CN107051558A - A kind of preparation method of the silver-colored photochemical catalyst of the silver-colored compound phosphoric acid of wolframic acid - Google Patents
A kind of preparation method of the silver-colored photochemical catalyst of the silver-colored compound phosphoric acid of wolframic acid Download PDFInfo
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- CN107051558A CN107051558A CN201710201017.7A CN201710201017A CN107051558A CN 107051558 A CN107051558 A CN 107051558A CN 201710201017 A CN201710201017 A CN 201710201017A CN 107051558 A CN107051558 A CN 107051558A
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- Prior art keywords
- silver
- wolframic acid
- colored
- acid
- colloid
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- 239000002253 acid Substances 0.000 title claims abstract description 48
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000003054 catalyst Substances 0.000 title claims abstract description 26
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 13
- 150000001875 compounds Chemical class 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000084 colloidal system Substances 0.000 claims abstract description 24
- 229910052709 silver Inorganic materials 0.000 claims abstract description 22
- 239000004332 silver Substances 0.000 claims abstract description 22
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical class [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 12
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 12
- 239000011734 sodium Substances 0.000 claims abstract description 12
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- NDYNABNWLRVCDO-UHFFFAOYSA-N phosphoric acid silver Chemical compound [Ag].P(O)(O)(O)=O NDYNABNWLRVCDO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 150000002500 ions Chemical class 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- XRRQZKOZJFDXON-UHFFFAOYSA-N nitric acid;silver Chemical compound [Ag].O[N+]([O-])=O XRRQZKOZJFDXON-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 3
- 239000010452 phosphate Substances 0.000 claims abstract description 3
- 238000004821 distillation Methods 0.000 claims abstract 2
- 238000003756 stirring Methods 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 4
- 229940100890 silver compound Drugs 0.000 description 4
- 150000003379 silver compounds Chemical class 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000004042 decolorization Methods 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus 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
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 241000220317 Rosa Species 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007539 photo-oxidation reaction Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 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
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1856—Phosphorus; Compounds thereof with iron group metals or platinum group metals with platinum group metals
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The present invention discloses a kind of preparation method of the silver-colored photochemical catalyst of the silver-colored compound phosphoric acid of wolframic acid, comprises the following steps that:12~16mmol silver nitrates are weighed, 18mmol/L silver nitrate solution is configured to, 6.6~8mmol sodium tungstates are weighed, 18mmol/L sodium tungstate solution is configured to;Both the above solution is mixed under 350~400 revs/min of rotating speed, colloid substance is formed, 3~4h is persistently stirred, sodium tungstate and nitric acid silver reaction in whipping process generate wolframic acid silver colloid;Wolframic acid silver colloid is placed in pellicle bag, with distillation water washing 3~4 times, get rid of dissociated ion, the wolframic acid silver colloid is added in the sodium radio-phosphate,P-32 solution that 60~80mL concentration is 3~4mol/L again, soaked 2~4 days, phosphoric acid silver nano-grain is formed on wolframic acid Argent grain surface, separation of solid and liquid, a kind of silver-colored photochemical catalyst of the silver-colored compound phosphoric acid of wolframic acid is made in deionized water washing solid 2~3 times, 75~105 DEG C of drying.This method is that catalyst and carrier are combined closely in carrier surface formation catalyst.
Description
Technical field
The present invention relates to a kind of preparation method of the silver-colored photochemical catalyst of the silver-colored compound phosphoric acid of wolframic acid, belong in environmental protection at sewage
Manage technical field.
Background technology
Traditional method for treating water efficiency is low, cost is high, there are secondary pollution problems, and waste water control always cannot be well
Solution.The development and application of nanometer technology are likely to thoroughly solve this problem.Start within 1972 to find TiO2Oxidation activity
Higher, chemical stability is good, harmless to the human body, and cost is low, pollution-free, has a wide range of application, thus is most paid attention to, but TiO2
Larger (such as anatase TiO of energy gap2Energy gap Eg=3.2eV), be only capable of absorb ultraviolet region (wavelength is less than
Light 387nm), the utilization ratio to solar energy is relatively low.
In contaminant degradation and production of energy field, conductor photocatalysis is one of most promising method.Work as energy
Amount will produce point of electron-hole pair when being more than or equal to the photon irradiation of semiconductor energy gap in photocatalyst surface
From this is the initial basic step of light-catalyzed reaction.In order to find efficient photochemical catalyst, numerous studies work is all concentrated on
In the influence factor for studying photocatalytic activity.In June, 2010, material research institution researcher has found that silver orthophosphate has light
The effect of catalyst, and photooxidation effect is to be currently known more than the decades of times of various photochemical catalysts.But due to silver orthophosphate itself
Unstable, easy self-reversal, causes catalyst degradation performance to reduce rapidly in photocatalysis.And it is that a nothing is stopped to improve photocatalysis effect
The work in border.Further, since nano particle is difficult to be separated from waste water after processing waste water, it is therefore desirable to which nano particle is loaded
On some carriers.The material synthesized on its surface is a kind of composite, can there is good photocatalysis effect.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to propose a kind of silver-colored photochemical catalyst of the silver-colored compound phosphoric acid of wolframic acid
Preparation method, this method is that catalyst and carrier are combined closely in carrier surface formation catalyst.
The technical solution adopted by the present invention is to use following steps:
1) 12~16mmol silver nitrates are weighed, 18mmol/L silver nitrate solution is configured to, 6.6~8mmol wolframic acids are weighed
Sodium, is configured to 18mmol/L sodium tungstate solution;
2) both the above solution is mixed under 350~400 revs/min of rotating speed, forms colloid substance, persistently stir 3
~4h, sodium tungstate and nitric acid silver reaction in whipping process generate wolframic acid silver colloid;
3) wolframic acid silver colloid is placed in pellicle bag, with water washing is distilled 3~4 times, gets rid of dissociated ion, then should
Wolframic acid silver colloid is added in the sodium radio-phosphate,P-32 solution that 60~80mL concentration is 3~4mol/L, is soaked 2~4 days, in wolframic acid Argent grain
Surface forms phosphoric acid silver nano-grain, and one kind is made in separation of solid and liquid, deionized water washing solid 2~3 times, 75~105 DEG C of drying
The silver-colored photochemical catalyst of wolframic acid silver compound phosphoric acid.
The beneficial effects of the invention are as follows:(1) this method utilizes the difference of solubility product constant, in wolframic acid silver surface formation solubility
The smaller phosphoric acid Argent grain of product constant.
(2) wolframic acid silver and silver orthophosphate are combined, synergy, and wolframic acid silver can be made preferably to play catalysis under visible light and made
With and good catalytic effect can be obtained.
Embodiment
Embodiment 1
12mmol silver nitrates are weighed, 18mmol/L silver nitrate solution is configured to, 6.6mmol sodium tungstates is weighed, is configured to
18mmol/L sodium tungstate solution;Both the above solution is mixed under 350 revs/min of rotating speed, colloid substance is formed, continued
3h is stirred, sodium tungstate and nitric acid silver reaction in whipping process generate wolframic acid silver colloid;Wolframic acid silver colloid is placed in pellicle bag
It is interior, with water washing is distilled 3 times, dissociated ion is got rid of, then the wolframic acid silver colloid is added to the phosphorus that 60mL concentration is 3mol/L
In acid sodium solution, soak 2 days, phosphoric acid silver nano-grain is formed on wolframic acid Argent grain surface, separation of solid and liquid, deionized water washing is solid
A kind of silver-colored photochemical catalyst of the silver-colored compound phosphoric acid of wolframic acid is made in body 2 times, 75 DEG C of drying.
Obtained wolframic acid silver compound phosphoric acid silver photochemical catalyst 0.5g is added into the acid red that 400mL concentration is 40mg/L to give up
In water, under the irradiation of 300w Metal halogen lamps, 30min is reacted, percent of decolourization is 95.1%, can be reused after catalyst separation.
Embodiment 2
16mmol silver nitrates are weighed, 18mmol/L silver nitrate solution is configured to, 8mmol sodium tungstates is weighed, is configured to
18mmol/L sodium tungstate solution;Both the above solution is mixed under 400 revs/min of rotating speed, colloid substance is formed, continued
4h is stirred, sodium tungstate and nitric acid silver reaction in whipping process generate wolframic acid silver colloid;Wolframic acid silver colloid is placed in pellicle bag
It is interior, with water washing is distilled 4 times, dissociated ion is got rid of, then the wolframic acid silver colloid is added to the phosphorus that 80mL concentration is 4mol/L
In acid sodium solution, soak 4 days, phosphoric acid silver nano-grain is formed on wolframic acid Argent grain surface, separation of solid and liquid, deionized water washing is solid
A kind of silver-colored photochemical catalyst of the silver-colored compound phosphoric acid of wolframic acid is made in body 3 times, 105 DEG C of drying.
Obtained wolframic acid silver compound phosphoric acid silver photochemical catalyst 0.5g is added into the gold orange 7 that 400mL concentration is 40mg/L to give up
In water, under the irradiation of 300w Metal halogen lamps, 30min is reacted, percent of decolourization is 97.6%, can be reused after catalyst separation.It is right
In identical waste water under the same conditions, the degradation efficiency of pure tungsten acid silver is 72.1%, substantially increases its action effect.
Embodiment 3
14mmol silver nitrates are weighed, 18mmol/L silver nitrate solution is configured to, 7mmol sodium tungstates is weighed, is configured to
18mmol/L sodium tungstate solution;Both the above solution is mixed under 400 revs/min of rotating speed, colloid substance is formed, continued
4h is stirred, sodium tungstate and nitric acid silver reaction in whipping process generate wolframic acid silver colloid;Wolframic acid silver colloid is placed in pellicle bag
It is interior, with water washing is distilled 4 times, dissociated ion is got rid of, then the wolframic acid silver colloid is added to the phosphorus that 60mL concentration is 4mol/L
In acid sodium solution, soak 3 days, phosphoric acid silver nano-grain is formed on wolframic acid Argent grain surface, separation of solid and liquid, deionized water washing is solid
A kind of silver-colored photochemical catalyst of the silver-colored compound phosphoric acid of wolframic acid is made in body 3 times, 105 DEG C of drying.
Obtained wolframic acid silver compound phosphoric acid silver photochemical catalyst 0.5g is added to the rose red b that 400mL concentration is 40mg/L
In waste water, under the irradiation of 300w Metal halogen lamps, 30min is reacted, percent of decolourization is 96.7%, can be reused after catalyst separation.
Claims (1)
1. the preparation method of the silver-colored photochemical catalyst of the silver-colored compound phosphoric acid of a kind of wolframic acid, it is characterized in that in turn including the following steps:
1) 12~16mmol silver nitrates are weighed, 18mmol/L silver nitrate solution is configured to, 6.6~8mmol sodium tungstates is weighed, matches somebody with somebody
It is set to 18mmol/L sodium tungstate solution;
2) both the above solution is mixed under 350~400 revs/min of rotating speed, forms colloid substance, persistently stir 3~4h,
Sodium tungstate and nitric acid silver reaction in whipping process, generate wolframic acid silver colloid;
3) wolframic acid silver colloid is placed in pellicle bag, with distillation water washing 3~4 times, gets rid of dissociated ion, then by the wolframic acid
Silver colloid is added in the sodium radio-phosphate,P-32 solution that 60~80mL concentration is 3~4mol/L, is soaked 2~4 days, on wolframic acid Argent grain surface
Phosphoric acid silver nano-grain is formed, a kind of wolframic acid is made in separation of solid and liquid, deionized water washing solid 2~3 times, 75~105 DEG C of drying
The silver-colored photochemical catalyst of silver-colored compound phosphoric acid.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102600869A (en) * | 2012-02-23 | 2012-07-25 | 常州水木环保科技有限公司 | Synthetic method of supported silver phosphate photocatalyst |
CN103990481A (en) * | 2014-06-04 | 2014-08-20 | 常州大学 | Preparation method of metavanadic silver/silver/silver phosphate composite catalyst |
CN105289674A (en) * | 2015-11-17 | 2016-02-03 | 中国科学院海洋研究所 | AgVO3/Ag3PO4 heterojunction composite photocatalyst and preparation method and application thereof |
CN106268804A (en) * | 2016-07-21 | 2017-01-04 | 吉林师范大学 | One step hydrothermal technique prepares Ag2o/Ag2wO4the method of nanometer rods |
CN106335926A (en) * | 2016-08-17 | 2017-01-18 | 哈尔滨理工大学 | Silver tungstate nanowire and preparation method thereof |
KR101698848B1 (en) * | 2014-04-28 | 2017-01-24 | 이화여자대학교 산학협력단 | Silver phosphate single crystal film, preparing method thereof, and photocatalyst including the same |
-
2017
- 2017-03-30 CN CN201710201017.7A patent/CN107051558A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102600869A (en) * | 2012-02-23 | 2012-07-25 | 常州水木环保科技有限公司 | Synthetic method of supported silver phosphate photocatalyst |
KR101698848B1 (en) * | 2014-04-28 | 2017-01-24 | 이화여자대학교 산학협력단 | Silver phosphate single crystal film, preparing method thereof, and photocatalyst including the same |
CN103990481A (en) * | 2014-06-04 | 2014-08-20 | 常州大学 | Preparation method of metavanadic silver/silver/silver phosphate composite catalyst |
CN105289674A (en) * | 2015-11-17 | 2016-02-03 | 中国科学院海洋研究所 | AgVO3/Ag3PO4 heterojunction composite photocatalyst and preparation method and application thereof |
CN106268804A (en) * | 2016-07-21 | 2017-01-04 | 吉林师范大学 | One step hydrothermal technique prepares Ag2o/Ag2wO4the method of nanometer rods |
CN106335926A (en) * | 2016-08-17 | 2017-01-18 | 哈尔滨理工大学 | Silver tungstate nanowire and preparation method thereof |
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Application publication date: 20170818 |