CN105016389B - A kind of lead molybdate nanocrystal of carbon shell cladding and preparation method thereof - Google Patents
A kind of lead molybdate nanocrystal of carbon shell cladding and preparation method thereof Download PDFInfo
- Publication number
- CN105016389B CN105016389B CN201510412852.6A CN201510412852A CN105016389B CN 105016389 B CN105016389 B CN 105016389B CN 201510412852 A CN201510412852 A CN 201510412852A CN 105016389 B CN105016389 B CN 105016389B
- Authority
- CN
- China
- Prior art keywords
- lead
- nanocrystal
- preparation
- cladding
- molybdate
- 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.)
- Expired - Fee Related
Links
Landscapes
- Carbon And Carbon Compounds (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to lead molybdate nanocrystal of a kind of carbon shell cladding and preparation method thereof, wherein use citric acid to control to synthesize the lead molybdate nano material of different carbon thickness of the shell, specifically, described preparation method is simple, novel, controllability is strong.Lead molybdate composite nanocrystal purity height, length and the width thereof of the carbon-coating cladding synthesized are about 100 nanometers and 50 ran, it addition, the separation of the carbon shell being coated with outside the lead molybdate composite obtained, more conducively electronics and transfer.As the cathode material of photoelectrocatalysis splitting water, its stability and catalytic efficiency can also be improved, and meet the research in terms of up-to-date clean energy resource and sustainable energy thereof.
Description
Technical field
The present invention relates to materials synthesis field, more particularly to the semiconductor nano material of a kind of carbon shell cladding
And the application that the semiconductor nano material of synthetic method and described carbon shell cladding is in hydrogen energy source field, more
Concretely relate to the lead molybdate nano material using citric acid to control to synthesize different carbon thickness of the shell,
The lead molybdate nano material being additionally related to prepared lead molybdate and carbon cladding thereof cracks at photoelectrocatalysis
Application in terms of water.
Background technology
Hydrogen is a kind of cleaning, free of contamination novel energy, is expected to substitute fossil fuels, meets whole world energy
Source demand, alleviating energy crisis.At present, utilize sunlight to carry out photoelectrocatalysis splitting water and prepare hydrogen tool
There are environmental protection and energy saving, the advantage such as sustainable, become focus of concern.But present stage light photoelectrocatalysis
Semi-conducting electrode material in splitting water device nevertheless suffers from serious restriction, causes photoelectrocatalysis splitting water
Produce hydrogen efficiency is low, industrialization cost high and the problem such as poor stability.
Lead molybdate is as the important p-type semiconductor material of a class, and its band-gap energy is 3.2eV, wherein
Valence-band is about-0.6eV, and conduction band energy is about 2.6eV, be conventional luminescence generated by light, scintillator,
Sensor and catalysis material.Additionally, relative to other common semiconductor material, lead molybdate is at nature
In with scheelite form exist, rich reserves, use cost is low.But p-type semiconductor is as photoelectrochemical
There is a serious defect in the cathode material learning decomposition water, it is simply that works long hours easily by electrolyte also
Former, stability is poor, and the life-span is comparatively short.Therefore, University of Texas-Austin of the U.S. has synthesized p-n junction
P-PbMoO4/n-Bi2O3Nano composite material, and test this material property at photoelectrocatalysis splitting water
Energy (J.Phys.Chem.Lett.2013,4,2707-2710).Test data show: the p-n junction of formation is received
The stability of nano composite material is improved.But this quasiconductor is compound with quasiconductor, reduces
The electric conductivity of material, have impact on its photocatalysis efficiency；And in preparation process, exist complex process,
The problem such as relatively costly.
Summary of the invention
In the present invention, inventor uses in solvent process for thermosynthesizing that citric acid is controlled prepares lead molybdate
And the lead molybdate of carbon cladding is nanocrystalline.Reaction solution adds different amounts of citric acid and can obtain carbon shell
Thickness is the lead molybdate nanocrystal of 2 to 20 nanometer claddings.Found by measurement, the carbon-coating outside lead molybdate
The electric conductivity of material can be promoted, stop lead molybdate to be corroded by electrolyte solution.Therefore prepared carbon shell
The lead molybdate nanocrystal of cladding is nanocrystalline relative to exposed lead molybdate, the effect of its photoelectrocatalysis splitting water
Rate and stability have obtained bigger lifting.
It is an object of the present invention to provide the lead molybdate nanocrystal of a kind of carbon shell cladding, described molybdic acid
The carbon thickness of the shell of lead nanocrystal is 2 to 20 nanometers, preferably 2 to 10 nanometers, more preferably 2 to
8 nanometers.Can be such as 2 nanometers, 5 nanometers or 8 nanometers, most preferably 2 nanometers, its length and width
Degree is about 50 to 100 nanometers and 20 to 50 ran.
Further object is that the preparation side of the lead molybdate nanocrystal that a kind of carbon shell cladding is provided
Method, described preparation method includes:
1) at room temperature, by three acetate hydrate lead that mol ratio is 1:1 and seven AMMONIUM MOLYBDATE(VI), Yi Jishi
Amount solvent add reactor polytetrafluoroethyllining lining in and stir 2 to 15 minutes；
2) three acetate hydrate lead and seven AMMONIUM MOLYBDATE(VI) based on 100 weight portions altogether, by 100-2000
The citric acid of weight portion joins aforesaid reaction vessel inside liner, is further continued for stirring 5 to 10 minutes；
3) after tightening kettle cover, reactor is put in the electric drying oven with forced convection of 100-240 degree, and keep
30-90 minute；
4) take out reactor and naturally cool to room temperature state, subsequently, with dehydrated alcohol with deionized water repeatedly
Intersection is centrifugal, washed product, and desciccate in vacuum drying oven.Thus obtained the product of white.
Preferably, the step of the preparation method of the lead molybdate nanocrystal being coated with at the carbon shell according to the present invention
1) one or more in solvent selected from methanol, ethanol and deionized water, more preferably deionized water in,
Three acetate hydrate lead and seven AMMONIUM MOLYBDATE(VI) based on 100 weight portions altogether, the amount of described solvent is 5-20
Weight portion.
Preferably, the step of the preparation method of the lead molybdate nanocrystal being coated with at the carbon shell according to the present invention
2) in, three acetate hydrate lead and seven AMMONIUM MOLYBDATE(VI) based on 100 weight portions altogether, the addition of citric acid
Amount is 100-1200 weight portion, preferably 100-1050 weight portion, more preferably 105-1050 weight portion,
Most preferably selected from 105 weight portions, 210 weight portions or 1050 weight portions.
Beneficial effect
Present invention have the advantage that: this type of synthetic method is simple, novel, controllability is strong.Utilize lemon
Lemon acid pyrolytic prepares the carbon nanometer layer of different-thickness, low cost, environmental protection, pollution-free.Synthesis
Lead molybdate composite nanocrystal purity height, length and the width thereof of material with carbon element cladding are about 100 nanometers and 50
Ran.It addition, obtain lead molybdate composite outside cladding carbon shell, more conducively electronics point
From with transfer.As the cathode material of Optical Electro-Chemistry decomposition water, its stability and catalytic efficiency can also obtain
Improve, also comply with the research in terms of up-to-date clean energy resource and sustainable energy thereof.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of embodiment product, and wherein photo 1 is according to embodiment 1
The lead molybdate nanocrystal of 2 nano-sized carbon shell claddings of preparation, photo 2 is 5 according to embodiment 2 preparation
The lead molybdate nanocrystal of nano-sized carbon shell cladding, photo 3 is the 8 nano-sized carbon shells according to embodiment 3 preparation
The lead molybdate nanocrystal of cladding, and the molybdenum that photo 4 is the uncoated carbon shell according to embodiment 4 preparation
Lead plumbate nanocrystal；
Fig. 2 is the X-ray powder diffraction figure of sample obtained according to embodiment, curve 1 in figure, 2,3,
4 represent the lead molybdate nanocrystal of the uncoated carbon shell according to embodiment 4 preparation, respectively according to embodiment 1
Preparation 2 nano-sized carbon shells cladding lead molybdate nanocrystal, according to embodiment 2 preparation 5 nano-sized carbon shells
The lead molybdate nanocrystal of cladding and the lead molybdate nanometer of the 8 nano-sized carbon shell claddings according to embodiment 3 preparation
Brilliant；
Fig. 3 is the high resolution electron microscope photo of sample obtained according to embodiment, photo 1 in figure, 2,
3,4 the lead molybdate nanocrystal of the uncoated carbon shell according to embodiment 4 preparation is represented respectively, according to enforcement
Example 1 preparation 2 nano-sized carbon shells cladding lead molybdate nanocrystal, according to embodiment 2 preparation 5 nanometers
The lead molybdate nanocrystal of carbon shell cladding and the lead molybdate of the 8 nano-sized carbon shell claddings according to embodiment 3 preparation
Nanocrystalline；
Fig. 4 is the Raman spectrogram of the sample obtained according to embodiment, and in figure, curve 1,2,3,4 is respectively
Represent the lead molybdate nanocrystal of the uncoated carbon shell according to embodiment 4 preparation, prepare according to embodiment 1
2 nano-sized carbon shells cladding lead molybdate nanocrystal, according to embodiment 2 preparation 5 nano-sized carbon shells cladding
Lead molybdate nanocrystal and according to embodiment 3 preparation 8 nano-sized carbon shells cladding lead molybdate nanocrystalline,
Wherein I, II represent D band and G band respectively, and its position is about 1363cm-1With 1595cm-1.With
Time D band and G band represent respectively is carbon and the orderly graphitic carbon of lack of alignment, this Raman spectrogram is said
Clear Lead molybdate nano crystal material is surface coated is carbon shell；
Fig. 5 is the linear sweep voltammetry curve when Optical Electro-Chemistry water-splitting of the sample according to embodiment acquisition
Figure, in figure, curve 1 represents the blank FTO (SnO of doped with fluorine of non-coated samples2Transparent conducting glass),
Curve 2,3,4,5 represents uncoated according to embodiment 4 preparation being coated on blank FTO respectively
The lead molybdate nanocrystal of carbon shell, 2 nano-sized carbon according to embodiment 1 preparation being coated on blank FTO
The lead molybdate nanocrystal of shell cladding, 5 nanometers according to embodiment 2 preparation being coated on blank FTO
The lead molybdate nanocrystal of carbon shell cladding, according to embodiment 3 preparation 8 be coated on blank FTO are received
The lead molybdate nanocrystal of rice carbon shell cladding.
Detailed description of the invention
Following example are enumerated only as the example of embodiment of the present invention, do not constitute the present invention
Any restriction, it will be appreciated by those skilled in the art that without departing from the present invention essence and design in the range of
Amendment each fall within protection scope of the present invention.
The instrument used in an embodiment has:
(model is x-ray powder diffraction instrument: Rigaku D/Max 2200PC, wherein copper KαRadiation
Diffractometer () and graphite monochromator scanning angle per minute from 10 °-80 ° and scanning speed
5.0°)；(model is transmission electron microscope: JEM100-CXII)；High-resolution-ration transmission electric-lens (model is:
GEOL-2010)；Raman spectrometer (model is: NEXUS 670), electrochemical workstation (model is:
CHI 660D), Optical Electro-Chemistry water-splitting tester (comprising: 350 watts of xenon lamps, the optical filtering of different wave length
Sheet, camera bellows, LP-3A laser power meter) (Beijing Heng Gong Instrument Ltd.).
The chemical reagent three acetate hydrate lead used and ammonium molybdate are commercially available reagent pure reagent.
The synthesis of the lead molybdate nanocrystal of embodiment 1:2 nano-sized carbon shell cladding
First three acetate hydrate lead (75.9 milligrams) and ammonium molybdate (35.3 milligrams) are at room temperature added
It is in the polytetrafluoroethyllining lining of 20 milliliters to volume, subsequently with liquid-transfering gun by 12.0 milliliters go
Ionized water joins in polytetrafluoroethyllining lining, and the solution of above-mentioned acquisition is placed on magnetic stirring apparatus stirring
10 minutes.
The citric acid of 105.0 milligrams is joined in above-mentioned liquid, more molten by what above-mentioned reaction liner obtained
Liquid stirs 5 minutes on magnetic stirring apparatus.
It follows that the reaction liner that will be equipped with precursor aqueous solution is put in the reactor of stainless steel casing, tighten
Kettle cover, then reactor is put in the electric drying oven with forced convection of 200 degree, and keep 1 hour.
After reaction terminates, the reactor of taking-up is cooled to room temperature state, the solution in reaction liner is turned
Move on in the centrifuge tube of 10ml, the solution dehydrated alcohol in centrifuge tube is intersected with deionization waterside and washes
Wash 3 times, be centrifuged and just obtained white precipitate；The white precipitate obtained is placed on the vacuum drying oven of 50 degree
In be dried just obtained final product.
The transmission electron microscope photo of the final products that the photo 1 of Fig. 1 is prepared for the present embodiment, this photograph
Its length and the width of sheet display preparation are about 50 to 100 nanometers and 20 to 50 ran；Fig. 2
In the X-ray powder diffraction figure of final products prepared for the present embodiment of curve 2, can from figure
Go out, synthesize the product degree of crystallinity obtained under hydrothermal conditions high；Photo 2 in Fig. 3 is the present embodiment system
The high resolution electron microscope photo of standby final products；The curve 2 of Fig. 4 is prepared for the present embodiment
The Raman spectrogram of finished product, has absorption band D band to carry with G in this Raman spectrum, and its position is about
1363cm-1With 1595cm-1, illustrate what lead molybdate nanocrystal outer surface prepared by the present embodiment was coated with
It it is carbon shell.
The lead molybdate nanocrystal of embodiment 2:5 nano-sized carbon shell cladding
In addition to adding the citric acid of 210.0 milligrams, prepare 5 according to the method that embodiment 1 is identical and receive
The lead molybdate nanocrystal of rice carbon shell cladding.
The transmission electron microscope photo of the final products that the photo 2 of Fig. 1 is prepared for the present embodiment, this photograph
Its length and the width of sheet display preparation are about 50 to 100 nanometers and 20 to 50 ran；Fig. 2
In the X-ray powder diffraction figure of final products prepared for the present embodiment of curve 3, can from figure
Go out, synthesize the product degree of crystallinity obtained under hydrothermal conditions high；Photo 3 in Fig. 3 is the present embodiment system
The high resolution electron microscope photo of standby final products；The curve 3 of Fig. 4 is prepared for the present embodiment
The Raman spectrogram of finished product, has absorption band D band to carry with G in this Raman spectrum, and its position is about
1363cm-1With 1595cm-1, illustrate what lead molybdate nanocrystal outer surface prepared by the present embodiment was coated with
It it is carbon shell.
The lead molybdate nanocrystal of embodiment 3:8 nano-sized carbon shell cladding
In addition to adding the citric acid of 1050 milligrams, prepare 8 according to the method that embodiment 1 is identical and receive
The lead molybdate nanocrystal of rice carbon shell cladding.
The transmission electron microscope photo of the final products that the photo 3 of Fig. 1 is prepared for the present embodiment, this photograph
Its length and the width of sheet display preparation are about 50 to 100 nanometers and 20 to 50 ran；Fig. 2
In the X-ray powder diffraction figure of final products prepared for the present embodiment of curve 4, can from figure
Go out, synthesize the product degree of crystallinity obtained under hydrothermal conditions high；Photo 4 in Fig. 3 is the present embodiment system
The high resolution electron microscope photo of standby final products；The curve 4 of Fig. 4 is prepared for the present embodiment
The Raman spectrogram of finished product, has absorption band D band to carry with G in this Raman spectrum, and its position is about
1363cm-1With 1595cm-1, illustrate what lead molybdate nanocrystal outer surface prepared by the present embodiment was coated with
It it is carbon shell.
Embodiment 4: the lead molybdate nanocrystal of uncoated carbon shell
In addition to without citric acid, prepare the molybdenum of uncoated carbon shell according to the method that embodiment 1 is identical
Lead plumbate nanocrystal.
The transmission electron microscope photo of the final products that the photo 1 of Fig. 1 is prepared for the present embodiment, this photograph
Its length and the width of sheet display preparation are about 50 to 100 nanometers and 20 to 50 ran；Fig. 2
In the X-ray powder diffraction figure of final products prepared for the present embodiment of curve 1, can from figure
Go out, synthesize the product degree of crystallinity obtained under hydrothermal conditions high；Photo 1 in Fig. 3 is the present embodiment system
The high resolution electron microscope photo of standby final products；The curve 1 of Fig. 4 is prepared for the present embodiment
The Raman spectrogram of finished product, has absorption band D band to carry with G in this Raman spectrum, and its position is about
1363cm-1With 1595cm-1, illustrate what lead molybdate nanocrystal outer surface prepared by the present embodiment was coated with
It it is carbon shell.
Test example: Optical Electro-Chemistry water-splitting is tested
The sample and the blank that use preparation in photoelectrocatalysis splitting water tester testing example 1 to 4 are mixed
The SnO of miscellaneous fluorine2The performance of the Optical Electro-Chemistry water-splitting of transparent conducting glass (FTO).
First, respectively by embodiment 1 to 4 preparation sample be dispersed in respectively in hexamethylene, then by
Drop coating is added to, above clean blank FTO, be dried 1 hour afterwards under the nitrogen atmosphere of 60 degree.So
After, the sample first step obtained is put into the electricity of 100 milliliters of aqueous solutions containing 0.5 mol sulfuric acid respectively
Xie Chizhong tests, and different samples obtains different density of photocurrent numerical value.Test result shows: compare
For the lead molybdate nanocrystal of the carbon-free shell cladding of preparation in embodiment 4, there is different-thickness carbon shell
The lead molybdate nanocrystal of cladding has preferable performance, meanwhile, molybdic acid in terms of Optical Electro-Chemistry water-splitting
Outside lead, the material with carbon element of cladding is more beneficial for separating and shifting and also improve material water-splitting of electronics
Stability.
Fig. 5 is the linear sweep voltammetry curve when Optical Electro-Chemistry water-splitting of the sample according to embodiment acquisition
Figure, in figure, curve 1 represents the blank FTO (the SnO2 transparent conducting glass of doped with fluorine) of non-coated samples,
Curve 2,3,4,5 represents uncoated according to embodiment 4 preparation being coated on blank FTO respectively
The lead molybdate nanocrystal of carbon shell, 2 nano-sized carbon according to embodiment 1 preparation being coated on blank FTO
The lead molybdate nanocrystal of shell cladding, 5 nanometers according to embodiment 2 preparation being coated on blank FTO
The lead molybdate nanocrystal of carbon shell cladding, according to embodiment 3 preparation 8 be coated on blank FTO
The lead molybdate nanocrystal of nano-sized carbon shell cladding can obtain from Fig. 5: compared to standard hydrogen electrode, real
Executing the lead molybdate nanocrystal of the 2 nano-sized carbon shells claddings that example 1 obtained, what embodiment 2 was obtained 5 receives
The lead molybdate nanocrystal of rice carbon shell cladding, the lead molybdate of the 8 nano-sized carbon shell claddings that embodiment 3 is obtained
Nanocrystal, the density of photocurrent of the lead molybdate nanocrystal of the non-carbon shell cladding that embodiment 4 is obtained divides
It is not 2.7,1.8,1.6,0.5 (milliamps per square centimeter).Meanwhile, further comparative result shows:
In the sample that the ownership is standby, the lead molybdate nanocrystal of the 2 nano-sized carbon shell claddings that embodiment 1 is obtained exists
Photoelectrocatalysis cracking Aquatic product hydrogen and stability aspect thereof are best.
Claims (9)
1. a preparation method for the lead molybdate nanocrystal of carbon shell cladding, described preparation method includes:
1) at room temperature, by three acetate hydrate lead that mol ratio is 1:1 and seven AMMONIUM MOLYBDATE(VI), Yi Jishi
Amount solvent add reactor polytetrafluoroethyllining lining in and stir 2 to 15 minutes；
2) three acetate hydrate lead and seven AMMONIUM MOLYBDATE(VI) based on 100 weight portions altogether, by 100-2000
The citric acid of weight portion joins aforesaid reaction vessel inside liner, is further continued for stirring 5 to 10 minutes；
3) after tightening kettle cover, reactor is put in the electric drying oven with forced convection of 100-240 degree, and keep
30-90 minute；
4) take out reactor and naturally cool to room temperature state, subsequently, intersect with deionized water with dehydrated alcohol
Centrifugal, washed product 2-5 time, and desciccate in vacuum drying oven, thus obtained white product
Product.
The preparation method of the lead molybdate nanocrystal of carbon shell the most according to claim 1 cladding, it is special
Levy and be, the step 1 in described preparation method) in solvent selected from methanol, ethanol and deionized water
One or more, three acetate hydrate lead and seven AMMONIUM MOLYBDATE(VI) based on 100 weight portions altogether, described molten
The amount of agent is 5-20 weight portion.
The preparation method of the lead molybdate nanocrystal of carbon shell the most according to claim 2 cladding, it is special
Levy and be, the step 1 in described preparation method) in solvent be deionized water.
The preparation method of the lead molybdate nanocrystal of carbon shell the most according to claim 1 cladding, it is special
Levy and be, the step 2 in described preparation method processed) in, three hydration second based on 100 weight portions altogether
Lead plumbate and seven AMMONIUM MOLYBDATE(VI), the addition of citric acid is 100-1200 weight portion.
The preparation method of the lead molybdate nanocrystal of carbon shell the most according to claim 4 cladding, it is special
Levy and be, the step 2 in described preparation method processed) in, three hydration second based on 100 weight portions altogether
Lead plumbate and seven AMMONIUM MOLYBDATE(VI), the addition of citric acid is 100-1050 weight portion.
The preparation method of the lead molybdate nanocrystal of carbon shell the most according to claim 4 cladding, it is special
Levy and be, the step 2 in described preparation method processed) in, three hydration second based on 100 weight portions altogether
Lead plumbate and seven AMMONIUM MOLYBDATE(VI), the addition of citric acid is 105 weight portions, 210 weight portions or 1050 weights
Amount part.
The preparation method of the lead molybdate nanocrystal of carbon shell the most according to claim 1 cladding, it is special
Levy and be, first 75.9 milligram of three acetate hydrate lead and 35.3 milligrams of ammonium molybdates are at room temperature joined appearance
Amassing is in the polytetrafluoroethyllining lining of 20 milliliters, is added by the deionized water of 12.0 milliliters with liquid-transfering gun subsequently
Enter in polytetrafluoroethyllining lining, the solution of above-mentioned acquisition be placed on magnetic stirring apparatus stirring 10 minutes,
Then the citric acid of 105.0 milligrams is joined in above-mentioned liquid, more molten by what above-mentioned reaction liner obtained
Liquid stirs 5 minutes on magnetic stirring apparatus, it follows that the reaction liner that will be equipped with precursor aqueous solution is put into not
In the reactor of rust outer steel shell, tighten kettle cover, then reactor is put into the electric heating forced air drying of 200 degree
In case, and keep 1 hour, after reaction terminates, the reactor of taking-up is cooled to room temperature state, will be anti-
Answer the solution in liner to transfer in the centrifuge tube of 10ml, by the solution dehydrated alcohol in centrifuge tube with
Deionization waterside cross washing 3 times, is centrifuged and has just obtained white precipitate；The white precipitate obtained is placed on
The vacuum drying oven of 50 degree is dried and has just obtained final product.
The preparation method of the lead molybdate nanocrystal of carbon shell the most according to claim 1 cladding, it is special
Levy and be, first 75.9 milligram of three acetate hydrate lead and 35.3 milligrams of ammonium molybdates are at room temperature joined appearance
Amassing is in the polytetrafluoroethyllining lining of 20 milliliters, is added by the deionized water of 12.0 milliliters with liquid-transfering gun subsequently
Enter in polytetrafluoroethyllining lining, the solution of above-mentioned acquisition be placed on magnetic stirring apparatus stirring 10 minutes,
Then the citric acid of 210.0 milligrams is joined in above-mentioned liquid, more molten by what above-mentioned reaction liner obtained
Liquid stirs 5 minutes on magnetic stirring apparatus, it follows that the reaction liner that will be equipped with precursor aqueous solution is put into not
In the reactor of rust outer steel shell, tighten kettle cover, then reactor is put into the electric heating forced air drying of 200 degree
In case, and keep 1 hour, after reaction terminates, the reactor of taking-up is cooled to room temperature state, will be anti-
Answer the solution in liner to transfer in the centrifuge tube of 10ml, by the solution dehydrated alcohol in centrifuge tube with
Deionization waterside cross washing 3 times, is centrifuged and has just obtained white precipitate；The white precipitate obtained is placed on
The vacuum drying oven of 50 degree is dried and has just obtained final product.
The preparation method of the lead molybdate nanocrystal of carbon shell the most according to claim 1 cladding, it is special
Levy and be, first 75.9 milligram of three acetate hydrate lead and 35.3 milligrams of ammonium molybdates are at room temperature joined appearance
Amassing is in the polytetrafluoroethyllining lining of 20 milliliters, is added by the deionized water of 12.0 milliliters with liquid-transfering gun subsequently
Enter in polytetrafluoroethyllining lining, the solution of above-mentioned acquisition be placed on magnetic stirring apparatus stirring 10 minutes,
Then the citric acid of 1050 milligrams is joined in above-mentioned liquid, then the solution that will obtain in above-mentioned reaction liner
Magnetic stirring apparatus stirs 5 minutes, it follows that the reaction liner that will be equipped with precursor aqueous solution is put into stainless
In the reactor of outer steel shell, tighten kettle cover, then reactor is put into the electric drying oven with forced convection of 200 degree
In, and keep 1 hour, after reaction terminates, the reactor of taking-up is cooled to room temperature state, will reaction
Solution in liner is transferred in the centrifuge tube of 10ml, by the solution dehydrated alcohol in centrifuge tube with go
Ion waterside cross washing 3 times, is centrifuged and has just obtained white precipitate；The white precipitate obtained is placed on 50
The vacuum drying oven of degree is dried and has just obtained final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510412852.6A CN105016389B (en) | 2015-07-14 | 2015-07-14 | A kind of lead molybdate nanocrystal of carbon shell cladding and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510412852.6A CN105016389B (en) | 2015-07-14 | 2015-07-14 | A kind of lead molybdate nanocrystal of carbon shell cladding and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105016389A CN105016389A (en) | 2015-11-04 |
| CN105016389B true CN105016389B (en) | 2016-10-19 |
Family
ID=54406769
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510412852.6A Expired - Fee Related CN105016389B (en) | 2015-07-14 | 2015-07-14 | A kind of lead molybdate nanocrystal of carbon shell cladding and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105016389B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106824086A (en) * | 2017-03-20 | 2017-06-13 | 东华理工大学 | A kind of carbosphere Quito point loads the preparation method of heterogeneous structure material |
| CN112891532B (en) * | 2021-01-27 | 2023-04-07 | 深圳技术大学 | Nano photo-thermal conversion material and preparation method and application thereof |
Family Cites Families (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3567477A (en) * | 1967-11-15 | 1971-03-02 | Du Pont | Molybdate orange pigment |
| JPH0673799B2 (en) * | 1988-01-30 | 1994-09-21 | 株式会社トーキン | Grinding method of PbMoO4 single crystal using c grindstone |
| JPH01305884A (en) * | 1988-06-03 | 1989-12-11 | Tokin Corp | Method of growing lead molybdate single crystal |
| US6331503B1 (en) * | 1998-04-15 | 2001-12-18 | Lehigh University | In-situ formation of metal-molybdate catalysts |
| RU2164562C1 (en) * | 2000-02-18 | 2001-03-27 | Аненков Александр Николаевич | Method of producing lead-tungstate scintillation single crystal |
| CN100489162C (en) * | 2003-12-30 | 2009-05-20 | 宁波大学 | Falling crucible method growth process for lead molybdate single crystal |
| CN102010006B (en) * | 2010-12-24 | 2012-05-30 | 金堆城钼业股份有限公司 | Synthesis method for lead molybdate |
| CN102071466B (en) * | 2010-12-24 | 2012-10-17 | 金堆城钼业股份有限公司 | Method for preparing lead molybdate polycrystalline material |
| CN102689922B (en) * | 2011-03-24 | 2017-04-19 | 杨春晓 | Lead compound nano-powder preparation method for recovery and manufacture of lead-acid battery |
| CN103387263B (en) * | 2013-07-11 | 2015-02-11 | 洛阳理工学院 | Lead molybdate nano crystal material and preparation method thereof |
| TWI499627B (en) * | 2013-10-11 | 2015-09-11 | Nanya Plastics Corp | A surface-coated inorganic filler molybdenum compound and use thereof |
| CN103754935B (en) * | 2014-01-07 | 2015-04-08 | 洛阳理工学院 | Method for synthesizing lead molybdate tower crystal at room temperature |
| CN103877984B (en) * | 2014-03-06 | 2016-01-20 | 同济大学 | Fe 3o 4cPbMoO 4the preparation method of core-shell magnetic nano material |
| CN105056965B (en) * | 2015-07-20 | 2017-11-28 | 长安大学 | Biological carbon ball load molybdic acid ferrous iron Fenton catalyst, preparation method and application |
-
2015
- 2015-07-14 CN CN201510412852.6A patent/CN105016389B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN105016389A (en) | 2015-11-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106521547B (en) | A kind of TiO2/RGO/C3N4The Preparation method and use of combination electrode | |
| Lv et al. | Graphitic carbon nitride decorated with C–N compounds broken by s-triazine unit as homojunction for photocatalytic H 2 evolution | |
| Guo et al. | Hierarchical TiO 2–CuInS 2 core–shell nanoarrays for photoelectrochemical water splitting | |
| CN104341006A (en) | Three-dimensional MoS2@MWNTs nanostructure and preparation method thereof | |
| CN112588303B (en) | Preparation method of selenium-bismuth oxide nanosheet and heterojunction type photoelectrode based on selenium-bismuth oxide nanosheet | |
| Wei et al. | Integrating Co (OH) 2 nanosheet arrays on graphene for efficient noble-metal-free EY-sensitized photocatalytic H 2 evolution | |
| CN106984337A (en) | CdS‑MoS2Nano particle co-doped black porous titanium dioxide photocatalysis agent | |
| CN106698365A (en) | Preparation method and application of hollow porous transition metal chalcogenide nanosheets | |
| Cheng et al. | Ag 2 S/Bi 2 S 3 co-sensitized TiO 2 nanorod arrays prepared on conductive glass as a photoanode for solar cells | |
| Sun et al. | Plasmonic coupling-boosted photothermal nanoreactor for efficient solar light-driven photocatalytic water splitting | |
| CN105836715A (en) | Self-assembly ternary sulfur molybdenum selenide nanotube with controllable composition and preparation method thereof | |
| Chen et al. | Quaternary two dimensional Zn–Ag–In–S nanosheets for highly efficient photocatalytic hydrogen generation | |
| CN104961159B (en) | A kind of nanometer tungsten oxide and one step vapour phase reduction preparation method and application | |
| CN105016389B (en) | A kind of lead molybdate nanocrystal of carbon shell cladding and preparation method thereof | |
| Chen et al. | Construction of Z-Scheme CdS/WO 3 Heterostructure on photonic crystals with high-efficiency photocatalysis performance | |
| Li et al. | Efficient photocathode performance of lithium ion doped LaFeO 3 nanorod arrays in hydrogen evolution | |
| CN104404565B (en) | Au/TiO2optoelectronic pole of nanotube composite construction and preparation method thereof | |
| CN102718491B (en) | Nanotube / powder blending phase metal oxide | |
| CN109957814A (en) | A kind of Bi-BiOI/TNA composite material and its application | |
| CN109133158B (en) | Locally oxidized SnS2Method for preparing thin slice and its product and use | |
| Shen | Combining microwave and ultrasound irradiation for rapid synthesis of nanowires: a case study on Pb (OH) Br | |
| CN102897722A (en) | Alpha-In2Se3 nano-grade flower-ball solvothermal synthesizing method | |
| Yu et al. | Preparation and characterization of CeO 2 decorated TiO 2 nanotube arrays photoelectrode and its enhanced photoelectrocatalytic efficiency for degradation of methyl orange | |
| CN114210315B (en) | Preparation and application of rare earth erbium modified pollen carbon composite photocatalyst | |
| Wang et al. | Construction of a novel direct Z-scheme heterostructure consisting of ReS2 nanoflowers and In2S3 nanohoneycombs for improving photoelectrochemical performance |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20161019 Termination date: 20200714 |