CN106391067A - AgI-Ag3PO4/OV-TiO2 compound photocatalyst and preparation method thereof - Google Patents
AgI-Ag3PO4/OV-TiO2 compound photocatalyst and preparation method thereof Download PDFInfo
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- CN106391067A CN106391067A CN201610781786.4A CN201610781786A CN106391067A CN 106391067 A CN106391067 A CN 106391067A CN 201610781786 A CN201610781786 A CN 201610781786A CN 106391067 A CN106391067 A CN 106391067A
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- tio
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- catalyst
- titanium dioxide
- ag3po4
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 52
- 229910000161 silver phosphate Inorganic materials 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000002131 composite material Substances 0.000 claims description 43
- 239000000243 solution Substances 0.000 claims description 17
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 10
- GETTZEONDQJALK-UHFFFAOYSA-N (trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=CC=C1 GETTZEONDQJALK-UHFFFAOYSA-N 0.000 claims description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 5
- 229960004756 ethanol Drugs 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 14
- 229940043267 rhodamine b Drugs 0.000 abstract description 14
- 238000006731 degradation reaction Methods 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 abstract description 8
- 230000015556 catabolic process Effects 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 3
- 229910052709 silver Inorganic materials 0.000 abstract description 3
- 239000004332 silver Substances 0.000 abstract description 2
- 238000001291 vacuum drying Methods 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract 2
- 229910000510 noble metal Inorganic materials 0.000 abstract 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract 1
- 238000011085 pressure filtration Methods 0.000 abstract 1
- 229910019142 PO4 Inorganic materials 0.000 description 13
- 238000005286 illumination Methods 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 229940019931 silver phosphate Drugs 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 description 3
- 229910021612 Silver iodide Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- JKFYKCYQEWQPTM-UHFFFAOYSA-N 2-azaniumyl-2-(4-fluorophenyl)acetate Chemical compound OC(=O)C(N)C1=CC=C(F)C=C1 JKFYKCYQEWQPTM-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229940045105 silver iodide Drugs 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
-
- B01J35/39—
Abstract
The invention discloses an AgI-Ag3PO4/OV-TiO2 compound photocatalyst, which is composed of AgI, Ag3PO4, and OV-TiO2. The invention further provides a preparation method of the compound photocatalyst. The method comprises a step of preparation of an oxygen vacancy type titanium dioxide and a step of preparation of an Ag3PO4/OV-TiO2 compound photocatalyst. The AgI-Ag3PO4/OV-TiO2 compound photocatalyst is obtained by dissolving the prepared Ag3PO4/OV-TiO2 compound photocatalyst in an ethanol solution, adding a NaI solution, performing dark stirring after the reaction is completed, performing reduced-pressure filtration, and performing vacuum drying after washing. The compound photocatalyst prepared from the method is high in reaction activity of photocatalytic degradation of rhodamine B that is an organic pollutant, and has the photocatalytic activity three times as much as that of pure Ag3PO4 in visible light. The use amount of noble metal silver is obviously reduced, and the compound photocatalyst has the same effect on degradation of phenol that is a colorless organic pollutant.
Description
Technical field
The invention belongs to materialogy field, it is related to a kind of catalyst, specifically AgI-Ag3PO4/OV-TiO2Complex light
Catalyst and preparation method thereof.
Background technology
Silver phosphate/oxygen vacancies type titanium dioxide (Ag3PO4/OV-TiO2) composite photo-catalyst is a kind of in radiation of visible light
Under there is the photocatalyst of photocatalytic activity, but its photocatalysis less stable, limit its practical application.
Content of the invention
For above-mentioned technical problem of the prior art, the invention provides AgI-Ag3PO4/OV-TiO2Composite photocatalyst
Agent and preparation method thereof, described this composite photo-catalyst and preparation method thereof will solve silver phosphate/oxygen of the prior art
Cavity type titanium dioxide (Ag3PO4/OV-TiO2) composite photo-catalyst photocatalysis less stable technical problem.
The invention provides AgI-Ag3PO4/OV-TiO2Composite photo-catalyst, described AgI, Ag3PO4And OV-TiO2's
Mol ratio is 1 × 10-3~ 2×10-1:1: 1~5.
Present invention also offers AgI-Ag3PO4/OV-TiO2The preparation method of composite photo-catalyst, comprises the steps:
1)One step preparing oxygen vacancies type titanium dioxide, titanium dioxide is added in a reaction vessel, adds trifluoro
Toluene and benzyl alcohol, using the ultraviolet light for 365nm for the wavelength 6 ~ 10 hours, described titanium dioxide, benzotrifluoride and benzene
The material ratio of methanol is 1kg:50~70L:7 ~ 9mol, reaction uses dehydrated alcohol and deionized water wash, then by solid after terminating
Sample is vacuum dried, then grind into powder obtains oxygen vacancies type titanium dioxide;
2)One preparation Ag3PO4/OV-TiO2The step of composite photo-catalyst, weighs oxygen vacancies type titanium dioxide, is dissolved in anhydrous
In ethanol, add AgNO3, described oxygen vacancies type titanium dioxide and AgNO3Mol ratio be 1:1 ~ 5, magnetic under the conditions of lucifuge
After power stirs 40 ~ 80 minutes, under continuous stirring containing Na2HPO3·12H2The aqueous solution of O adds, described oxygen vacancies type
Titanium dioxide and Na2HPO3·12H2The mol ratio of O is 1:1 ~ 5, stir 3 ~ 8 hours, then sucking filtration, using absolute ethanol washing,
Again solid is vacuum dried, obtains Ag3PO4/OV-TiO2Composite photo-catalyst;
3)By the above-mentioned Ag preparing3PO4/OV-TiO2Composite catalyst is dissolved in ethanol solution, and ultrasonic agitation is after 3 ~ 10 minutes,
Continuously stirred 0.03 ~ 1 hour on magnetic stirring apparatuss, then NaI solution is added in above-mentioned solution, described Ag3PO4/
OV-TiO2The mol ratio of composite catalyst and NaI solution is 1: 1×10-3~ 2×10-1;Lucifuge stirring 1 ~ 3 after reaction completely
Hour, it is vacuum dried after the sucking filtration that then reduces pressure, washing, obtain AgI-Ag3PO4/OV-TiO2Composite photo-catalyst.
Present invention employs a kind of simple sedimentation method, successfully prepare AgI-Ag3PO4/OV-TiO2Composite photocatalyst
Agent, the reactivity of prepared composite photo-catalyst photocatalysis degradation organic contaminant rhodamine B is higher, light under visible light
Catalysis activity is than pure Ag3PO4Exceed twice, and significantly reduce the usage amount of noble silver, to colourless organic pollution phenol
Degraded equally effective.
The present invention compares with prior art, and its technological progress is significant.The present invention is in silver phosphate/oxygen vacancies type titanium dioxide
Titanium (Ag3PO4/OV-TiO2) composite photo-catalyst basis on, synthesized a kind of higher high activity silver iodide of stability-
Silver phosphate/oxygen defect type titanium dioxide (AgI-Ag3PO4/OV-TiO2) composite photo-catalyst.The preparation method of the present invention is simple,
And the photocatalytic activity height of product, good stability are it is not necessary to the equipment of complex and expensive, synthesis condition are gentle.Be conducive to extensive
Popularization, can be used for the improvement of the organic pollutions such as dyestuff, phenol.
Brief description
Fig. 1 is the AgI-Ag of the present invention3PO4/OV-TiO2(1:5)The X-ray diffraction of composite photo-catalyst(XRD)Figure.
Fig. 2 is the AgI-Ag of the present invention3PO4/OV-TiO2(1:5)The Flied emission transmission electron microscope picture of composite photo-catalyst.
Fig. 3 is the AgI-Ag of the present invention3PO4/OV-TiO2(1:5)、(1:1)Composite photo-catalyst utilizes as photocatalyst
Visible ray(Wavelength is more than 420nm)The active situation of light degradation colored dye, rhodamine B.
Fig. 4 is the color change in dye, rhodamine B solution degradation process.
Fig. 5 is the AgI-Ag of the present invention3PO4/OV-TiO2(1:5)Composite photo-catalyst utilizes visible ray as photocatalyst
(Wavelength is more than 420nm)The steadiness of light degradation colored dye, rhodamine B in triplicate.
Fig. 6 is the AgI-Ag of the present invention3PO4/OV-TiO2(1:5)Closing light catalyst utilizes visible ray as photocatalyst
(Wavelength is more than 420nm)The active situation of the colourless phenol of light degradation.
Specific embodiment
Embodiment 1
The preparation process of material is as follows:P25 titanium dioxide 1g is moved in 100ml beaker, adds 60ml benzotrifluoride and 8mmol
Benzyl alcohol, using the ultraviolet light for 365nm for the wavelength 8 hours.With the solid after dehydrated alcohol and deionized water cyclic washing
Sample is vacuum dried, and grind into powder obtains oxygen vacancies type titanium dioxide afterwards(OV-TiO2).
Weigh 0.4g OV-TiO2Powder is dissolved in 180ml dehydrated alcohol and adds 1.019g AgNO3Magnetic under the conditions of lucifuge
After power stirs 60 minutes, under continuous stirring containing 0.358g Na2HPO3·12H2The 20ml aqueous solution of O is added dropwise over, and drips
, at 1 drop/sec, after being stirred for 5 hours after being added dropwise to complete, sucking filtration, the solid of dehydrated alcohol cyclic washing are in vacuum drying for acceleration
60 degree of dryings of case, obtain the Ag of high light catalysis activity3PO4/OV-TiO2(1:5) composite photo-catalyst.{ weigh 0.08g simultaneously
OV-TiO2Powder presses above-mentioned steps, obtains the Ag of high light catalysis activity3PO4/OV-TiO2(1:1) composite photo-catalyst.}
By the above-mentioned Ag preparing3PO4/OV-TiO2(1:5)Composite catalyst takes 0.25g to be dissolved in the ethanol solution of 20ml, surpasses
Sound stir 5 minutes after continuously stirred 0.5 hour on magnetic stirring apparatuss, weigh 0.006gNaI and be dissolved in 1ml deionized water then
It is added dropwise to above-mentioned solution, be vacuum dried after decompression filtering and washing after lucifuge stirs 2 hours after completion of dropping, obtain AgI-
Ag3PO4/OV-TiO2(1:5) composite photo-catalyst.Described AgI-Ag3PO4/OV-TiO2(1:5) X of composite photo-catalyst penetrates
Line diffraction(XRD)Figure is as shown in figure 1, Flied emission transmission electron microscope picture is as shown in Figure 2.{ take 0.25g Ag simultaneously3PO4/OV-TiO2
(1:1) composite photo-catalyst is pressed above-mentioned steps and is prepared, and obtains AgI-Ag3PO4/OV-TiO2(1:1) composite photo-catalyst.}
Embodiment 2
By the AgI-Ag obtaining3PO4/OV-TiO2(1:1)、(1:5)Composite visible light catalyst carries out rhodamine B photocatalysis fall
Solution.Weigh 0.1g AgI-Ag respectively3PO4/OV-TiO2(1:1)、(1:5)Composite photo catalyst powder adds 100 mL rhodamines
In B solution (20 mg/L), lucifuge stirs 60 min, makes rhodamine B solution reach absorption/desorption equilibrium in catalyst surface.So
Open light source afterwards and carry out light-catalyzed reaction, reaction certain time takes 4 mL reactant liquors, through ultracentrifugal supernatant, using Shimadzu
UV2550 spectrophotometer detects.Become according to the concentration that the change of absorbance at solution 554nm determines rhodamine B in solution
Change.Light source utilizes 300W xenon lamp, and making incident illumination using optical filter is visible ray(420nm<λ<800nm).High using 10cm
Water layer filters the infrared ray in light source, prevents reacting liquid temperature from raising, and makes light degradation reaction temperature stable in room temperature state.Luo Dan
In bright B solution degradation process there is significant change in color, as shown in Figure 3.
Embodiment 3
The degraded situation of rhodamine B is as shown in figure 4, simple Ag3PO4As rhodamine B during photocatalyst in illumination 26 min
Substantially completely degrade afterwards, Ag3PO4/OV-TiO2(1:1)、(1:5)Composite is photocatalyst, and rhodamine B is in illumination 16
Substantially completely degrade after min, AgI-Ag3PO4/OV-TiO2(1:1)、(1:5)Composite is photocatalyst, and rhodamine B is in light
According to 5 min about after substantially completely degraded show AgI-Ag3PO4/OV-TiO2Composite photo-catalyst has more efficient visible ray
Photocatalysis performance.
Embodiment 4
Repeat rhodamine B degradation three times as shown in figure 5, Ag3PO4/OV-TiO2Composite be photocatalyst when, in triplicate after
Activity reduces the soonest, works as Ag3PO4Take second place during as photocatalyst, and AgI-Ag3PO4/OV-TiO2Composite is photocatalyst
When, still there is after rhodamine B degradation preferable photocatalytic activity in triplicate.
Embodiment 5
Prepared composite photo-catalyst also has the ability of degradation of phenol.As shown in fig. 6, simple Ag3PO4As photocatalysis
During agent, phenol is degraded to less than 40%, Ag after illumination 200min3PO4/OV-TiO2(1:5) composite is photocatalyst, phenol
In illumination 120min about after be degraded to 35%, and AgI-Ag3PO4/OV-TiO2(1:5)When composite is photocatalyst, phenol
30% just can be degraded to after illumination 60min.
Claims (2)
1. a kind of AgI-Ag3PO4/OV-TiO2Composite photo-catalyst it is characterised in that:By AgI, Ag3PO4And OV-TiO2Composition,
Described AgI, Ag3PO4And OV-TiO2Mol ratio be 1 × 10-3~ 2×10-1:1: 1~5.
2. the AgI-Ag described in claim 13PO4/OV-TiO2The preparation method of composite photo-catalyst it is characterised in that include as
Lower step:
1)One step preparing oxygen vacancies type titanium dioxide, titanium dioxide is added in a reaction vessel, adds trifluoro
Toluene and benzyl alcohol, using the ultraviolet light for 365nm for the wavelength 6 ~ 10 hours, described titanium dioxide, benzotrifluoride and benzene
The material ratio of methanol is 1kg:50~70L:7 ~ 9mol, reaction uses dehydrated alcohol and deionized water wash, then by solid after terminating
Sample is vacuum dried, then grind into powder obtains oxygen vacancies type titanium dioxide;
2)One preparation Ag3PO4/OV-TiO2The step of composite photo-catalyst, weighs oxygen vacancies type titanium dioxide, is dissolved in anhydrous
In ethanol, add AgNO3, described oxygen vacancies type titanium dioxide and AgNO3Mol ratio be 1:1 ~ 5, magnetic under the conditions of lucifuge
After power stirs 40 ~ 80 minutes, under continuous stirring containing Na2HPO3·12H2The aqueous solution of O adds, described oxygen vacancies type
Titanium dioxide and Na2HPO3·12H2The mol ratio of O is 1:1 ~ 5, stir 3 ~ 8 hours, then sucking filtration, using absolute ethanol washing,
Again solid is vacuum dried, obtains Ag3PO4/OV-TiO2Composite photo-catalyst;
3)By the above-mentioned Ag preparing3PO4/OV-TiO2Composite catalyst is dissolved in ethanol solution, and ultrasonic agitation is after 3 ~ 10 minutes,
Continuously stirred 0.03 ~ 1 hour on magnetic stirring apparatuss, then NaI solution is added in above-mentioned solution, described Ag3PO4/
OV-TiO2The mol ratio of composite catalyst and NaI solution is 1: 1×10-3~ 2×10-1;Lucifuge stirring 1 ~ 3 after reaction completely
Hour, it is vacuum dried after the sucking filtration that then reduces pressure, washing, obtain AgI-Ag3PO4/OV-TiO2Composite photo-catalyst.
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Cited By (1)
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CN108579775A (en) * | 2018-05-15 | 2018-09-28 | 浙江大学城市学院 | A kind of silver orthophosphate/silver/titanium dioxide nano flower composite material and the preparation method and application thereof |
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CN101327438A (en) * | 2008-01-10 | 2008-12-24 | 武汉理工大学 | Method for preparing AgI/TiO2 nano compound photocatalyst |
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2016
- 2016-08-30 CN CN201610781786.4A patent/CN106391067A/en active Pending
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CN101327438A (en) * | 2008-01-10 | 2008-12-24 | 武汉理工大学 | Method for preparing AgI/TiO2 nano compound photocatalyst |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108579775A (en) * | 2018-05-15 | 2018-09-28 | 浙江大学城市学院 | A kind of silver orthophosphate/silver/titanium dioxide nano flower composite material and the preparation method and application thereof |
CN108579775B (en) * | 2018-05-15 | 2020-09-11 | 浙江大学城市学院 | Silver phosphate/silver/titanium dioxide nanoflower composite material and preparation method and application thereof |
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