CN110632488B - Device and method for testing contact electrical characteristics of graphene nanocrystalline carbon film - Google Patents
Device and method for testing contact electrical characteristics of graphene nanocrystalline carbon film Download PDFInfo
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Abstract
The invention discloses a device and a method for testing contact electrical characteristics of a graphene nano-crystal carbon film, wherein the device comprises a metal base, a P-type silicon substrate, the graphene nano-crystal carbon film and a conductive probe which can be contacted with the graphene nano-crystal carbon film in a stacked mode, the metal base and the graphene nano-crystal carbon film are electrically connected through conductive silver paste, and the conductive probe is electrically connected with the metal base. According to the method, based on different contact stages of the conductive probe and the graphene nano-crystal carbon film, a constant voltage mode and a variable voltage mode are adopted to respectively carry out contact electrical characteristic tests on the graphene nano-crystal carbon film, and corresponding electrical characteristic data are obtained. The contact electrical characteristics of the graphene nano-crystal carbon film are tested, and the larger the average nano-crystal size of the graphene nano-crystal carbon film is, the better conductivity is shown, and the method has important significance for the application of the graphene nano-crystal carbon film on the surface of a micro-nano device.
Description
Technical Field
The invention relates to the technical field of nano carbon film electrical parameter measurement, in particular to a device and a method for testing contact electrical characteristics of a graphene nano crystal carbon film.
Background
With the development of the microelectronics and microelectromechanical systems industries, graphene-based microelectromechanical systems are very promising candidates for the next generation of miniaturized, lightweight and ultra-sensitive devices. However, in the research of various graphene-based components, it was found that the tested electrical properties deviate from the theoretical values, wherein the main reason is that the contact electrical characteristics of graphene when contacting with metal or other semiconductor elements are changed, which affects the performance of graphene transistors and graphene-based electrodesAn important factor. In addition, because the thickness of single-layer graphene is only 0.34nm, the nano surface application requirements under various macro scales are difficult to meet, the functional thin film is one of effective means for improving the performance of the device, and the carbon film containing the graphene nanocrystalline embedded layer has good combination potential of physicochemical, mechanical and optical properties because of sp in the thin film2The bonded graphene layer has super lubricity, electrical conductivity, magnetism and photovoltaics. However, the graphene embedded nano-crystalline carbon film also causes the change of electrical properties due to the nano-crystalline structure transformation under the contact action, thereby affecting the reliability of the nano-device.
The prior art has obtained a method for controlling the size of graphene nanocrystals in a carbon film by ECR electron irradiation density under a closed magnetic field, the average size of the graphene nanocrystals of the carbon film prepared by the method is gradually increased from 1.09nm to 2.69nm, the carbon film with the size has good photoelectric and magnetoelectric effects and great potential in optical, magnetic and electric sensing applications, and the contact electrical characteristics of the surface of the graphene nanocrystal carbon film have not been studied.
Therefore, there is a need in the prior art to develop a method for testing the surface characteristics of an electron-irradiated graphene nanocrystalline carbon film, so as to provide a good performance test for the application of the carbon film on a sensing device.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a method for testing the contact electrical characteristics of a graphene nano-crystalline carbon film, which aims to measure the contact electrical characteristics of the graphene nano-crystalline carbon film and solve the technical problem of application of the graphene nano-crystalline carbon film in micro-nano scale.
The utility model provides a test device of graphite alkene nano crystal carbon film contact electrical property, wherein, metal base, P type silicon substrate, graphite alkene nano crystal carbon film that include to and with the conductive probe that graphite alkene nano crystal carbon film contactable, metal base with graphite alkene nano crystal carbon film passes through conductive silver thick liquid electricity and connects, conductive probe wire and metal base electricity are connected.
A method for testing contact electrical characteristics of a graphene nanocrystalline carbon film comprises the following steps:
adjusting the contact area of the conductive probe and the graphene nano-crystal carbon film, so that the contact stage of the conductive probe and the graphene nano-crystal carbon film comprises a loading contact stage, a load-holding contact stage and an unloading contact stage; and respectively carrying out contact electrical characteristic tests in a constant voltage mode and a variable voltage mode on the graphene nano-crystalline carbon film at different contact stages to obtain corresponding electrical characteristic data.
The method for testing the contact electrical characteristics of the graphene nano-crystalline carbon film, wherein the step of testing the contact electrical characteristics of the graphene nano-crystalline carbon film in a constant pressure mode at different contact stages comprises the following steps:
and applying fixed voltage in the loading contact stage, the loading contact stage and the unloading contact stage of the conductive probe and the graphene nano-crystalline carbon film, and applying 0 to the maximum load in the loading contact stage to obtain a corresponding current value when the contact area of the conductive probe and the graphene nano-crystalline carbon film is changed from 0 to the maximum value. The method for testing the contact electrical characteristics of the graphene nano-crystalline carbon film is characterized in that the fixed voltage is 2-8V.
The method for testing the contact electrical characteristics of the graphene nano-crystalline carbon film is characterized in that the maximum load in the loading contact stage is 500-2000 mu N.
The method for testing the contact electrical characteristics of the graphene nano-crystalline carbon film, wherein the step of testing the contact electrical characteristics of the graphene nano-crystalline carbon film in a voltage transformation mode at different contact stages comprises the following steps:
and applying a variable voltage of-5V to 5V at the stage of load-holding contact between the conductive probe and the graphene nano-crystalline carbon film, and testing the volt-ampere characteristic curve of the graphene nano-crystalline carbon film under different voltages.
The method for testing the contact electrical characteristics of the graphene nanocrystalline carbon film is characterized in that the increasing step of the variable voltage is 0.1V.
The method for testing the contact electrical characteristics of the graphene nanocrystalline carbon film comprises the steps that the included angle of the conical surface of the conductive probe is 142.3 degrees, and the curvature radius of the needle tip is 150 nm.
Has the advantages that: according to the method for testing the contact electrical characteristics of the graphene nano-crystal carbon film, the contact electrical characteristics of the graphene nano-crystal carbon film are respectively tested by using the conductive probe and the graphene nano-crystal carbon film in different contact stages in a constant voltage mode and a variable voltage mode, and corresponding electrical characteristic data are obtained. The contact electrical characteristics of the graphene nano-crystal carbon film are tested, and the larger the average nano-crystal size of the graphene nano-crystal carbon film is, the better conductivity is shown, and the method has important significance for the application of the graphene nano-crystal carbon film on the surface of a micro-nano device.
Drawings
Fig. 1 is a schematic structural diagram of a preferred embodiment of a testing apparatus for electrical contact characteristics of a graphene nano-crystalline carbon film according to the present invention.
FIG. 2 shows an electron irradiation density of 35.2mA/cm2TEM surface-like photographs of the carbon films were prepared.
FIG. 3 is a graph showing the response current with respect to the press-in depth after a contact electrical characteristic test was performed on a carbon film having an average nanocrystal size of 1.189nm in a constant voltage mode at an input voltage of 2V and a ballast of 500. mu.N.
FIG. 4 is a graph showing the response current with respect to the press-in depth after a contact electrical characteristic test was performed on a carbon film having an average nanocrystal size of 1.349nm in a constant voltage mode at an input voltage of 8V and a ballast of 2000 μ N.
FIG. 5 is a voltammogram obtained by performing a contact electrical characteristic test on a carbon film having an average nanocrystal size of 1.189nm by applying 500-2000 μ N ballast in a variable voltage mode.
FIG. 6 is a voltammetric response graph obtained by performing a contact electrical characteristic test on a carbon film having an average nanocrystal size of 1.349nm by applying 500-2000 μ N ballast in a variable voltage mode.
Detailed Description
The invention provides a device and a method for testing contact electrical characteristics of a graphene nanocrystalline carbon film, and in order to make the purpose, technical scheme and effect of the invention clearer and clearer, the invention is further described in detail below by referring to the attached drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, fig. 1 is a schematic structural diagram of a preferred embodiment of a device for testing contact electrical characteristics of a graphene nano-crystal carbon film according to the present invention, as shown in the figure, the device includes a metal base 10, a P-type silicon substrate 20, a graphene nano-crystal carbon film 30, and a conductive probe 40 contactable with the graphene nano-crystal carbon film 30, the metal base 10 and the graphene nano-crystal carbon film 30 are electrically connected through a conductive silver paste 50, the conductive probe 40 and the metal base 10 are electrically connected through a conductive wire, and a driving voltage 60 and an ammeter 70 are disposed between the conductive probe 40 and the metal base 10.
The testing device for the contact electrical characteristics of the graphene nano-crystal carbon film based on the embodiment can accurately test the contact electrical characteristics of the graphene nano-crystal carbon film, and provides good performance test data for the application of the graphene nano-crystal carbon film on a sensing device.
In some embodiments, the graphene nano-crystalline carbon film is prepared by ECR electron irradiation, and in the present embodiment, the electron irradiation density of the graphene nano-crystalline carbon film is from 3.2mA/cm during the preparation process2Gradually increased to 184.0mA/cm2The calculation method of the electron irradiation density is to divide the substrate current collected during the carbon film deposition by the substrate area, and the carbon film influenced by the electron irradiation density in the range is adopted, the average size of the graphene nano-crystal is increased from 0.917nm to 1.349nm, and the carbon film has good photoelectric and magnetoelectric effects and great potential in optical, magnetic and electric sensing applications.
In some embodiments, the graphene nano-crystalline carbon film contact electrical characteristics are tested based on the graphene nano-crystalline carbon film contact electrical characteristics testing device, which specifically includes the following steps:
adjusting the contact area of the conductive probe and the graphene nano-crystal carbon film, so that the contact stage of the conductive probe and the graphene nano-crystal carbon film comprises a loading contact stage, a load-holding contact stage and an unloading contact stage; and respectively carrying out contact electrical characteristic tests in a constant voltage mode and a variable voltage mode on the graphene nano-crystalline carbon film at different contact stages to obtain corresponding electrical characteristic data.
Specifically, a graphene nano-crystalline carbon film sample is cut into a proper size by a diamond cutting pen, conductive silver paste is sequentially adhered to a metal base, then the base is installed in a nano-indenter, and the graphene nano-crystalline carbon film contact electrical characteristic testing device is calibrated before each test is started. In the testing process, a conductive probe is adopted to contact the surface of the graphene nano-crystal carbon film, and the contact electrical characteristic test in a constant voltage mode and a variable voltage mode is respectively carried out on the graphene nano-crystal carbon film to obtain corresponding electrical characteristic data, wherein the contact stage of the conductive probe and the graphene nano-crystal carbon film comprises a loading contact stage, a load-holding contact stage and an unloading contact stage, wherein the loading contact stage refers to that the contact area of the conductive probe and the graphene nano-crystal carbon film is increased from zero, and the load-holding contact stage is reached when the contact area reaches the maximum value; and unloading the probe after a certain period of time, namely the unloading stage refers to the process that the contact area between the conductive probe and the graphene nanocrystalline carbon film is changed from the maximum value to zero.
In some embodiments, the performing the contact electrical characteristic test of the graphene nano-crystalline carbon film in a constant pressure mode at different contact stages comprises the steps of: and applying fixed voltage in the loading contact stage, the load-holding contact stage and the unloading contact stage of the conductive probe and the graphene nano-crystal carbon film, and applying 0 to the maximum load in the loading stage to obtain a corresponding current value when the contact area of the conductive probe and the graphene nano-crystal carbon film is changed from 0 to the maximum value, namely testing the change rule of the contact current of the graphene nano-crystal carbon film along with the contact area.
In some embodiments, a fixed voltage of 2-8V is applied during the three phases of contact, and the maximum load of the contact loading phase is 500-. In the loading contact process, the contact area of the probe and the carbon film is increased from zero to reach the maximum value when reaching the load-holding stage, and the maximum value range of the contact area is 0.0744-0.3064 mu m2And the corresponding response current is changed from 0 to the maximum value in the change process, and the maximum value range of the response current is 1.089-65.32 muA. And unloading the probe after the load is maintained for a period of time, wherein the contact area between the probe and the carbon film and the maximum load current are changed from the maximum value to zero. The fixed voltage is 2-8V.
In some embodiments, the performing the contact electrical characteristic test of the graphene nanocrystalline carbon film in a transformation mode at different contact stages comprises the steps of: and applying a variable voltage of-5V to 5V at the stage of load-holding contact between the conductive probe and the graphene nano-crystalline carbon film, and testing the volt-ampere characteristic curve of the graphene nano-crystalline carbon film under different voltages.
In some embodiments, in the transformer mode: no voltage is applied in the loading contact stage and the unloading contact stage, the contact area between the probe and the carbon film is increased from zero to the maximum value in the load-holding stage, and the maximum value of the contact area ranges from 0.0744 to 0.3064 mu m according to different ballasts2. And when the contact area reaches the maximum value in the load-holding stage, applying a variable voltage of-5V, wherein the step size is 0.1V, and obtaining a corresponding volt-ampere characteristic curve according to the difference between the average nanocrystalline size of each sample and the ballast, wherein the volt-ampere response current difference range is 12.1-54.49 muA, and the current value corresponding to minus 5V is subtracted from the current value corresponding to plus 5V.
In some embodiments, the conductive probe has a cone included angle of 142.3 degrees and a tip curvature radius of 150 nm.
The technical solution of the present invention is further illustrated by the following specific examples:
example 1
1) The electron irradiation density during the deposition of the graphene nanocrystalline carbon film in this embodiment was 3.2mA/cm2And the average size of the graphene nanocrystals in the carbon film is 0.917 nm.
2) The contact electrical characteristics of the graphene nano-crystalline carbon film are tested in a constant-voltage mode and a variable-voltage mode, a fixed voltage of +2V and a load of 500 mu N are applied in the constant-voltage mode, and the contact area is changed from 0 to 0.0744 mu m2The corresponding response current changes from 0 to 1.514 mua during the change. Applying a load of 500-2000 μ N in a Sweep mode, wherein the contact area of the load-holding part is 0.0784-0.221 μm2The volt-ampere response current difference is 19.87-35.92 muA.
Example 2
1) The electron irradiation density during the deposition of the graphene nanocrystalline carbon film in this embodiment was 35.2mA/cm2FIG. 2 shows a TEM nanocrystal image of the surface of the carbon film, which shows that the carbon film contains graphene nanocrystals, and the average size of the graphene nanocrystals in the carbon film is 1.189nm。
2) The contact electrical characteristics of the graphene nano-crystalline carbon film are respectively tested in two modes of constant voltage and variable voltage at different positions, as shown in fig. 3, a fixed voltage of +2V and a load of 500 μ N are applied in the constant voltage mode, and the contact area is changed from 0 to 0.0825 μm2The corresponding response current changes from 0 to 1.089 muA during the change. As shown in FIG. 5, a load of 500-2000 μ N is applied in the variable voltage mode, and the contact area at the load-holding position is 0.0841-0.2403 μm2The difference of the volt-ampere response current is 26.32-40.72 muA.
Example 3
1) The electron irradiation density during the deposition of the graphene nanocrystalline carbon film in this embodiment was 86.4mA/cm2(ii) a The average size of the nanocrystalline graphene in the carbon film is 1.295 nm.
2) Respectively carrying out contact electrical characteristic tests in a constant voltage mode and a variable voltage mode on different positions of the graphene nano-crystalline carbon film, applying a fixed voltage of +5V and a load of 2000 mu N in the constant voltage mode, and obtaining that the contact area is changed from 0 to 0.2450 mu m2The corresponding response current changes from 0 to 24.09 mua during the change. Applying a load of 500-2000 μ N in a variable voltage mode, wherein the contact area of the load-holding part is 0.0875-0.2936 μm2The volt-ampere response current difference is 12.095-42.43 muA.
Example 4
1) The electron irradiation density during the deposition of the graphene nanocrystalline carbon film in this embodiment was 116.8mA/cm2And the average size of graphene nanocrystals in the carbon film is 1.269 nm.
2) Respectively carrying out contact electrical characteristic tests in two modes of constant voltage and variable voltage on different positions of the graphene nano-crystalline carbon film, applying a fixed voltage of +5V and a load of 1000 mu N in the constant voltage mode, and obtaining that the contact area is changed from 0 to 0.1880 mu m2The corresponding response current changes from 0 to 15.58 mua during the change. Applying a load of 500-2000 μ N in a variable voltage mode, wherein the contact area of the load-holding part is 0.1052-0.3242 μm2The difference of the volt-ampere response current is 25.89-40.2 muA.
Example 5
1) The electron irradiation density during the deposition of the graphene nanocrystalline carbon film in this embodiment is 164.20 mA-cm2(ii) a The average size of graphene nanocrystals in the carbon film was 1.349 nm.
3) The contact electrical characteristics of the graphene nano-crystalline carbon film are respectively tested in two modes of constant voltage and variable voltage at different positions, as shown in FIG. 4, a constant voltage of +8V and a load of 2000 μ N are applied in the constant voltage mode, and the contact area is obtained to be changed from 0 to 0.2672 μm2The corresponding response current changes from 0 to 53.06 mua during the change. As shown in FIG. 6, a load of 500-2000 μ N is applied in the voltage transformation mode, and the contact area at the load-holding position is 0.0868-0.2828 μm2The volt-ampere response current difference is 35.24-54.49 muA.
In summary, the present invention provides a method for testing contact electrical characteristics of a graphene nano-crystalline carbon film, which comprises contacting a conductive berckvich probe with a carbon surface, and testing the contact electrical characteristics of the graphene nano-crystalline carbon film by applying a load varying within a range of 500-2000 μ N. The sample to be tested is prepared by electron irradiation, and the nano-crystal size is 0.917-1.349 nm. The carbon film is subjected to two contact electrical property tests of constant pressure and variable pressure, and the contact process is divided into three stages: load, and unload. The constant pressure mode is that a fixed load of 2-8V is applied in three stages of contact, and the contact area is changed from 0 to the maximum value. According to the difference between the average nanocrystalline size and the ballasting of each sample, the maximum value of the contact area ranges from 0.0744 to 0.3064 mu m2. The corresponding response current changes from 0 to the maximum value in the change process, and the maximum value range of the response current is 1.089-65.32 muA. In the voltage transformation mode, a variable voltage of-5V is applied in the load holding stage, the step size is 0.1V, and the difference range of the volt-ampere response current is 12.1-54.49 muA according to the difference between the average nanocrystalline size and the ballast of each sample. The larger the average nanocrystalline size is, the better conductivity is shown, and the method has important significance for the surface application of the graphene nanocrystalline carbon film and the micro-nano device.
It should be understood that the technical solutions and concepts of the present invention may be equally replaced or changed by those skilled in the art, and all such changes or substitutions should fall within the protection scope of the appended claims.
Claims (5)
1. A contact electrical characteristic testing method of a graphene nano-crystal carbon film based on a contact electrical characteristic testing device of the graphene nano-crystal carbon film is characterized in that the contact electrical characteristic testing device of the graphene nano-crystal carbon film comprises a metal base, a P-type silicon substrate, the graphene nano-crystal carbon film and a conductive probe which can be contacted with the graphene nano-crystal carbon film, wherein the metal base is electrically connected with the graphene nano-crystal carbon film through conductive silver paste, and the conductive probe is electrically connected with the metal base through a lead; the test method comprises the following steps:
adjusting the contact area of the conductive probe and the graphene nano-crystal carbon film, so that the contact stage of the conductive probe and the graphene nano-crystal carbon film comprises a loading contact stage, a load-holding contact stage and an unloading contact stage;
respectively carrying out contact electrical characteristic tests in a constant voltage mode and a variable voltage mode on the graphene nano-crystal carbon film at different contact stages to obtain corresponding electrical characteristic data;
wherein, the contact electrical characteristic test of the graphene nano-crystalline carbon film in a constant pressure mode at different contact stages comprises the following steps:
applying fixed voltage in the loading contact stage, the load-holding contact stage and the unloading contact stage of the conductive probe and the graphene nano-crystal carbon film, and applying 0 to the maximum load in the loading contact stage to obtain a corresponding current value when the contact area of the conductive probe and the graphene nano-crystal carbon film is changed from 0 to the maximum value;
the contact electrical characteristic test of the graphene nano-crystalline carbon film in a voltage transformation mode at different contact stages comprises the following steps:
and applying a variable voltage of-5V to 5V at the stage of load-holding contact between the conductive probe and the graphene nano-crystalline carbon film, and testing the volt-ampere characteristic curve of the graphene nano-crystalline carbon film under different voltages.
2. The method for testing contact electrical characteristics of a graphene nanocrystalline carbon film according to claim 1, wherein the fixed voltage is 2-8V.
3. The method for testing the contact electrical characteristics of the graphene nano-crystalline carbon film as claimed in claim 1, wherein the maximum load in the loading contact stage is 500-.
4. The method for testing the contact electrical characteristics of the graphene nano-crystalline carbon film according to claim 1, wherein the increase step of the variable voltage is 0.1V.
5. The method for testing the contact electrical characteristics of the graphene nano-crystalline carbon film according to claim 1, wherein the included angle of the conical surface of the conductive probe is 142.3 degrees, and the radius of curvature of the tip is 150 nm.
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