CN101734615A - Method for preparing metal/titanium dioxide composite nano material at low temperature by gamma-irradiation - Google Patents
Method for preparing metal/titanium dioxide composite nano material at low temperature by gamma-irradiation Download PDFInfo
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- CN101734615A CN101734615A CN200910073254A CN200910073254A CN101734615A CN 101734615 A CN101734615 A CN 101734615A CN 200910073254 A CN200910073254 A CN 200910073254A CN 200910073254 A CN200910073254 A CN 200910073254A CN 101734615 A CN101734615 A CN 101734615A
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Abstract
The invention provides a method for preparing a metal/titanium dioxide composite nano material at low temperature by gamma-irradiation, which relates to a method for preparing a metal/titanium dioxide composite nano material. The invention solves the problems that the preparation of the metal/titanium dioxide composite material in the prior art needs a high-temperature reaction and needs to be introduced with a large amount of reducers or organic stabilizers, the obtained product has poor dispersivity and low photocatalytic activity, and the size and the pattern of metal particles generated by reduction are still difficult to control even if a gamma-irradiation reduction method is adopted. The method comprises the following steps of: (1) preparing a precursor solution of titanium; (2) preparing pulpous liquid; (3) preparing TiO2 transparent sol; (4) adding a metal precursor solution and isopropanol into the transparent sol to obtain mixed reaction liquid, introducing nitrogen gas and carrying out gamma-ray radiation reduction by a 60Co source after sealing to obtain metal/titanium dioxide composite sol; and (5) drying or coating to obtain the metal/titanium dioxide composite nano material. In the invention, the size and the distribution of the metal particles are controllable, a template agent does not need to be added, the high-temperature reaction is not needed, and the product has good dispersivity and high photocatalytic activity.
Description
Technical field
The present invention relates to prepare the method for metal/titanium dioxide composite nano material.
Background technology
Mainly concentrate on about the preparation research of metal in the control growth of size, pattern and metallic dispersiveness etc., can pass through accomplished in many ways now, as chemical method, electrochemical process, phonochemistry method or photocatalytic method etc.But, the reduction of metal ion process has generally all been introduced a large amount of reducing agents, organic formwork agent or microemulsion system etc. in these methods, and need pyroreaction, and this class material is difficult to separate fully from system after reaction finishes, still have partial action at catalyst surface, to play certain inhibitory action to its catalytic activity, and cause the product dispersiveness that obtains bad, photocatalytic activity is low.
At present, γ-radiation the reducing process that comprises metal ion salt solution is widely used in the synthetic of metal nanoparticle, the free radical that solvent produces under the irradiation of gamma-radiation has stronger reducing power, can spontaneous under the condition of no additional reducing agent the solution metal ion be reduced into metal.Yet the gamma-irradiation reducing process is expanded so far as yet to the preparation of the composite that can be used as photochemical catalyst, and its main cause is under the situation of no template agent existence in the system, the metal particle size and the difficult problem of pattern control that still exist reduction to generate.
Summary of the invention
The present invention seeks to prepare metal in the prior art in order to solve, existing needs pyroreaction, need to introduce a large amount of reducing agents or organic stabilizer, the products therefrom dispersiveness is bad, photocatalytic activity is low, adopt the gamma-irradiation reducing process to have the problem of particle size and pattern control difficulty, and the method for gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature is provided.
The method of gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature is carried out according to the following steps: one, the presoma with titanium adds in the alcohol, and the precursor concentration that is mixed with titanium is the solution of 0.1~0.5mol/L; Two, get 10~50mL step 1 solution, under room temperature, stirring condition, be added drop-wise in 10~50mL distilled water, dropwise back warming-in-water to 60~80 ℃ of continuation and stir 30~100min, get pulpous state liquid; Three, pulpous state liquid separates to such an extent that precipitate through centrifuge, adds the acid solution that 50~300mL concentration is 0.05~5.0mol/L then, and 4~20h is stirred in the sealing back under 60~80 ℃ condition, add 100~400mL distilled water again, gets TiO
2Vitreosol; Four, get 10~100mL TiO
2Vitreosol, adding 20~300 μ L concentration is metal precursor solution and the 3~20mL isopropyl alcohol of 0.1~1mol/L, gets mixed reaction solution, feeds nitrogen then, seals bottleneck behind 10~30min, uses again
60Gamma-radiation radiation reduction 10~60h is carried out in the Co source, and dose of radiation is 2 * 10
4~2 * 10
2Gy/h gets the metal/titanium dioxide complex sol; Five, metal/titanium dioxide complex sol drying or coating obtain Powdered respectively or film shape metal/titanium dioxide composite nano material; Wherein the presoma of titanium is titanium sulfate, titanyl sulfate, titanium tetrachloride, butyl titanate or isopropyl titanate in the step 1; Alcohol is ethanol or isopropyl alcohol in the step 1; Acid solution is hydrochloric acid, acetic acid, nitric acid or above-mentioned two kinds of acid by 1: 1 mixed in molar ratio in the step 3; Metal precursor is one or both in silver nitrate, gold chloride, chloroplatinic acid, the nickel nitrate in the step 4.
The present invention adopts being radiated at of gamma-radiation to produce e in the aqueous solution
-, H
2O
+Deng species, following reaction takes place respectively with hydrone, generate e
Aq -With OH,
H
2O
++H
2O→H
3O
++·OH
e
-+H
2O→e
aq -
Wherein oxidized form free radical OH is caught by isopropyl alcohol excessive in the system, and e
Aq -Have stronger reducing power, can spontaneous under the condition of no additional reducing agent the solution metal ion be reduced into metal; Compare with other method of reducing, this ionising radiation method can guarantee that reduction class species homogeneous phase in system that solvent produces distributes, and has just guaranteed that also the metallic of even formation is grown at the stabilizing agent surface in situ in ionization and excitation process.The present invention can obtain anatase phase TiO respectively by at low temperatures titanium precursor body hydrolysate being carried out peptization
2Particle Cluster and rutile be TiO mutually
2Nanometer rods, this TiO
2Crystal has water-soluble (or water dispersible) of height, though product still maintains the characteristic of out-phase system on nanoscale, can not think that owing to there is obvious limit to be similar in macro-scale a kind of macroscopical homogeneous dispersion is.Therefore, the present invention adopts the gamma-irradiation method of reducing at water-soluble TiO
2The plane of crystal carrying metal particles is by newly-generated water-soluble TiO
2Crystal is as the stabilizing agent of effective separation and fixing metal nano particle, thereby avoid introducing the organic ligand that suppresses the nano-sized metal particles reunion and grow up in the irradiation reduction process, not only can provide size, metallic that character is adjustable as dressing agent, the more important thing is the photochemical catalyst with " cleaning " surface that can obtain to be used for special dimension.
Raw material among the present invention is cheap to be easy to get, easy and simple to handle, need not add any template agent, does not need high-temperature high-voltage reaction, makes laboratory mass preparation and even suitability for industrialized production become possibility.Employing the present invention can obtain the anatase and red schorl phase titanium dioxide composite of metal load respectively, the product good dispersion, and the transparent homogeneous of product, pattern is controlled, and the photocatalytic activity height, and character is very stable, obviously is better than the P25 powder sample of using always.The gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature can be widely used as catalysis material, solar cell and electrode material among the present invention, can be used in and administers waste water, purifies air, aspect such as opto-electronic conversion.
Description of drawings
Fig. 1 is the transmission electron microscope picture of the low multiplication factor of gained metal/titanium dioxide composite nano material in the specific embodiment 17; Fig. 2 is the transmission electron microscope picture of gained metal/titanium dioxide composite nano material high-amplification-factor in the specific embodiment 17; Fig. 3 is the Fourier transform figure (FFT) of gained metal/titanium dioxide composite nano material in the specific embodiment 17; Fig. 4 is the XRD figure of gained metal/titanium dioxide composite nano material in the specific embodiment 17, wherein ▲ and expression TiO
2Characteristic diffraction peak, ● the expression Ag characteristic diffraction peak; Fig. 5 is gained metal/titanium dioxide composite nano material and a commodity P25 powder sample difference photocatalytically degradating organic dye methylene blue in the specific embodiment 17, and its degradation rate is curve map over time, and wherein ■ represents TiO
2, represents Ag/TiO
2, ▲ expression P25; Fig. 6 is the transmission electron microscope picture of the low multiplication factor of gained metal/titanium dioxide composite nano material in the specific embodiment 18; Fig. 7 is the transmission electron microscope picture of gained metal/titanium dioxide composite nano material high-amplification-factor in the specific embodiment 18; Fig. 8 is the Fourier transform figure (FFT) of gained metal/titanium dioxide composite nano material in the specific embodiment 18; Fig. 9 is the XRD figure of gained metal/titanium dioxide composite nano material in the specific embodiment 18, wherein
Expression TiO
2Characteristic diffraction peak, ★ represents the characteristic diffraction peak of Au; Figure 10 is gained metal/titanium dioxide composite nano material and a commodity P25 powder sample difference photocatalytically degradating organic dye methylene blue in the specific embodiment 18, and its degradation rate is curve map over time, wherein ● expression TiO
2(R), zero expression Au/TiO
2(R), ▲ expression P25.
The specific embodiment
The specific embodiment one: the method for present embodiment gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature is carried out according to the following steps: one, the presoma with titanium adds in the alcohol, and the precursor concentration that is mixed with titanium is the solution of 0.1~0.5mol/L; Two, get 10~50mL step 1 solution, under room temperature, stirring condition, be added drop-wise in 10~50mL distilled water, dropwise back warming-in-water to 60~80 ℃ of continuation and stir 30~100min, get pulpous state liquid; Three, pulpous state liquid separates to such an extent that precipitate through centrifuge, adds the acid solution that 50~300mL concentration is 0.05~5.0mol/L then, and 4~20h is stirred in the sealing back under 60~80 ℃ condition, add 100~400mL distilled water again, gets TiO
2Vitreosol; Four, get 10~100mL TiO
2Vitreosol, adding 20~300 μ L concentration is metal precursor solution and the 3~20mL isopropyl alcohol of 0.1~1mol/L, gets mixed reaction solution, feeds nitrogen then, seals bottleneck behind 10~30min, uses again
60Gamma-radiation radiation reduction 10~60h is carried out in the Co source, and dose of radiation is 2 * 10
4~2 * 10
2Gy/h gets the metal/titanium dioxide complex sol; Five, metal/titanium dioxide complex sol drying or coating obtain Powdered respectively or film shape metal/titanium dioxide composite nano material; Wherein the presoma of titanium is titanium sulfate, titanyl sulfate, titanium tetrachloride, butyl titanate or isopropyl titanate in the step 1; Alcohol is ethanol or isopropyl alcohol in the step 1; Acid solution is hydrochloric acid, acetic acid, nitric acid or above-mentioned two kinds of acid by 1: 1 mixed in molar ratio in the step 3; Metal precursor is one or both in silver nitrate, gold chloride, chloroplatinic acid, the nickel nitrate in the step 4.
Speed of agitator is 300~1000 rev/mins in the present embodiment, and centrifuge speed is 3000~8000 rev/mins.
The specific embodiment two: present embodiment and the specific embodiment one are different is that the precursor concentration that is mixed with titanium in the step 1 is the solution of 0.2~0.4mol/L.Other step and parameter are identical with the specific embodiment one.
The specific embodiment three: present embodiment and the specific embodiment one are different is that the precursor concentration that is mixed with titanium in the step 1 is the solution of 0.3mol/L.Other step and parameter are identical with the specific embodiment one.
The specific embodiment four: present embodiment and the specific embodiment one are different is that the precursor concentration that is mixed with titanium in the step 1 is the solution of 0.1mol/L.Other step and parameter are identical with the specific embodiment one.
The specific embodiment five: present embodiment and the specific embodiment one are different is that the precursor concentration that is mixed with titanium in the step 1 is the solution of 0.5mol/L.Other step and parameter are identical with the specific embodiment one.
The specific embodiment six: what present embodiment and the specific embodiment one, two, three, four or five were different is to get 20~40mL step 1 solution in the step 2, under room temperature, stirring condition, be added drop-wise in 20~40mL distilled water, dropwise back warming-in-water to 65~75 ℃ of continuation and stir 40~90min.Other step and parameter are identical with the specific embodiment one, two, three, four or five.
The specific embodiment seven: what present embodiment and the specific embodiment one, two, three, four or five were different is to get 30mL step 1 solution in the step 2, under room temperature, stirring condition, be added drop-wise in the 30mL distilled water, dropwise ℃ continuation of back warming-in-water to 70 and stir 80min.Other step and parameter are identical with the specific embodiment one, two, three, four or five.
The specific embodiment eight: present embodiment and the specific embodiment seven are different is that to add acid solution and the 100~200mL concentration that 100~200mL concentration is 0.5~3.0mol/L in the step 3 be the aqueous slkali of 0.5~3.0mol/L, and 6~18h is stirred in the sealing back under 65~75 ℃ condition.Other step and parameter are identical with the specific embodiment seven.
The specific embodiment nine: present embodiment and the specific embodiment seven are different is that to add 180mL concentration in the step 3 be that acid solution and the 180mL concentration of 2.0mol/L is the aqueous slkali of 2.0mol/L, and 16h is stirred in the sealing back under 70 ℃ condition.Other step and parameter are identical with the specific embodiment seven.
The specific embodiment ten: what present embodiment was different with the specific embodiment eight or nine is to get 20~90mL TiO in the step 4
2Vitreosol, adding 50~200 μ L concentration is metal precursor solution and the 5~18mL isopropyl alcohol of 0.4~0.8mol/L.Other step and parameter are identical with the specific embodiment eight or nine.
The specific embodiment 11: what present embodiment was different with the specific embodiment eight or nine is to get 50mL TiO in the step 4
2Vitreosol adds metal precursor solution and 12mL isopropyl alcohol that 100 μ L concentration are 0.5mol/L.Other step and parameter are identical with the specific embodiment eight or 92.
The specific embodiment 12: what present embodiment and the specific embodiment 11 were different is to use in the step 4
60Gamma-radiation radiation reductase 12 0~50h is carried out in the Co source, and dose of radiation is 2 * 10
4Gy/h.Other step and parameter are identical with the specific embodiment 11.
The specific embodiment 13: what present embodiment and the specific embodiment 11 were different is to use in the step 4
60Gamma-radiation radiation reduction 30h is carried out in the Co source, and dose of radiation is 2 * 10
2Gy/h.Other step and parameter are identical with the specific embodiment 11.
The specific embodiment 14: present embodiment and the specific embodiment one, two, three, four, five, eight, nine, 12 or 13 are different is to dropwise back warming-in-water to 60~80 ℃ in the step 2 to continue to stir 30~100min, can also add the aqueous slkali that 50~300mL concentration is 0.05~5.0mol/L, 4~20h is stirred in the sealing back under 60~80 ℃ condition, get pulpous state liquid.Other step and parameter are identical with the specific embodiment one, two, three, four, five, eight, nine, 12 or 13.
The specific embodiment 15: what present embodiment and the specific embodiment 14 were different is that aqueous slkali is NaOH, potassium hydroxide or sodium carbonate in the step 2.Other step and parameter are identical with the specific embodiment 14.
The specific embodiment 16: present embodiment and the specific embodiment 15 are different be in the step 3 pulpous state liquid through centrifuge separate precipitation, and be washed with distilled water to supernatant pH value near neutral, add the acid solution that 50~300mL concentration is 0.05~5.0mol/L then, 4~20h is stirred in the sealing back under 60~80 ℃ condition, add 100~400mL distilled water again, get TiO
2Vitreosol.Other step and parameter are identical with the specific embodiment 15.
The distilled water washing is a foreign ion of removing precipitation surface absorption in the present embodiment.
The specific embodiment 17: the method for present embodiment gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature is carried out according to the following steps: one, the presoma with titanium adds in the alcohol, and the precursor concentration that is mixed with titanium is the solution of 0.35mol/L; Two, get 25mL step 1 solution, under room temperature, stirring condition, be added drop-wise in the 30mL distilled water, dropwise ℃ continuation of back warming-in-water to 70 and stir 50min, get pulpous state liquid; Three, pulpous state liquid separates to such an extent that precipitate through centrifuge, adds the acid solution that 80mL concentration is 0.055mol/L then, and 4h is stirred in the sealing back under 70 ℃ condition, add 300mL distilled water again, gets TiO
2Vitreosol; Four, get 50mL TiO
2Vitreosol adds metal precursor solution and 5mL isopropyl alcohol that 270 μ L concentration are 0.33mol/L, gets mixed reaction solution, feeds nitrogen then, seals bottleneck behind the 15min, uses again
60Gamma-radiation radiation reductase 12 0h is carried out in the Co source, and dose of radiation is 2 * 10
3Gy/h gets the metal/titanium dioxide complex sol; Five, metal/titanium dioxide complex sol drying or coating obtain Powdered respectively or film shape metal/titanium dioxide composite nano material; Wherein the presoma of titanium is a titanium sulfate in the step 1; Alcohol is ethanol in the step 1; Acid solution is a nitric acid in the step 3; Metal precursor is a silver nitrate in the step 4.
Speed of agitator is 500 rev/mins in the present embodiment, and centrifuge speed is 6000 rev/mins.
Gained metal/titanium dioxide composite nano material in the present embodiment, by Fig. 1,2 and 3 as can be known, product good dispersion, TiO
2The particle diameter of nano particle distributes and is positioned at 5~8nm, and the Ag nano particle is 1~2nm; The XRD testing result as shown in Figure 4, titanium dioxide is the anatase phase in the metal/titanium dioxide composite nano material, and crystal property is good.
Gained metal/titanium dioxide composite nano material and commodity P25 powder sample are respectively got 10mg in the present embodiment, be diluted with water to 10mL, regulate the pH value of the two consistent then, 0.2% aqueous solution of methylene blue that adds 40 μ L again, be statically placed in the down irradiation of high-pressure sodium lamp of 100W, the photocatalytically degradating organic dye methylene blue, the degradation rate of observing dyestuff respectively is situation over time, as shown in Figure 5, TiO
2Crystal its photocatalytic activity behind the area load metal all is significantly increased, and obviously is better than the commodity P25 type photochemical catalyst of using always.
The specific embodiment 18: the method for present embodiment gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature is carried out according to the following steps: one, the presoma with titanium adds in the alcohol, and the precursor concentration that is mixed with titanium is the solution of 0.35mol/L; Two, get 25mL step 1 solution, under room temperature, stirring condition, be added drop-wise in the 30mL distilled water, dropwise back warming-in-water to 60~80 ℃ of continuation and stir 30~100min, can also add the aqueous slkali that 50~300mL concentration is 0.05~5.0mol/L, 4~20h is stirred in the sealing back under 60~80 ℃ condition, get pulpous state liquid; Three, pulpous state liquid separates to such an extent that precipitate through centrifuge, and be washed with distilled water to supernatant pH value near neutral, and adding the acid solution that 50~300mL concentration is 0.05~5.0mol/L then, 4~20h is stirred in the sealing back under 60~80 ℃ condition, add 100~400mL distilled water again, get TiO
2Vitreosol; Four, get 50mL TiO
2Vitreosol adds metal precursor solution and 5mL isopropyl alcohol that 60 μ L concentration are 0.33mol/L, gets mixed reaction solution, feeds nitrogen then, seals bottleneck behind the 15min, uses again
60Gamma-radiation radiation reductase 12 0h is carried out in the Co source, and dose of radiation is 2 * 10
3Gy/h gets the metal/titanium dioxide complex sol; Five, metal/titanium dioxide complex sol drying or coating obtain Powdered respectively or film shape metal/titanium dioxide composite nano material; Wherein the presoma of titanium is titanium sulfate, titanyl sulfate, titanium tetrachloride, butyl titanate or isopropyl titanate in the step 1; Alcohol is ethanol in the step 1; Aqueous slkali is a NaOH in the step 2; Acid solution is a nitric acid in the step 3; Metal precursor is a gold chloride in the step 4.
Speed of agitator is 500 rev/mins in the present embodiment, and centrifuge speed is 6000 rev/mins.
Gained metal/titanium dioxide composite nano material in the present embodiment, by Fig. 6,7 and 8 as can be known, product good dispersion, TiO
2The nanometer rods even size distribution, aspect ratio is about 6~8, the about 20~30nm of the central diameter of nanometer rods, the Au nano particle is about 1~2nm; The XRD testing result as shown in Figure 9, titanium dioxide is the rutile phase in the metal/titanium dioxide composite nano material, and crystal property is good.
Gained metal/titanium dioxide composite nano material and commodity P25 powder sample difference photocatalytically degradating organic dye methylene blue in the present embodiment, maximum absorption band time-dependent variation in intensity curve in its uv-visible absorption spectra, as shown in Figure 10, TiO
2Crystal its photocatalytic activity behind the area load metal all is significantly increased, and obviously is better than the commodity P25 type photochemical catalyst of using always.
Claims (10)
1. the method for gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature, the method that it is characterized in that the gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature is carried out according to the following steps: one, the presoma with titanium adds in the alcohol, and the precursor concentration that is mixed with titanium is the solution of 0.1~0.5mol/L; Two, get 10~50mL step 1 solution, under room temperature, stirring condition, be added drop-wise in 10~50mL distilled water, dropwise back warming-in-water to 60~80 ℃ of continuation and stir 30~100min, get pulpous state liquid; Three, pulpous state liquid separates to such an extent that precipitate through centrifuge, adds the acid solution that 50~300mL concentration is 0.05~5.0mol/L then, and 4~20h is stirred in the sealing back under 60~80 ℃ condition, add 100~400mL distilled water again, gets TiO
2Vitreosol; Four, get 10~100mL TiO
2Vitreosol, adding 20~300 μ L concentration is metal precursor solution and the 3~20mL isopropyl alcohol of 0.1~1mol/L, gets mixed reaction solution, feeds nitrogen then, seals bottleneck behind 10~30min, uses again
60Gamma-radiation radiation reduction 10~60h is carried out in the Co source, and dose of radiation is 2 * 10
4~2 * 10
2Gy/h gets the metal/titanium dioxide complex sol; Five, metal/titanium dioxide complex sol drying or coating obtain Powdered respectively or film shape metal/titanium dioxide composite nano material; Wherein the presoma of titanium is titanium sulfate, titanyl sulfate, titanium tetrachloride, butyl titanate or isopropyl titanate in the step 1; Alcohol is ethanol or isopropyl alcohol in the step 1; Acid solution is hydrochloric acid, acetic acid, nitric acid or above-mentioned two kinds of acid by 1: 1 mixed in molar ratio in the step 3; Metal precursor is one or both in silver nitrate, gold chloride, chloroplatinic acid, the nickel nitrate in the step 4.
2. the method for gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature according to claim 1, the precursor concentration that it is characterized in that being mixed with in the step 1 titanium is the solution of 0.2~0.4mol/L.
3. the method for gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature according to claim 1, the precursor concentration that it is characterized in that being mixed with in the step 1 titanium is the solution of 0.3mol/L.
4. according to the method for claim 1,2 or 3 described gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature, it is characterized in that getting in the step 2 30mL step 1 solution, under room temperature, stirring condition, be added drop-wise in the 30mL distilled water, dropwise ℃ continuation of back warming-in-water to 70 and stir 80min.
5. the method for gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature according to claim 4 is characterized in that adding 180mL concentration in the step 3 is the acid solution of 2.0mol/L, and 16h is stirred in the sealing back under 70 ℃ condition.
6. the method for gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature according to claim 5 is characterized in that getting in the step 4 50mL TiO
2Vitreosol adds metal precursor solution and 12mL isopropyl alcohol that 100 μ L concentration are 0.5mol/L.
7. the method for gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature according to claim 6 is characterized in that using in the step 4
60Gamma-radiation radiation reduction 30h is carried out in the Co source, and dose of radiation is 2 * 10
2Gy/h.
8. according to the method for claim 1,2,3,5,6 or 7 described gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature, it is characterized in that dropwising in the step 2 back warming-in-water to 60~80 ℃ of continuation and stir 30~100min, can also add the aqueous slkali that 50~300mL concentration is 0.05~5.0mol/L, 4~20h is stirred in the sealing back under 60~80 ℃ condition, get pulpous state liquid.
9. the method for gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature according to claim 8 is characterized in that aqueous slkali is NaOH, potassium hydroxide or sodium carbonate in the step 2.
10. the method for gamma-irradiation preparing metal/titanium dioxide composite nano material at low temperature according to claim 9, it is characterized in that pulpous state liquid separates to such an extent that precipitate through centrifuge in the step 3, and be washed with distilled water to supernatant pH value near neutral, add the acid solution that 50~300mL concentration is 0.05~5.0mol/L then, 4~20h is stirred in the sealing back under 60~80 ℃ condition, add 100~400mL distilled water again, get TiO
2Vitreosol.
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