CN116083084A - Method for inducing zero band gap two-dimensional material fluorescence by fluorination - Google Patents
Method for inducing zero band gap two-dimensional material fluorescence by fluorination Download PDFInfo
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- CN116083084A CN116083084A CN202211477161.0A CN202211477161A CN116083084A CN 116083084 A CN116083084 A CN 116083084A CN 202211477161 A CN202211477161 A CN 202211477161A CN 116083084 A CN116083084 A CN 116083084A
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- 239000000463 material Substances 0.000 title claims abstract description 54
- 238000003682 fluorination reaction Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 32
- 230000001939 inductive effect Effects 0.000 title claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 230000005284 excitation Effects 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 6
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000011737 fluorine Substances 0.000 claims abstract description 3
- 229920000642 polymer Polymers 0.000 claims abstract description 3
- HPQRSQFZILKRDH-UHFFFAOYSA-M chloro(trimethyl)plumbane Chemical compound C[Pb](C)(C)Cl HPQRSQFZILKRDH-UHFFFAOYSA-M 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- 229910021389 graphene Inorganic materials 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000002033 PVDF binder Substances 0.000 claims description 4
- 229920002313 fluoropolymer Polymers 0.000 claims description 4
- 239000004811 fluoropolymer Substances 0.000 claims description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000007791 liquid phase Substances 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 229920002620 polyvinyl fluoride Polymers 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 claims description 2
- 230000005283 ground state Effects 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 9
- 238000002189 fluorescence spectrum Methods 0.000 description 6
- 239000012159 carrier gas Substances 0.000 description 4
- 125000001153 fluoro group Chemical group F* 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 239000002390 adhesive tape Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000005424 photoluminescence Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/26—Materials of the light emitting region
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/26—Materials of the light emitting region
- H01L33/34—Materials of the light emitting region containing only elements of group IV of the periodic system
Abstract
The invention relates to a method for inducing zero band gap two-dimensional material fluorescence by fluorination, belonging to the technical field of two-dimensional materials. The preparation method comprises the following steps of transferring a zero-band gap two-dimensional material to the surface of a substrate to obtain a sample; the sample and the fluorine-containing polymer are added into a heating container, and are fluorinated to obtain the two-dimensional material with fluorescence. The preparation method enables the original non-luminous zero-band-gap two-dimensional material to show good fluorescence characteristics while not changing the conductivity, and the energy band of the material is opened through the fluorination process, so that the lowest point of the conduction band and the highest point of the valence band of the material are far away from the fermi level, electrons are transited from the valence band to the conduction band under the excitation of a certain light source, and the material is transited from the ground state to the excitation state. Then, the electrons in the conduction band recombine with holes in the valence band, thereby releasing the excess energy in the form of light, returning the material to the ground state, and the intensity of the emitted light changes with the wavelength, thereby exhibiting fluorescence characteristics.
Description
Technical Field
The invention belongs to the technical field of two-dimensional materials, and particularly relates to a method for inducing zero-band gap two-dimensional material fluorescence by fluorination.
Background
In recent years, two-dimensional materials have been widely studied for their unique photoelectric properties, and in particular, the fluorescence optical properties of two-dimensional materials. In order to adjust the fluorescence properties of two-dimensional materials and expand their applications, researchers have studied the doping of impurity atoms, such as nitrogen, sulfur, chlorine, etc., and have been shown to be effective in creating new phenomena and some unexpected properties. However, the fluorescence characteristics of the zero-bandgap two-dimensional material have not been studied so far in the prior art. The charge of the zero-band-gap two-dimensional material is free flowing, the property of the zero-band-gap two-dimensional material is not required to be expressed through energy excitation, and the zero-band-gap two-dimensional material cannot be used as a conventional transistor channel material due to the natural zero-band-gap property of the zero-band-gap two-dimensional material, so that the zero-band-gap two-dimensional material cannot be applied to the current electronic industry, and the application of the zero-band-gap two-dimensional material in the field of semiconductors is greatly hindered.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for inducing fluorescence of a zero-band-gap two-dimensional material by fluorination.
It is a first object of the present invention to provide a method for fluorination-induced fluorescence of zero-bandgap two-dimensional materials, comprising the steps of,
(1) Transferring the zero band gap two-dimensional material to the surface of a substrate to obtain a sample;
(2) And (3) adding the sample obtained in the step (1) and the fluorine-containing polymer into a heating container, and carrying out fluorination to obtain the two-dimensional material with fluorescence.
In one embodiment of the present invention, in step (1), the zero-bandgap two-dimensional material is graphene or tungsten telluride.
In one embodiment of the present invention, in step (1), the zero-bandgap two-dimensional material has a thickness of 1-20nm.
In one embodiment of the present invention, in step (1), the material of the substrate is silicon, potassium tantalate, or strontium titanate. The substrate has good material stability, high heat conduction performance and strong antistatic capability, and meets the requirements of the semiconductor industry.
In one embodiment of the present invention, in step (1), the transferring method is a mechanical lift-off method, a liquid phase lift-off method, or a CVD growth method.
In one embodiment of the invention, in step (2), the fluoropolymer is polyvinylidene fluoride and/or polyvinyl fluoride. The fluoropolymer has excellent chemical resistance, excellent high temperature resistance, color change resistance and oxidation resistance.
In one embodiment of the invention, in step (2), the fluorination is carried out by heating to 300-440 ℃ for 30-40min and maintaining the temperature for 30-120min. The fluorine atoms in the fluoropolymer can be burst out at the temperature, and the heat preservation is to dope the fluorine atoms into the two-dimensional material as much as possible.
In one embodiment of the invention, in step (2), the fluorination is performed under a nitrogen atmosphere; the purity of the nitrogen is more than 99.999%.
A second object of the present invention is to provide a two-dimensional material with fluorescence prepared by the method.
In one embodiment of the invention, the excitation wavelength of the two-dimensional material with fluorescence is 550-700nm.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) The preparation method of the invention enables the original non-luminous zero-band-gap two-dimensional material to show good fluorescence characteristics while not changing the conductivity, and the energy band of the zero-band-gap two-dimensional material is opened through the fluorination process, so that the lowest point of the conduction band and the highest point of the valence band of the zero-band-gap two-dimensional material are far away from the fermi level, electrons are transited from the valence band to the conduction band under the excitation of a certain light source, and the zero-band-gap two-dimensional material is transited from the ground state to the excitation state. Then, electrons in the conduction band can be recombined with holes in the valence band, and the redundant energy is released in the form of light, and the two-dimensional material is returned to the ground state, and the intensity of the emitted light changes with the wavelength, so that the fluorescence characteristic of the zero-band gap two-dimensional material is displayed.
(2) The two-dimensional material with fluorescence disclosed by the invention can make up the defects of the traditional fluorescent material to a certain extent, and has great potential and application prospects in the field of photoluminescence or the field of photoelectric devices.
Drawings
In order that the invention may be more readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings, in which:
FIG. 1 is a flow chart of the present invention for preparing a two-dimensional material having fluorescence.
FIG. 2 is a graph showing fluorescence spectra of graphene before and after fluorination in test example 1 of the present invention.
FIG. 3 is a graph showing fluorescence spectra of tungsten telluride fluoride having different thicknesses and different fluorination times in test example 2 of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the invention and practice it.
Example 1
Referring to fig. 1, a method for inducing fluorescence of a zero-bandgap two-dimensional material by fluorination specifically comprises the following steps:
transferring graphene from a graphite crystal block to the surface of monocrystalline silicon by using an adhesive tape through a mechanical stripping method to obtain a sample, wherein the thickness of the graphene on the surface of the sample is 1-10nm; the sample and 0.2g PVDF were placed on the left and right sides of the quartz boat, respectively, and placed in a tube furnace for heating. In the whole heating process, nitrogen with the purity of 99.999% is used as carrier gas, the carrier gas is initially kept at room temperature, gradually rises to 350 ℃ within 30min, and gradually falls to room temperature after being kept constant for 60min, so that the graphene with fluorescence is obtained.
Example 2
Referring to fig. 1, a method for inducing fluorescence of a zero-bandgap two-dimensional material by fluorination specifically comprises the following steps:
transferring tungsten telluride from the tungsten telluride bulk material to the surface of monocrystalline silicon by using an adhesive tape through a mechanical stripping method to obtain a sample, wherein the thickness of the tungsten telluride on the surface of the sample is 1-20nm; the sample and 0.2g PVDF were placed on the left and right sides of the quartz boat, respectively, and placed in a tube furnace for heating. In the whole heating process, nitrogen with the purity of 99.999% is used as carrier gas, the carrier gas is initially kept at room temperature, gradually rises to 350 ℃ within 30min, and gradually falls to room temperature after being kept constant for 60min, so that the tungsten telluride with fluorescence is obtained.
Test example 1
Fluorescence spectrum tests were performed on graphene before and after fluorination based on example 1, and the results are shown in fig. 2. The fluorescence intensity changes with laser of different wavelengths, and the graphene film under the irradiation of fluorine atoms shows good fluorescence characteristics between 550nm and 700nm after doping, obvious photoluminescence characteristic peaks of graphene are shown at 561nm, the fluorescence intensity of the fluorinated graphene film at 582nm is about 5 times greater than that of the graphene film before fluorination, and the conductivity of the graphene before and after fluorination is not changed. Therefore, in practical application, the fluorination process method can meet the requirement of enhancing the fluorescence effect of the graphene film while not changing the conductivity of the graphene, and has application prospects in the fields of optical sensing devices and the like.
Test example 2
The fluorescence spectrum test was performed on tungsten telluride fluoride based on example 2, and the results are shown in fig. 3. FIG. 3a is a graph showing fluorescence spectra of tungsten telluride having different thicknesses after fluorination, wherein the fluorescence intensity varies with laser light having different wavelengths. After fluorine atom doping, the tungsten telluride film under light irradiation also shows good fluorescence characteristics between 550nm and 700nm, particularly the 5nm tungsten telluride film shows the most excellent fluorescence performance after fluorination, and the light-emitting intensity of the tungsten telluride film is about 4 times stronger at 582nm than that of the 30nm tungsten telluride film, which means that the thinner tungsten telluride film has stronger fluorescence performance after fluorination. FIG. 3b is a graph of fluorescence spectra of tungsten telluride thin films measured after different fluorination times, wherein the longer the fluorination time is, the stronger the luminous intensity, and when the fluorination time exceeds 30min, the fluorination reaction is saturated, so that the luminous intensity of the fluorination time of 30min is similar to that of the fluorination time of 40min, and the requirement of the fluorescence effect of the tungsten telluride thin films can be met by selecting the fluorination time of 30 min.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations and modifications of the present invention will be apparent to those of ordinary skill in the art in light of the foregoing description. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (10)
1. A method for inducing fluorescence of zero-band-gap two-dimensional materials by fluorination is characterized by comprising the following steps,
(1) Transferring the zero band gap two-dimensional material to the surface of a substrate to obtain a sample;
(2) And (3) adding the sample obtained in the step (1) and the fluorine-containing polymer into a heating container, and carrying out fluorination to obtain the two-dimensional material with fluorescence.
2. The method of claim 1, wherein in step (1), the zero-bandgap two-dimensional material is graphene or tungsten telluride.
3. The method of claim 1, wherein in step (1), the zero-bandgap two-dimensional material has a thickness of 1-20nm.
4. The method of claim 1, wherein in step (1), the substrate is silicon, potassium tantalate, or strontium titanate.
5. The method of claim 1, wherein in step (1), the transfer method is a mechanical lift-off method, a liquid phase lift-off method, or a CVD growth method.
6. The method of claim 1, wherein in step (2), the fluoropolymer is polyvinylidene fluoride and/or polyvinyl fluoride.
7. The method of claim 1, wherein in step (2), the fluorination is performed by heating to 300-440 ℃ for 30-40min, and maintaining the temperature for 30-120min.
8. The method of claim 1, wherein in step (2), the fluorination is performed under nitrogen atmosphere; the purity of the nitrogen is more than 99.999%.
9. A two-dimensional material with fluorescence produced by the method of any one of claims 1-8.
10. The two-dimensional material with fluorescence according to claim 9, wherein the excitation wavelength of the two-dimensional material with fluorescence is 550-700nm.
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| CN202211477161.0A CN116083084B (en) | 2022-11-23 | 2022-11-23 | Method for inducing zero band gap two-dimensional material fluorescence by fluorination |
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| CN202211477161.0A CN116083084B (en) | 2022-11-23 | 2022-11-23 | Method for inducing zero band gap two-dimensional material fluorescence by fluorination |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110303121A1 (en) * | 2010-06-10 | 2011-12-15 | The University Of Manchester | Functionalized graphene and methods of manufacturing the same |
| CN105565310A (en) * | 2016-03-02 | 2016-05-11 | 桂林理工大学 | Method for preparing fluorine doped graphene quantum dot with excellent optical properties |
| CN105645398A (en) * | 2016-03-10 | 2016-06-08 | 上海大学 | Method for stripping preparation of large-scale fluorinated graphene by supercritical carbon dioxide |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110303121A1 (en) * | 2010-06-10 | 2011-12-15 | The University Of Manchester | Functionalized graphene and methods of manufacturing the same |
| CN105565310A (en) * | 2016-03-02 | 2016-05-11 | 桂林理工大学 | Method for preparing fluorine doped graphene quantum dot with excellent optical properties |
| CN105645398A (en) * | 2016-03-10 | 2016-06-08 | 上海大学 | Method for stripping preparation of large-scale fluorinated graphene by supercritical carbon dioxide |
Non-Patent Citations (2)
| Title |
|---|
| KI-JOON JEON ET AL.: ""Fluorographene: A Wide Bandgap Semiconductor with Ultraviolet Luminescence"", ACS NANO, vol. 5, no. 2, pages 1042 - 1046 * |
| ZHAOFENG WANG ET AL.: ""Cooperatively exfoliated fluorinated graphene with full-color emission"", RSC ADVANCES, vol. 2, pages 11681 - 11686 * |
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