CN111039279A - Graphene-like material and preparation method and application thereof - Google Patents

Graphene-like material and preparation method and application thereof Download PDF

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CN111039279A
CN111039279A CN201811187544.8A CN201811187544A CN111039279A CN 111039279 A CN111039279 A CN 111039279A CN 201811187544 A CN201811187544 A CN 201811187544A CN 111039279 A CN111039279 A CN 111039279A
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graphene
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江浪
张静
段惠
郭玉国
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Institute of Chemistry CAS
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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    • H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having a potential-jump barrier or a surface barrier
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Abstract

The invention discloses a graphene-like thin film material and a preparation method and application thereof. The method comprises the following steps: and preparing the graphene-like on a substrate by using organic micromolecules as a carbon source and utilizing a normal-pressure physical meteorological transmission method. The material prepared by the invention can also be used for preparing organic functional devices such as organic field effect transistors and organic logic circuits such as inverters and oscillators, and further applied to large-scale integrated circuits. The material can also be applied to lithium batteries.

Description

Graphene-like material and preparation method and application thereof
Technical Field
The invention belongs to the field of materials, and relates to a graphene-like material, and a preparation method and application thereof.
Background
Due to its unique properties, graphene has attracted a great deal of attention in both theoretical research and applications. The development and utilization of graphene-like materials have been an important research direction for researchers. However, for graphene preparation, complicated processes such as high temperature, metal catalyst, transfer and the like always restrict the wide application of the graphene.
Disclosure of Invention
The invention aims to provide a graphene-like material, and a preparation method and application thereof.
The method for preparing the graphene-like material comprises the following steps:
and preparing the graphene-like material on a substrate by using organic micromolecules as a carbon source and utilizing an atmospheric pressure physical vapor transport process (APPVT).
In the above method, the organic small molecule is any one of the following compounds (also shown in fig. 1):
Figure BDA0001826639250000011
x ═ Br, F, I, Cl, or H; r1To R11Are both selected from any one of X and H.
The method further comprises the following steps: prior to said preparing, said carbon source is compressed.
The purpose of pressing is to effectively control the sublimation rate of the feedstock and to precisely control the growth rate of the sample.
The pressing method is a physical pressing method;
specifically, the pressing conditions are as follows: pressing for 1-3 minutes under the condition of 10-20 MPa; specifically, the pressing was carried out at 15MPa for 2 minutes.
The substrate is selected from at least one of a conductive substrate, a non-conductive substrate and a flexible substrate; specifically, the metal material is selected from any one of glass, ceramic, silicon chip, copper sheet, nickel sheet, foam copper, foam nickel, gold and silver.
In the normal-pressure physical meteorological transmission method, the temperature is more than 500 ℃; specifically 500 ℃ and 650 ℃; specifically 550 ℃, 600 ℃ or 650 ℃; the time is 1h-10 h; in particular 5 h; the carrier gas is inert gas; specifically argon; the flow rate of the carrier gas is 0.05-0.50 sccm; specifically 0.5 sccm.
In addition, the graphene-like material prepared by the method and the application of the graphene-like material as an organic semiconductor layer in the preparation of organic functional devices and as an electrode in the preparation of any one of organic logic circuits, integrated circuits and lithium batteries also belong to the protection scope of the invention.
Wherein, the organic functional device can be an organic field effect transistor;
the organic logic circuit may be specifically any one of an inverter and an oscillator.
More specifically, the organic field effect transistor comprises a substrate, a gate electrode, an insulating layer, a source electrode, a drain electrode and an organic semiconductor layer, and the preparation method comprises the following steps:
1) with cleaning of the gate electrode substrate.
Mixing 1X 1cm2The silicon wafer with the insulating layer was first ultrasonically cleaned with deionized water and then treated with Piranha (H)2O2:H2SO43:7), boiling, finally ultrasonic cleaning with deionized water and isopropanol in sequence, and drying with nitrogen.
2) And (4) preparing the organic field effect transistor.
Preparing the graphene film on the substrate cleaned in the step 1), and preparing a source electrode and a drain electrode by a thermal evaporation method.
The preparation method of the electrode in the integrated circuit comprises the following steps:
1) spin-coating photoresist on the graphene-like thin film, and then placing the graphene-like thin film under a photoetching mask plate for exposure and development to obtain a patterned source drain electrode;
2) making O to the patterned electrode2Plasma treatment (power 100W, time 10 min);
3) and soaking the electrode in an acetone solution to remove the photoresist. The channel ratio of the graphene film electrode is 20/1.
The organic logic circuit inverter comprises a substrate, a gate electrode, an insulating layer, a source electrode, a drain electrode and an organic semiconductor layer, and the preparation method comprises the following steps:
1) preparing a source electrode and a drain electrode by adopting the electrode preparation method;
2) the preparation of the semiconductor layer comprises the following steps:
1) preparing CMUT solutions with different concentrations respectively;
2) preparing a CMUT organic field effect transistor device by using the prepared graphene-like thin film electrode and adopting a direct drip method;
3) preparing a standing DPA crystal by adopting a PVT method;
4) transferring a DPA crystal to the electrode by using the prepared graphene-like thin film electrode to prepare a DPA organic field effect transistor device;
3) the source electrode of the CMUT organic field effect transistor is connected with the drain electrode of the DPA organic field effect transistor;
4) and testing the performance of the device. Using a keithley model 4200 semiconductor tester at room temperature (298K) and under air conditions (10)5Pa) were tested for field effect transistors, inverters.
The lithium battery may specifically include: the lithium ion battery comprises a negative electrode substrate, metal lithium, an electrolyte, a diaphragm and a positive electrode.
The negative electrode substrate can be a copper sheet, a foam copper and other conductive substrates.
The electrolyte is a commercial electrolyte, and can be an ether electrolyte or an ester electrolyte.
The positive electrode may be LiFePO4、LiMn2O4、LiNi0.5Mn1.5O4、LiNi0.5Mn0.5O2And the like.
The preparation method comprises the following steps:
1) preparing the negative electrode base material modified by the graphene-like film. The graphene-like thin film is prepared on a conductive substrate (such as a copper sheet, a copper foam and the like) in the same way as the method.
2) A negative electrode containing metal lithium was prepared. And rapidly transferring the modified substrate into a glove box with water and oxygen value contents lower than 0.1ppm, matching with the metal lithium, and assembling the battery by using commercial electrolyte to deposit the metal lithium. Preferred commercial electrolytes are ether and ester electrolytes. The current density of the lithium metal deposition is 0.01-20mA cm-2Preferably 0.5 to 10mA cm-2. The capacity of the deposition surface is 0.01-20mAh cm-2Preferably 0.5-8mAh cm-2。
3) And preparing the positive electrode. Mixing the positive electrode, conductive carbon black and polyvinylidene chloride according to the mass ratio of 8:1:1, adding N-methyl pyrrolidone to prepare uniform slurry, uniformly coating the uniform slurry on an aluminum foil current collector, drying in vacuum, and slicing to obtain the working positive electrode.
4) And assembling the full cell. The metallic lithium negative electrode obtained in the second step was matched with the positive electrode in the third step, and a full cell was assembled using a commercial electrolyte.
The invention uses organic micromolecular material as carbon source, adopts normal pressure physical meteorology transmission method (APPVT), successfully prepares a graphene-like material on any substrate without metal catalyst, transfer and low temperature, shows excellent electrical performance, and has good application prospect in organic field effect transistor, organic logic circuit and lithium battery.
The method of the invention has the following characteristics and advantages:
1. the raw material cost is low and rich (namely, hexabromobenzene is a commercial material and is cheap to purchase);
2. the preparation process is simple and quick (namely, no metal catalyst, no transfer, direct preparation on any substrate and low preparation temperature);
3. the thickness of the film can be regulated and controlled by controlling the growth temperature of the graphene-like film, so that the conductivity of the film can be further regulated and controlled;
4. can realize large-area preparation of various substrates, such as glass, ceramics, silicon wafers and the like;
5. the material prepared by the invention can also be used for preparing organic functional devices such as organic field effect transistors, sensors and solar cells and organic logic circuits such as inverters and oscillators, and is applied to large-scale integrated circuits.
Drawings
Fig. 1 shows the raw materials for preparing the graphene-like thin film according to the present invention.
FIG. 2 is a) optical microscope image of a graphene-like thin film prepared from hexabromobenzene; b) an AFM image; c) XPS high resolution of C1 s; d) raman plots at different preparation temperatures.
FIG. 3 is a schematic structural diagram of a) an organic field effect transistor of a graphene-like thin film prepared from hexabromobenzene; b) IV curve; c) transfer curve and d) output curve.
FIG. 4 is a schematic view of a) electrodes of graphene-like thin films prepared from hexabromobenzene; b) transition profile of field effect transistor based on CMUT and c) DPA as organic semiconductor; d) inverter electrical characteristics based on the above P-and n-type organic semiconductors.
FIG. 5 is a) optical microscope image of a graphene-like thin film prepared from hexachlorobenzene; b) AFM drawing.
FIG. 6 is a) Raman spectrum of a graphene-like thin film prepared from hexachlorobenzene; b) IV curve; c) transfer curve and d) output curve.
FIG. 7 is a) optical microscope image of a graphene-like thin film prepared from anthracene; b) AFM drawing.
Fig. 8 is a) raman spectrum of a graphene-like thin film prepared from anthracene; b) IV curve; c) transfer curve and d) output curve.
FIG. 9 is a) optical microscope image of a graphene-like thin film prepared from 2, 6-dibromoanthracene; b) AFM drawing.
FIG. 10 is a) Raman spectrum of graphene-like thin film prepared from 2, 6-dibromoanthracene; b) IV curve; c) transfer curve and d) output curve.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
Example 1
Preparation of C-Br graphene film
(1) Pressing a raw material hexabromobenzene by a physical tabletting method at 15MPa for 2 minutes to prepare 150mg of flaky solid;
(2) preparing a C-Br type graphene film;
placing the flaky solid obtained in the step 1) in a quartz boat, placing a cleaned silicon wafer in a deposition area, and preparing by using a normal-pressure physical meteorological transmission method, wherein high-purity argon is used as carrier gas, the gas flow rate is 0.5sccm, the temperature is 550 ℃, and the time is 5 hours, so that the C-Br type graphene film is obtained.
Optical microscopic picture, AFM picture, XPS high resolution picture of C1s and Raman picture under different preparation temperatures of the graphene filmAs shown in fig. 2. As can be seen from fig. 2, a is a sample prepared by the film on a silicon wafer, and the sample can form a large-area uniform film on a substrate, wherein an inset is an electrode prepared by the C-Br type graphene film. The thickness was 2.6nm as seen in AFM panel b. In the graph C, the XPS analysis of the sample can detect three elements of C, Br and O, wherein O may be adsorbed in the air. Further, high-resolution XPS analysis of C1s shows that C-Br bonds exist in the sample, and further shows that the C-Br bonds in hexabromobenzene are incompletely broken to form a C-Br type graphene film. In the graph d, at 1350cm-1,1580cm-1And 2735cm-1The D, G, and 2D peaks, respectively.
Preparation of two, C-Br type graphene thin film organic field effect transistor
(1) With cleaning of the gate electrode substrate.
Mixing 1X 1cm2The silicon wafer with the insulating layer was first ultrasonically cleaned with deionized water and then treated with Piranha (H)2O2:H2SO43:7), boiling, finally ultrasonic cleaning with deionized water and isopropanol in sequence, and drying with nitrogen.
(2) Preparation of organic field effect transistor
Preparing the C-Br type graphene film on the substrate cleaned in the step 1), and preparing a source electrode and a drain electrode by adopting a thermal evaporation method.
The structure, the IV curve, the transfer curve and the output curve of the organic field effect transistor are shown in fig. 3, and as can be seen from the graph, a in fig. 3 is a schematic structural diagram of the organic field effect transistor, bottom gate top contact is adopted, a C-Br type graphene film is an organic semiconductor layer, and 40nm gold is a source electrode and a drain electrode. In the b in the graph in FIG. 3, when the voltage is-1 to 1V, the current is very high, and the conductance is 188.74S/cm. In fig. 3, C is a transfer curve of the C — Br graphene-based thin film as an organic semiconductor layer, and when VDS is-1V, the mobility of the thin film is 0.39cm2V-1s-1. In fig. 3 d is the output curve.
Preparation of three, C-Br type graphene film electrode
1) Spin-coating photoresist on the C-Br type graphene film, and then placing the C-Br type graphene film under a photoetching mask plate for exposure and development to obtain a patterned source drain electrode;
2) making O to the patterned electrode2Plasma treatment (power 100W, time 10 min);
3) soaking the electrode in acetone solution to remove the photoresist
4) The channel ratio of the C-Br type graphene thin film electrode prepared in the above manner is 20/1.
A schematic of this electrode is shown as a in figure 4.
Preparation and test of organic circuit inverter
The organic logic circuit inverter comprises a substrate, a gate electrode, an insulating layer, a source electrode, a drain electrode and an organic semiconductor layer, and the preparation method comprises the following steps:
the first step is as follows: preparing a source electrode and a drain electrode by adopting the electrode preparation method;
the second step is that: the preparation of the semiconductor layer comprises the following steps:
1) preparing CMUT solutions with different concentrations respectively;
2) preparing a CMUT organic field effect transistor device by using the prepared C-Br type graphene film electrode and adopting a direct dripping method;
3) preparing DPA crystals by adopting a PVT method;
4) transferring a DPA crystal to the electrode by using the prepared C-Br type graphene film electrode to prepare a DPA organic field effect transistor device;
the third step: the source electrode of the CMUT organic field effect transistor is connected with the drain electrode of the DPA organic field effect transistor;
the fourth step: and testing the performance of the device. Using a keithley model 4200 semiconductor tester at room temperature (298K) and under air conditions (10)5Pa) were tested for field effect transistors, inverters. The test results are shown in fig. 4 as b, c and d. As can be seen from the figure, the CMUT and DPA field effect transistors based on the above structure have mobility at 0.153 and 0.191cm at 40V voltage, respectively2V-1s-1On-off ratio>104(ii) a The inverter has a gain of 5.2 at 20V.
Application of lithium battery
1) Preparing the C-Br type graphene film modified negative electrode substrate. Preparing the C-Br type graphene film on the foam copper in the same way as the method.
2) A negative electrode containing metal lithium was prepared. Rapidly transferring the modified substrate into a glove box with water and oxygen content lower than 0.1ppm, matching with metal lithium, and assembling the battery at a current density of 1mA cm by using DOL/DME (volume ratio of 1:1) electrolyte-2Bottom deposition 3mAh cm-2Deposition of lithium metal.
3) And preparing the positive electrode. The anode LiFePO is added4Mixing the conductive carbon black and the polyvinylidene chloride according to the mass ratio of 8:1:1, adding N-methyl pyrrolidone to prepare uniform slurry, uniformly coating the uniform slurry on an aluminum foil current collector, drying in vacuum, and slicing to obtain the working anode.
4) And assembling the full cell. And matching the metal lithium cathode obtained in the third step with the anode obtained in the fourth step, and assembling the whole battery by using DOL/DME (volume ratio of 1:1) electrolyte. Test at 0.1C, LiFePO4The capacity of (A) is 0.1C 155mAh g-1The capacity retention was 90% after 0.1c cycles of 200 cycles.
Or;
1) preparing the C-Br type graphene film modified negative electrode substrate. Preparing the graphene-like film on the copper sheet in the same way as the method.
2) A negative electrode containing metal lithium was prepared. Rapidly transferring the modified substrate into a glove box with water and oxygen content lower than 0.1ppm, matching with metallic lithium, and assembling the battery at a current density of 0.5mA cm by using EC/DMC/DEC (volume ratio of 1:1:1) electrolyte-2Lower deposition 2mAh cm-2Deposition of lithium metal.
3) And preparing the positive electrode. Mixing the positive electrode LiMn2O4Mixing the conductive carbon black and the polyvinylidene chloride according to the mass ratio of 8:1:1, adding N-methyl pyrrolidone to prepare uniform slurry, uniformly coating the uniform slurry on an aluminum foil current collector, drying in vacuum, and slicing to obtain the working anode.
4) And assembling the full cell. Matching the negative pole of the metal lithium obtained in the third step with the positive pole obtained in the fourth step, and using EC/DMC-DEC (volume ratio 1:1:1) electrolyte was used to assemble a full cell. Testing at 0.1C, LiMn2O4Capacity of 120mAh g-1And the capacity retention rate is 85 percent after 0.1c circulation for 200 circles.
Example 2
Preparation of C-Cl graphene film
(1) Pressing the raw material hexachlorobenzene for 2 minutes under 15MPa by a physical tabletting method to prepare 150mg of flaky solid;
(2) preparing a C-Cl graphene film;
placing the flaky solid obtained in the step 1) in a quartz boat, placing a cleaned silicon wafer in a deposition area, and preparing by using a normal-pressure physical meteorological transmission method, wherein high-purity argon is used as carrier gas, the gas flow rate is 0.5sccm, the temperature is 600 ℃ at normal pressure, and the C-Cl graphene film is obtained after 5 hours.
An optical microscope image and an AFM image of the graphene film are shown in FIG. 5; the raman spectrum is shown in fig. 6. As can be seen from FIG. 5, a is a sample of the film prepared on a silicon wafer, which can form a large area uniform film on the substrate. The thickness in AFM FIG. 6, b, was 2.5 nm. A in FIG. 6 at 1348cm-1,1584cm-1And 2756cm-1The D, G, and 2D peaks, respectively.
Preparation of two, C-Cl graphene thin film organic field effect transistor
(1) With cleaning of the gate electrode substrate.
Mixing 1X 1cm2The silicon wafer with the insulating layer was first ultrasonically cleaned with deionized water and then treated with Piranha (H)2O2:H2SO43:7), boiling, finally ultrasonic cleaning with deionized water and isopropanol in sequence, and drying with nitrogen.
(2) Preparation of organic field effect transistor
Preparing the C-Cl graphene film on the substrate cleaned in the step 1), and preparing a source electrode and a drain electrode by adopting a thermal evaporation method.
The transfer curve and the output curve of the organic field effect transistor are shown as c and d in fig. 6. As can be seen from the figure, the C-Cl type graphene film is used as an organic semiconductor layer,and constructing the field effect transistor by adopting bottom gate top contact. The film had a mobility of 0.46cm at VDS-1V2V-1s-1. In fig. 6 d is the output curve.
Example 3
Preparation of graphene-like thin film
(1) Pressing raw material anthracene for 2 minutes under 15MPa by a physical tabletting method to prepare 150mg of flaky solid;
(2) preparing a graphene-like film;
placing the flaky solid obtained in the step 1) in a quartz boat, placing a cleaned silicon wafer in a deposition area, and preparing by using a normal-pressure physical meteorological transmission method, wherein high-purity argon is used as a carrier gas, the gas flow rate is 0.5sccm, the temperature is 650 ℃, and the graphene film is prepared and obtained after 5 hours.
An optical microscope image and an AFM image of the graphene film are shown in FIG. 7; the raman spectrum is shown in fig. 8. As can be seen from FIG. 7, a is a sample of the film prepared on a silicon wafer, which can form a large area uniform film on the substrate. The thickness was 1.1nm as seen in AFM panel b. In a of FIG. 8, at 1352cm-1,1568cm-1And 2750cm-1The D, G, and 2D peaks, respectively.
Preparation of graphene-like thin film organic field effect transistor
(1) With cleaning of the gate electrode substrate.
Mixing 1X 1cm2The silicon wafer with the insulating layer was first ultrasonically cleaned with deionized water and then treated with Piranha (H)2O2:H2SO43:7), boiling, finally ultrasonic cleaning with deionized water and isopropanol in sequence, and drying with nitrogen.
(2) Preparation of organic field effect transistor
Preparing the graphene film on the substrate cleaned in the step 1), and preparing a source electrode and a drain electrode by a thermal evaporation method.
The transfer curve and the output curve of the organic field effect transistor are shown as c and d in fig. 8. As can be seen from the figure, the graphene film is taken as an organic semiconductor layer, and the field effect crystal is constructed by adopting bottom-gate top contactBody tube. The film has a mobility of 3.1X 10 at VDS-1V-3cm2V-1s-1. In fig. 8, d is an output curve, and the graphene-like thin film has good controllability.
Example 4
Preparation of C-Br graphene film
(1) Pressing a raw material 2, 6-dibromoanthracene for 2 minutes under 15MPa by a physical tabletting method to prepare 150mg of flaky solid;
(2) preparing a C-Br graphene film;
placing the flaky solid obtained in the step 1) in a quartz boat, placing a cleaned silicon wafer in a deposition area, and preparing by using a normal-pressure physical meteorological transmission method, wherein high-purity argon is used as carrier gas, the gas flow rate is 0.5sccm, the temperature is 550 ℃, and the C-Br type graphene film is obtained after 5 hours.
An optical microscope picture and an AFM picture of the graphene film are shown in FIG. 9; the raman spectrum is shown in fig. 10. As can be seen from FIG. 9, a is a sample of the film prepared on a silicon wafer, which can form a large area uniform film on the substrate. The thickness was 6.3nm as seen in AFM panel b. In fig. 10, a is 1345cm-1,1550cm-1And 2750cm-1The D, G, and 2D peaks, respectively.
Preparation of two, C-Br type graphene thin film organic field effect transistor
(1) With cleaning of the gate electrode substrate.
Mixing 1X 1cm2The silicon wafer with the insulating layer was first ultrasonically cleaned with deionized water and then treated with Piranha (H)2O2:H2SO43:7), boiling, finally ultrasonic cleaning with deionized water and isopropanol in sequence, and drying with nitrogen.
(2) Preparation of organic field effect transistor
Preparing the C-Br type graphene film on the substrate cleaned in the step 1), and preparing a source electrode and a drain electrode by adopting a thermal evaporation method.
The transfer curve and the output curve of the organic field effect transistor are shown as c and d in fig. 10. As can be seen from the figure, the graphene film is organicAnd a semiconductor layer, wherein a field effect transistor is constructed by adopting bottom gate top contact. The film had a mobility of 8.65cm at VDS-1V2V-1s-1. In fig. 10 d is the output curve.

Claims (10)

1. A method of preparing a graphene-like, comprising:
and preparing the graphene-like on a substrate by using organic micromolecules as a carbon source and utilizing a normal-pressure physical meteorological transmission method.
2. The method of claim 1, wherein: the organic small molecule is any one of the following compounds:
Figure FDA0001826639240000011
x ═ Br, F, I, Cl, or H; r1To R11Are both selected from any one of X and H.
3. The method according to claim 1 or 2, characterized in that: the method further comprises the following steps: prior to said preparing, said carbon source is compressed.
4. The method of claim 3, wherein: the pressing conditions are as follows: pressing for 1-3 minutes under the condition of 15-25 MPa; specifically, the pressing was carried out at 20MPa for 2 minutes.
5. The method according to any one of claims 1-4, wherein: the substrate is selected from at least one of a conductive substrate, a non-conductive substrate and a flexible substrate; specifically, the metal material is selected from any one of glass, ceramic, silicon chip, copper sheet, nickel sheet, foam copper, foam nickel, gold and silver.
6. The method according to any one of claims 1-5, wherein: in the normal-pressure physical meteorological transmission method, the temperature is more than 500 ℃; specifically 500 ℃ and 650 ℃; the time is 1h-10 h; in particular 5 h;
the carrier gas is inert gas; specifically argon; the flow rate of the carrier gas is 0.05-0.50 sccm; specifically 0.5 sccm.
7. A graphene-like material prepared by the method of any one of claims 1 to 6.
8. Use of the graphene-like material of claim 7 as an organic semiconductor layer in the preparation of organic functional devices.
9. Use of the graphene-like material of claim 7 as an electrode in the preparation of any one of organic logic circuits, integrated circuits and lithium batteries.
10. Use according to claim 8 or 9, characterized in that: the organic functional device is an organic field effect transistor;
the organic logic circuit is any one of an inverter and an oscillator.
CN201811187544.8A 2018-10-12 2018-10-12 Graphene-like material and preparation method and application thereof Pending CN111039279A (en)

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Application publication date: 20200421