preparation method of nano-tube array, its feature exist In：Solution temperature described in step 2) is 20-60 DEG C, dissolution time 20min-4h.
  5. 5. the controlling type metal ion doping TiO in situ as described in claim 12The preparation method of nano-tube array, its feature exist In：Described titanium alloy be TA5, TA6, TA7, TA10, TA11, TA12, TA13, TA14, TA15, TA16, TA17, TA18, TA19、TA20、TA21、TA22、TA23、TA24、TA25、TA26、TA28、TB2、TB3、TB4、TB5、TB6、TB7、TB8、TB9、 TB10、TB11、TC1、TC2、TC3、TC4、TC6、TC8、TC9、TC10、TC11、TC15、TC16、TC17、TC18、TC19、 TC20, TC21, TC22, TC23, TC24, TC25 or TC26.
  6. 6. the controlling type metal ion doping TiO in situ as described in claim 12The preparation method of nano-tube array, its feature exist In：Described fluorine-containing solution is organic solution or the inorganic solution of hydrofluoric acid containing containing ammonium fluoride.
  7. 7. the controlling type metal ion doping TiO in situ as described in claim 62The preparation method of nano-tube array, its feature exist In：Described fluorine-containing solution is the aqueous solution of the ethylene glycol containing ammonium fluoride, glycerin solution or hydrofluoric acid containing.
  8. 8. the controlling type metal ion doping TiO in situ as described in claim 12The preparation method of nano-tube array, its feature exist In：Described metal ion original position is doped to Al, Cu, Fe, Sn, V, Cr, Mo, Nb, Mn, Ni, Zr, Ta, W, Nd, Ru and Pd ion In single ionic doping or different kinds of ions codope.
  9. 9. the controlling type metal ion doping TiO in situ as described in claim 12The preparation method of nano-tube array, its feature exist In：Described acid solution is HCl, H2SO4、HNO3Or H3PO4Solution, described aqueous slkali are NaOH, KOH, Ca (OH)2Or Mg (OH)2Solution.
  10. 10. the controlling type metal ion doping TiO in situ as described in claim 12The preparation method of nano-tube array, its feature It is：The acid solution pH added is 1-4, and it is 10-13 that the aqueous slkali added, which controls pH,.
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