CN1593749A - Process for preparing nanometer titanium dioxide membrane photocatalyst - Google Patents
Process for preparing nanometer titanium dioxide membrane photocatalyst Download PDFInfo
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- CN1593749A CN1593749A CN 200410025755 CN200410025755A CN1593749A CN 1593749 A CN1593749 A CN 1593749A CN 200410025755 CN200410025755 CN 200410025755 CN 200410025755 A CN200410025755 A CN 200410025755A CN 1593749 A CN1593749 A CN 1593749A
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Abstract
The invention relates to a kind of manufacturing method of millimicron titanium dioxide photocatalyst, especially also relates to a manufacturing method of crystal-form controllable titanium dioxide photocatalyst in low temperature. It uses micro emulsifiable solution to hydro heating synthesis, and the feature of which is as follows: make the titanium source hydrolyze in the acid micro emulsifiable solution under certain condition; through adjusting the proportion of negative ion in water phase, the titanium dioxide micro emulsifiable solution can be get; then after crystallizing with hydro heating and emulsion resolving in pressure pan that having the inside lining of polytetrafluoroethylene (PTFE), the anatase and the rutile crystal-form proportion controllable titanium dioxide photocatalyst can be acquired.
Description
Technical field
The present invention relates to a kind of preparation method of nano titanium dioxide photocatalyst, particularly a kind of preparation method of the photochemical catalyst of controllable-crystal nano titanium dioxide at low temperatures.
Background technology
In recent years; along with the pay attention to day by day of people to environmental protection; what three waste discharge such as organic wastewater and vehicle exhaust required improves constantly; the heterogeneous catalysis material of semiconductor is as a kind of environmentally friendly new catalytic material, particularly is subjected to countries in the world government and researcher's extensive concern aspect the organic sewage processing in environmental improvement.Because it is simple to operate that it uses, only need to carry out at normal temperature and pressure; And can thoroughly destroy pollutant in the empty G﹠W, and making it permineralization is innocuous substances such as carbon dioxide, water, avoids advantages such as secondary pollution, the heterogeneous catalysis material of semiconductor becomes replenishing of traditional pollution treatment material just gradually, demonstrates tempting application prospect.At present, the multiphase photocatalysis material of academia's research photocatalytic degradation environmental contaminants mostly concentrates on metal oxide and the metal sulfide semiconductor material, as titanium dioxide, zinc oxide, tungstic acid, tin ash, di-iron trioxide, cadmium sulfide etc.In numerous conductor photocatalysis materials, titanium dioxide is because of characteristics such as its catalytic activity height, safety non-toxic, chemical property are stable, with low cost, is acknowledged as the environment-friendly type catalysis material of the tool exploitation future in environment pollution treatment field.The common crystal formation of titanium dioxide has three kinds: Detitanium-ore-type, rutile-type and brookite type, because the brookite type titanium dioxide instability, research mainly concentrates on anatase and the rutile.It is generally acknowledged that anatase is than the photocatalytic activity height of rutile; But R.R.Bacsa, J.C.Yu etc. find also that under study for action a certain proportion of anatase has higher photocatalytic activity with the more single titanium dioxide mutually of rutile mixed crystal.Report among the Appl.Catal.B 16 (1998) 19 that anatase, rutile mixed crystal ratio are that 7: 3 o'clock photocatalytic activities are best; Report among the J.Photochem.Photobiol.A 111 (1997) 199 that anatase, rutile mixed crystal ratio are more can improve photocatalytic activity at 9: 1; And the ratio of reporting anatase in anatase, the rutile mixed crystal among the J.Phys.Chem.B 105 (2001) 2417 surpasses 5%, and photocatalytic activity just can improve greatly.Therefore, preparation anatase, the controlled titanic oxide material of rutile crystal type ratio and study its influence and just seem very meaningful to photocatalytic activity.
The preparation method of nano titanium dioxide photocatalyst is a lot, and sol-gel process is domestic and international the most frequently used a kind of method, but the titanium dioxide that sol-gel process prepares is unformed, shows any photocatalytic activity hardly.In order to obtain the titanium dioxide that the degree of crystallinity height has photocatalytic activity, just need carry out high-temperature heat treatment.Raising along with heat treatment temperature, will cause titanium dioxide granule to be grown up and the decline of specific area, titanium dioxide optical catalyst is the same with other catalysis materials, improves activity in order there to be more chain carrier to participate in reaction, all needs big specific area and little particle size.Therefore, low temperature prepares titanium dioxide and just seems necessary.A kind of good low temperature preparation method and the microemulsion hydrothermal synthesis method be can yet be regarded as.Reported low temperature, acid condition among the Langmuir15 (1999) 8822 down with synthetic pure Detitanium-ore-type and the rutile titanium dioxide of microemulsion hydro-thermal, but it is studied to the influence of pure Detitanium-ore-type and rutile titanium dioxide formation to hydro-thermal time, hydrothermal temperature and microemulsion acidity.The present invention is exactly on this research basis, and the anionic proportioning of microemulsion aqueous phase prepares anatase at low temperatures and the rutile crystal type ratio is controlled, the high specific surface area titanic oxide photochemical catalyst by regulating.
Summary of the invention
The technical issues that need to address of the present invention are to have proposed a kind of low temperature to prepare anatase and rutile, and crystal form ratio is controlled, the method for high specific surface area titanic oxide photochemical catalyst.
To achieve these goals, utilize the microemulsion hydrothermal synthesis method, with the hydrolysis under the certain condition in acid microemulsion of titanium source, and by regulating the anionic proportioning of aqueous phase, make titanium dioxide micro latex, change over to then to have and carry out hydro-thermal breakdown of emulsion crystallization in the teflon-lined autoclave, obtain the controlled titanium dioxide optical catalyst material of anatase and rutile crystal type ratio.
The condition of described acid microemulsion is: Triton X-100, n-hexyl alcohol, cyclohexane volume ratio are 5: 3: 8 in the microemulsion oil phase.Described hydrolysising condition control: temperature is 10-60 ℃, and the time is 1-12 hour.The acidity of described microemulsion water is 2-10M, preferred 5M.Described titanium source is one or more the combination in butyl titanate, metatitanic acid isopropyl ester, metatitanic acid second fat, metatitanic acid formicester, titanium tetrachloride, the titanium sulfate.The molar concentration in titanium source is preferably 1-0.05M, preferred 0.5-0.1M.
Described anion is chlorion and sulfate ion.The chlorion source is one or both combinations in hydrochloric acid, ammonium chloride, potassium chloride, the sodium chloride, and the sulfate ion source is one or both combinations in sulfuric acid, ammonium sulfate, potassium sulfate, the sodium sulphate.Described sulfate ion accounts for the 0.32%-1.6% of chlorion and sulfate ion mole total amount.
Hydro-thermal breakdown of emulsion crystallization condition is: temperature is 100-160 ℃, and the time is 8-24 hour
This law is hydro-thermal breakdown of emulsion titanium dioxide micro latex at low temperatures, makes it slowly gentle brilliant anatase, rutile or both mixed crystal of forming that change., the most levigate through infra-red drying after alcohol, water washing be neutrality to pH, promptly obtain the titanium dioxide powder photochemical catalyst.
The method that said low temperature prepares anatase and the controlled titanium dioxide optical catalyst of rutile crystal type ratio among the present invention can also be used to prepare the nano titanium dioxide photocatalyst film except that can preparing the powder nano titanium dioxide photocatalyst.
The photocatalytic activity of titanium dioxide powder photochemical catalyst is to investigate the degradation and decolorization situation of methyl orange solution in nano-titanium dioxide powder suspension system by illumination to test.Waste water from dyestuff is one of industrial wastewater of present difficult degradation, and its toxicity is big, and color and luster is dark, serious harm ecological environment.This colored compound of methyl orange than difficult degradation, because azo and quinoid structure that it has under acid and alkali condition also are the agent structures of dye composition, select it as a kind of simulation dye discoloration compound, in handling organic dye waste water, have certain representativeness.Titanium dioxide powder photocatalytic activity experiment to methyl orange degradation in the aqueous solution is that the suspension by high voltage mercury lamp radiation nano titanium oxide and methyl orange carries out under the effect of magnetic agitation.Detailed process is as follows: the nano-titanium dioxide powder that takes by weighing 0.06g, the methyl orange solution (the pH value of solution value is its value 6.4-6.7 naturally) of measuring 60ml40mg/l is in quartz test tube, put into magnetic stir bar again, made suspension in ultrasonic 20 minutes, place on the magnetic stirring apparatus pre-absorption 30min to make it to reach the adsorption-desorption balance in test tube, sampling is carried out light-catalyzed reaction then as the light degradation initial concentration under 300W uviol lamp (maximum wavelength 365nm).Sampling is tested its absorbance with the ultraviolet-visible diffuse reflection spectrum again with filter membrane elimination titanium dioxide powder behind the reaction 80min, calculates percent of decolourization.
The physical property of titanium dioxide powder photochemical catalyst characterizes and comprises: X-ray diffraction (XRD) characterizes phase structure, phase composition and crystallite dimension size, specific area with nitrogen adsorption device characterization titanium dioxide powder, with ultraviolet-visible spectrophotometer test light catalytic degradation decolouring situation, characterize titanium dioxide powder surface sulphate-containing ion situation with Fourier infrared spectrum (FTIR).
Description of drawings
Fig. 1 is the XRD figure spectrum of the resultant titanium dioxide powder of embodiment 1-5.
Fig. 2 is that embodiment 1-5 prepares titanium dioxide powder XRD figure spectrum and calculates anatase content, obtains sulfate ion addition and anatase relation with contents fitted figure.
Fig. 3 is the FFIR of embodiment 1 and 5 resultant titanium dioxide powders.
Fig. 4 is the photocatalytic activity figure of the resultant titanium dioxide powder degraded of embodiment 1-5 methyl orange
The specific embodiment
Embodiment 1
The method of the synthetic crystal with controllable crystal forms titanium dioxide optical catalyst of low temperature microemulsion hydro-thermal is as follows: 10ml Triton X-100 and 6ml n-hexyl alcohol, 16ml cyclohexane are added in the single port flask of 100ml, with magnetic stirrer evenly after, add 4ml dissolving 0.0682g (NH
4)
2SO
410M hydrochloric acid, use constant pressure funnel under 25 ℃, to drip the 3.4ml butyl titanate again with 10/min.Dropwise, constant speed stirs 6h makes its hydrolysis complete, obtains the yellow transparent microemulsion.Microemulsion has been changed in the teflon-lined autoclave, be incubated 13h down at 120 ℃.Treat that autoclave is cooled to room temperature, be neutral with ethanol and water washing sample to pH value respectively, put into the dry 12h of IR bake and obtain sample, the sample name is designated as S-1.28, and the percentage composition that expression microemulsion aqueous phase sulfate ion accounts for chlorion and sulfate ion mole total amount is 1.28%.
Embodiment 2
Add 0.0599g (NH in the hydrochloric acid
4)
2SO
4, except that the amount difference of the sulfate ion that adds, other reaction condition such as titanium source, titanium source hydrolysis temperature time, aqueous phase anion source, microemulsion acidity and hydro-thermal time-temperature etc. are all identical with embodiment 1, obtain sample and are designated as S-1.12.
Embodiment 3
Add 0.0512g (NH in the hydrochloric acid
4)
2SO
4, except that the amount difference of the sulfate ion that adds, other reaction condition such as titanium source, titanium source hydrolysis temperature time, aqueous phase anion source, microemulsion acidity and hydro-thermal time-temperature etc. are all identical with embodiment 1, obtain sample and are designated as S-0.96.
Embodiment 4
Add 0.0426g (NH in the hydrochloric acid
4)
2SO
4, except that the amount difference of the sulfate ion that adds, other reaction condition such as titanium source, titanium source hydrolysis temperature time, aqueous phase anion source, microemulsion acidity and hydro-thermal time-temperature etc. are all identical with embodiment 1, obtain sample and are designated as S-0.80.
Embodiment 5
Add 0.0341g (NH in the hydrochloric acid
4)
2SO
4, except that the amount difference of the sulfate ion that adds, other reaction condition such as titanium source, titanium source hydrolysis temperature time, aqueous phase anion source, microemulsion acidity and hydro-thermal time-temperature etc. are all identical with embodiment 1, obtain sample and are designated as S-0.64.
Fig. 1 makes the XRD figure spectrum of titanium dioxide powder for the microemulsion hydro-thermal is synthetic.Increase along with the sulfate ion addition as can be seen from Figure 1, the content ordered increase of anatase, rutile content then successively decreases in order.By the Scherrer formula calculate anatase in all samples mutually and the grain size of rutile phase all between the 10-15 nanometer.
Fig. 2 has shown sulfate ion consumption and anatase relation with contents fitted figure.Its sample anatase content can calculate by formula (1).Can find that from Fig. 2 microemulsion aqueous phase sulfate ion content and anatase content have good linear relationship (its coefficient correlation is 0.99859).This shows that we can be by regulating microemulsion aqueous phase Cl
-, SO
4 2-Ratio control the crystal form ratio of titanium dioxide optical catalyst within the specific limits.
K＝0.79 f
A＞0.2
K＝0.68 f
A≤0.2
F wherein
ABe anatase content, I
R, I
ABe respectively the intensity of 110 of 101 of anatases and rutile in the XRD figure spectrum.
In order to get rid of the influence of sample surfaces different in kind to photocatalytic activity, we have chosen the highest and minimum two samples of anatase content and have carried out the FFIR sign.Fig. 4 is the FFIR of sample S-1.28 and S-0.64.Can find that from scheming to go up us the infrared spectrum of two samples is extremely similar, at 1200-1040cm
-1All there is poor absorption at the place, the characteristic frequency that is absorbed as the double coordination sulfate ion herein, and this illustrates that all preparation titanium dioxide powder surface naturies are identical, promptly all contains a small amount of double coordination sulfate ion.At 3410cm
-1And 1630cm
-1Absorption be respectively the flexural vibrations and the stretching vibration of OH key; 579cm
-1The place is the absorption of Ti-O key.
Photocatalytic activity figure when Fig. 5 is the methyl orange solution 80min of 5 kinds of titanium dioxide powders degraded 40mg/l.When we can find that anatase content is 74.2% (sample S-1.12) from figure, has best photocatalytic activity; And anatase content is when being 15.3% (sample S-0.64), and photocatalytic activity is the poorest.113,131,147,169,162m the specific area that records sample S-1.28-S-0.64 with the nitrogen adsorption device is respectively:
2/ g, the best sample of photocatalytic activity is not the highest sample of specific area, this shows that specific area is not the topmost factor that influences photocatalytic activity in our experiment.The result that comprehensive sample surfaces character, specific area and photocatalytic activity etc. obtain, we can draw a conclusion: the photocatalytic activity of 5 kinds of titanium dioxide powders is not both because it contains the anatase and the rutile of different amounts, promptly in anatase and rutile mixed crystal, contain a certain amount of rutile, help photocatalytic activity and improve; The existence of a large amount of rutile then is unfavorable for photocatalytic degradation.
Embodiment 6
The method of the synthetic crystal with controllable crystal forms titanium dioxide optical catalyst of low temperature microemulsion hydro-thermal is as follows: 10ml Triton X-100 and 6ml n-hexyl alcohol, 16ml cyclohexane are added in the single port flask of 100ml, with magnetic stirrer evenly after, add 4ml dissolving 0.0733g Na
2SO
45M hydrochloric acid, use again constant pressure funnel under 10 ℃ with 10/min Dropwise 5 .7ml metatitanic acid isopropyl ester.Dropwise, constant speed stirs 1h makes its hydrolysis complete, obtains the yellow transparent microemulsion.Microemulsion has been changed in the teflon-lined autoclave, be incubated 16h down at 100 ℃.Treat that autoclave is cooled to room temperature, be neutral with ethanol and water washing sample to pH value respectively, put into the dry 12h of IR bake and obtain sample.
Embodiment 7
The method of the synthetic crystal with controllable crystal forms titanium dioxide optical catalyst of low temperature microemulsion hydro-thermal is as follows: 10ml Triton X-100 and 6ml n-hexyl alcohol, 16ml cyclohexane are added in the single port flask of 100ml, with magnetic stirrer evenly after, add 4ml dissolving 0.0367gNa
2SO
412M hydrochloric acid, use constant pressure funnel under 10 ℃, to drip 1.2ml metatitanic acid isopropyl ester again with 10/min.Dropwise, constant speed stirs 12h makes its hydrolysis complete, obtains the yellow transparent microemulsion.Microemulsion has been changed in the teflon-lined autoclave, be incubated 10h down at 140 ℃.Treat that autoclave is cooled to room temperature, be neutral with ethanol and water washing sample to pH value respectively, put into the dry 12h of IR bake and obtain sample.
In embodiment 6,7, the anionic proportioning of microemulsion aqueous phase is identical with embodiment 1,5 respectively, and different is titanium source, titanium source hydrolysis temperature time, aqueous phase anion source, microemulsion acidity and hydro-thermal time-temperature.We utilize the intensity of 110 of 101 of anatases and rutile in the XRD figure spectrum to calculate by formula (1) and find, among the embodiment 6,7 content of anatase respectively with embodiment 1,5 in the content of anatase very close.Conditions such as this explanation titanium source, titanium source hydrolysis temperature time, aqueous phase anion source, microemulsion acidity and hydro-thermal time-temperature are not main to the influence of titanium dioxide powder crystal formation content, and the anionic proportioning of microemulsion aqueous phase is only topmost influence factor.Therefore, we can control the crystal form ratio of rutile and anatase by the anionic proportioning of simple adjusting microemulsion aqueous phase.The photocatalytic activity of the titanium dioxide powder that embodiment 6,7 is prepared will be lower than the activity of embodiment 1,5 preparation powders respectively, and this may be because sodium ion is present in the titanium dioxide crystal surface and is unfavorable for due to the photocatalysis.
Claims (10)
1, a kind of preparation method of nano titanium dioxide photocatalyst, utilize the microemulsion hydrothermal synthesis method, it is characterized in that: with the hydrolysis under the certain condition in acid microemulsion of titanium source, and by regulating the anionic proportioning of aqueous phase, make titanium dioxide micro latex, change over to then to have and carry out hydro-thermal breakdown of emulsion crystallization in the teflon-lined autoclave, obtain the controlled titanium dioxide optical catalyst material of anatase and rutile crystal type ratio.
2, preparation method as claimed in claim 1 is characterized in that described titanium source is one or more the combination in butyl titanate, metatitanic acid isopropyl ester, metatitanic acid second fat, metatitanic acid formicester, titanium tetrachloride, the titanium sulfate.
3, preparation method as claimed in claim 2 is characterized in that described titanium source molar concentration in microemulsion is 1-0.05M.
4, preparation method as claimed in claim 3 is characterized in that the preferred 0.5-0.1M of described titanium source molar concentration in microemulsion.
5, preparation method as claimed in claim 1, the acidity that it is characterized in that described microemulsion water is 8-12M.
6, preparation method as claimed in claim 1, it is characterized in that described hydrolysising condition is: temperature is 10-60 ℃, the time is 1-12 hour.
7, preparation method as claimed in claim 1 is characterized in that described anion is chlorion and sulfate ion.
8, preparation method as claimed in claim 6, it is characterized in that described chlorion source is one or both combinations in hydrochloric acid, ammonium chloride, potassium chloride, the sodium chloride, the sulfate ion source is one or both combinations in sulfuric acid, ammonium sulfate, potassium sulfate, the sodium sulphate.
9, preparation method as claimed in claim 6 is characterized in that described sulfate ion accounts for the 0.32%-1.6% of chlorion and sulfate ion mole total amount.
10, preparation method as claimed in claim 1, it is characterized in that described hydro-thermal breakdown of emulsion crystallization condition is: temperature is 100-140 ℃, and the time is 10-16 hour.
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| CN100450936C (en) * | 2007-02-16 | 2009-01-14 | 武汉大学 | Preparation method of Nano TiO2 composite sol having visible light catalytic activation |
| CN102126750A (en) * | 2010-12-31 | 2011-07-20 | 东莞市明天纳米科技有限公司 | Preparation method of anatase nano titanium dioxide |
| CN102151561A (en) * | 2011-01-22 | 2011-08-17 | 浙江理工大学 | Photocatalyst consisting of carbon nanotubes loaded with titanium dioxide and preparation method thereof |
| CN103537286A (en) * | 2013-10-28 | 2014-01-29 | 湛江师范学院 | Single-step hydrothermal micro-emulsion method for preparing iron-doped nano titanium dioxide powder |
| CN105126800A (en) * | 2015-08-24 | 2015-12-09 | 苏州聚康新材料科技有限公司 | Granite-loaded nano titanium dioxide photo-catalytic material and preparation method therefor |
| CN105195125A (en) * | 2015-08-24 | 2015-12-30 | 苏州聚康新材料科技有限公司 | Feldspar loaded nano-titanium dioxide photocatalytic material and preparation method thereof |
| CN106367809A (en) * | 2016-10-31 | 2017-02-01 | 南昌大学 | Method for preparing monocrystalline anatase TiO2 nanorod array with superhydrophilicity |
| CN106622198A (en) * | 2016-11-29 | 2017-05-10 | 湖北大学 | Composite nano-structured titanium dioxide photocatalyst and preparation method thereof |
| CN107253736A (en) * | 2017-08-16 | 2017-10-17 | 四川理工学院 | A kind of preparation method of anatase titanium dioxide monocrystalline |
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| CN111790414A (en) * | 2020-08-10 | 2020-10-20 | 齐鲁工业大学 | Mixed crystal TiO2BiOBr composite material and preparation method and application thereof |
| CN111847505A (en) * | 2020-06-17 | 2020-10-30 | 山东师范大学 | Method for preparing titanium dioxide based on ternary eutectic solvent, titanium dioxide material and application |
| CN113135591A (en) * | 2021-03-24 | 2021-07-20 | 湖北文理学院 | Preparation method of titanium dioxide nanorod array |
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| CN100450936C (en) * | 2007-02-16 | 2009-01-14 | 武汉大学 | Preparation method of Nano TiO2 composite sol having visible light catalytic activation |
| CN102126750A (en) * | 2010-12-31 | 2011-07-20 | 东莞市明天纳米科技有限公司 | Preparation method of anatase nano titanium dioxide |
| CN102126750B (en) * | 2010-12-31 | 2013-08-28 | 东莞市明天纳米科技有限公司 | Preparation method of anatase nano titanium dioxide |
| CN102151561A (en) * | 2011-01-22 | 2011-08-17 | 浙江理工大学 | Photocatalyst consisting of carbon nanotubes loaded with titanium dioxide and preparation method thereof |
| CN103537286A (en) * | 2013-10-28 | 2014-01-29 | 湛江师范学院 | Single-step hydrothermal micro-emulsion method for preparing iron-doped nano titanium dioxide powder |
| CN103537286B (en) * | 2013-10-28 | 2015-06-17 | 湛江师范学院 | Single-step hydrothermal micro-emulsion method for preparing iron-doped nano titanium dioxide powder |
| CN105126800A (en) * | 2015-08-24 | 2015-12-09 | 苏州聚康新材料科技有限公司 | Granite-loaded nano titanium dioxide photo-catalytic material and preparation method therefor |
| CN105195125A (en) * | 2015-08-24 | 2015-12-30 | 苏州聚康新材料科技有限公司 | Feldspar loaded nano-titanium dioxide photocatalytic material and preparation method thereof |
| CN106367809A (en) * | 2016-10-31 | 2017-02-01 | 南昌大学 | Method for preparing monocrystalline anatase TiO2 nanorod array with superhydrophilicity |
| CN106622198A (en) * | 2016-11-29 | 2017-05-10 | 湖北大学 | Composite nano-structured titanium dioxide photocatalyst and preparation method thereof |
| CN106622198B (en) * | 2016-11-29 | 2019-07-23 | 湖北大学 | A kind of composite nanostructure titanium dioxide optical catalyst and preparation method thereof |
| CN107253736A (en) * | 2017-08-16 | 2017-10-17 | 四川理工学院 | A kind of preparation method of anatase titanium dioxide monocrystalline |
| CN107253736B (en) * | 2017-08-16 | 2019-03-12 | 四川理工学院 | A kind of preparation method of anatase titanium dioxide monocrystalline |
| CN108246067A (en) * | 2018-01-19 | 2018-07-06 | 宿迁艾润科技有限公司 | A kind of smell photocatalysis purifier |
| CN111847505A (en) * | 2020-06-17 | 2020-10-30 | 山东师范大学 | Method for preparing titanium dioxide based on ternary eutectic solvent, titanium dioxide material and application |
| CN111847505B (en) * | 2020-06-17 | 2023-03-07 | 山东师范大学 | Method for preparing titanium dioxide based on ternary eutectic solvent, titanium dioxide material and application |
| CN111790414A (en) * | 2020-08-10 | 2020-10-20 | 齐鲁工业大学 | Mixed crystal TiO2BiOBr composite material and preparation method and application thereof |
| CN113135591A (en) * | 2021-03-24 | 2021-07-20 | 湖北文理学院 | Preparation method of titanium dioxide nanorod array |
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