CN104028290A - Method for preparing sulfur-nitrogen co-doped nanometer titanium dioxide through rapid sol-gel process - Google Patents
Method for preparing sulfur-nitrogen co-doped nanometer titanium dioxide through rapid sol-gel process Download PDFInfo
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Abstract
The invention discloses a method for preparing sulfur-nitrogen co-doped nanometer titanium dioxide through a rapid sol-gel process. The method specifically comprises the following steps: step 1. preparing a sulfur-nitrogen co-doped nanometer titanium dioxide sol-gel precursor; step 2. adding deionized water into the sulfur-nitrogen co-doped nanometer titanium dioxide sol-gel precursor obtained in the step 1, stirring and standing to obtain wet gel; step 3. putting the wet gel obtained in the step 2 into a drying oven, drying at the temperature of 70-90 DEG C to obtain dried gel in which the solvent and moisture are removed; and step 4. sequentially grinding and calcining the dried gel obtained in the step 3 to obtain anatase type sulfur-nitrogen co-doped nanometer titanium dioxide. According to the method for preparing the sulfur-nitrogen co-doped nanometer titanium dioxide through the rapid sol-gel process, a sulfur-nitrogen co-doped nanometer titanium dioxide photocatalyst with visible-light activity can be prepared, a white flocculent is avoided in the gelling process, and the production cycle is shortened.
Description
Technical field
The invention belongs to catalysis material preparation method technical field, relate to a kind of method that fast sol-gel is prepared sulfur and nitrogen co-doped nano titanium oxide.
Background technology:
In the research of semiconductor nano photochemical catalyst, TiO
2have advantages of that oxidability is strong, nontoxic, biochemistry and photochemical stability good, thereby the core status in photocatalysis research always.But, due to TiO
2the energy gap of (anatase) is large, under the exciting of ultraviolet light, could show catalytic activity, and sunshine medium ultraviolet light energy only accounts for 4%, and visible light energy accounts for 43%.Doping vario-property TiO how
2, make its photocatalytic activity and catalytic efficiency be improved the focus that becomes current research.
Doping is incorporated into a certain amount of impurity in the lattice of titanium dioxide exactly, thereby affect the generation of electron hole pair, compound and transmittance process, therefore the photocatalytic activity of titanium dioxide also changes, and the energy level of foreign ion may be arranged in the forbidden band of titanium dioxide, the level structure that causes semiconductor crystal changes, thereby has expanded absorption optical wavelength range.The doping of sulphur and nitrogen is at TiO
2middle introducing Lattice Oxygen vacancy, or partial oxygen vacancy replaced by sulphur and nitrogen, makes TiO
2taboo width, thereby expand the response range of sunshine, ultraviolet light and visible ray are all had more by force and are absorbed, aspect degradation of contaminant, show common nano-TiO
2incomparable photocatalysis efficiency.
Utilize sol-gel process to prepare TiO
2photochemical catalyst is a kind of common method, but exists the cycle to grow and easily generate the shortcoming of white floccule.
Summary of the invention
The object of the present invention is to provide a kind of fast sol-gel to prepare the method for sulfur and nitrogen co-doped nano titanium oxide, can prepare the sulfur and nitrogen co-doped nano titanium oxide with visible light activity, not only in gel process, can adularescent flocculent deposit not generate, also shortened the production cycle.
The technical solution adopted in the present invention is that fast sol-gel is prepared the method for sulfur and nitrogen co-doped nano titanium oxide, specifically according to following steps, implements:
Step 1, prepare sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor;
Step 2, remove ionized water and add in the sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor obtaining through step 1, through stirring, after standing, obtain sulfur and nitrogen co-doped nano titanium oxide wet gel;
Step 3, the sulfur and nitrogen co-doped nano titanium oxide wet gel obtaining through step 2 is put into baking oven, under 70 ℃～90 ℃ conditions, carry out drying and processing, obtain removing the sulfur and nitrogen co-doped nano titanium oxide xerogel of solvent and moisture;
Step 4, by the sulfur and nitrogen co-doped nano titanium oxide xerogel obtaining through step 3 successively through grinding, obtain the sulfur and nitrogen co-doped nano titanium oxide of Detitanium-ore-type after calcining.
Feature of the present invention is also:
Step 1 is specifically implemented according to following steps:
Step 1.1, under room temperature, be that 10～15:1 measures respectively absolute ethyl alcohol and butyl titanate by volume;
Step 1.2, according to the consumption of butyl titanate in step 1.1, get respectively thiocarbamide and urea, the mol ratio of thiocarbamide, urea, butyl titanate is 0.25～1:0.5～1:1;
Step 1.3, the absolute ethyl alcohol measuring in step 1.1 is mixed with butyl titanate, preparation obtains mixture A;
Step 1.4, the thiocarbamide in step 1.2 and urea are added in the mixture A obtaining through step 1.3, obtain mixture B;
Step 1.5, get diluted acid and add in the mixture B obtaining through step 1.4, regulate the concentration of mixture B, until the pH value of mixture B is 3～4, complete the acidity adjustment to mixture B;
Step 1.6, the mixture B that regulates acidity through step 1.5 is stirred to 10min～30min, obtain sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor.
Diluted acid in step 1.5 is that mass percent concentration is rare nitric acid of 4%～6%.
Step 2 is specifically implemented according to following steps:
Step 2.1, by the deionized water that measures of the absolute ethyl alcohol measuring in step 1.1, the volume ratio 0.05～0.1:1 of deionized water and absolute ethyl alcohol;
Step 2.2, the deionized water measuring through step 2.1 is added dropwise in the sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor obtaining through step 1, dropwise rear stirring 20min～40min, standing 40min～90min again, obtains sulfur and nitrogen co-doped nano titanium oxide wet gel afterwards.
In step 2.2, adopt constant pressure funnel that deionized water is added dropwise in sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor.
Step 4 is specifically implemented according to following steps:
Step 4.1, the sulfur and nitrogen co-doped nano titanium oxide obtaining through step 3 is ground to 5min～15min, obtain sulfur and nitrogen co-doped nano titanium oxide dry gel powder;
Step 4.2, the sulfur and nitrogen co-doped nano titanium oxide dry gel powder obtaining through step 4.1 is poured in crucible, under 400 ℃～550 ℃ conditions, calcined 3.5h～4.5h, obtain the sulfur and nitrogen co-doped nano titanium oxide of Detitanium-ore-type.
What in step 4.2, calcining adopted is Muffle furnace.
Beneficial effect of the present invention is:
1) method that fast sol-gel of the present invention is prepared sulfur and nitrogen co-doped nano titanium oxide has changed traditional sol-gel process, traditional sol-gel process all can add water when dissolving thiocarbamide and urea, and the method is that in the end a step just drips water, in order to solve the problem that easily generates white floccule in sol-gel process, long shortcoming experimental period that overcomes Study on Synthesis of Nanocrystal Titanium Dionide, process operation is very simple;
2) the sulfur and nitrogen co-doped nano titanium oxide UV, visible light optical absorption edge red shift that the method for utilizing fast sol-gel of the present invention to prepare sulfur and nitrogen co-doped nano titanium oxide is prepared, electron-hole recombination rate reduce, and photocatalysis efficiency improves;
3) the sulfur and nitrogen co-doped nano titanium oxide crystal grain that the method for utilizing fast sol-gel of the present invention to prepare sulfur and nitrogen co-doped nano titanium oxide is prepared is little, and titania is between 10nm～15nm.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the sulfur and nitrogen co-doped nano titanium oxide prepared of the method for utilizing fast sol-gel of the present invention to prepare sulfur and nitrogen co-doped nano titanium oxide;
Fig. 2 is the sulfur and nitrogen co-doped nano titanium oxide prepared of the method for utilizing fast sol-gel of the present invention to prepare sulfur and nitrogen co-doped nano titanium oxide and the UV-Vis DRS abosrption spectrogram of common nano titanium oxide;
Fig. 3 is the XPS figure of the sulfur and nitrogen co-doped nano titanium oxide prepared of the method for utilizing fast sol-gel of the present invention to prepare sulfur and nitrogen co-doped nano titanium oxide;
Fig. 4 is the sulfur and nitrogen co-doped nano titanium oxide prepared of the method for utilizing fast sol-gel of the present invention to prepare sulfur and nitrogen co-doped nano titanium oxide and the degraded figure of common nano titanium dioxide photocatalysis weak acid red.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Fast sol-gel of the present invention is prepared the method for sulfur and nitrogen co-doped nano titanium oxide, specifically according to following steps, implements:
Step 1, prepare sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor:
Step 1.1, under room temperature, be that 10～15:1 measures respectively absolute ethyl alcohol and butyl titanate by volume;
Step 1.2, according to the consumption of butyl titanate in step 1.1, get respectively thiocarbamide and urea, the mol ratio of thiocarbamide, urea, butyl titanate is 0.25～1:0.5～1:1;
Step 1.3, the absolute ethyl alcohol measuring in step 1.1 is mixed with butyl titanate, preparation obtains mixture A;
Step 1.4, the thiocarbamide in step 1.2 and urea are added in the mixture A obtaining through step 1.3, obtain mixture B;
Step 1.5, to get mass percent concentration be that rare nitric acid of 4%～6% adds in the mixture B obtaining through step 1.4, regulates the concentration of mixture B, until the pH value of mixture B is 3～4, completes the acidity adjustment to mixture B;
Step 1.6, the mixture B that regulates acidity through step 1.5 is stirred to 10min～30min, obtain sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor.
Step 2, remove ionized water and add in the sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor obtaining through step 1, through stirring, after standing, obtain sulfur and nitrogen co-doped nano titanium oxide wet gel:
Step 2.1, by the deionized water that measures of the absolute ethyl alcohol measuring in step 1.1, the volume ratio 0.05～0.1:1 of deionized water and absolute ethyl alcohol;
Step 2.2, the deionized water measuring through step 2.1 is slowly added dropwise in the sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor obtaining through step 1 with constant pressure funnel, dropwise rear stirring 20min～40min, standing 40min～90min again, obtains sulfur and nitrogen co-doped nano titanium oxide wet gel afterwards.
Step 3, the wet gel obtaining through step 2 is put into baking oven, under 70 ℃～90 ℃ conditions, carry out drying and processing, obtain removing the sulfur and nitrogen co-doped nano titanium oxide xerogel of solvent and moisture;
Step 4, by the sulfur and nitrogen co-doped nano titanium oxide xerogel obtaining through step 3 successively through grinding, obtain the sulfur and nitrogen co-doped nano titanium oxide of Detitanium-ore-type after calcining:
Step 4.1, the sulfur and nitrogen co-doped nano titanium oxide obtaining through step 3 is ground to 5min～15min, obtain sulfur and nitrogen co-doped nano titanium oxide dry gel powder;
Step 4.2, the sulfur and nitrogen co-doped nano titanium oxide dry gel powder obtaining through step 4.1 is poured in crucible, under 400 ℃～550 ℃ conditions, in Muffle furnace, calcined 3.5h～4.5h, obtain the sulfur and nitrogen co-doped nano titanium oxide of Detitanium-ore-type.
Fig. 1 is S-N-TiO
2photochemical catalyst XRD collection of illustrative plates can be found: S-N-TiO from Fig. 1
2the diffraction maximum peak shape of photochemical catalyst is rather sharp-pointed, and crystal formation forming degree is high, and its particle diameter is 12.94nm; This shows the sulfur and nitrogen co-doped nano-TiO of preparing
2be that nanoscale and moulding are good, particle diameter is very little, illustrates that the doping of sulphur, nitrogen effectively suppresses the particle diameter growth of photochemical catalyst, improves the activity of photochemical catalyst.
Fig. 2 is TiO
2, S-N-TiO
2photochemical catalyst UV-Vis collection of illustrative plates, as can be seen from Figure 2: pure nano-TiO
2absorption spectrum mainly concentrate at ultraviolet region; Nano-TiO through the doping of sulphur nitrogen
2spectral response range is widened, and not only at ultraviolet region, has stronger absorption, and still has stronger absorption at visible region.
Fig. 3 is S-N-TiO
2the XPS of photochemical catalyst composes entirely, as can be seen from Figure 3: S-N-TiO
2by S, N, Ti, O and a small amount of C, formed, show that S and N are all doped into TiO
2in photochemical catalyst.
Fig. 4 TiO
2, S-N-TiO
2photocatalyst for degrading weak acid red, as can be seen from Figure 4: S-N-TiO
2the degradation rate of photochemical catalyst is always higher than pure nano-TiO
2, S-N-TiO during to 120min
2the degradation rate of photochemical catalyst approaches 100%, shows that the doping of S and N effectively improves the activity of catalyst.
Embodiment 1
Under room temperature, for 10:1, measure respectively absolute ethyl alcohol and butyl titanate by volume, according to the amount of the butyl titanate measuring, get respectively thiocarbamide and urea, the mol ratio of thiocarbamide, urea, butyl titanate is 0.25:1:1; The absolute ethyl alcohol measuring is mixed with butyl titanate, and preparation obtains mixture A; Thiocarbamide and urea are added in mixture A, obtain mixture B; Get mass percent concentration and be rare nitric acid of 5% and add in mixture B, regulate the concentration of mixture B, until the pH value of mixture B is 3.5; The mixture B that regulates acidity is stirred to 20min, obtain sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor;
Amount by the absolute ethyl alcohol measuring measures deionized water, the volume ratio 0.05:1 of deionized water and absolute ethyl alcohol; The deionized water measuring is slowly added dropwise in sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor with constant pressure funnel, dropwises rear stirring 30min, standing 60min again, obtains sulfur and nitrogen co-doped nano titanium oxide wet gel afterwards;
The sulfur and nitrogen co-doped nano titanium oxide wet gel obtaining is put into baking oven, under 80 ℃ of conditions, carry out drying and processing, drying time is 4h, obtains removing the sulfur and nitrogen co-doped nano titanium oxide xerogel of solvent and moisture;
The sulfur and nitrogen co-doped nano titanium oxide xerogel obtaining is ground to 10min, obtain sulfur and nitrogen co-doped nano titanium oxide dry gel powder; The sulfur and nitrogen co-doped nano titanium oxide dry gel powder obtaining is poured in crucible, under 450 ℃ of conditions, in Muffle furnace, calcined 4h, obtain the sulfur and nitrogen co-doped nano titanium oxide of Detitanium-ore-type.
The average grain diameter that records the sulfur and nitrogen co-doped nano titanium oxide of Detitanium-ore-type is 12.56nm, sulfur and nitrogen co-doped nano-TiO
2absorption edge red shift is to 595nm, and energy gap is reduced to 2.08eV.
Embodiment 2
Under room temperature, for 12:1, measure respectively absolute ethyl alcohol and butyl titanate by volume, according to the butyl titanate measuring, get respectively thiocarbamide and urea, the mol ratio of thiocarbamide, urea, butyl titanate is 0.5:1:1; The absolute ethyl alcohol measuring is mixed with butyl titanate, and preparation obtains mixture A; Thiocarbamide and urea are added in mixture A, obtain mixture B; Get mass percent concentration and be rare nitric acid of 4% and add in mixture B, regulate the concentration of mixture B, until the pH value of mixture B is 3; The mixture B that regulates acidity is stirred to 10min, obtain sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor;
Amount by the absolute ethyl alcohol measuring measures deionized water, the volume ratio 0.07:1 of deionized water and absolute ethyl alcohol; The deionized water measuring is slowly added dropwise in sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor with constant pressure funnel, dropwises rear stirring 20min, standing 40min again, obtains sulfur and nitrogen co-doped nano titanium oxide wet gel afterwards;
The sulfur and nitrogen co-doped nano titanium oxide wet gel obtaining is put into baking oven, under 70 ℃ of conditions, carry out drying and processing, drying time is 4.5h, obtains removing the sulfur and nitrogen co-doped nano titanium oxide xerogel of solvent and moisture;
The sulfur and nitrogen co-doped nano titanium oxide xerogel obtaining is ground to 5min, obtain sulfur and nitrogen co-doped nano titanium oxide dry gel powder; The sulfur and nitrogen co-doped nano titanium oxide dry gel powder obtaining is poured in crucible, under 400 ℃ of conditions, in Muffle furnace, calcined 4.5h, obtain the sulfur and nitrogen co-doped nano titanium oxide of Detitanium-ore-type.
The average grain diameter that records the sulfur and nitrogen co-doped nano titanium oxide of Detitanium-ore-type is 10.42nm, sulfur and nitrogen co-doped nano-TiO
2absorption edge red shift is to 568nm, and energy gap is reduced to 2.18eV.
Embodiment 3
Under room temperature, for 15:1, measure respectively absolute ethyl alcohol and butyl titanate by volume, according to the butyl titanate measuring, get respectively thiocarbamide and urea, the mol ratio of thiocarbamide, urea, butyl titanate is 0.75:1:1; The absolute ethyl alcohol measuring is mixed with butyl titanate, and preparation obtains mixture A; Thiocarbamide and urea are added in mixture A, obtain mixture B; Get mass percent concentration and be rare nitric acid of 4% and add in mixture B, regulate the concentration of mixture B, until the pH value of mixture B is 4; The mixture B that regulates acidity is stirred to 13min, obtain sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor;
Amount by the absolute ethyl alcohol measuring measures deionized water, the volume ratio 0.1:1 of deionized water and absolute ethyl alcohol; The deionized water measuring is slowly added dropwise in sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor with constant pressure funnel, dropwises rear stirring 40min, standing 90min again, obtains sulfur and nitrogen co-doped nano titanium oxide wet gel afterwards;
The sulfur and nitrogen co-doped nano titanium oxide wet gel obtaining is put into baking oven, under 90 ℃ of conditions, carry out drying and processing, drying time is 3.5h, obtains removing the sulfur and nitrogen co-doped nano titanium oxide xerogel of solvent and moisture;
The sulfur and nitrogen co-doped nano titanium oxide xerogel obtaining is ground to 15min, obtain sulfur and nitrogen co-doped nano titanium oxide dry gel powder; The sulfur and nitrogen co-doped nano titanium oxide dry gel powder obtaining is poured in crucible, under 550 ℃ of conditions, in Muffle furnace, calcined 3.5h, obtain the sulfur and nitrogen co-doped nano titanium oxide of Detitanium-ore-type.
The average grain diameter that records the sulfur and nitrogen co-doped nano titanium oxide of Detitanium-ore-type is 12.94nm, sulfur and nitrogen co-doped nano-TiO
2absorption edge red shift is to 588nm, and energy gap is reduced to 2.11eV.
It is Detitanium-ore-type that the sulphur nitrogen that the method that adopts fast sol-gel of the present invention to prepare sulfur and nitrogen co-doped nano titanium oxide prepares is mixed nano titanium oxide altogether, and particle size is between 10nm～15nm.
The method that fast sol-gel of the present invention is prepared sulfur and nitrogen co-doped nano titanium oxide has changed traditional sol-gel process, traditional sol-gel process all can add water when dissolving thiocarbamide and urea, and the method is that in the end a step just drips water, in order to solve the problem that easily generates white floccule in sol-gel process, long shortcoming experimental period that overcomes Study on Synthesis of Nanocrystal Titanium Dionide, process operation is very simple.
Claims (7)
1. fast sol-gel is prepared the method for sulfur and nitrogen co-doped nano titanium oxide, it is characterized in that, specifically according to following steps, implements:
Step 1, prepare sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor;
Step 2, remove ionized water and add in the sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor obtaining through step 1, through stirring, after standing, obtain sulfur and nitrogen co-doped nano titanium oxide wet gel;
Step 3, the sulfur and nitrogen co-doped nano titanium oxide wet gel obtaining through step 2 is put into baking oven, under 70 ℃～90 ℃ conditions, carry out drying and processing, obtain removing the sulfur and nitrogen co-doped nano titanium oxide xerogel of solvent and moisture;
Step 4, by the sulfur and nitrogen co-doped nano titanium oxide xerogel obtaining through step 3 successively through grinding, obtain the sulfur and nitrogen co-doped nano titanium oxide of Detitanium-ore-type after calcining.
2. fast sol-gel according to claim 1 is prepared the method for sulfur and nitrogen co-doped nano titanium oxide, it is characterized in that, described step 1 is specifically implemented according to following steps:
Step 1.1, under room temperature, be that 10～15:1 measures respectively absolute ethyl alcohol and butyl titanate by volume;
Step 1.2, according to the consumption of butyl titanate in step 1.1, get respectively thiocarbamide and urea, the mol ratio of thiocarbamide, urea, butyl titanate is 0.25～1:0.5～1:1;
Step 1.3, the absolute ethyl alcohol measuring in step 1.1 is mixed with butyl titanate, preparation obtains mixture A;
Step 1.4, the thiocarbamide in step 1.2 and urea are added in the mixture A obtaining through step 1.3, obtain mixture B;
Step 1.5, get diluted acid and add in the mixture B obtaining through step 1.4, regulate the concentration of mixture B, until the pH value of mixture B is 3～4, complete the acidity adjustment to mixture B;
Step 1.6, the mixture B that regulates acidity through step 1.5 is stirred to 10min～30min, obtain sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor.
3. fast sol-gel according to claim 2 is prepared the method for sulfur and nitrogen co-doped nano titanium oxide, it is characterized in that, the diluted acid in described step 1.5 is that mass percent concentration is rare nitric acid of 4%～6%.
4. fast sol-gel according to claim 1 is prepared the method for sulfur and nitrogen co-doped nano titanium oxide, it is characterized in that, described step 2 is specifically implemented according to following steps:
Step 2.1, by the deionized water that measures of the absolute ethyl alcohol measuring in step 1.1, the volume ratio 0.05～0.1:1 of deionized water and absolute ethyl alcohol;
Step 2.2, the deionized water measuring through step 2.1 is added dropwise in the sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor obtaining through step 1, dropwise rear stirring 20min～40min, standing 40min～90min again, obtains sulfur and nitrogen co-doped nano titanium oxide wet gel afterwards.
5. fast sol-gel according to claim 4 is prepared the method for sulfur and nitrogen co-doped nano titanium oxide, it is characterized in that, in described step 2.2, adopt constant pressure funnel that deionized water is added dropwise in sulfur and nitrogen co-doped nano titanic oxide sol-Gel Precursor.
6. fast sol-gel according to claim 1 is prepared the method for sulfur and nitrogen co-doped nano titanium oxide, it is characterized in that, described step 4 is specifically implemented according to following steps:
Step 4.1, the sulfur and nitrogen co-doped nano titanium oxide obtaining through step 3 is ground to 5min～15min, obtain sulfur and nitrogen co-doped nano titanium oxide dry gel powder;
Step 4.2, the sulfur and nitrogen co-doped nano titanium oxide dry gel powder obtaining through step 4.1 is poured in crucible, under 400 ℃～550 ℃ conditions, calcined 3.5h～4.5h, obtain the sulfur and nitrogen co-doped nano titanium oxide of Detitanium-ore-type.
7. fast sol-gel according to claim 6 is prepared the method for sulfur and nitrogen co-doped nano titanium oxide, it is characterized in that, what in described step 4.2, calcining adopted is Muffle furnace.
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| CN108906107A (en) * | 2018-07-06 | 2018-11-30 | 广东海洋大学 | A kind of preparation method of sulfur and nitrogen co-doped titanium dioxide |
| CN109574333A (en) * | 2018-12-06 | 2019-04-05 | 东南大学 | A kind of copper modification nitrogen-doped titanium dioxide material and its preparation method and application |
| CN111924872A (en) * | 2020-08-10 | 2020-11-13 | 东莞世皓新材料生物科技有限公司 | Method for preparing modified nano zinc oxide by sol-gel process |
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