CN109216501A - The preparation method and application of photoelectric response material based on graphene - Google Patents
The preparation method and application of photoelectric response material based on graphene Download PDFInfo
- Publication number
- CN109216501A CN109216501A CN201810838175.8A CN201810838175A CN109216501A CN 109216501 A CN109216501 A CN 109216501A CN 201810838175 A CN201810838175 A CN 201810838175A CN 109216501 A CN109216501 A CN 109216501A
- Authority
- CN
- China
- Prior art keywords
- graphene
- added
- container
- preparation
- graphene oxide
- 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.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 101
- 230000004044 response Effects 0.000 title claims abstract description 61
- 239000000463 material Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 113
- 235000019441 ethanol Nutrition 0.000 claims abstract description 46
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000725 suspension Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000002604 ultrasonography Methods 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000005119 centrifugation Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000000746 purification Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 44
- 229910002804 graphite Inorganic materials 0.000 claims description 26
- 239000010439 graphite Substances 0.000 claims description 26
- 230000003647 oxidation Effects 0.000 claims description 26
- 238000007254 oxidation reaction Methods 0.000 claims description 26
- 239000000047 product Substances 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 239000012153 distilled water Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 13
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- 229910052681 coesite Inorganic materials 0.000 claims description 10
- 229910052906 cristobalite Inorganic materials 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 10
- 238000010907 mechanical stirring Methods 0.000 claims description 10
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- 229910052682 stishovite Inorganic materials 0.000 claims description 10
- 239000000758 substrate Substances 0.000 claims description 10
- 229910052905 tridymite Inorganic materials 0.000 claims description 10
- 239000002131 composite material Substances 0.000 claims description 9
- 229910021382 natural graphite Inorganic materials 0.000 claims description 9
- 239000004570 mortar (masonry) Substances 0.000 claims description 7
- 241000238370 Sepia Species 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 238000001259 photo etching Methods 0.000 claims description 5
- 239000012286 potassium permanganate Substances 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- 235000019394 potassium persulphate Nutrition 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 238000004448 titration Methods 0.000 claims description 5
- 150000001336 alkenes Chemical class 0.000 claims description 4
- 239000004575 stone Substances 0.000 claims description 4
- -1 after mixing evenly Chemical compound 0.000 claims description 3
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims 1
- 229910044991 metal oxide Inorganic materials 0.000 claims 1
- 150000004706 metal oxides Chemical class 0.000 claims 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 30
- 239000011787 zinc oxide Substances 0.000 description 15
- 229960001296 zinc oxide Drugs 0.000 description 15
- 239000011701 zinc Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 9
- 238000001514 detection method Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 230000035945 sensitivity Effects 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000004891 communication Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000013307 optical fiber Substances 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/0328—Inorganic materials including, apart from doping materials or other impurities, semiconductor materials provided for in two or more of groups H01L31/0272 - H01L31/032
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The present invention provides a kind of preparation method and applications of photoelectric response material based on graphene, which comprises ethyl alcohol is added into graphene oxide, obtains graphene oxide suspension；The graphene oxide suspension is placed in the container containing ethyl alcohol and carries out ultrasound；Zn (Ac) is added into container2·2H2The ethanol solution of O is ultrasonic again, wherein the Zn (Ac) of addition2·2H2The mass ratio of O and graphene oxide is 1:1；The ethanol solution of NaOH is added into container, wherein the mass ratio of the NaOH of addition and graphene oxide is 0.12~0.14:1；After stirring the mixture for uniformly, reacted in a water bath；It after cooling, is rinsed respectively through ethyl alcohol, centrifugation purification 2~3 times, finally prepares the photoelectric response material based on graphene.The present invention can reduce cost, shorten the response time.
Description
Technical field
The present invention relates to technical field of optical fiber communication, more particularly to a kind of system of photoelectric response material based on graphene
Preparation Method and application.
Background technique
In recent years, it with the development of science and technology optical fiber communication technology is rapidly developed, is led in the test of optical fiber communication technology
It is often needed in domain using photodetector, photodetector is based on the object for causing illuminated material electrical properties to change by radiation
Phenomenon is managed, optical signal is converted to electric signal, and examine the device of optical signal by detection electric signal.Photodetector is light
One kind of detector has detectivity high, and time response is fast, can measure to the transient change of optical radiation power,
There is apparent optical wavelength selection characteristic simultaneously.
It needs in photodetector using photoelectric response material, it is traditional based on cadmium sulfide, cadmium selenide visible light wave range
Photo resistance and photoelectric response material based on vulcanized lead infrared band are widely used in photodetector, but these tradition
Material have the shortcomings that higher cost, response time are long, the final cost and sensitivity for influencing photodetector.
Summary of the invention
In view of the above situation, an aspect of of the present present invention provides a kind of preparation side of photoelectric response material based on graphene
Method solves the problems, such as that higher cost, response time are slow.
A kind of preparation method of the photoelectric response material based on graphene, comprising:
Ethyl alcohol is added into graphene oxide, obtains graphene oxide suspension；
The graphene oxide suspension is placed in the container containing ethyl alcohol and carries out ultrasound；
Zn (Ac) is added into container2·2H2The ethanol solution of O is ultrasonic again, wherein the Zn (Ac) of addition2·2H2O and
The mass ratio of graphene oxide is 1:1；
The ethanol solution of NaOH is added into container, wherein the mass ratio of the NaOH of addition and graphene oxide is 0.12
~0.14:1；
After stirring the mixture for uniformly, reacted in a water bath；
It after cooling, is rinsed respectively through ethyl alcohol, centrifugation purification 2~3 times, finally prepares the photoelectricity based on graphene and ring
Answer material.
The preparation method of the photoelectric response material based on graphene provided according to the present invention is finally prepared based on graphite
The composite photoelectric responsive materials of alkene and Zinc oxide nanoparticle, cost is relatively low for material requested, what test result showed to prepare
The average diameter of nanometer monocrystalline zinc oxide particle in photoelectric response material is 4.6~5.4nm, these particles are evenly distributed on also
Former graphene surface, wherein due to not having molecule connection, the contact performance at interface between Zinc oxide nanoparticle and graphene
It is greatly improved, this is finally made to have fast and efficiently response special ultraviolet light based on the photoelectric response material of graphene
Point.
In addition, the preparation method of the above-mentioned photoelectric response material based on graphene according to the present invention, can also have as
Under additional technical characteristic:
Further, before described the step of ethyl alcohol is added into graphene oxide powder, the method also includes oxidations
The preparation of graphene, specifically includes:
Step 11, the pre-oxidation of graphite:
Dense H is added into container2SO4, it is then placed in mechanical stirring in oil bath pan, sequentially adds natural graphite, persulfuric acid
Potassium, P2O5, after mixing evenly, distilled water is slowly added in 70~80 DEG C of reaction 3h into container after being cooled to room temperature, control is held
Temperature in device is no more than 80 DEG C；Mixed solution is filtered by vacuum, obtained filter cake is placed in clean beaker, again plus
Enter distilled water dilution, then filters, until filtrate is in neutrality, filter cake is finally put into 80 DEG C of air dry ovens dry 10~
12h obtains pre-oxidation product；
Step 12, the oxidation of graphite:
Step 121, dense H is added into beaker under condition of ice bath2SO4, the pre-oxidation product that upper step is obtained grinds
After be added in beaker, stir evenly, finely ground KMnO be slowly added4Powder, sufficiently reaction 4h；
Step 122, beaker is transferred to and is previously heated in 35 DEG C of oil bath pans, mechanical stirring reacts 2h, and reaction is completed
Afterwards, distilled water is slowly added with titration bottle, the temperature in beaker is kept to be no more than 80 DEG C, solution is in sepia at this time；
Step 123, oil bath temperature is risen to 95 DEG C, mechanic whirl-nett reaction 30min, solution is in faint yellow, into beaker
H is added2O2, solution becomes glassy yellow by faint yellow, and 10% hydrochloric acid solution is then added, removes the complete metal oxygen of unreacted
Compound, then product is washed to solution repeatedly with distilled water and is in neutrality, finally slimy product is freeze-dried；
Step 13, it grinds:
After the product being freeze-dried in previous step is fully ground with agate mortar, the graphite oxide is obtained；
Step 14, disperse:
Tube-type atmosphere furnace is previously heated to 700 DEG C, and is passed through protective gas N2, the graphite oxide is put into nickel crucible
In, it is then placed in the tube-type atmosphere furnace, keeps the temperature 8~10min, the graphene oxide is finally made.
Further, described that the graphene oxide suspension is placed in the container containing ethyl alcohol to the step for carrying out ultrasound
In, ultrasonic time is 8~10min.
Further, described that Zn (Ac) is added into container2·2H2The ethanol solution of O is again in ultrasonic step, ultrasound
Time is 5~6min.
Further, it is described stir the mixture for uniformly after, in the step of being reacted in a water bath, water-bath is adjusted
Are as follows: it is reacted 1~1.5 hour in 70~80 DEG C of water-baths.
Further, in the step 11, the natural graphite, the persulfuric acid of mass ratio 2.5:1.5:1.8 are sequentially added
Potassium, P2O5。
Further, in the step 121, the KMnO4The quality of powder is 4~5 times of the natural graphite quality.
Further, it in the step 13, after agate mortar is fully ground, sieves with 100 mesh sieve, obtains the graphite oxide.
Another aspect of the present invention also provides a kind of answering for the photoelectric response material based on graphene of above method preparation
With the photoelectric response material based on graphene is used to prepare photodetector, comprising the following steps:
Use partial size for 300mm SiO2SiO is obtained by thermal oxide2/ Si substrate；
Using photoetching technique in the SiO2/ Si substrate prepares the interdigital electrode that adjacent spacing is 5 μm；
Ethanol solution containing the photoelectric response material based on graphene is dripped in interdigital electrode, at room temperature certainly
It so dries, to prepare photodetector.
The photodetector finally prepared is to the detection sensitivity of ultraviolet light up to 1.03~1.05*104, to the sound of ultraviolet light
Up to 7.6~9.2s between seasonable, compared with prior art, there is advantage.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Fig. 1 is the flow chart of the preparation method of the photoelectric response material based on graphene of embodiment of the present invention.
Specific embodiment
To facilitate the understanding of the present invention, a more comprehensive description of the invention is given in the following sections with reference to the relevant attached drawings.In attached drawing
Give several embodiments of the invention.But the invention can be realized in many different forms, however it is not limited to this paper institute
The embodiment of description.On the contrary, purpose of providing these embodiments is make it is more thorough and comprehensive to the disclosure.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term " and or " used herein includes one or more phases
Any and all combinations of the listed item of pass.
Referring to Fig. 1, embodiments of the present invention provide a kind of preparation side of photoelectric response material based on graphene
Method, comprising:
Step 1, ethyl alcohol is added into graphene oxide, obtains graphene oxide suspension；
Step 2, the graphene oxide suspension is placed in the container containing ethyl alcohol and carries out ultrasound；
Step 3, Zn (Ac) is added into container2·2H2The ethanol solution of O is ultrasonic again, wherein the Zn (Ac) of addition2·
2H2The mass ratio of O and graphene oxide is 1:1；
Step 4, the ethanol solution of NaOH is added into container, wherein the NaOH of addition and the mass ratio of graphene oxide
For 0.12~0.14:1；
Step 5, it after stirring the mixture for uniformly, is reacted in a water bath；
Step 6, it after cooling, rinses, centrifugation purification 2~3 times, finally prepares described based on graphene through ethyl alcohol respectively
Photoelectric response material.
The preparation method of the photoelectric response material based on graphene provided according to the present invention is finally prepared based on graphite
The composite photoelectric responsive materials of alkene and Zinc oxide nanoparticle, cost is relatively low for material requested, what test result showed to prepare
The average diameter of nanometer monocrystalline zinc oxide particle in photoelectric response material is 5nm, these particles are evenly distributed on reduction graphite
Alkene surface, wherein due to not having molecule connection between Zinc oxide nanoparticle and graphene, the contact performance at interface is obtained very
Big raising finally makes this have fast and efficiently features of response to ultraviolet light based on the photoelectric response material of graphene.
Divide multiple embodiments that the embodiment of the present invention is further detailed below.The embodiment of the present invention be not limited to
Under specific embodiment.Within the scope of the unchanged main rights, implementation can appropriate be changed.
Embodiment one
A kind of preparation method of the photoelectric response material based on graphene, comprising:
Step 11, the pre-oxidation of graphite:
Dense H is added into container2SO4, it is then placed in mechanical stirring in oil bath pan, sequentially adds mass ratio 2.5:1.5:1.8
Natural graphite, potassium peroxydisulfate, P2O5, after mixing evenly, 70 DEG C of reaction 3h are slowly added after being cooled to room temperature into container
Distilled water, the temperature controlled in container are no more than 80 DEG C；Mixed solution is filtered by vacuum, obtained filter cake is placed in clean
In beaker, distilled water dilution is added again, then filter, until filtrate is in neutrality, filter cake is finally put into 80 DEG C of air blast and is done
Dry 10h in dry case, obtains pre-oxidation product；
Step 12, the oxidation of graphite:
Step 121, dense H is added into beaker under condition of ice bath2SO4, the pre-oxidation product that upper step is obtained grinds
After be added in beaker, stir evenly, finely ground KMnO be slowly added4Powder, the KMnO4The quality of powder is the day
4 times of right graphite quality, sufficiently reaction 4h；
Step 122, beaker is transferred to and is previously heated in 35 DEG C of oil bath pans, mechanical stirring reacts 2h, and reaction is completed
Afterwards, distilled water is slowly added with titration bottle, the temperature in beaker is kept to be no more than 80 DEG C, solution is in sepia at this time；
Step 123, oil bath temperature is risen to 95 DEG C, mechanic whirl-nett reaction 30min, solution is in faint yellow, into beaker
H is added2O2, solution becomes glassy yellow by faint yellow, and 10% hydrochloric acid solution is then added, removes the complete metal oxygen of unreacted
Compound, then product is washed to solution repeatedly with distilled water and is in neutrality, finally slimy product is freeze-dried；
Step 13, it grinds:
It after the product being freeze-dried in previous step is fully ground with agate mortar, sieves with 100 mesh sieve, obtains the oxidation stone
Ink；
Step 14, disperse:
Tube-type atmosphere furnace is previously heated to 700 DEG C, and is passed through protective gas N2, the graphite oxide is put into nickel crucible
In, it is then placed in the tube-type atmosphere furnace, keeps the temperature 8min, the graphene oxide is finally made；
Step 15, ethyl alcohol is added into graphene oxide, obtains graphene oxide suspension；
Step 16, the graphene oxide suspension is placed in the container containing ethyl alcohol and carries out ultrasound, ultrasonic time is
8min；
Step 17, Zn (Ac) is added into container2·2H2The ethanol solution of O ultrasound 5min again, wherein the Zn of addition
(Ac)2·2H2The mass ratio of O and graphene oxide is 1:1；
Step 18, the ethanol solution of NaOH is added into container, wherein the NaOH of addition and the mass ratio of graphene oxide
For 0.12:1；
Step 19, it after stirring the mixture for uniformly, is reacted in a water bath, water-bath is adjusted are as follows: in 70 DEG C of water-baths
Reaction 1 hour；
Step 20, it after cooling, rinses, centrifugation purification 2~3 times, finally prepares described based on graphene through ethyl alcohol respectively
Photoelectric response material.
Show the nanometer monocrystalline zinc oxide in photoelectric response material that the present embodiment is prepared by Electronic Speculum test result
The average diameter of grain is 4.6nm, and nanometer monocrystalline zinc oxide particle is evenly distributed on reduced graphene surface, zinc-oxide nano
There is no molecule connection between grain and graphene, the contact performance at interface is greatly improved, this is finally made to be based on graphene
Photoelectric response material there is fast and efficiently features of response to ultraviolet light.
The present embodiment also proposes the application of the above-mentioned photoelectric response material based on graphene prepared, will be obtained described
Photoelectric response material based on graphene is used to prepare photodetector, comprising the following steps:
Step 201, use partial size for 300mm SiO2SiO is obtained by thermal oxide2/ Si substrate；
Step 202, using photoetching technique in the SiO2/ Si substrate prepares the interdigital electrode that adjacent spacing is 5 μm；
Step 203, the ethanol solution containing the photoelectric response material based on graphene is dripped in interdigital electrode,
Naturally dry at room temperature, to prepare photodetector.
By electrical testing, the photodetector finally prepared reaches 1.03*10 to the detection sensitivity of ultraviolet light4, right
The response time of ultraviolet light reaches 7.6s.
Embodiment two
A kind of preparation method of the photoelectric response material based on graphene, comprising:
Step 11, the pre-oxidation of graphite:
Dense H is added into container2SO4, it is then placed in mechanical stirring in oil bath pan, sequentially adds mass ratio 2.5:1.5:1.8
Natural graphite, potassium peroxydisulfate, P2O5, after mixing evenly, 75 DEG C of reaction 3h are slowly added after being cooled to room temperature into container
Distilled water, the temperature controlled in container are no more than 80 DEG C；Mixed solution is filtered by vacuum, obtained filter cake is placed in clean
In beaker, distilled water dilution is added again, then filter, until filtrate is in neutrality, filter cake is finally put into 80 DEG C of air blast and is done
Dry 11h in dry case, obtains pre-oxidation product；
Step 12, the oxidation of graphite:
Step 121, dense H is added into beaker under condition of ice bath2SO4, the pre-oxidation product that upper step is obtained grinds
After be added in beaker, stir evenly, finely ground KMnO be slowly added4Powder, the KMnO4The quality of powder is the day
4.5 times of right graphite quality, sufficiently reaction 4h；
Step 122, beaker is transferred to and is previously heated in 35 DEG C of oil bath pans, mechanical stirring reacts 2h, and reaction is completed
Afterwards, distilled water is slowly added with titration bottle, the temperature in beaker is kept to be no more than 80 DEG C, solution is in sepia at this time；
Step 123, oil bath temperature is risen to 95 DEG C, mechanic whirl-nett reaction 30min, solution is in faint yellow, into beaker
H is added2O2, solution becomes glassy yellow by faint yellow, and 10% hydrochloric acid solution is then added, removes the complete metal oxygen of unreacted
Compound, then product is washed to solution repeatedly with distilled water and is in neutrality, finally slimy product is freeze-dried；
Step 13, it grinds:
It after the product being freeze-dried in previous step is fully ground with agate mortar, sieves with 100 mesh sieve, obtains the oxidation stone
Ink；
Step 14, disperse:
Tube-type atmosphere furnace is previously heated to 700 DEG C, and is passed through protective gas N2, the graphite oxide is put into nickel crucible
In, it is then placed in the tube-type atmosphere furnace, keeps the temperature 9min, the graphene oxide is finally made；
Step 15, ethyl alcohol is added into graphene oxide, obtains graphene oxide suspension；
Step 16, the graphene oxide suspension is placed in the container containing ethyl alcohol and carries out ultrasound, ultrasonic time is
9min；
Step 17, Zn (Ac) is added into container2·2H2The ethanol solution of O ultrasound 5min again, wherein the Zn of addition
(Ac)2·2H2The mass ratio of O and graphene oxide is 1:1；
Step 18, the ethanol solution of NaOH is added into container, wherein the NaOH of addition and the mass ratio of graphene oxide
For 0.13:1；
Step 19, it after stirring the mixture for uniformly, is reacted in a water bath, water-bath is adjusted are as follows: in 75 DEG C of water-baths
Reaction 1.3 hours；
Step 20, it after cooling, rinses, centrifugation purification 2~3 times, finally prepares described based on graphene through ethyl alcohol respectively
Photoelectric response material.
Show the nanometer monocrystalline zinc oxide in photoelectric response material that the present embodiment is prepared by Electronic Speculum test result
The average diameter of grain is 4.9nm, and nanometer monocrystalline zinc oxide particle is evenly distributed on reduced graphene surface, zinc-oxide nano
There is no molecule connection between grain and graphene, the contact performance at interface is greatly improved, this is finally made to be based on graphene
Photoelectric response material there is fast and efficiently features of response to ultraviolet light.
The present embodiment also proposes the application of the above-mentioned photoelectric response material based on graphene prepared, will be obtained described
Photoelectric response material based on graphene is used to prepare photodetector, comprising the following steps:
Step 201, use partial size for 300mm SiO2SiO is obtained by thermal oxide2/ Si substrate；
Step 202, using photoetching technique in the SiO2/ Si substrate prepares the interdigital electrode that adjacent spacing is 5 μm；
Step 203, the ethanol solution containing the photoelectric response material based on graphene is dripped in interdigital electrode,
Naturally dry at room temperature, to prepare photodetector.
By electrical testing, the photodetector finally prepared reaches 1.05*10 to the detection sensitivity of ultraviolet light4, right
The response time of ultraviolet light reaches 8.4s.
Embodiment three
A kind of preparation method of the photoelectric response material based on graphene, comprising:
Step 11, the pre-oxidation of graphite:
Dense H is added into container2SO4, it is then placed in mechanical stirring in oil bath pan, sequentially adds mass ratio 2.5:1.5:1.8
Natural graphite, potassium peroxydisulfate, P2O5, after mixing evenly, 80 DEG C of reaction 3h are slowly added after being cooled to room temperature into container
Distilled water, the temperature controlled in container are no more than 80 DEG C；Mixed solution is filtered by vacuum, obtained filter cake is placed in clean
In beaker, distilled water dilution is added again, then filter, until filtrate is in neutrality, filter cake is finally put into 80 DEG C of air blast and is done
Dry 12h in dry case, obtains pre-oxidation product；
Step 12, the oxidation of graphite:
Step 121, dense H is added into beaker under condition of ice bath2SO4, the pre-oxidation product that upper step is obtained grinds
After be added in beaker, stir evenly, finely ground KMnO be slowly added4Powder, the KMnO4The quality of powder is the day
5 times of right graphite quality, sufficiently reaction 4h；
Step 122, beaker is transferred to and is previously heated in 35 DEG C of oil bath pans, mechanical stirring reacts 2h, and reaction is completed
Afterwards, distilled water is slowly added with titration bottle, the temperature in beaker is kept to be no more than 80 DEG C, solution is in sepia at this time；
Step 123, oil bath temperature is risen to 95 DEG C, mechanic whirl-nett reaction 30min, solution is in faint yellow, into beaker
H is added2O2, solution becomes glassy yellow by faint yellow, and 10% hydrochloric acid solution is then added, removes the complete metal oxygen of unreacted
Compound, then product is washed to solution repeatedly with distilled water and is in neutrality, finally slimy product is freeze-dried；
Step 13, it grinds:
It after the product being freeze-dried in previous step is fully ground with agate mortar, sieves with 100 mesh sieve, obtains the oxidation stone
Ink；
Step 14, disperse:
Tube-type atmosphere furnace is previously heated to 700 DEG C, and is passed through protective gas N2, the graphite oxide is put into nickel crucible
In, it is then placed in the tube-type atmosphere furnace, keeps the temperature 10min, the graphene oxide is finally made；
Step 15, ethyl alcohol is added into graphene oxide, obtains graphene oxide suspension；
Step 16, the graphene oxide suspension is placed in the container containing ethyl alcohol and carries out ultrasound, ultrasonic time is
10min；
Step 17, Zn (Ac) is added into container2·2H2The ethanol solution of O ultrasound 6min again, wherein the Zn of addition
(Ac)2·2H2The mass ratio of O and graphene oxide is 1:1；
Step 18, the ethanol solution of NaOH is added into container, wherein the NaOH of addition and the mass ratio of graphene oxide
For 0.14:1；
Step 19, it after stirring the mixture for uniformly, is reacted in a water bath, water-bath is adjusted are as follows: in 80 DEG C of water-baths
Reaction 1.5 hours；
Step 20, it after cooling, rinses, centrifugation purification 2~3 times, finally prepares described based on graphene through ethyl alcohol respectively
Photoelectric response material.
Show the nanometer monocrystalline zinc oxide in photoelectric response material that the present embodiment is prepared by Electronic Speculum test result
The average diameter of grain is 5.4nm, and nanometer monocrystalline zinc oxide particle is evenly distributed on reduced graphene surface, zinc-oxide nano
There is no molecule connection between grain and graphene, the contact performance at interface is greatly improved, this is finally made to be based on graphene
Photoelectric response material there is fast and efficiently features of response to ultraviolet light.
The present embodiment also proposes the application of the above-mentioned photoelectric response material based on graphene prepared, will be obtained described
Photoelectric response material based on graphene is used to prepare photodetector, comprising the following steps:
Step 201, use partial size for 300mm SiO2SiO is obtained by thermal oxide2/ Si substrate；
Step 202, using photoetching technique in the SiO2/ Si substrate prepares the interdigital electrode that adjacent spacing is 5 μm；
Step 203, the ethanol solution containing the photoelectric response material based on graphene is dripped in interdigital electrode,
Naturally dry at room temperature, to prepare photodetector.
By electrical testing, the photodetector finally prepared reaches 1.05*10 to the detection sensitivity of ultraviolet light4, right
The response time of ultraviolet light reaches 9.2s.
The photodetector that upper table compared preparing using the method for above three embodiments and the prior art is to ultraviolet
The detection sensitivity of light and the response time of ultraviolet light, from table, it is apparent that using three embodiments of the present invention
The photodetector that method is finally prepared is superior to existing skill to the detection sensitivity of ultraviolet light and the response time of ultraviolet light
Art has a clear superiority.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (9)
1. a kind of preparation method of the photoelectric response material based on graphene characterized by comprising
Ethyl alcohol is added into graphene oxide, obtains graphene oxide suspension；
The graphene oxide suspension is placed in the container containing ethyl alcohol and carries out ultrasound；
Zn (Ac) is added into container2·2H2The ethanol solution of O is ultrasonic again, wherein the Zn (Ac) of addition2·2H2O and oxidation
The mass ratio of graphene is 1:1；
The ethanol solution of NaOH is added into container, wherein the mass ratio of the NaOH of addition and graphene oxide is 0.12~
0.14:1；
After stirring the mixture for uniformly, reacted in a water bath；
It after cooling, is rinsed respectively through ethyl alcohol, centrifugation purification 2~3 times, finally prepares the photoelectric respone material based on graphene
Material.
2. the preparation method of graphene composite material according to claim 1, which is characterized in that described to graphene oxide
Before the step of ethyl alcohol is added in powder, the method also includes the preparations of graphene oxide, specifically include:
Step 11, the pre-oxidation of graphite:
Dense H is added into container2SO4, be then placed in mechanical stirring in oil bath pan, sequentially add natural graphite, potassium peroxydisulfate,
P2O5, after mixing evenly, distilled water is slowly added in 70~80 DEG C of reaction 3h into container after being cooled to room temperature, and controls in container
Temperature be no more than 80 DEG C；Mixed solution is filtered by vacuum, obtained filter cake is placed in clean beaker, is added steams again
Distilled water dilution, then filter, until filtrate is in neutrality, filter cake is finally put into 80 DEG C of air dry ovens dry 10~12h,
Obtain pre-oxidation product；
Step 12, the oxidation of graphite:
Step 121, dense H is added into beaker under condition of ice bath2SO4, add after the pre-oxidation product grinding that upper step is obtained
Enter into beaker, stir evenly, finely ground KMnO is slowly added4Powder, sufficiently reaction 4h；
Step 122, beaker is transferred to and is previously heated in 35 DEG C of oil bath pans, mechanical stirring reacts 2h, after the reaction was completed, uses
Distilled water is slowly added in titration bottle, and the temperature in beaker is kept to be no more than 80 DEG C, and solution is in sepia at this time；
Step 123, oil bath temperature is risen to 95 DEG C, mechanic whirl-nett reaction 30min, solution is added in faint yellow into beaker
H2O2, solution becomes glassy yellow by faint yellow, and 10% hydrochloric acid solution is then added, removes the complete metal oxide of unreacted,
Product is washed to solution with distilled water repeatedly again and is in neutrality, is finally freeze-dried slimy product；
Step 13, it grinds:
After the product being freeze-dried in previous step is fully ground with agate mortar, the graphite oxide is obtained；
Step 14, disperse:
Tube-type atmosphere furnace is previously heated to 700 DEG C, and is passed through protective gas N2, the graphite oxide is put into nickel crucible, so
After be put into the tube-type atmosphere furnace, keep the temperature 8~10min, the graphene oxide is finally made.
3. the preparation method of graphene composite material according to claim 1, which is characterized in that described by the oxidation stone
Black alkene suspension is placed in the container containing ethyl alcohol in the step for carrying out ultrasound, and ultrasonic time is 8~10min.
4. the preparation method of graphene composite material according to claim 1, which is characterized in that described to be added into container
Zn(Ac)2·2H2For the ethanol solution of O again in the step of ultrasound, ultrasonic time is 5~6min.
5. the preparation method of graphene composite material according to claim 1, which is characterized in that described to stir the mixture for
After uniformly, in the step of being reacted in a water bath, water-bath is adjusted are as follows: is reacted 1~1.5 hour in 70~80 DEG C of water-baths.
6. the preparation method of graphene composite material according to claim 2, which is characterized in that in the step 11, according to
The secondary natural graphite, potassium peroxydisulfate, the P that mass ratio 2.5:1.5:1.8 is added2O5。
7. the preparation method of graphene composite material according to claim 2, which is characterized in that in the step 121, institute
State KMnO4The quality of powder is 4~5 times of the natural graphite quality.
8. the preparation method of graphene composite material according to claim 2, which is characterized in that in the step 13, Ma
It after Nao mortar is fully ground, sieves with 100 mesh sieve, obtains the graphite oxide.
9. the application of the photoelectric response material based on graphene prepared by claim 1, which is characterized in that described will be based on graphite
The photoelectric response material of alkene is used to prepare photodetector, comprising the following steps:
Use partial size for 300mm SiO2SiO is obtained by thermal oxide2/ Si substrate；
Using photoetching technique in the SiO2/ Si substrate prepares the interdigital electrode that adjacent spacing is 5 μm；
Ethanol solution containing the photoelectric response material based on graphene is dripped in interdigital electrode, is dried in the air naturally at room temperature
It is dry, to prepare photodetector.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810838175.8A CN109216501A (en) | 2018-07-26 | 2018-07-26 | The preparation method and application of photoelectric response material based on graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810838175.8A CN109216501A (en) | 2018-07-26 | 2018-07-26 | The preparation method and application of photoelectric response material based on graphene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109216501A true CN109216501A (en) | 2019-01-15 |
Family
ID=64990738
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810838175.8A Pending CN109216501A (en) | 2018-07-26 | 2018-07-26 | The preparation method and application of photoelectric response material based on graphene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109216501A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111653647A (en) * | 2020-04-22 | 2020-09-11 | 中山大学 | Preparation method of interdigital electrode and application of interdigital electrode in photoelectric detection field |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110268647A1 (en) * | 2010-04-22 | 2011-11-03 | Max-Planck-Gesellschaft zur Foerd. der Wisse. e.V. | Producing two-dimensional sandwich nanomaterials based on graphene |
| CN102543464A (en) * | 2011-12-13 | 2012-07-04 | 西北师范大学 | ZnO/reduced graphene oxide/polypyrrole ternary composite material preparation method, and application of the ternary composite material |
| CN102921416A (en) * | 2012-11-05 | 2013-02-13 | 江苏大学 | Nano composite photocatalytic material and method for preparing same |
| CN105839084A (en) * | 2015-07-08 | 2016-08-10 | 北京工业大学 | Method for preparation of porous WO3/rGO composite film by Sol-Gel |
| CN106374118A (en) * | 2016-10-14 | 2017-02-01 | 济南大学 | ZnO/rGO composite material with efficient electro-catalysis oxygen reduction performance |
| CN107902641A (en) * | 2017-09-19 | 2018-04-13 | 太原理工大学 | A kind of preparation method of functionalization reduced graphene |
-
2018
- 2018-07-26 CN CN201810838175.8A patent/CN109216501A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110268647A1 (en) * | 2010-04-22 | 2011-11-03 | Max-Planck-Gesellschaft zur Foerd. der Wisse. e.V. | Producing two-dimensional sandwich nanomaterials based on graphene |
| CN102543464A (en) * | 2011-12-13 | 2012-07-04 | 西北师范大学 | ZnO/reduced graphene oxide/polypyrrole ternary composite material preparation method, and application of the ternary composite material |
| CN102921416A (en) * | 2012-11-05 | 2013-02-13 | 江苏大学 | Nano composite photocatalytic material and method for preparing same |
| CN105839084A (en) * | 2015-07-08 | 2016-08-10 | 北京工业大学 | Method for preparation of porous WO3/rGO composite film by Sol-Gel |
| CN106374118A (en) * | 2016-10-14 | 2017-02-01 | 济南大学 | ZnO/rGO composite material with efficient electro-catalysis oxygen reduction performance |
| CN107902641A (en) * | 2017-09-19 | 2018-04-13 | 太原理工大学 | A kind of preparation method of functionalization reduced graphene |
Non-Patent Citations (3)
| Title |
|---|
| ZHAOYAO ZHAN等: "Self-powered, visible-light photodetector based on thermally reduced grapheneoxide–ZnO (rGO–ZnO) hybrid nanostructure", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
| 张丹慧等: "《贵金属-石墨烯纳米复合材料的合成及性能》", 31 December 2015, 国防工业出版社 * |
| 杨杰: "石墨烯复合材料的制备与结构性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111653647A (en) * | 2020-04-22 | 2020-09-11 | 中山大学 | Preparation method of interdigital electrode and application of interdigital electrode in photoelectric detection field |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Ji et al. | VO2/ZnS core-shell nanoparticle for the adaptive infrared camouflage application with modified color and enhanced oxidation resistance | |
| Xu et al. | Controllable reduced black titania with enhanced photoelectrochemical water splitting performance | |
| CN110669515B (en) | Two-photon near-infrared carbon dot with high brightness and ultra-narrow half-peak width and preparation method thereof | |
| Zhang et al. | ZnO-carbon nanofibers for stable, high response, and selective H2S sensors | |
| CN110291042B (en) | Mixed powder for forming black film and method for producing same | |
| CN105000806B (en) | A kind of silica-based solar cell back side silver paste lead-free glass powder and preparation method thereof | |
| JP2023067932A (en) | infrared photovoltaic device | |
| WO2021164124A1 (en) | Preparation method for spherical silica powder filler, powder filler obtained thereby and use thereof | |
| CN102659410A (en) | High near-infrared reflectivity nano-ceramic pigment and preparation method thereof | |
| CN105957966A (en) | REO (rare earth oxide) down-conversion material perovskite solar cell and preparation method | |
| CN108893114B (en) | Lead-free halide perovskite quantum dot and preparation method thereof | |
| CN109216501A (en) | The preparation method and application of photoelectric response material based on graphene | |
| CN111678881A (en) | Air pollutant detector based on graphene infrared emission unit | |
| Yang et al. | A self-powered high performance UV-Vis-NIR broadband photodetector based on β-Bi 2 O 3 nanoparticles through defect engineering | |
| Long et al. | Novel organic–inorganic hybrid powder SrGa 12 O 19: Mn 2+–ethyl cellulose for efficient latent fingerprint recognition via time-gated fluorescence | |
| George et al. | Synthesis and characterization of environmentally benign calcium-doped Pr2Mo2O9 pigments: applications in coloring of plastics | |
| JP2008166178A (en) | Conductive tin oxide powder, and its manufacturing method | |
| Ganesh et al. | Photo sensing properties of yttrium doped In2S3 thin film fabricated by low prize nebulizer spray pyrolysis technique | |
| CN109292820A (en) | VO2/ ZnO bilayer film and preparation method thereof | |
| CN103922421B (en) | Method for preparing alpha-Fe2O3 | |
| WO2012070760A1 (en) | Titanium dioxide nanoparticles for fabricating photo-electrode for efficient, longlasting dye-sensitized solar cell and fabrication method thereof | |
| Ratep | Preparation and characterization of silicate glasses from waste agriculture materials (rice husk and peanut peel) | |
| CN109682867B (en) | Micron-sized tin dioxide gas-sensitive material and preparation method and application thereof | |
| CN102765744B (en) | One-step preparation method of zinc oxide quantum dots | |
| Wang et al. | Graphene quantum dot-sensitized GaP@ ZnO nanocomposite for high-performance UV photodetectors |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190115 |
|
| RJ01 | Rejection of invention patent application after publication |