CN106745166A - A kind of synthetic method of quantum dot cerium oxide/modified oxidized cerium nano material - Google Patents
A kind of synthetic method of quantum dot cerium oxide/modified oxidized cerium nano material Download PDFInfo
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- 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
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- 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
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- Y02P20/00—Technologies relating to chemical industry
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- Y02P20/133—Renewable energy sources, e.g. sunlight
Abstract
The invention discloses a kind of synthetic method of quantum dot cerium oxide/modified oxidized cerium nano material; belong to solar energy, photocatalysis nano material, environmental sanitation, purification of air and green agriculture plant protection art; by adding a certain amount of cerium salt in certain alcohol water mixed solution; by controlling pH condition; it is precipitated thing; isothermal reaction in a kettle. again, can synthesize the quantum dot cerium oxide of about 5nm.Adding metal chloride, nitric acid compound and gold chloride of certain mol proportion example etc. in system simultaneously can form the quantum dot cerium oxide of different metal doping or modification.The present invention uses hydro-thermal method, can synthesize pure quantum dot cerium oxide with a series of Bu Tong element modified quantum dot cerium oxide；The present invention uses solvent heat, and quantum dot cerium oxide and modified quantum dot cerium oxide nano materials can be prepared by controlling reaction condition, and the material of preparation has the actual application values such as exhaust fume catalytic is processed and pathogenic microorganism is controlled.
Description
Technical field
The invention belongs to solar energy, photocatalysis nano material, environmental sanitation, purification of air and green agriculture plant protection neck
A kind of domain, and in particular to the synthetic method of quantum dot cerium oxide or modified oxidized cerium nano material.
Background technology
CeO2It is a kind of wide variety of inorganic material, its stable chemical nature is nontoxic, is most abundant in rare earth element
Element, is even more abundant in China's content.CeO2Performance is related to do polishing material, catalyst, catalyst carrier（Auxiliary agent）, ultraviolet
Absorbent, fuel-cell electrolyte, vehicle exhaust absorbent, electronic ceramics etc..Nano material is due to small size Xiao Ying ﹑ tables
Face effect is answered ﹑ to measure sub- size effect and answers ﹑ macro quanta tunnel effects and Dielectric confinement effect, and this series of effects result in nano material
All show in terms of many physics such as fusing point, vapour pressure, optical property, chemical reactivity, magnetic, superconduction and plastic deformation and chemistry
Special performance is shown.Cerium oxide is made into nano material can more improve its application value.
Cerium oxide is widely used in degradable organic pollutant and kills the micro- life of cause of disease as a kind of catalysis material in recent years
Thing is studied, and is the nano material that a kind of novel photocatalysis prevent and treat pathogen.Relative to chemical reagent such as traditional utilization antibiotic
The method for preventing and treating pathogen has the advantage that.One is sterilized thoroughly, due to the high activity hydroxyl radical free radical activity that photocatalysis is produced
The free radicals such as oxygen can not only kill pathogen can also degrade pathogen generation toxin.Secondly sterilization spectrum, photocatalysis is killed
The mechanism of bacterium is different with traditional chemistry and antibiotic sterilization mechanism, all has bactericidal effect to nearly all pathogen.Thirdly
Photo-catalyst utilizes sunlight as driving force, energy-conservation, environmental protection, but pure CeO2Energy gap~2.58 ev,
Only can be by part excited by visible light in sunshine, while light activated carrier is also easily combined, therefore by preparing particle diameter
Less nano particle and compound grade cerium modified to pure oxidation develop visible light-responded quantum dot CeO2It is beneficial to improve
Its actual application value.
Adulterated using technology or can improve CeO with other semiconductors couplings2Visible light-responded and catalytic effect.So
And the CeO for synthesizing2The problems such as material is due to particle diameter, catalytic efficiency and other performances have much room for improvement.
The content of the invention
The technical problem to be solved in the present invention is directed to current material and there is particle diameter greatly, the performance shortcoming not high such as catalysis,
There is provided a kind of using a kind of easy method quantum dot cerium oxide/modified oxidized cerium nano material of synthesis.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of synthetic method of quantum dot cerium oxide/modified oxidized cerium nano material, step is as follows：
（1）Cerium salt is dissolved in alcoholic solution and forms cerium solution, be subsequently adding slaine, fully add NaOH after dissolving
The pH of ethanol solution regulation system is 3 ~ 6, stirs to form mixed solution；
（2）By step（1）Obtained mixed solution pours into reactor the isothermal reaction 1-12h under conditions of 120 ~ 250 DEG C, obtains
To sediment；
（3）By step（2）The sediment for obtaining is washed with water and ethanol, and quantum dot cerium oxide/modified oxidized cerium is obtained after drying
Nano material.
The step（1）In cerium salt be CeCl3Or Ce (NO3)3, described alcohol is methyl alcohol or ethanol, described slaine
For the chloride or copper of copper, palladium, silver, gold, manganese, niobium, tungsten, neodymium, nickel, platinum, gold or cadmium, palladium, silver, gold, manganese, niobium, tungsten, neodymium, nickel,
The nitric acid thing of platinum, gold or cadmium.
The step（1）The molar concentration of cerium salt is 0.05 ~ 0.3mol/L in the mixed solution for obtaining.
The step（1）The ratio between amount of material of middle cerium salt and slaine is 1:0~0.2.
The step（2）Middle reaction temperature is 160 ~ 200 DEG C.
The step（2）The middle reaction time is 2 ~ 10h.
The molar concentration scope of present invention cerium salt in each specific reaction system in giving, the content concn model of modified metal element
Enclose and different alcohol used, modified Nano material can be obtained in scope, in the optimization range for being further given, can
To obtain the more preferable modified quantum dot nano material of bactericidal property.Modified Nano material in the present invention is visible light-responded height
Effect catalytically bactericidal process material, key factor be in this preparation method can will be metal-doped or load to ceria, improve it
Visible absorption and raising catalytic performance.Temperature conditionss needed for present invention reaction, can not crystallization well less than 120 DEG C；120
When more than DEG C, Emission in Cubic ceria can be obtained, temperature is higher, resulting materials crystallization is better, after 250 DEG C, reaction danger
Dangerous increase.Required reaction time, reaction time>2h can be obtained by it is material modified, the extension time be conducive to reaction enter completely
OK, crystal grain crystallization is conducive to.
Design principle of the present invention is as follows：
Cerium salt and slaine are well mixed in alcohol hydrating agents, add a certain amount of NaOH to form precipitation, then by water
Thermal response, single step reaction prepares metal-doped or modification modified quantum dot cerium dioxide nano material.
The present invention has the advantage that and technique effect：
1. the present invention is mixed using different metal salt and cerium salt, in different solvents, is prepared for a series of metal-modifieds or doping
Modified quantum dot nano material.
2. raw material of the present invention is cheap, and cost is relatively low, does not use dispersant, simple to operate, it is easy to control.
3. the quantum-dot modified nano material prepared by the present invention, can kill bacterium under visible light.
Brief description of the drawings
Fig. 1 is Cu/CeO prepared by the embodiment of the present invention 12XRD spectra；
Fig. 2 is Cu/CeO prepared by the embodiment of the present invention 12Ultraviolet-visible absorption collection of illustrative plates；
Fig. 3 is Cu/CeO prepared by the embodiment of the present invention 12TEM photos；
Fig. 4 is Cu/CeO prepared by the embodiment of the present invention 12XPS spectrum figure；
Fig. 5 is Cu/CeO prepared by the embodiment of the present invention 12Killing curve figure；
Fig. 6 is CeO prepared by the embodiment of the present invention 22TEM figure；
Fig. 7 is Cu/CeO prepared by the embodiment of the present invention 32TEM figure；
Fig. 8 is Pd/CeO prepared by the embodiment of the present invention 42TEM figure.
Specific embodiment
With reference to specific embodiment, the present invention will be further described.It should be understood that following examples are merely to illustrate this
Invention can make one not for limitation the scope of the present invention, the person skilled in the art in the field according to the content of foregoing invention
A little nonessential modifications and adaptations.
Embodiment 1
The quantum-dot modified cerium oxide nano materials Cu/CeO of the present embodiment2Synthetic method, step is as follows：
（1）Room temperature, in the presence of magnetic agitation, by 6mmol (2.24g) CeCl3∙7H2O（Purity is 99.99%）Add
The alcohol hydrating agents of cerium chloride are formed in 30mL methanol solutions, 3.6mmol is subsequently adding（0.62g）CuCl2∙2H2O（Purity is
99%）, it is stirred vigorously 20 minutes, fully dissolving, 30mL is contained into 42mmol（1.73g）NaOH（Purity is 97%）Methyl alcohol it is molten
Liquid and above-mentioned solution mix（The PH=4.5 of adjustment system）, mixture is stirred vigorously half an hour；
（2）By step（1）The mixed system for obtaining is imported in the reactor of the polytetrafluoroethyllining lining of 100mL volumes, at 200 DEG C
Lower insulation 4 hours, obtains deposit；
（3）Then, by gained deposit ethanol and water washing several times, Cu/CeO is obtained after being dried at 80 DEG C2Powder, sample
It is designated as A.
XRD analysis are carried out to the sample for obtaining using German Bruker companies D8 Advance types X-ray diffractometers.As schemed
1 XRD spectra for showing sample, XRD spectra display sample is Emission in Cubic ceria and Emission in Cubic copper.It is public using FDAC
Department U-3900H ultraviolet-visible solid diffusing reflection instruments sample light absorbs are analyzed, as shown in Figure 2 prepare material have compared with
Good visible absorption effect.
The appearance structure of sample is obtained using the type transmission electron microscope observation of JEOL 2100, sample is illustrated in figure 3
The TEM photos of product, as a result visible, gained CeO2Size be about 5nm, it is relatively uniform.Using Thermo Fischer Scient Inc.
Element contained by the x-ray photoelectron spectroscopy test sample of ESCALAB250, is illustrated in figure 4 the XPS figures of sample.
Visible light photocatalysis experiment is carried out using the xenon source of Beijing Bo Feilai Science and Technology Ltd.s, as shown in Figure 5 system
Have under standby material visible-light well kill Escherichia coli (Escherichia coli) effect.
Embodiment 2
The quantum dot cerium oxide nano materials CeO of the present embodiment2Synthetic method, step is as follows：
（1）Room temperature, in the presence of magnetic agitation, by 3mmol (1.12g) CeCl3∙7H2O（Purity is 99.99%）Add
The alcohol hydrating agents of the cerium chloride formed in 30mL ethanol waters, wherein ethanol mass fraction are 95%, are stirred vigorously 20 minutes,
Fully dissolving, 9mmol is contained by 30mL（0.37g）NaOH（Purity is 97%）95% ethanol solution and above-mentioned solution mixing（Adjustment
System PH=3）, mixture is stirred vigorously half an hour；
（2）By step（1）The mixed system solution for obtaining is imported in the reactor of the polytetrafluoroethyllining lining of 100mL volumes,
2 hours are incubated at 160 DEG C, deposit is obtained；
（3）Gained deposit is washed several times with water and ethanol, pure CeO is obtained after being dried at 80 DEG C2Powder, sample is designated as B.
Embodiment 3
The synthetic method of the quantum-dot modified cerium oxide nano materials Cu/CeO2 of the present embodiment, step is as follows：
（1）Room temperature, in the presence of magnetic agitation, by 10.5mmol (3.92g) CeCl3∙7H2O（Purity is 99.99%）Plus
Enter the pure water mixture of formation cerium chloride in 30mL95% methanol solutions, be subsequently adding 1.05mmol (0.46g) Cu (NO3)2∙6H2O
（Purity is 99.99%）, it is stirred vigorously 20 minutes, fully dissolving, 30mL is contained into 42mmol（1.73g）NaOH（Purity is 97%）'s
95% methanol solution and above-mentioned solution mix（Adjustment system PH=4.5）, mixture is stirred vigorously half an hour；
（2）By step（1）The mixed system solution for obtaining is imported in the reactor of the polytetrafluoroethyllining lining of 100mL volumes,
6 hours are incubated at 180 DEG C, deposit is obtained；
（3）By gained deposit ethanol and water washing several times, Cu/CeO is obtained after being dried at 80 DEG C2Powder, sample is designated as
C。
Sample is detected using the equipment of embodiment 1, the pattern of sample is illustrated in figure 6 the TEM photos of sample C,
Gained Cu/CeO2Uniformity is preferable.XRD spectra display sample is Emission in Cubic ceria and Emission in Cubic copper.
Embodiment 4
The synthetic method of the quantum-dot modified cerium oxide nano materials Cu/CeO2 of the present embodiment, step is as follows：
（1）Room temperature, in the presence of magnetic agitation, by 18mmol（6.72g）CeCl3∙7H2O（Purity is 99.99%）Add
The alcohol hydrating agents of cerium chloride are formed in 30mL ethanol solutions, 3.6mmol is subsequently adding（0.64g）PdCl2（Purity is 99.99%）,
It is stirred vigorously 20 minutes, fully dissolving, 30mL is contained into 90mmol（3.71g）NaOH（Purity is 97%）Ethanol solution and upper
Solution mixing (adjustment system PH=6) is stated, mixture is stirred vigorously half an hour；
（2）By step（1）The mixed system for obtaining is imported in the reactor of the polytetrafluoroethyllining lining of 100mL volumes, at 200 DEG C
Lower insulation 10 hours, obtains deposit；
（3）By gained deposit ethanol and water washing several times, Pd/CeO is obtained after being dried at 80 DEG C2Powder, sample is designated as
D。
Sample is detected using the equipment of embodiment 1, the pattern of sample is illustrated in figure 7 the TEM photos of sample D,
It is quantum dot Pd/CeO2.XRD spectra display sample is Emission in Cubic ceria.
Other slaines etc. act on identical in the present invention, can obtain material modified, therefore do not providing embodiment
On the premise of, can be it is envisioned that identical technique effect.
General principle of the invention and principal character and advantages of the present invention has been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the simply explanation described in above-described embodiment and specification
Principle of the invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appending claims and
Its equivalent thereof.
Claims (6)
1. the synthetic method of a kind of quantum dot cerium oxide/modified oxidized cerium nano material, it is characterised in that step is as follows：
（1）Cerium salt is dissolved in alcoholic solution and forms cerium solution, be subsequently adding slaine, fully add NaOH after dissolving
The pH of alcoholic solution regulation system is 3 ~ 6, stirs to form mixed solution；
（2）By step（1）Obtained mixed solution pours into reactor the isothermal reaction 1-12h under conditions of 120 ~ 250 DEG C, obtains
To deposit；
（3）By step（2）The sediment for obtaining is washed with water and ethanol, and quantum dot cerium oxide/modified oxidized cerium is obtained after drying
Nano material.
2. the synthetic method of quantum dot cerium oxide according to claim 1/modified oxidized cerium nano material, its feature exists
In：The step（1）In cerium salt be CeCl3∙7H2O or Ce (NO3)3∙6H2O, described alcohol is methyl alcohol that mass fraction is 95%
The aqueous solution or mass fraction are 95% ethanol water, described slaine is copper, palladium, silver, gold, manganese, niobium, tungsten, neodymium, nickel,
The chloride or copper of platinum, gold or cadmium, palladium, silver, gold, manganese, niobium, tungsten, neodymium, nickel, platinum, the nitric acid thing of gold or cadmium.
3. the synthetic method of quantum dot cerium oxide according to claim 1/modified oxidized cerium nano material, its feature exists
In：The step（1）The molar concentration of cerium salt is 0.05 ~ 0.3mol/L in the mixed solution for obtaining.
4. the synthetic method of quantum dot cerium oxide according to claim 1/modified oxidized cerium nano material, its feature exists
In：The step（1）The ratio between amount of material of middle cerium salt and slaine is 1:0~0.2.
5. the synthetic method of quantum dot cerium oxide according to claim 1/modified oxidized cerium nano material, its feature exists
In：The step（2）Middle reaction temperature is 160 ~ 200 DEG C.
6. the synthetic method of quantum dot cerium oxide according to claim 1/modified oxidized cerium nano material, its feature exists
In：The step（2）The middle reaction time is 2 ~ 10h.
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Cited By (6)
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| CN107651703A (en) * | 2017-09-19 | 2018-02-02 | 天津大学 | The preparation method of particular crystal plane nano ceric oxide |
| CN109110793A (en) * | 2018-03-22 | 2019-01-01 | 云南大学 | A kind of preparation method of alumina load nano-cerium oxide compound gold and ru oxide |
| CN109651360A (en) * | 2018-12-19 | 2019-04-19 | 云南大学 | A kind of method that the compound gold of nano-cerium oxide prepares fibrauretine with ru oxide photocatalysis |
| CN110367280A (en) * | 2019-08-09 | 2019-10-25 | 大连民族大学 | A kind of Ag/CeO2Antibacterial agent and preparation method thereof |
| CN111280176A (en) * | 2019-08-28 | 2020-06-16 | 大连民族大学 | Au/CeO2Bactericide and preparation method and application thereof |
| CN113054145A (en) * | 2019-12-28 | 2021-06-29 | Tcl集团股份有限公司 | Composite material, preparation method and application thereof, light-emitting diode and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107651703A (en) * | 2017-09-19 | 2018-02-02 | 天津大学 | The preparation method of particular crystal plane nano ceric oxide |
| CN109110793A (en) * | 2018-03-22 | 2019-01-01 | 云南大学 | A kind of preparation method of alumina load nano-cerium oxide compound gold and ru oxide |
| CN109651360A (en) * | 2018-12-19 | 2019-04-19 | 云南大学 | A kind of method that the compound gold of nano-cerium oxide prepares fibrauretine with ru oxide photocatalysis |
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