CN106735166A - A kind of EuWO4(OH) preparation method of nanobelt and its composite - Google Patents
A kind of EuWO4(OH) preparation method of nanobelt and its composite Download PDFInfo
- Publication number
- CN106735166A CN106735166A CN201611138429.2A CN201611138429A CN106735166A CN 106735166 A CN106735166 A CN 106735166A CN 201611138429 A CN201611138429 A CN 201611138429A CN 106735166 A CN106735166 A CN 106735166A
- Authority
- CN
- China
- Prior art keywords
- euwo
- nanobelt
- preparation
- europium
- alkaline
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002127 nanobelt Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002131 composite material Substances 0.000 title claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000010931 gold Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(3+);trinitrate Chemical compound [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 claims abstract description 11
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 10
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims abstract description 6
- 238000006552 photochemical reaction Methods 0.000 claims abstract description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 18
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 13
- 229910052693 Europium Inorganic materials 0.000 claims description 12
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- -1 polytetrafluoroethylene Polymers 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000005119 centrifugation Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 244000248349 Citrus limon Species 0.000 claims 1
- 235000005979 Citrus limon Nutrition 0.000 claims 1
- 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 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 abstract description 17
- 239000000463 material Substances 0.000 abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- NQYDFSLFJNXWJE-UHFFFAOYSA-N europium;hydrate Chemical compound O.[Eu] NQYDFSLFJNXWJE-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- WKFWYTXUPOVMSF-UHFFFAOYSA-M [Eu].O[W]=O Chemical compound [Eu].O[W]=O WKFWYTXUPOVMSF-UHFFFAOYSA-M 0.000 abstract 1
- 230000008878 coupling Effects 0.000 abstract 1
- 238000010168 coupling process Methods 0.000 abstract 1
- 238000005859 coupling reaction Methods 0.000 abstract 1
- 238000001514 detection method Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- BRSVJNYNWNMJKC-UHFFFAOYSA-N [Cl].[Au] Chemical compound [Cl].[Au] BRSVJNYNWNMJKC-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 230000005779 cell damage Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 150000002019 disulfides Chemical class 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000019491 signal transduction Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0551—Flake form nanoparticles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
- C01F17/32—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 oxide or hydroxide being the only anion, e.g. NaCeO2 or MgxCayEuO
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/32—Titanates; Germanates; Molybdates; Tungstates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/17—Nanostrips, nanoribbons or nanobelts, i.e. solid nanofibres with two significantly differing dimensions between 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention relates to a kind of EuWO4(OH) preparation method of nanobelt and its composite, belongs to technical field of nanometer material preparation.By hydro-thermal method, with ammonium tungstate, thiocarbamide, europium nitrate and water are raw material, under specific reaction condition, can be with one-step synthesis method hydroxyl tungsten oxide europium nanobelt.Then nanobelt and gold chloride are synthesized into EuWO under conditions of photochemical reaction4(OH)/Au composites, this material is used for detecting hydrogen peroxide by the method for fluorescence.This material is easy to operate in preparation, with short production cycle, low production cost, and yield is high and no coupling product, is easy to be commercialized a large amount of preparations.
Description
Technical field
The present invention develops a kind of EuWO4(OH) preparation method of nanobelt and its composite, is related to function nano material
Material preparing technical field.
Technical background
On basic science and the aspect of application, two-dimentional transition metal dichalcogenide has become the material being popular
Material.In recent years, application of these materials in electronics and photoelectronics is widely inquired into.Due to most of two-dimentional transition
The band gap of metal disulfides is in visible ray near infrared wavelength region so that these materials are suitable for optical transmitting set, light electric-examination
Survey device and solar cell etc..Different from III-V semiconductors, the optical property of two-dimentional transition metal dichalcogenide is by with strong knot
The exciton for closing energy (about 300meV) and large radius (~1.6nm) is determined.But its luminescent quantum yield is very low, that is,
Say, the quantity of the electron-hole pair of the photon ratio generation of material radiation is much lower.Therefore, researcher attempts development has
Luminous efficiency two-dimensional material higher.
Rare earth compound is significant due to the potentiality of its practical application in various fields, and for example light dress
Put, medical diagnosis, biochemical probes, the catalysis of sensor and some technical significant process.Rare earth oxyhydroxide is used as rare earth
The compound of oxide, in their light, magnetic, heat and electrical property aspect are studied in detail.So far, only
The report of the synthesis of a small number of two-dimensional nano pieces on these rare earth compounds.Cao et al. by microwave-hydrothermal method 160 DEG C~
Synthesize NdWO at 220 DEG C4(OH) powder.Lee et al. prepares SmWO by hydro-thermal method4(OH) nanometer sheet, but product is impure, wherein
Contain Sm2WO6Nanometer sheet, and this slice, thin piece is thicker.Therefore, it is necessary to develop new reflection condition to overcome these to limit.
H2O2It is considered as the related active material of cellular damage, and is the important adjuster of eukaryotic signal transduction.
Therefore, H2O2Detection have great importance, had many methods so far.In these inspection policies, optical means is base
In the direct method that the living things catalysis of Au nano particles grows, this is the Au nano particles due to catalysis generation in about 540nm ripples
The surface plasma body resonant vibration of strong point.Due to extinction coefficient and absorption spectrum wide high, Au nano particles are typically used as lighting
Quencher and energy acceptor, and serve as conductive channel to promote electro transfer.
The content of the invention
Cheap, the excellent performance it is an object of the invention to provide a kind of raw material, the one-step synthesis with huge commercial value
Method obtain EuWO4(OH) nanobelt, and EuWO4(OH) preparation method of/Au composites.
In order to the technical scheme for solving above-mentioned one of technical problem proposition is：A kind of alkaline wolframic acid europium EuWO4 (OH)
The preparation method of nanobelt, comprises the following steps：
In mass ratio it is 1 by ammonium tungstate, thiocarbamide and europium nitrate：2.9~3.1:0.4~0.7 mixing, with water as solvent, plus
Enter in the water heating kettle with polytetrafluoroethylene (PTFE) as inner bag, 23-25h is heated at 210-230 DEG C, reaction terminates rear natural cooling, will
The product centrifugation that obtains of reaction, is washed three times with ethanol, then washes three times and obtain EuWO4(OH) nanobelt.
Preferably, in mass ratio it is 1 by ammonium tungstate, thiocarbamide and europium nitrate:3:0.5 mixing.
Preferably, add in the water heating kettle with polytetrafluoroethylene (PTFE) as inner bag, 24h is heated at 220 DEG C.
In order to the technical scheme for solving above-mentioned one of technical problem proposition is：A kind of alkaline wolframic acid europium EuWO4(OH)
Nanobelt, alkaline wolframic acid europium EuWO is prepared according to above-mentioned preparation method4(OH) nanobelt.
In order to the technical scheme for solving above-mentioned one of technical problem proposition is, described alkaline wolframic acid europium EuWO4
(OH) nanobelt prepares EuWO4(OH) method of/Au composites, by sodium citrate, gold chloride and above-mentioned EuWO4(OH) receive
Rice band mixing, by photochemical reaction 4 hours, after reaction terminates, will react the product centrifugation for obtaining, and wash three times and be obtained
EuWO4(OH)/Au composites.
Preferably, the mol ratio by sodium citrate, gold chloride is 3:1.
Beneficial effect:
The present invention develops that a kind of raw material is cheap and easy to get, and low production cost, yield is high, and the step for being adapted to large-scale production is closed
Into the method for alkaline wolframic acid europium EuWO4 (OH) nanobelt.The present invention passes through hydro-thermal method, is with ammonium tungstate, thiocarbamide, europium nitrate and water
Raw material, under specific reaction condition, can be with one-step synthesis method hydroxyl EuWO4(OH) nanobelt.Then by nanobelt and chlorine gold
Acid synthesizes EuWO under conditions of photochemical reaction4(OH)/Au composites, this material is used for by the method for fluorescent quenching
Detection hydrogen peroxide, test limit reaches 0.2mM.
(1) product of the invention detects and sign that good product purity, yield is high through various methods.
(2) synthetic method of the invention is hydro-thermal method, simple to operate.
(3) raw material of the invention, cheap and easy to get, low production cost.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of sample in embodiment 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of sample in comparative example 1.
Fig. 3 is the X-ray single crystal diffraction figure of sample in embodiment 1.
Fig. 4 is the fluorescence spectrum of detection hydrogen peroxide in embodiment 6.
Fig. 5 is the corresponding relative intensity of fluorescence figure of hydrogen peroxide of various concentrations in embodiment 6.
Specific embodiment
For a better understanding of the present invention, technical scheme is illustrated below by specific embodiment.
Embodiment 1：
By ammonium tungstate (42mg), thiocarbamide (128mg), after europium nitrate (20mg) and the mixing of 19.44mL water, heating for dissolving, so
It is added to afterwards in the water heating kettle that 25mL polytetrafluoroethylene (PTFE) is inner bag, is put into the baking oven for being warming up to 220 DEG C in advance, it is anti-at 220 DEG C
Answer 24 hours.After reaction terminates, room temperature environment natural cooling is placed on.The white solid for obtaining will be reacted and pass through centrifugation (second
Alcohol is washed three times, and water is washed three times again), finally give target product EuWO4(OH) nanobelt.Fig. 1 is shown the scanning electricity of product
Mirror figure, it will be seen that product is a kind of strip material.Fig. 3 is shown the X-ray single crystal diffraction figure of product, peak and standard on spectrogram
Card JCPDS card No.23-0428 match, and do not have miscellaneous peak, it can be seen that the purity of alkaline molybdic acid europium is very high.
Comparative example 1：
By ammonium tungstate (425mg), thiocarbamide (1285mg), after europium nitrate (4.7mg) and the mixing of 19.44mL water, heating for dissolving,
It is then added in the water heating kettle that 25mL polytetrafluoroethylene (PTFE) is inner bag, the baking oven for being warming up to 220 DEG C in advance is put into, at 220 DEG C
Reaction 24 hours.After reaction terminates, room temperature environment natural cooling is placed on.The white solid for obtaining will be reacted and pass through centrifugation
(ethanol is washed three times, and water is washed three times again), finally gives target product EuWO4(OH) nanometer sheet.Fig. 2 is shown the scanning of product
Electron microscope, it will be seen that product is flaky material.
Embodiment 2：
By ammonium tungstate (42mg), thiocarbamide (121mg), after europium nitrate (16mg) and the mixing of 19.44mL water, heating for dissolving, so
It is added to afterwards in the water heating kettle that 25mL polytetrafluoroethylene (PTFE) is inner bag, is put into the baking oven for being warming up to 230 DEG C in advance, it is anti-at 230 DEG C
Answer 25 hours.After reaction terminates, room temperature environment natural cooling is placed on.The white solid for obtaining will be reacted and pass through centrifugation (second
Alcohol is washed three times, and water is washed three times again), finally give target product EuWO4(OH) nanobelt.
Embodiment 3：
By ammonium tungstate (42mg), thiocarbamide (130mg), after europium nitrate (30mg) and the mixing of 19.44mL water, heating for dissolving, so
It is added to afterwards in the water heating kettle that 25mL polytetrafluoroethylene (PTFE) is inner bag, is put into the baking oven for being warming up to 210 DEG C in advance, it is anti-at 210 DEG C
Answer 23 hours.After reaction terminates, room temperature environment natural cooling is placed on.The white solid for obtaining will be reacted and pass through centrifugation (second
Alcohol is washed three times, and water is washed three times again), finally give target product EuWO4(OH) nanobelt.
Embodiment 4：
By ammonium tungstate (42mg), thiocarbamide (128mg), after europium nitrate (28mg) and the mixing of 19.44mL water, heating for dissolving, so
It is added to afterwards in the water heating kettle that 25mL polytetrafluoroethylene (PTFE) is inner bag, is put into the baking oven for being warming up to 210 DEG C in advance, it is anti-at 210 DEG C
Answer 24 hours.After reaction terminates, room temperature environment natural cooling is placed on.The white solid for obtaining will be reacted and pass through centrifugation (second
Alcohol is washed three times, and water is washed three times again), finally give target product EuWO4(OH) nanobelt.
Embodiment 5：
Take the EuWO of 0.36mg4(OH) nanobelt is dissolved in the water of 9mL, sequentially add 90 μ L sodium citrate (30mM) and
The gold chloride (30mM) of 30 μ L, then shines 4h with halogen light.Solution centrifugal is concentrated into 2mL by reaction after terminating, you can obtained
EuWO4(OH)/Au composite nano materials.
Embodiment 6：
Take the EuWO of the 0.02mg/mL of 1mL4(OH)/Au solution is separately added into 0.204 μ L, 0.41 μ L, 0.616 μ L, 0.82
μL、1.024μL、1.536μL、2.048μL、4.096μL H2O2(3% now matches somebody with somebody) be made into 0.2mM, 0.4mM, 0.6mM, 0.8mM,
1.0mM, 1.5mM, 2.0mM, 4.0mM, hydrogen peroxide is detected by the intensity of fluorescence.Fig. 4 is the fluorescence light for detecting hydrogen peroxide
Spectrogram, Fig. 5 is the relative intensity linear graph of fluorescence under different hydrogen peroxide concentrations.From this two width figure, we can see that the material
There is preferable sensitivity to detection hydrogen peroxide, detection is limited to 0.2mM.
The concrete technical scheme being not limited to described in above-described embodiment of the invention, the technology that all use equivalents are formed
Scheme is the protection domain of application claims.
Claims (6)
1. a kind of alkaline wolframic acid europium EuWO4(OH) preparation method of nanobelt, it is characterised in that：Comprise the following steps：
In mass ratio it is 1 by ammonium tungstate, thiocarbamide and europium nitrate：2.9~3.1:0.4~0.7 mixing, with water as solvent, add with
During polytetrafluoroethylene (PTFE) is for the water heating kettle of inner bag, 23-25h is heated at 210-230 DEG C, reaction terminates rear natural cooling, will react
The product centrifugation for obtaining, is washed three times with ethanol, then is washed three times and obtained EuWO4(OH) nanobelt.
2. alkaline wolframic acid europium EuWO according to claim 14(OH) preparation method of nanobelt, it is characterised in that：By wolframic acid
Ammonium, thiocarbamide and europium nitrate are 1 in mass ratio:3:0.5 mixing.
3. alkaline wolframic acid europium EuWO according to claim 14(OH) preparation method of nanobelt, it is characterised in that：Add with
During polytetrafluoroethylene (PTFE) is for the water heating kettle of inner bag, 24h is heated at 220 DEG C.
4. a kind of alkaline wolframic acid europium EuWO4(OH) nanobelt, it is characterised in that：Preparation side according to claim 1,2 or 3
Method prepares alkaline wolframic acid europium EuWO4(OH) nanobelt.
5. alkaline wolframic acid europium EuWO according to claim 44(OH) nanobelt prepares EuWO4(OH) side of/Au composites
Method, it is characterised in that：By sodium citrate, gold chloride and EuWO4(OH) nanobelt mixing, by photochemical reaction 4 hours, reaction
After end, the product centrifugation for obtaining will be reacted, wash three prepared EuWO4(OH)/Au composites.
6. preparation EuWO according to claim 54(OH) method of)/Au composites, it is characterised in that：It is described by lemon
Sour sodium, the mol ratio of gold chloride are 3:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611138429.2A CN106735166B (en) | 2016-12-12 | 2016-12-12 | A kind of EuWO4(OH) preparation method of nanobelt and its composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611138429.2A CN106735166B (en) | 2016-12-12 | 2016-12-12 | A kind of EuWO4(OH) preparation method of nanobelt and its composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106735166A true CN106735166A (en) | 2017-05-31 |
| CN106735166B CN106735166B (en) | 2018-10-12 |
Family
ID=58879913
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611138429.2A Active CN106735166B (en) | 2016-12-12 | 2016-12-12 | A kind of EuWO4(OH) preparation method of nanobelt and its composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106735166B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103333689A (en) * | 2013-07-11 | 2013-10-02 | 黑龙江大学 | Method of thermosynthesis of SrWO4:Ln3<+> nanoribbon with solvent |
| CN103508492A (en) * | 2013-09-27 | 2014-01-15 | 陕西科技大学 | Method for rapidly preparing NdWO4(OH) nanopowder |
| CN103922412A (en) * | 2014-04-17 | 2014-07-16 | 陕西科技大学 | Method for preparing flaky SmWO4(OH) with microwave hydrothermal method |
| CN103991913A (en) * | 2014-05-29 | 2014-08-20 | 陕西科技大学 | Method for preparing CoWO4 nano powder material by adopting microwave-hydrothermal method |
| CN104722298A (en) * | 2015-03-26 | 2015-06-24 | 电子科技大学 | Method for preparing titania composite nano-gold photocatalyst |
| US20150174659A1 (en) * | 2010-12-09 | 2015-06-25 | Carestream Health, Inc. | Nanowire preparation methods, compositions, and articles |
| CN106076367A (en) * | 2016-06-12 | 2016-11-09 | 江苏大学 | One prepares CdS/CoWO4the method of heterojunction composite photocatalyst |
-
2016
- 2016-12-12 CN CN201611138429.2A patent/CN106735166B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150174659A1 (en) * | 2010-12-09 | 2015-06-25 | Carestream Health, Inc. | Nanowire preparation methods, compositions, and articles |
| CN103333689A (en) * | 2013-07-11 | 2013-10-02 | 黑龙江大学 | Method of thermosynthesis of SrWO4:Ln3<+> nanoribbon with solvent |
| CN103508492A (en) * | 2013-09-27 | 2014-01-15 | 陕西科技大学 | Method for rapidly preparing NdWO4(OH) nanopowder |
| CN103922412A (en) * | 2014-04-17 | 2014-07-16 | 陕西科技大学 | Method for preparing flaky SmWO4(OH) with microwave hydrothermal method |
| CN103991913A (en) * | 2014-05-29 | 2014-08-20 | 陕西科技大学 | Method for preparing CoWO4 nano powder material by adopting microwave-hydrothermal method |
| CN104722298A (en) * | 2015-03-26 | 2015-06-24 | 电子科技大学 | Method for preparing titania composite nano-gold photocatalyst |
| CN106076367A (en) * | 2016-06-12 | 2016-11-09 | 江苏大学 | One prepares CdS/CoWO4the method of heterojunction composite photocatalyst |
Non-Patent Citations (4)
| Title |
|---|
| YING-HUI LI等: "A hydrothermal assisted method to prepare Samarium Tungstate sheets at lowered reaction temperature", 《MATERIALS LETTERS》 * |
| 刘栋梁等: "表面活性剂对Bi２ WO６ 片层纳米晶形貌及其光致发光性能的影响", 《功能材料》 * |
| 吴菊: "水热法合成钨酸盐材料的纳米结构", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 曹丽云等: "NdWO4 （OH ）粉体的微波水热法合成及其光催化性能", 《陕西科技大学学报》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106735166B (en) | 2018-10-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Tong et al. | Near‐infrared, heavy metal‐free colloidal “Giant” core/shell quantum dots | |
| Zhu et al. | Hydrogenated blue titania with high solar absorption and greatly improved photocatalysis | |
| Naik et al. | Influence of Cu doping on ZnO nanoparticles for improved structural, optical, electrochemical properties and their applications in efficient detection of latent fingerprints | |
| Song et al. | Tumor cell-targeted Zn 3 In 2 S 6 and Ag–Zn–In–S quantum dots for color adjustable luminophores | |
| CN110627046B (en) | Nitrogen-doped graphene quantum dot and preparation method and application thereof | |
| CN109283235B (en) | Based on NSCQDs/Bi2S3Photoelectrochemical sensor and preparation method thereof | |
| Yang et al. | Multifunctional N-doped graphene quantum dots towards tetracycline detection, temperature sensing and high-performance WLEDs | |
| CN110240148B (en) | Tungsten diselenide/redox graphene composite structure with metal structure and preparation method thereof | |
| Li et al. | Near-infrared photoactive Yb-MOF functionalized with a large conjugate ionic liquid: synthesis and application for photoelectrochemical immunosensing of carcinoma embryonic antigen | |
| CN107670674A (en) | Indium sulfide material of rare earth element codope and its preparation method and application | |
| Dhandapani et al. | A potential forecast of carbon quantum dots (CQDs) as an ultrasensitive and selective fluorescence probe for Hg (II) ions sensing | |
| CN108587607B (en) | Luminescent metal organic framework material for detecting thiocyanate ions in water and preparation method and application thereof | |
| Zhang et al. | A sandwiched photoelectrochemical biosensing platform for detecting Cytokeratin-19 fragments based on Ag2S-sensitized BiOI/Bi2S3 heterostructure amplified by sulfur and nitrogen co-doped carbon quantum dots | |
| CN110373184A (en) | A kind of synthetic method of high yield red fluorescence carbon quantum dot material | |
| CN109507255A (en) | A kind of Preparation method and use of bismuth/carbonitride photoelectric material | |
| CN108659831A (en) | A kind of method that one kettle way prepares Solid substrate room temperature phosphorescence carbon dots | |
| Jiang et al. | Synthesis of Zn0· 1Cd0· 9S heterostructure with N-doped graphene quantum dots and graphene for enhancing photoelectric performance in UV–visible light | |
| Zhang et al. | ZnO/C nanocomposite grafted molecularly imprinted polymers as photoelectrochemical sensing interface for ultrasensitive and selective detection of chloramphenicol | |
| Xiao‐Yan et al. | Crown daisy leaf waste–derived carbon dots: A simple and green fluorescent probe for copper ion | |
| CN107603604A (en) | A kind of copper nanocluster fluorescent material and preparation method thereof | |
| Li et al. | Green synthesis of multifunctional carbon nanodots and their applications as a smart nanothermometer and Cr (VI) ions sensor | |
| Chen et al. | Synthesis and hybridization of CuInS 2 nanocrystals for emerging applications | |
| CN109735325A (en) | A kind of composite material using quantum dot enhancing up-conversion luminescence | |
| CN106735166B (en) | A kind of EuWO4(OH) preparation method of nanobelt and its composite material | |
| CN105907391A (en) | Method for preparing carbon quantum dots by aldehyde precursor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |