CN113828293A - Improve TiO2Method for surface photovoltage - Google Patents

Improve TiO2Method for surface photovoltage Download PDF

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CN113828293A
CN113828293A CN202111232657.7A CN202111232657A CN113828293A CN 113828293 A CN113828293 A CN 113828293A CN 202111232657 A CN202111232657 A CN 202111232657A CN 113828293 A CN113828293 A CN 113828293A
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straw
tio
surface photovoltage
carbon
ethyl alcohol
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CN113828293B (en
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陈久福
钟俊波
黄生田
李建章
李敏娇
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Sichuan University of Science and Engineering
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Sichuan University of Science and Engineering
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063—Titanium; Oxides or hydroxides thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties

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Abstract

The invention relates to a method for improving TiO content2Method of surface photovoltage. The method comprises the following steps: drying, powdering and screening the straw cores, and roasting in an inert atmosphere to obtain straw carbon; dispersing a certain amount of straw carbon and butyl titanate into absolute ethyl alcohol; dropwise adding deionized water into a straw carbon-butyl titanate-absolute ethyl alcohol suspension system by using a constant flow pump, stirring, transferring the suspension into a hydrothermal reaction kettle for hydrothermal treatment, carrying out vacuum filtration, washing with deionized water and absolute ethyl alcohol, drying, and grinding to obtain the TiO with enhanced surface photovoltage signals2And (3) sampling. The application can obviously improve TiO content by the auxiliary preparation of proper amount of straw carbon2Surface photovoltage signal of, this study was directed to propelling TiO2The practical application of the photocatalytic material has practical significance. In addition, the surface photovoltage signal of the invention is obviously enhanced TiO2The preparation method has the advantages that the raw materials are low in price and easy to realize; meanwhile, the waste straw is recycled, and the environment is protected.

Description

Improve TiO2Method for surface photovoltage
Technical Field
The invention relates to the field of material chemistry, in particular to the field of photocatalytic materials, and specifically relates to a method for improving TiO content2Method for surface photovoltage。
Background
Titanium dioxide (TiO)2) The photocatalyst is a most ideal photocatalyst because of the advantages of low cost, stability, no toxicity, excellent performance and the like, and is known to be the most ideal photocatalyst in the degradation of organic pollutants by the photocatalyst2As a photocatalyst, there is a limitation in its use: TiO 22The forbidden band width of the light source is about 3.2eV, and the light source can only be driven by ultraviolet light (the wavelength is less than or equal to 385nm), which seriously hinders the practical application of the light source under the irradiation of visible light. Furthermore, TiO2The photo-generated electrons and holes have higher recombination rate, and the scale application of the photo-generated electrons and holes is further limited. Therefore, it is imperative to improve the separation of photogenerated carriers. To make TiO2The method has a satisfactory effect on photocatalytic organic pollutant degradation, and the modification of titanium dioxide is urgently needed to improve the photocatalytic performance of titanium dioxide.
Heterogeneous photocatalytic reactions mainly occur on the surface of the photocatalyst, so that the surface properties (structural properties, surface hydroxyl content, surface trapping states, oxygen vacancies and the like) of the photocatalyst inevitably affect the response capability of the photocatalyst to light, the separating behavior of photo-generated charges and the adsorption capability of organic pollutants, thereby affecting the photocatalytic activity. Thus, by modifying or manipulating TiO2The surface property of the photo-generated electron-hole pair is an effective strategy for improving the photocatalytic activity.
The photocatalytic reaction is a physical and chemical process which occurs on the surface of a photocatalyst, and many studies show that TiO is modified by carbon materials2Is an effective method for improving the photocatalytic performance. The carbon material can be used as a good conductor of electrons, thereby accelerating e-/h+And (4) separating the pairs. In recent years, biomass charcoal using renewable waste biomass and agricultural and sideline products (such as sorghum straws and corn straws) as raw materials is considered as a bright star in the field of environmental protection. The biomass charcoal has the characteristics of easily available raw materials, good heat conductivity, rich surface functional groups and the like, so that the biomass charcoal becomes an ideal material for preparing the photocatalyst with excellent performance. The carbon material is used for modifying the photocatalytic material, and the photocatalytic material with excellent photocatalytic performance is expected to be obtained.
When the photocatalyst absorbs a certain amount of photon energy, photo-generated charges are generated. The separation of the photo-generated electrons and holes results in a change in the surface barrier of the photocatalyst. The difference between the surface barrier in light and the surface barrier in the dark produces an electrical signal that is captured and processed to form a surface photovoltage spectrum. High surface photovoltages benefit from an efficient photogenerated carrier separation speed. Among all the factors that influence photocatalytic activity, the rate of photogenerated charge separation plays a primary role. The high separation speed of the photon-generated carriers is beneficial to generating more active free radicals, thereby accelerating the degradation of environmental pollutants and showing high photocatalytic performance.
Disclosure of Invention
The invention provides a method for improving TiO content based on the problems in the prior art2The method for surface photovoltage adopts cheap raw materials, is easy to realize, realizes the reutilization of waste straws, is beneficial to environmental protection, and prepares the obtained TiO2The surface photovoltage signal is obviously enhanced in the range of 300-400 nm.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
improve TiO2A method of surface photovoltage comprising the steps of:
step one, drying, powdering and screening straw cores, and roasting in an inert atmosphere to obtain straw carbon for later use;
secondly, dispersing the straw carbon and the butyl titanate into absolute ethyl alcohol to obtain a suspension system for later use;
thirdly, dropwise adding deionized water into a straw carbon-butyl titanate-absolute ethyl alcohol suspension system by using a constant flow pump, and stirring to form a suspension; transferring the suspension into a hydrothermal reaction kettle for hydrothermal treatment, performing reduced pressure suction filtration, washing, drying and grinding to obtain the TiO with enhanced surface photovoltage signal2。
As a preferred embodiment in this application, in the first step, the straw core is any one of a sorghum straw core or a corn straw core.
As a preferred embodiment of the present application, in the first step, the straw core is sieved to have a particle size of 80-150 mesh.
As a preferred embodiment of the present application, in the first step, the inert atmosphere is N2Ar or NH3Any one of them.
As a preferred embodiment of the present application, in the first step, the inert atmosphere calcination temperature is 600-900 ℃.
As a preferred embodiment of the present application, in the first step, the inert atmosphere calcination time is 1 to 3 hours.
As a better embodiment in the application, in the second step, the mass ratio of the straw carbon to the tetrabutyl titanate is 0.1-5.5%.
As a preferred embodiment of the present application, in the second step, the ratio of the mass g of tetrabutyl titanate to the volume mL of absolute ethanol is from 2:1 to 1:2, preferably 1: 2.
As a preferred embodiment of the present application, in the third step, the volume ratio of the deionized water to the absolute ethyl alcohol is 1:2 to 2:1, preferably 2: 1.
As a preferred embodiment of the present application, in the third step, the temperature of the hydrothermal reaction is 140 ℃ to 180 ℃.
As a preferred embodiment of the present application, in the third step, the hydrothermal reaction time is 12 to 24 hours.
The TiO with the enhanced surface photovoltage signal is prepared by the method2The surface photovoltage signal of the photocatalytic material is obviously enhanced in the range of 300-400 nm.
Compared with the prior art, the invention has the beneficial effects that:
first, the surface photovoltage signal of the invention is obviously enhanced TiO2The preparation method has the advantages of cheap raw materials and low cost, and can realize the reutilization of the waste straws.
(II) TiO prepared by auxiliary preparation of proper amount of straw carbon2The surface photovoltage signal is obviously enhanced in the range of 300-400 nm, which has important practical significance for improving the photocatalytic activity.
Drawings
FIG. 1 shows TiO prepared without adding straw charcoal2XRD pattern of the sample.
FIG. 2 shows TiO prepared without adding straw charcoal2And the surface photovoltage signals of the samples obtained in example 1.
FIG. 3 shows TiO prepared without adding straw charcoal2And the surface photovoltage signal of the sample obtained in example 2.
FIG. 4 shows TiO prepared without adding straw charcoal2And the surface photovoltage signal of the sample obtained in example 3.
FIG. 5 shows TiO prepared without adding straw charcoal2And the surface photovoltage signal of the sample obtained in example 4.
FIG. 6 shows TiO prepared without adding straw charcoal2And the surface photovoltage signals of the samples obtained in example 5.
FIG. 7 shows TiO prepared without adding straw charcoal2And the surface photovoltage signals of the samples obtained in example 6.
FIG. 8 shows TiO prepared without adding straw charcoal2And the surface photovoltage signal of the sample obtained in example 7.
FIG. 9 shows TiO prepared without straw char2And the surface photovoltage signals of the samples obtained in example 8.
FIG. 10 shows TiO prepared without straw char2And the surface photovoltage signal of the sample obtained in example 9.
FIG. 11 shows TiO prepared without straw char2And the surface photovoltage signals of the samples obtained in example 10.
FIG. 12 shows TiO prepared without straw char2And the surface photovoltage signal of the sample obtained in example 11.
FIG. 13 shows TiO prepared without straw char2And the surface photovoltage signal of the sample obtained in example 12.
FIG. 14 shows TiO prepared without straw char2And the surface photovoltage signal of the sample obtained in example 13.
FIG. 15 shows TiO prepared without straw char2And the surface photovoltage signal of the sample obtained in example 14.
FIG. 16 shows TiO prepared without straw charcoal2And the surface photovoltage signal of the sample obtained in example 15.
FIG. 17 shows TiO prepared without straw charcoal2And the surface photovoltage signals of the samples obtained in example 16.
Detailed Description
Improve TiO2A method of surface photovoltage comprising the steps of:
step one, drying, powdering and screening straw cores, and roasting in an inert atmosphere to obtain straw carbon for later use;
secondly, dispersing the straw carbon and the butyl titanate into absolute ethyl alcohol to obtain a suspension system for later use;
thirdly, dropwise adding deionized water into a straw carbon-butyl titanate-absolute ethyl alcohol suspension system by using a constant flow pump, and stirring to form a suspension; transferring the suspension into a hydrothermal reaction kettle for hydrothermal treatment, performing reduced pressure suction filtration, washing, drying and grinding to obtain the TiO with enhanced surface photovoltage signal2。
Preferably, in the first step, the straw core is any one of sorghum or corn straw.
Preferably, in the first step, the inert atmosphere is N as a preferred embodiment of the present application2Ar or NH3Any one of them.
Preferably, in the first step, the inert atmosphere roasting temperature is 600-900 ℃.
Preferably, in the first step, the inert atmosphere roasting time is 1-3 h.
Preferably, in the second step, the mass ratio of the straw carbon to the tetrabutyl titanate is 0.1-5.5%.
Preferably, in the second step, the ratio of the mass g of tetrabutyl titanate to the volume mL of absolute ethanol is 1: 2.
Preferably, in the third step, the volume ratio of the deionized water to the absolute ethyl alcohol is 2: 1.
Preferably, in the third step, the temperature of the hydrothermal reaction is 140-180 ℃.
Preferably, in the third step, the hydrothermal reaction time is 12-24 h.
The TiO with the enhanced surface photovoltage signal prepared by the method2The surface photovoltage signal of the photocatalytic material is obviously enhanced in a range of 300-400 nm.
In order to facilitate the understanding of the present invention, the catalyst and the preparation method thereof will be further described with reference to the accompanying drawings and the detailed description. It should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples.
In the present document,% represents wt% unless otherwise specified.
In the examples described below, XRD was tested on a DX-2600X-ray diffractometer; the surface photovoltage test is carried out on a surface photovoltage spectrum assembled in Jilin university, a xenon lamp is used as a light source, a phase-locked amplifier is used for amplifying an acquired signal, a sample is pressed between conductive glass and a metal copper base, the wavelength test range is 300-400 nm, and the specific test method and the operation adopt conventional technical means.
Comparative example 1:
1) weighing 10g of butyl titanate, dissolving in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the solution by using a constant flow pump; and (3) continuously stirring the formed suspension system for 30min, then transferring the suspension system into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 24h at 180 ℃, and naturally cooling to room temperature.
2) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2The optical voltage signal and XRD were measured. FIG. 1 shows the TiO prepared2The XRD spectrum of the product shows that the prepared sample is TiO with anatase and rutile coexisting2。
Example 1:
this example shows surface photovoltage signal enhanced TiO2The preparation process is as follows:
1) collecting corn straws, peeling, taking straw cores, drying the straw cores for later use, fully crushing the dried straw cores by using a portable high-speed universal crusher (DFT-200), and sieving the crushed straw cores by using a 100-mesh sieve; roasting the screened straw powder for 1.5h at 600 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.01g of the straw carbon, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; and (3) continuously stirring the formed suspension system for 30min, then transferring the suspension system into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 24h at 180 ℃, and naturally cooling to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical voltage signal.
Compared with the comparative example 1, the straw carbon obtained by roasting for 1.5 hours at the temperature of 600 ℃ is added, and the mass ratio of the straw carbon to the butyl titanate is 0.1%.
Fig. 2 is a graph comparing surface photovoltage signals of samples obtained in example 1 and comparative example 1. As can be seen from FIG. 2, TiO prepared by the aid of straw carbon2And TiO prepared without the assistance of straw carbon in the range of 300-400 nm2The surface photovoltage signal is obviously enhanced, and the TiO can be enhanced by the auxiliary preparation of proper amount of straw carbon2A surface photovoltage signal.
Example 2:
this example shows surface photovoltage signal enhanced TiO2The preparation process is as follows:
1) collecting sorghum straws, peeling, taking straw cores, drying the straw cores for later use, fully crushing the dried straw cores by using a portable high-speed universal crusher (DFT-200), and sieving the crushed straw cores by using a 100-mesh sieve; roasting the screened straw powder for 2 hours at 700 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.1g of the straw carbon, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; the formed suspension system is continuously stirred for 30min, then transferred into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, subjected to hydrothermal reaction for 20h at 140 ℃, and naturally cooled to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical voltage signal.
Compared with the comparative example 1, the straw carbon obtained by roasting for 2 hours at 700 ℃ is added, the mass ratio of the straw carbon to the butyl titanate is 1 percent, the hydrothermal temperature is 140 ℃, and the hydrothermal time is 20 hours.
Fig. 3 is a graph comparing surface photovoltage signals of samples obtained in example 2 and comparative example 1. As can be seen from FIG. 3, TiO produced with the aid of straw charcoal2And TiO prepared without the assistance of straw carbon in the range of 300-400 nm2The surface photovoltage signal is obviously enhanced, and the TiO can be enhanced by the auxiliary preparation of proper amount of straw carbon2A surface photovoltage signal.
Example 3:
this example shows surface photovoltage signal enhanced TiO2The preparation process is as follows:
1) collecting corn straws, peeling, taking straw cores, drying the straw cores for later use, fully crushing the dried straw cores by using a portable high-speed universal crusher (DFT-200), and sieving the crushed straw cores by using a 100-mesh sieve; roasting the screened straw powder for 3 hours at 750 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.2g of the straw carbon, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; the formed suspension system is continuously stirred for 30min, then transferred into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, subjected to hydrothermal reaction for 16h at 150 ℃, and naturally cooled to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical surface voltage signal.
Compared with the comparative example 1, the straw carbon obtained by roasting for 3 hours at 750 ℃ is added, the mass ratio of the straw carbon to the butyl titanate is 2%, the hydrothermal temperature is 150 ℃, and the hydrothermal time is 16 hours.
Fig. 4 is a graph comparing surface photovoltage signals of samples obtained in example 3 and comparative example 1. As can be seen from FIG. 4, the straw charcoal-assisted preparationOf TiO 22And TiO prepared without the assistance of straw carbon in the range of 300-400 nm2The surface photovoltage signal is obviously enhanced, and the TiO can be enhanced by the auxiliary preparation of proper amount of straw carbon2A surface photovoltage signal.
Example 4:
this example shows surface photovoltage signal enhanced TiO2The preparation process is as follows:
1) collecting corn straws, peeling, taking straw cores, drying the straw cores for later use, fully crushing the dried straw cores by using a portable high-speed universal crusher (DFT-200), and sieving the crushed straw cores by using a 100-mesh sieve; roasting the screened straw powder for 1.5h at 800 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.3g of the straw carbon, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; the formed suspension system is continuously stirred for 30min, then transferred into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, subjected to hydrothermal reaction at 160 ℃ for 18h, and naturally cooled to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical voltage signal.
Compared with the comparative example 1, the straw carbon obtained by roasting at 800 ℃ for 1.5h is added, the mass ratio of the straw carbon to the butyl titanate is 3%, the hydrothermal temperature is 160 ℃, and the hydrothermal time is 18 h.
Fig. 5 is a graph comparing surface photovoltage signals of samples obtained in example 4 and comparative example 1. As can be seen from FIG. 5, TiO produced with the aid of straw charcoal2And TiO prepared without the assistance of straw carbon in the range of 300-400 nm2The surface photovoltage signal is obviously enhanced, and the TiO can be enhanced by the auxiliary preparation of proper amount of straw carbon2A surface photovoltage signal.
Example 5:
1) collecting straws, peeling, taking straw cores, drying for later use, fully crushing the dried straw cores by using a portable high-speed universal crusher (DFT-200), and sieving by using a 100-mesh sieve; roasting the screened straw powder for 2 hours at 850 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.4g of the straw carbon, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; the formed suspension system is continuously stirred for 30min, then transferred into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, subjected to hydrothermal reaction for 20h at 170 ℃, and naturally cooled to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical voltage signal.
Compared with the comparative example 1, the straw carbon obtained by roasting for 2 hours at 850 ℃ is added, the mass ratio of the straw carbon to the butyl titanate is 4 percent, the hydrothermal temperature is 170 ℃, and the hydrothermal time is 20 hours.
Fig. 6 is a graph comparing surface photovoltage signals of samples obtained in example 5 and comparative example 1. As can be seen from FIG. 6, TiO prepared by the aid of straw carbon2And TiO prepared without the assistance of straw carbon in the range of 300-400 nm2The surface photovoltage signal is obviously enhanced, and the TiO can be enhanced by the auxiliary preparation of proper amount of straw carbon2A surface photovoltage signal.
Example 6:
1) collecting straws, peeling, taking straw cores, drying for later use, fully crushing the dried straw cores by using a portable high-speed universal crusher (DFT-200), and sieving by using a 100-mesh sieve; roasting the screened straw powder for 2.5 hours at 900 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.5g of the straw carbon, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; the formed suspension system is continuously stirred for 30min, then transferred into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, subjected to hydrothermal reaction for 22h at 165 ℃, and naturally cooled to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical voltage signal.
Compared with the comparative example 1, the straw carbon obtained by roasting for 2.5 hours at 900 ℃ is added, the mass ratio of the straw carbon to the butyl titanate is 5%, the hydrothermal temperature is 165 ℃, and the hydrothermal time is 22 hours.
Fig. 7 is a graph comparing surface photovoltage signals of samples obtained in example 6 and comparative example 1. As can be seen from FIG. 7, TiO produced with the aid of straw charcoal2And TiO prepared without the assistance of straw carbon in the range of 300-400 nm2The surface photovoltage signal is obviously enhanced, and the TiO can be enhanced by the auxiliary preparation of proper amount of straw carbon2A surface photovoltage signal.
Example 7:
this example shows surface photovoltage signal enhanced TiO2The preparation process is as follows:
1) collecting straws, peeling, taking straw cores, drying for later use, fully crushing the dried straw cores by using a portable high-speed universal crusher (DFT-200), and sieving by using a 100-mesh sieve; roasting the screened straw powder for 3 hours at 650 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.55g of the straw carbon, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; the formed suspension system was stirred for 30min, then transferred to a 100mL teflon-lined hydrothermal reaction kettle, subjected to hydrothermal reaction at 175 ℃ for 24h, and naturally cooled to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical voltage signal.
Compared with the comparative example 1, the straw carbon obtained by roasting for 3 hours at 650 ℃ is added, the mass ratio of the straw carbon to the butyl titanate is 5.5%, and the hydrothermal temperature is 175 ℃.
FIG. 8 is a graph comparing the surface photovoltage signals of the samples obtained in example 7 and comparative example 1. As can be seen from FIG. 8, TiO produced with the aid of straw charcoal2And TiO prepared without the assistance of straw carbon in the range of 300-400 nm2The surface photovoltage signal is obviously enhanced, and the TiO can be enhanced by the auxiliary preparation of proper amount of straw carbon2A surface photovoltage signal.
Example 8:
the surface photovoltage signal of the embodiment is subtractedWeak TiO2The specific preparation process comprises the following steps:
1) collecting straws, peeling, taking straw cores, drying for later use, fully crushing the dried straw cores by using a portable high-speed universal crusher (DFT-200), and sieving by using a 100-mesh sieve; roasting the screened straw powder for 1.8h at 820 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.6g of the straw carbon, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; the formed suspension system is continuously stirred for 30min, then transferred into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, subjected to hydrothermal reaction for 19h at 180 ℃, and naturally cooled to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical voltage signal.
Compared with the comparative example 1, the straw carbon obtained by roasting at 820 ℃ for 1.8h is added, the mass ratio of the straw carbon to the butyl titanate is 6%, and the hydrothermal time is 19 h.
Fig. 9 is a graph comparing surface photovoltage signals of samples obtained in example 8 and comparative example 1. As can be seen from FIG. 8, TiO produced with the aid of straw charcoal2And TiO prepared without the assistance of straw carbon in the range of 300-400 nm2Obviously weakening surface photovoltage signals and preparing TiO with the assistance of excessive straw carbon2The surface photovoltage signal is attenuated.
Example 9:
this example surface photovoltage signal-attenuated TiO2The preparation process is as follows:
1) collecting straws, peeling, taking straw cores, drying for later use, fully crushing the dried straw cores by using a portable high-speed universal crusher (DFT-200), and sieving by using a 100-mesh sieve; roasting the screened straw powder for 2 hours at 500 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.1g of the straw carbon, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; and (3) continuously stirring the formed suspension system for 30min, then transferring the suspension system into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 24h at 180 ℃, and naturally cooling to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical voltage signal.
Compared with the comparative example 1, the straw carbon obtained by roasting for 2 hours at 500 ℃ is added, and the mass ratio of the straw carbon to the butyl titanate is 1%.
FIG. 10 is a graph comparing the surface photovoltage signals of the samples obtained in example 9 and comparative example 1. As can be seen from FIG. 10, TiO produced with the aid of straw charcoal2And TiO prepared without the assistance of straw carbon in the range of 300-400 nm2The surface photovoltage signal is obviously reduced, and the roasting temperature of the straw carbon is too low2The surface photovoltage signal decreases.
Example 10:
this example surface photovoltage signal-attenuated TiO2The preparation process is as follows:
1) collecting straws, peeling, taking straw cores, drying for later use, fully crushing the dried straw cores by using a portable high-speed universal crusher (DFT-200), and sieving by using a 100-mesh sieve; roasting the screened straw powder for 1h at 920 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.4g of the straw carbon, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; and (3) continuously stirring the formed suspension system for 30min, then transferring the suspension system into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 24h at 180 ℃, and naturally cooling to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical voltage signal.
Compared with the comparative example 1, the straw carbon obtained by roasting for 1 hour at 920 ℃ is added, and the mass ratio of the straw carbon to the butyl titanate is 4%.
FIG. 11 is a graph comparing the surface photovoltage signals of the samples obtained in example 10 and comparative example 1. As can be seen from FIG. 11It can be seen that TiO prepared with the aid of straw carbon2And TiO prepared without the assistance of straw carbon in the range of 300-400 nm2The surface photovoltage signal is obviously reduced, and the roasting temperature of the straw carbon is overhigh2The surface photovoltage signal decreases.
Example 11:
this example surface photovoltage signal-attenuated TiO2The preparation process is as follows:
1) collecting corn straws, peeling, taking straw cores, drying the straw cores for later use, fully crushing the dried straw cores by using a portable high-speed universal crusher (DFT-200), and sieving the crushed straw cores by using a 100-mesh sieve; roasting the screened straw powder for 3.5 hours at 900 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.2g of the straw carbon, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; the formed suspension system is continuously stirred for 30min, then transferred into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, subjected to hydrothermal reaction at 140 ℃ for 18h, and naturally cooled to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical voltage signal.
Compared with the comparative example 1, the straw carbon obtained by roasting for 3.5 hours at 900 ℃ is added, the mass ratio of the straw carbon to the butyl titanate is 0.1%, the hydrothermal temperature is 140 ℃, and the hydrothermal time is 18 hours.
FIG. 12 is a graph comparing the surface photovoltage signals of the samples obtained in example 11 and comparative example 1. As can be seen from FIG. 12, TiO produced with the aid of straw charcoal can be seen2And TiO prepared without the assistance of straw carbon in the range of 300-400 nm2Obviously reduces the surface photovoltage signal and prolongs the roasting time of the straw carbon to be TiO2The surface photovoltage signal decreases.
Example 12:
this example surface photovoltage signal-attenuated TiO2The preparation process is as follows:
1) collecting corn straws, peeling, taking straw cores, drying the straw cores for later use, fully crushing the dried straw cores by using a portable high-speed universal crusher (DFT-200), and sieving the crushed straw cores by using a 100-mesh sieve; roasting the screened straw powder for 1h at 700 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.1g of the straw carbon, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; the formed suspension system is continuously stirred for 30min, then transferred into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, subjected to hydrothermal reaction for 24h at 130 ℃, and naturally cooled to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical voltage signal.
Compared with the comparative example 1, the straw carbon obtained by roasting for 1h at 700 ℃ is added, the mass ratio of the straw carbon to the butyl titanate is 1%, and the hydrothermal temperature is 130 ℃.
Fig. 13 is a graph comparing surface photovoltage signals of samples obtained in example 12 and comparative example 1. As can be seen from FIG. 13, TiO produced with the aid of straw charcoal can be seen2And TiO prepared without the assistance of straw carbon in the range of 300-400 nm2TiO (titanium dioxide) with remarkably reduced surface photovoltage signal and excessively low hydrothermal temperature2The surface photovoltage signal decreases.
Example 13:
this example surface photovoltage signal-attenuated TiO2The preparation process is as follows:
1) collecting corn straws, peeling, taking straw cores, drying the straw cores for later use, fully crushing the dried straw cores by using a portable high-speed universal crusher (DFT-200), and sieving the crushed straw cores by using a 100-mesh sieve; roasting the screened straw powder for 2 hours at 600 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.2g of the straw carbon, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; the formed suspension system is continuously stirred for 30min, then transferred into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, subjected to hydrothermal reaction for 18h at 190 ℃, and naturally cooled to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical voltage signal.
Compared with the comparative example 1, the straw carbon obtained by roasting for 2 hours at the temperature of 600 ℃ is added, the mass ratio of the straw carbon to the butyl titanate is 0.1%, the hydrothermal temperature is 190 ℃, and the hydrothermal time is 18 hours.
FIG. 14 is a graph comparing the surface photovoltage signals of the samples obtained in example 13 and comparative example 1. As can be seen from FIG. 13, TiO produced with the aid of straw charcoal can be seen2And TiO prepared without the assistance of straw carbon in the range of 300-400 nm2The surface photovoltage signal is obviously reduced, and the hydrothermal temperature of the reaction is overhigh2The surface photovoltage signal is attenuated.
Example 14:
this example surface photovoltage signal-attenuated TiO2The preparation process is as follows:
1) collecting corn straws, peeling, taking straw cores, drying the straw cores for later use, fully crushing the dried straw cores by using a portable high-speed universal crusher (DFT-200), and sieving the crushed straw cores by using a 100-mesh sieve; roasting the screened straw powder for 0.5h at 600 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.3g of the straw carbon, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; and (3) continuously stirring the formed suspension system for 30min, then transferring the suspension system into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 24h at 180 ℃, and naturally cooling to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical voltage signal.
Compared with the comparative example 1, the straw carbon obtained by roasting for 0.5h at 600 ℃ is added, and the mass ratio of the straw carbon to the butyl titanate is 0.1%.
FIG. 15 is a graph comparing the surface photovoltage signals of the samples obtained in example 14 and comparative example 1. As can be seen from FIG. 15, TiO produced with the aid of straw charcoal can be seen2In aTiO prepared in 300-400 nm range without assistance of straw carbon2The surface photovoltage signal is obviously reduced, and the roasting time of the straw carbon is too short2The surface photovoltage signal decreases.
Example 15:
this example surface photovoltage signal-attenuated TiO2The preparation process is as follows:
1) collecting corn straws, taking the skin, drying the skin for later use, fully crushing the dried straw skin by using a portable high-speed universal crusher (DFT-200), and sieving the crushed straw skin by using a 100-mesh sieve; roasting the screened straw skin powder for 2 hours at 600 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.1g of the straw charcoal, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; and (3) continuously stirring the formed suspension system for 30min, then transferring the suspension system into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 24h at 180 ℃, and naturally cooling to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical voltage signal.
Compared with the comparative example 1, the straw skin carbon obtained by roasting for 2 hours at the temperature of 600 ℃ is added, and the mass ratio of the straw skin carbon to the butyl titanate is 1%.
FIG. 16 is a graph comparing the surface photovoltage signals of the samples obtained in example 15 and comparative example 1. As can be seen from FIG. 16, it can be seen that TiO prepared by the aid of straw charcoal2And TiO prepared without the assistance of straw skin charcoal in a range of 300-400 nm2The surface photovoltage signal is obviously reduced, and the auxiliary preparation of the straw charcoal leads to TiO2The surface photovoltage signal decreases.
Example 16:
this example surface photovoltage signal-attenuated TiO2The preparation process is as follows:
1) collecting sorghum straws, taking skins, drying the skins for later use, fully crushing the dried straw skins by using a portable high-speed universal crusher (DFT-200), and screening by using a 100-mesh sieve; roasting the screened straw skin powder for 3 hours at 700 ℃ in an inert atmosphere for later use;
2) weighing 10g of butyl titanate and 0.3g of the straw charcoal, dispersing in 20mL of absolute ethyl alcohol, stirring for 30min, and slowly dropwise adding 40mL of deionized water into the suspension system by using a constant flow pump; and (3) continuously stirring the formed suspension system for 30min, then transferring the suspension system into a 100mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 24h at 180 ℃, and naturally cooling to room temperature.
3) Washing with deionized water and anhydrous ethanol for 3 times, respectively, drying at 60 deg.C for 3 hr until the solid is completely dried, and grinding to obtain TiO2And testing the optical voltage signal.
Compared with the comparative example 1, the straw skin carbon obtained by roasting for 3 hours at 700 ℃ is added, and the mass ratio of the straw skin carbon to the butyl titanate is 3%.
Fig. 17 is a graph comparing surface photovoltage signals of samples obtained in example 16 and comparative example 1. As can be seen from FIG. 17, it can be seen that TiO prepared with the assistance of straw charcoal2And TiO prepared without the assistance of straw skin charcoal in a range of 300-400 nm2The surface photovoltage signal is obviously reduced, and the auxiliary preparation of the straw charcoal leads to TiO2The surface photovoltage signal decreases.
Although the present invention has been described in detail with reference to specific embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention encompassed by the appended claims.

Claims (10)

1. Improve TiO2Method of surface photovoltage, characterized in that it comprises the following steps:
step one, drying, powdering and screening straw cores, and roasting under an inert atmosphere condition to obtain straw carbon for later use;
secondly, dispersing the straw carbon and the butyl titanate into absolute ethyl alcohol to obtain a suspension system for later use;
thirdly, dropwise adding deionized water into the straw carbon-butyl titanate-absolute ethyl alcohol suspension system by using a constant flow pump, and stirring to form suspensionTurbid liquid; transferring the suspension into a hydrothermal reaction kettle for hydrothermal treatment, performing reduced pressure suction filtration, washing, drying and grinding to obtain the TiO with enhanced surface photovoltage signal2。
2. The method of claim 1, wherein the TiO-enhancing agent is selected from the group consisting of2A method of surface photovoltage, characterized by: the straw core is any one of a corn straw core or a sorghum straw core.
3. The method of claim 1, wherein the TiO-enhancing agent is selected from the group consisting of2A method of surface photovoltage, characterized by: inert atmosphere is N2Ar, or NH3Any one of them.
4. The method of claim 1, wherein the TiO-enhancing agent is selected from the group consisting of2A method of surface photovoltage, characterized by: the roasting temperature of the inert atmosphere of the straws is 600-900 ℃, and the roasting time is 1-3 h.
5. The method of claim 1, wherein the TiO-enhancing agent is selected from the group consisting of2A method of surface photovoltage, characterized by: in the second step, the mass ratio of the straw carbon to the butyl titanate is 0.1-5.5%; the ratio of the mass g of the butyl titanate to the volume mL of the absolute ethyl alcohol is 2:1-1: 2.
6. The method of claim 1, wherein the TiO-enhancing agent is selected from the group consisting of2A method of surface photovoltage, characterized by: in the second step and the third step, the volume ratio of the deionized water to the absolute ethyl alcohol is 1:2-2: 1.
7. The method of claim 1, wherein the TiO-enhancing agent is selected from the group consisting of2A method of surface photovoltage, characterized by: in the third step, the temperature of the hydrothermal reaction is 140-180 ℃.
8. The method of claim 1, wherein the TiO-enhancing agent is selected from the group consisting of2A method of surface photovoltage, characterized by: in the third step, the hydrothermal reaction time is 12-24 h.
9. TiO prepared by the process of any one of claims 1 to 8 having surface photovoltage signal enhancement2A photocatalytic material.
10. The TiO of claim 92A photocatalytic material characterized by: TiO 22The surface photovoltage signal is obviously enhanced in the range of 300-400 nm.
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