CN109119499B - Diamond radiation detector and preparation method thereof - Google Patents

Diamond radiation detector and preparation method thereof Download PDF

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CN109119499B
CN109119499B CN201710495046.9A CN201710495046A CN109119499B CN 109119499 B CN109119499 B CN 109119499B CN 201710495046 A CN201710495046 A CN 201710495046A CN 109119499 B CN109119499 B CN 109119499B
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graphene
diamond
graphene layer
heterostructure
layer
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CN109119499A (en
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戴丹
林正得
江南
刘颖
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Ningbo Institute of Material Technology and Engineering of CAS
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    • 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
    • H01L31/08—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 in which radiation controls flow of current through the device, e.g. photoresistors
    • H01L31/085—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 in which radiation controls flow of current through the device, e.g. photoresistors the device being sensitive to very short wavelength, e.g. X-ray, Gamma-rays
    • 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
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    • H01L31/028—Inorganic materials including, apart from doping material or other impurities, only elements of Group IV of the Periodic Table
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    • 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
    • H01L31/08—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 in which radiation controls flow of current through the device, e.g. photoresistors
    • H01L31/10—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 in which radiation controls flow of current through the device, e.g. photoresistors characterised by potential barriers, e.g. phototransistors
    • H01L31/115—Devices sensitive to very short wavelength, e.g. X-rays, gamma-rays or corpuscular radiation
    • H01L31/118—Devices sensitive to very short wavelength, e.g. X-rays, gamma-rays or corpuscular radiation of the surface barrier or shallow PN junction detector type, e.g. surface barrier alpha-particle detectors
    • H01L31/1185—Devices sensitive to very short wavelength, e.g. X-rays, gamma-rays or corpuscular radiation of the surface barrier or shallow PN junction detector type, e.g. surface barrier alpha-particle detectors of the shallow PN junction detector type
    • 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
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Abstract

The invention relates to a diamond radiation detector and a preparation method thereof. Specifically, in the present invention, the diamond radiation detector has excellent ohmic contact property and X-ray response sensitivity. The method has the characteristics of simple process, low cost, easiness in operation and the like, and can be used for quickly and efficiently preparing the graphene-diamond heterostructure with excellent bonding performance between the graphene layer and the diamond substrate so as to prepare the graphene-diamond detector.

Description

Diamond radiation detector and preparation method thereof
Technical Field
The invention relates to the field of materials, in particular to a diamond radiation detector and a preparation method thereof.
Background
The diamond material has the advantages of large forbidden band width, high carrier mobility, high breakdown electric field intensity, high temperature and high pressure resistance and can operate in extreme environments. The diamond detector has the advantages of low noise, small leakage current, strong radiation resistance, fast time response and the like.
However, ohmic contacts are a bottleneck problem in the development of probing devices. In order to conduct the generated electron-hole pairs to an external circuit to form an electrical signal, a suitable electrode needs to be applied to the diamond to form a good electrical contact-a non-rectifying (ohmic) contact between the electrode and the diamond. The ohmic contact does not create significant additional resistance and does not significantly alter the internal equilibrium carrier concentration. The ohmic contact has a linear symmetrical current-voltage relation and is characterized by no potential barrier and extremely high surface recombination velocity. However, diamond is a wide bandgap (5.5eV) material, and when diamond is in contact with metal, Schottky (Schottky) rectifying contact is easily formed due to an interface barrier. Moreover, the diamond surface is difficult to realize high dosage doping, so that an electrode with ohmic contact is difficult to manufacture on the diamond.
Graphene is receiving a great deal of attention due to its excellent physical properties. Graphene is a carbon-carbon atom sp2Bonded, honeycomb-like, regularly arranged, and only monoatomic thick carbon materials with many previously unseen properties, such as ultra high carrier mobility (2 × 10)6cm2The material has the advantages of being 1,000 times of silicon in terms of Vs, ultrahigh in thermal conductivity (the theoretical value reaches 5,300W/mK), high in light transmittance, excellent in mechanical property, capable of achieving the normal-temperature quantum Hall effect and the like, and capable of being applied to the fields of ultrafast electronic components, photovoltaic cell electrodes, high-sensitivity sensors and the like. Sp relative to diamond3Three-dimensional structure, graphene is periodic sp2The bonding has a very good compatibility with the lattice lengths of the two being close (about 2% difference). Another feature is that both materials have very high thermal conductivity, providing an effective heat sink when fabricated into an assembly, avoiding thermal failure.
The graphene and the diamond are matched to form a heterostructure, which is a novel structure developed in recent years, and only a few literature reports exist at present, so that the development potential of the heterostructure is shown to be great. The inventor of Shanghai university (CN201610315723, using spin coating method to coat graphene oxide on diamond film, then reducing graphene oxide to obtain graphene, then using vacuum evaporation or electron beam evaporation method to fabricate gold electrode on the surface thereof, making graphene-gold two-layer system, and annealing in nitrogen atmosphere to form ohmic contact electrode, IBM group published graphene radio frequency assembly paper on Nature, and CVD graphene was pasted on diamond-like carbon film (DLC) substrate by transfer method to fabricate device with line width of 40 nm, compared with silicon substrate, DLC film has higher phonon energy (165meV) and lower carrier trap density, thereby greatly improving graphene device performance, its cut-off frequency reaches 155GHz, U.S. Rivers team uses lift-off method to paste graphene on nano diamond film, and finds that current-carrying capacity (UC-carrying capacity) of the device is 20 times higher than that of using it, reaching 18 mu A/nm2And is favorable for developing high-power and large-current-density electronic components. The graphene/diamond heterostructure not only can not damage the essential characteristics of graphene and diamond, but also can reduce the component by the mutual high heat conduction efficiencyNoise ratio, improving reliability. However, since graphene is usually grown by copper foil catalytic CVD, it must be transferred from the copper foil to the diamond surface, and the transfer process has the defects of easy contamination, structural damage, poor interface compatibility, and poor bonding property.
Based on this, there is a need in the art for a graphene-diamond heterostructure with excellent bonding properties for the fabrication of diamond radiation detectors.
Disclosure of Invention
The invention aims to provide a graphene-diamond heterostructure with excellent bonding performance for preparing a diamond radiation detector.
In a first aspect of the invention, there is provided a graphene-diamond probe comprising a graphene-diamond heterostructure and a housing for enclosing the graphene-diamond heterostructure.
In another preferred example, the graphene-diamond heterostructure comprises a diamond substrate and a first graphene layer and a second graphene layer bonded to the surface of the diamond substrate, the first graphene layer and the second graphene layer each being grown in situ on the surface of the diamond substrate.
In another preferred embodiment, the "binding" is covalent bonding.
In another preferred embodiment, the diamond substrate has a thickness of 0.1 to 10mm, preferably 0.2to 5mm, more preferably 0.3 to 3 mm.
In another preferred example, the graphene layer is single-layer graphene, double-layer graphene or multi-layer graphene, and is preferably single-layer graphene.
In another preferred embodiment, the thickness of the single graphene layer is 0.1-0.5nm, preferably 0.2-0.4 nm.
In another preferred embodiment, the bond of the graphene layer and the diamond substrate is an ohmic contact.
In another preferred example, the graphene layer and the diamond substrate are bonded in a manner selected from the group consisting of:
1) the first and second graphene layers are bonded to two opposing major surfaces of the diamond substrate, respectively (as shown in figure 5 a);
2) the first and second graphene layers are bonded to one major surface of the diamond substrate without direct contact between the two graphene layers (as shown in figure 5 b);
3) the first graphene layer and the second graphene layer are arranged on one main surface of the diamond substrate, the first graphene layer is a plurality of (such as 3-20) graphene coatings arranged in parallel at intervals, the second graphene layer is a square graphene coating, the first graphene layer is positioned in a square of the second graphene layer, and the first graphene layer and the second graphene layer are not in direct contact (as shown in fig. 5 c);
4) the first graphene layer and the second graphene layer are disposed on one main surface of the diamond substrate, the first graphene layer and the second graphene layer are both of an interdigital structure, the first graphene layer and the second graphene layer are disposed in a crossed manner, and the first graphene layer and the second graphene layer are not in direct contact (as shown in fig. 5 d).
In another preferred example, the housing has a pin therein, and the housing and the graphene-diamond heterostructure are combined as follows: the first graphene layer of the graphene-diamond heterostructure is welded with the pins of the shell through welding wires or conductive adhesives, and the second graphene layer of the graphene-diamond heterostructure is welded with the inner bottom surface of the shell through the conductive adhesives or the welding wires.
In another preferred example, the housing fully encapsulates the graphene-diamond heterostructure.
In another preferred embodiment, the pins of the housing extend through a surface of the housing, and there are projections on an outer surface of the housing.
In another preferred example, the outer bottom surface corresponding to the inner bottom surface of the shell is provided with a second pin.
In another preferred embodiment, the housing is a conductive material selected from the group consisting of:
1) copper, nickel, or alloys thereof;
2) copper plating alloy;
3) a conductive rubber;
4) and (6) conducting masking cloth.
In another preferred embodiment, the detector has one or more characteristics selected from the group consisting of:
1) after biasing, the dark current of the detector and the bias voltage are basically in a linear relation;
2) the detector has a 3.4 × 10 for X-rays-20～2.9×10-1Coulomb/gurley response sensitivity.
In another preferred embodiment, the detector is prepared by the method of the second aspect of the present invention.
In a second aspect of the present invention, there is provided a method for manufacturing a graphene-diamond probe, the method comprising the steps of:
i) providing a graphene-diamond heterostructure and a housing;
ii) encapsulating the graphene-diamond heterostructure with the housing, resulting in the graphene-diamond probe.
In another preferred example, the graphene-diamond heterostructure is prepared as follows:
1) providing a coated diamond and an etching solution;
2) treating the coated diamond at a high temperature to obtain a treated coated diamond;
3) and etching the treated coated diamond obtained in the step 2) by using the etching solution to obtain the graphene-diamond heterostructure.
In another preferred example, the coated diamond comprises a diamond matrix and a metal dielectric film coated on the surface of the diamond matrix.
In another preferred example, the metal dielectric film is plated on the surface of the diamond matrix by a process selected from the group consisting of: electron beam evaporation, thermal evaporation, magnetron sputtering, or a combination thereof.
In another preferred embodiment, the diamond substrate is selected from the group consisting of: single crystal, polycrystalline, nanocrystalline.
In another preferred example, the diamond substrate is a single crystal.
In another preferred embodiment, the thickness of the metal dielectric film is 1-1000 nm, preferably 3-500 nm, and more preferably 5-200 nm.
In another preferred embodiment, the metal dielectric film is a transition metal film selected from the group consisting of: a copper film, a nickel film, a gold film, a platinum film, an iron film, or a composite film thereof.
In another preferred example, the etching solution comprises the following components: CuSO4+HCl+H 20、(NH4)2S2O8+H2O。
In another preferred example, in the etching solution, CuSO4HCl and H2The dosage ratio of 0 is 1-5g:3-10 ml: 3-10ml, preferably 1-3 g: 3-8 ml: 3-8 ml.
In another preferred example, (NH) is contained in the etching solution4)2S2O8And H2The dosage ratio of 0 is 4-28g:200-1200ml, preferably 1-14 g:200 and 600 ml.
In another preferred embodiment, the treatment temperature of the high-temperature treatment is 750-; and/or
The treatment time of the high-temperature treatment at the treatment temperature is 1-240min, preferably 10-120min, and more preferably 13-60 min.
In another preferred example, the high temperature treatment is performed in a tube furnace.
In another preferred example, H is continuously introduced into the processing chamber during the high-temperature treatment2Preferably, H2The amount of the introduced gas is 3to 20sccm, preferably 5to 15 sccm.
In another preferred embodiment, the pressure in the process chamber during the high temperature process is 0.05 to 0.5Torr, preferably 0.10 to 0.2 Torr.
In another preferred embodiment, the processing time of the etching treatment is 1-200min, preferably 10-180min, and more preferably 20-150 min.
It is to be understood that within the scope of the present invention, the above-described features of the present invention and those specifically described below (e.g., in the examples) may be combined with each other to form new or preferred embodiments. Not to be reiterated herein, but to the extent of space.
Drawings
Fig. 1 is a schematic structural diagram of the graphene-diamond heterostructures obtained in examples 1-9.
Fig. 2 is a schematic structural view of the graphene-diamond probe obtained in example 10.
Fig. 3 is a graph showing a change in dark current with a bias voltage of the graphene-diamond probe 1 obtained in example 10.
Fig. 4 is a graph showing the variation of the sensitivity of the graphene-diamond detector 1 obtained in example 10 with respect to the X-ray energy.
Fig. 5 is a schematic diagram of several exemplary placement configurations of the graphene-diamond heterostructure of the present invention.
Detailed Description
The invention provides a graphene-diamond heterostructure with excellent graphene layer and diamond substrate bonding performance, which is prepared by the inventor through long-term and deep research. Because the graphene layer grows on the surface of the diamond in situ, the graphene layer is pure in components, the bonding performance of the graphene layer and the diamond is excellent, the structure of the graphene layer is relatively complete, and the interface compatibility of the graphene layer and the diamond is good. Further, the graphene-diamond detector with excellent ohmic contact performance and X-ray response sensitivity is obtained by packaging the graphene-diamond heterostructure. On this basis, the inventors have completed the present invention.
Term(s) for
As used herein, the terms "graphene-diamond heterostructure", "diamond-graphene heterostructure" or "heterostructure" are used interchangeably.
As used herein, the terms "diamond radiation detector" and "graphene-diamond detector" are used interchangeably.
Diamond radiation detector
The invention provides a graphene-diamond detector, which comprises a graphene-diamond heterostructure and a shell used for packaging the graphene-diamond heterostructure.
In the present invention, the graphene-diamond heterostructure comprises a diamond substrate and a first graphene layer and a second graphene layer bonded to a surface of the diamond substrate, both of the first graphene layer and the second graphene layer being grown in situ on the surface of the diamond substrate.
In another preferred embodiment, the thickness of the diamond substrate is not particularly limited, and can be adjusted within a wide range according to actual needs, and is preferably 0.1 to 10mm, more preferably 0.2to 5mm, and still more preferably 0.3 to 3 mm.
Typically, the graphene layer is single-layer graphene, double-layer graphene or multi-layer graphene, preferably single-layer graphene.
In another preferred embodiment, the thickness of the single graphene layer is not particularly limited, and can be adjusted within a wide range according to actual needs, and is preferably 0.1-0.5nm, and more preferably 0.2-0.4 nm.
In another preferred embodiment, the bond of the graphene layer and the diamond substrate is an ohmic contact.
It is to be understood that, in the present invention, the bonding manner of the graphene layer and the diamond substrate includes (but is not limited to) the following group:
1) the first and second graphene layers are bonded to two opposing major surfaces of the diamond substrate, respectively (as shown in figure 5 a);
2) the first and second graphene layers are bonded to one major surface of the diamond substrate without direct contact between the two graphene layers (as shown in figure 5 b);
3) the first graphene layer and the second graphene layer are arranged on one main surface of the diamond substrate, the first graphene layer is a plurality of (such as 3-20) graphene coatings arranged in parallel at intervals, the second graphene layer is a square graphene coating, the first graphene layer is positioned in a square of the second graphene layer, and the first graphene layer and the second graphene layer are not in direct contact (as shown in fig. 5 c);
4) the first graphene layer and the second graphene layer are disposed on one main surface of the diamond substrate, the first graphene layer and the second graphene layer are both of an interdigital structure, the first graphene layer and the second graphene layer are disposed in a crossed manner, and the first graphene layer and the second graphene layer are not in direct contact (as shown in fig. 5 d).
Fig. 1 is a schematic structural diagram of the graphene-diamond heterostructures obtained in examples 1-9.
Fig. 2 is a schematic structural view of the graphene-diamond probe obtained in example 10.
It will be appreciated that the detector has a very good response sensitivity to X-rays, UV light, gamma rays or alpha particles.
Preparation method
The invention also provides a preparation method of the graphene-diamond detector, which comprises the following steps:
i) providing a graphene-diamond heterostructure and a housing;
ii) encapsulating the graphene-diamond heterostructure with the housing, resulting in the graphene-diamond probe.
It is to be understood that the graphene-diamond heterostructure is prepared as follows:
1) providing a coated diamond and an etching solution;
2) treating the coated diamond at a high temperature to obtain a treated coated diamond;
3) and etching the treated coated diamond obtained in the step 2) by using the etching solution to obtain the graphene-diamond heterostructure.
Typically, the coated diamond comprises a diamond substrate and a metal dielectric film coated on the surface of the diamond substrate.
In another preferred embodiment, the metal dielectric film is plated on the surface of the diamond matrix by a process selected from the group consisting of (but not limited to): electron beam evaporation, thermal evaporation, magnetron sputtering, or a combination thereof.
In another preferred embodiment, the diamond substrate is selected from the group consisting of: single crystal, polycrystalline, nanocrystalline.
In another preferred example, the diamond substrate is a single crystal.
In another preferred embodiment, the thickness of the metal dielectric film is 1-1000 nm, preferably 3-500 nm, and more preferably 5-200 nm.
In another preferred embodiment, the metal dielectric film is a transition group metal film selected from the group consisting of (but not limited to): a copper film, a nickel film, a gold film, a platinum film, an iron film, or a composite film thereof.
In the invention, the treatment temperature of the high-temperature treatment is 750-1200 ℃, preferably 800-1100 ℃, and more preferably 800-1050 ℃; and/or
The treatment time of the high-temperature treatment at the treatment temperature is 1-240min, preferably 10-120min, and more preferably 13-60 min.
In another preferred example, the high temperature treatment is performed in a tube furnace.
In another preferred example, H is continuously introduced into the processing chamber during the high-temperature treatment2Preferably, H2The amount of the introduced gas is 3to 20sccm, preferably 5to 15 sccm.
In another preferred embodiment, the pressure in the process chamber during the high temperature process is 0.05 to 0.5Torr, preferably 0.10 to 0.2 Torr.
In another preferred embodiment, the processing time of the etching treatment is 1-200min, preferably 10-180min, and more preferably 20-150 min.
In the invention, the method is characterized in that a graphene layer with strong bonding force is grown in situ on the diamond by using an annealing method in a hydrogen atmosphere to form the ohmic contact electrode of graphene. The graphene ohmic contact electrode disclosed by the invention is strong in binding force, has a good ohmic contact characteristic, can obviously improve the functions of the obtained device, and is simple in process.
Typically, the method comprises the steps of:
(1) cleaning the diamond;
(2) plating a metal dielectric film with the thickness of 1-1000 nm on the surface of the diamond cleaned and dried in the step (1) by using a plating device;
(3) putting the diamond (including single crystal and polycrystal) plated with the metal dielectric film in the step (2) into a tubular furnace, quickly heating to 600-1150 ℃, then annealing for 1-240min, quickly cooling to room temperature, and only continuously introducing 1-150 sccm of hydrogen in the whole reaction process in the tubular furnace;
(4) putting the sample which finishes growth in the step (3) into etching liquid, etching the residual metal dielectric film on the surface of the sample, and washing the sample by using deionized water to obtain a diamond-graphene heterostructure;
(5) and packaging the diamond-graphene heterostructure by using a shell to obtain the graphene-diamond detector.
According to the method, the graphene film is formed in situ by the diamond under the condition of rapid cooling by utilizing the catalytic action of the metal dielectric film on the diamond, and finally the residual metal dielectric film on the surface of the obtained sample is etched, so that the high-performance graphene electrode is obtained. Further, the graphene/diamond probe is formed by encapsulation. Good ohmic contact is formed between the graphene and the diamond.
It should be understood that, in the present invention, graphene-diamond heterostructures with different relative positions of the graphene layer and the diamond substrate can be prepared according to actual needs, so as to obtain graphene-diamond detectors with different structures. Specifically, graphene layers arranged at different positions can be obtained by adjusting the position of the metal dielectric film plated on the surface of the diamond matrix. Several typical positional arrangements of graphene-diamond heterostructures are shown in fig. 5, where a) is an opposing sandwich structure, b) is a photoconductive structure, c) is a coplanar sandwich structure, d) is an interdigitated structure. The graphene-diamond detector assembled by any one of the four structures has excellent ohmic contact performance and X-ray response sensitivity.
Compared with the prior art, the invention has the following main advantages:
(1) the method has the characteristics of simple process, low cost, easy operation and the like;
(2) the method can effectively avoid the problems of pollution, structural damage and the like caused by the transfer of the traditional graphene to the surface of the diamond;
(3) the method grows the graphene layer on the diamond in situ, so that the interface compatibility of the graphene layer and the diamond is good, and the bonding performance of the graphene layer and the diamond is more excellent compared with the case of using an external carbon source;
(4) since the graphene layer has more excellent bonding performance with the diamond, the electrode comprising the graphene-diamond heterostructure of the invention has excellent electrical properties, and when the electrode is in contact with a metal electrode, Schottky (Schottky) rectifying contact formed by an interface barrier can be avoided;
(5) the graphene-diamond detector has good signal-to-noise ratio, irradiation resistance and response speed.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out according to conventional conditions or according to conditions recommended by the manufacturers. Unless otherwise indicated, percentages and parts are by weight.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred embodiments and materials described herein are intended to be exemplary only.
Example 1 graphene-diamond heterostructure 1
Putting the diamond plated with the nickel film with the thickness of 5nm into a tubular furnace, quickly heating to 1000 ℃, annealing for 15min, then quickly cooling to room temperature, and only continuously introducing H of 8sccm into the furnace in the whole growth stage2And the pressure was maintained at 0.11 Torr. After the growth is finished, the sample is put into etching solution (CuSO)4:HCl:H20-1 g:5ml:5ml) for 40min, and removing the residual nickel film on the surface to obtain the graphene-diamond heterostructure 1. Wherein the diamond substrate has a thickness of 0.3 mm.
Raman characterization showed: the wave number of the graphene-diamond heterostructure 1 is 1580cm-1Has a characteristic peak G of graphene at a wave number of 2689cm-1The graphene has a characteristic peak 2D of graphene, the ratio of the 2D peak to the G peak is 1.13, and the graphene is single-layer graphene. The thickness of the graphene is 0.3 nm. The graphene/diamond (i.e. graphene-diamond heterostructure) is not damaged by ultrasound in acid and alkali.
Example 2 graphene-diamond heterostructure 2
Putting the diamond plated with the copper film with the thickness of 10nm into a tube furnace, quickly heating to 1000 ℃, annealing for 15min, then quickly cooling to room temperature, and only continuously introducing H of 8sccm into the furnace in the whole growth stage2And the pressure was maintained at 0.12 Torr. After the growth is finished, the sample is put into etching solution (CuSO)4:HCl:H20-1 g:5ml:5ml) for 40min, and removing the residual copper film on the surface of the graphene-diamond heterostructure to obtain the graphene-diamond heterostructure 2. Wherein the diamond substrate has a thickness of 1 mm.
Raman characterization showed: the wave number of the graphene-diamond heterostructure 2 is 1583cm-1Has a characteristic peak G of graphene at a wave number of 2692cm-1The graphene has a characteristic peak 2D of graphene, the ratio of the 2D peak to the G peak is 1.20, and the graphene is single-layer graphene. The thickness of the graphene is 0.3 nm. The structure of the graphene/diamond cannot be damaged by ultrasonic treatment in acid and alkali.
Example 3 graphene-diamond heterostructure 3
Will be plated with 10Putting diamond with copper/nickel film of 0nm thickness into a tube furnace, rapidly heating to 1000 deg.C, annealing for 15min, rapidly cooling to room temperature, and continuously introducing H of 8sccm into the furnace during the whole growth stage2And the pressure was maintained at 0.13 Torr. After the growth is finished, the sample is put into etching liquid ((NH)4)2S2O8:H20-4 g:200ml) for 40min, and removing the residual copper/nickel film on the surface of the graphene/diamond heterostructure to obtain the graphene-diamond heterostructure 3. Wherein the diamond substrate has a thickness of 1 mm.
Raman characterization showed: the graphene-diamond heterostructure 3 is at the wave number of 1586cm-1Has a characteristic peak G of graphene at a wave number of 2692cm-1The graphene has a characteristic peak 2D peak, the ratio of the 2D peak to the G peak is 0.75, and the graphene is multilayer graphene. The thickness of the graphene is 0.9 nm. The structure of the graphene/diamond cannot be damaged by ultrasonic treatment in acid and alkali.
Example 4 graphene-diamond heterostructure 4
Putting diamond plated with copper/nickel film with thickness of 100nm into a tube furnace, rapidly heating to 950 ℃, annealing for 15min, rapidly cooling to room temperature, and continuously introducing H of 8sccm into the furnace in the whole growth stage2And the pressure was maintained at 0.13 Torr. After the growth is finished, the sample is put into etching solution (CuSO)4:HCl:H20-1 g:5ml:5ml) for 40min, and removing the residual copper/nickel film on the surface of the graphene/diamond heterostructure to obtain the graphene-diamond heterostructure 4. Wherein the diamond substrate has a thickness of 0.5 mm.
Raman characterization showed: the graphene-diamond heterostructure 4 is at a wave number of 1580cm-1Has a characteristic peak G of graphene at a wave number of 2692cm-1The graphene has a characteristic peak 2D of graphene, the ratio of the 2D peak to the G peak is 0.90, and the graphene is multilayer graphene. The thickness of the graphene is 1.2 nm. The structure of the graphene/diamond cannot be damaged by ultrasonic treatment in acid and alkali.
Example 5 graphene-diamond heterostructure 5
Putting the diamond plated with the copper/nickel film with the thickness of 10nm into a tube furnace, quickly heating to 1050 ℃, annealing for 15min, then quickly cooling to room temperature, and finishingOnly 8sccm H is continuously introduced into the furnace in each growth stage2And the pressure was maintained at 0.12 Torr. After the growth is finished, the sample is put into etching solution (CuSO)4:HCl:H20-1 g:5ml:5ml) for 40min, and removing the residual copper film on the surface to obtain the graphene-diamond heterostructure 5. Wherein the diamond substrate has a thickness of 1 mm.
Raman characterization showed: the graphene-diamond heterostructure 5 is at a wave number of 1583cm-1Has a characteristic peak G of graphene at a wave number of 2696cm-1The graphene has a characteristic peak 2D of graphene, the ratio of the 2D peak to the G peak is 0.80, and the graphene is multilayer graphene. The thickness of the graphene is 0.6 nm. The structure of the graphene/diamond cannot be damaged by ultrasonic treatment in acid and alkali.
Example 6 graphene-diamond heterostructure 6
Putting the diamond plated with the nickel film with the thickness of 5nm into a tube furnace, quickly heating to 800 ℃, annealing for 15min, then quickly cooling to room temperature, and only continuously introducing 10sccm of H into the furnace in the whole growth stage2And the pressure is maintained at 0.11Torr to 0.14 Torr. After the growth is finished, the sample is put into etching liquid ((NH)4)2S2O8:H20-8 g:600ml) for 40min, and removing the nickel film remained on the surface of the graphene-diamond heterostructure to obtain the graphene-diamond heterostructure 6. Wherein the diamond substrate has a thickness of 0.5 mm.
Raman characterization showed: the graphene-diamond heterostructure 6 is 1582cm in wave number-1Has a characteristic peak G of graphene at a wave number of 2693cm-1The graphene has a characteristic peak 2D of graphene, the ratio of the 2D peak to the G peak is 1.80, and the graphene is single-layer graphene.
Example 7 graphene-diamond heterostructure 7
Putting the diamond plated with the nickel film with the thickness of 20nm into a tubular furnace, quickly heating to 1050 ℃, annealing for 30min, then quickly cooling to room temperature, and only continuously introducing 10sccm H into the furnace in the whole growth stage2And the pressure is maintained at 0.11Torr to 0.14 Torr. After the growth is finished, the sample is put into etching solution (CuSO)4:HCl:H20-1 g:5ml:5ml) for 40min, and etching the surface thereofAnd removing the residual nickel film to obtain the graphene-diamond heterostructure 7. Wherein the diamond substrate has a thickness of 1 mm.
Raman characterization showed: the graphene-diamond heterostructure 7 is at the wave number of 1581cm-1Has a characteristic peak G of graphene at a wave number of 2688cm-1The graphene has a characteristic peak 2D of graphene, the ratio of the 2D peak to the G peak is 0.65, and the graphene is multilayer graphene.
Example 8 graphene-diamond heterostructure 8
Putting the diamond plated with the copper/nickel film with the thickness of 20nm into a tubular furnace, quickly heating to 1050 ℃, annealing for 30min, then quickly cooling to room temperature, and only continuously introducing 10sccm of H into the furnace in the whole growth stage2And the pressure is maintained at 0.11Torr to 0.14 Torr. After the growth is finished, the sample is put into etching solution (CuSO)4:HCl:H20-1 g:5ml:5ml) for 40min, and removing the residual copper/nickel film on the surface of the graphene/diamond heterostructure to obtain the graphene-diamond heterostructure 8. Wherein the diamond substrate has a thickness of 0.5 mm.
Raman characterization showed: the graphene-diamond heterostructure 8 is at the wave number of 1580cm-1Has a characteristic peak G of graphene at a wave number of 2695cm-1The graphene has a characteristic peak 2D peak, the ratio of the 2D peak to the G peak is 0.78, and the graphene is multilayer graphene.
Example 9 graphene-diamond heterostructure 9
Putting the diamond plated with the nickel film with the thickness of 30nm into a tubular furnace, quickly heating to 1000 ℃, annealing for 30min, then quickly cooling to room temperature, and only continuously introducing 10sccm H into the furnace in the whole growth stage2And the pressure is maintained at 0.11Torr to 0.14 Torr. After the growth is finished, the sample is put into etching solution (CuSO)4:HCl:H20-1 g:5ml:5ml) for 40min, and removing the nickel film remained on the surface of the graphene-diamond heterostructure 9. Wherein the diamond substrate has a thickness of 1.5 mm.
Raman characterization showed: in the graphene-diamond heterostructure 9, at a wave number of 1583cm-1Has a characteristic peak G of graphene at a wave number of 2694cm-1Is provided with grapheneThe ratio of the 2D peak to the G peak is 0.80, and the graphene is multilayer graphene.
Example 10 graphene-diamond probe
The graphene-diamond heterostructures 1-9 prepared in examples 1-9 were respectively encapsulated using a housing to obtain graphene-diamond detectors 1-9.
Specifically, the packaging method of the detector is as follows: welding one graphene surface of the graphene-diamond heterostructure and one pin of the shell by a platinum wire, welding the whole surface of the other graphene surface of the graphene-diamond heterostructure and the bottom surface of the shell by silver adhesive, and welding the bottom surface of the shell and one pin by the platinum wire.
The dark current and sensitivity of the detector are important performance parameters of the detector. The invention adopts MOXTEKMagPro 60keV 12Watt X-ray Source, and utilizes the Agilent B2902A Precision Source/Measure Unit test instrument, the front side (ray incidence side) of the detector is connected with a signal, the back side of the detector is connected with high voltage, and the detector is in the dark for detecting the performance.
Fig. 3 is a graph showing a change in dark current with a bias voltage of the graphene-diamond probe 1 obtained in example 10.
As can be seen from fig. 3: when the bias voltage is within 600V, the dark current is less than 400nA, and the dark current has a good linear relation with the voltage, which indicates that excellent ohmic contact is obtained between graphene and diamond in the graphene-diamond detector.
Fig. 4 is a graph showing the variation of the sensitivity of the graphene-diamond detector 1 obtained in example 10 with respect to the X-ray energy.
From FIG. 4 it can be seen that the detector 1 has a voltage of 3.4 × 10 in the energy range of 3-20keV and in the voltage range of 30-150V-9～2.9×10-8Coulomb/gurley response sensitivity.
The graphene-diamond detectors 2-9 have similar performance to the graphene-diamond detector 1.
Comparative example 1 graphene-diamond heterostructure C1 (low annealing temperature)
Putting the diamond plated with the nickel film with the thickness of 5nm into a tube furnace, and quickly heating toAnnealing at 400 deg.C for 15min, rapidly cooling to room temperature, and introducing H of 8sccm into the furnace continuously during the whole growth stage2And the pressure was maintained at 0.11 Torr. After the growth is finished, the sample is put into etching solution (CuSO)4:HCl:H20-1 g:5ml:5ml) for 40min, and removing the residual nickel film on the surface to obtain the graphene-diamond heterostructure C1.
According to the detection, in the graphene-diamond heterostructure C1, although a graphene layer can grow on a diamond substrate, the graphene layer is discontinuous, so that the graphene-diamond probe C1 further assembled by the graphene-diamond heterostructure C1 has no electrical property and no detection signal.
Comparative example 2 graphene-diamond heterostructure C2 (short annealing time)
Putting the diamond plated with the nickel film with the thickness of 5nm into a tube furnace, quickly heating to 800 ℃, annealing for 10 seconds, then quickly cooling to room temperature, and only continuously introducing 10sccm of H into the furnace in the whole growth stage2And the pressure is maintained at 0.11Torr to 0.14 Torr. After the growth is finished, the sample is put into etching solution (CuSO)4:HCl:H20-1 g:5ml:5ml) for 40min, and removing the residual nickel film on the surface to obtain the graphene-diamond heterostructure C2.
According to the detection, in the graphene-diamond heterostructure C2, although a graphene layer can grow on a diamond substrate, the graphene layer is discontinuous, so that the graphene-diamond probe C2 further assembled by the graphene-diamond heterostructure C2 has no electrical property and no detection signal.
All documents referred to herein are incorporated by reference into this application as if each were individually incorporated by reference. Furthermore, it should be understood that various changes and modifications of the present invention can be made by those skilled in the art after reading the above teachings of the present invention, and these equivalents also fall within the scope of the present invention as defined by the appended claims.

Claims (12)

1. A graphene-diamond probe, wherein the probe comprises a graphene-diamond heterostructure and a housing for encapsulating the graphene-diamond heterostructure;
the graphene-diamond heterostructure comprises a diamond substrate and a first graphene layer and a second graphene layer which are bonded on the surface of the diamond substrate, wherein the first graphene layer and the second graphene layer are both obtained by in-situ growth on the surface of the diamond substrate;
the graphene layer is single-layer graphene;
the detector is prepared as follows:
i) providing a graphene-diamond heterostructure and a housing;
ii) encapsulating the graphene-diamond heterostructure with the housing, resulting in the graphene-diamond probe;
the graphene-diamond heterostructure is prepared as follows:
1) providing a coated diamond and an etching solution;
2) treating the coated diamond at a high temperature to obtain a treated coated diamond;
3) etching the treated coated diamond obtained in the step 2) by using the etching solution to obtain the graphene-diamond heterostructure;
during the high-temperature treatment, the pressure in the treatment cavity is 0.11-0.14 Torr;
the coated diamond comprises a diamond matrix and a metal dielectric film coated on the surface of the diamond matrix.
2. A probe as claimed in claim 1, in which the thickness of the single graphene layer is 0.1-0.5 nm.
3. A probe as claimed in claim 1, in which the single graphene layer has a thickness of 0.2to 0.4 nm.
4. The probe of claim 1, wherein the graphene layer and the diamond substrate are bonded in a manner selected from the group consisting of:
1) the first graphene layer and the second graphene layer are bonded to two opposite major surfaces of the diamond substrate, respectively;
2) the first graphene layer and the second graphene layer are bonded to one major surface of the diamond substrate without direct contact between the two graphene layers.
5. The probe of claim 1, wherein the graphene layer and the diamond substrate are bonded as follows: the first graphene layer and the second graphene layer are arranged on one main surface of the diamond substrate, the first graphene layer is a plurality of graphene coatings arranged at intervals in parallel, the second graphene layer is a square graphene coating, the first graphene layer is located in a square of the second graphene layer, and the first graphene layer is not in direct contact with the second graphene layer.
6. The probe of claim 1, wherein the graphene layer and the diamond substrate are bonded as follows: the first graphene layer and the second graphene layer are arranged on one main surface of the diamond substrate, the first graphene layer and the second graphene layer are of an interdigital structure, the first graphene layer and the second graphene layer are arranged in a cross mode, and the first graphene layer and the second graphene layer are not in direct contact.
7. The probe of claim 1, wherein the housing has a pin therein, and wherein the housing and the graphene-diamond heterostructure are combined as follows: the first graphene layer of the graphene-diamond heterostructure is welded with the pins of the shell through welding wires or conductive adhesives, and the second graphene layer of the graphene-diamond heterostructure is welded with the inner bottom surface of the shell through the conductive adhesives or the welding wires.
8. The probe of claim 1, wherein the probe has one or more characteristics selected from the group consisting of:
1) after biasing, the dark current of the detector and the bias voltage are basically in a linear relation;
2) the detector has a 3.4 × 10 for X-rays-20~2.9×10-1Coulomb/gurley response sensitivity.
9. A method of manufacturing the graphene-diamond probe according to claim 1, wherein the method comprises the steps of:
i) providing a graphene-diamond heterostructure and a housing;
ii) encapsulating the graphene-diamond heterostructure with the housing, resulting in the graphene-diamond probe;
the graphene-diamond heterostructure is prepared as follows:
1) providing a coated diamond and an etching solution;
2) treating the coated diamond at a high temperature to obtain a treated coated diamond;
3) etching the treated coated diamond obtained in the step 2) by using the etching solution to obtain the graphene-diamond heterostructure;
during the high-temperature treatment, the pressure in the treatment cavity is 0.11-0.14 Torr;
the coated diamond comprises a diamond matrix and a metal dielectric film coated on the surface of the diamond matrix.
10. The method of claim 9,
during the high temperature treatment, the pressure in the process chamber was 0.11 Torr.
11. The method of claim 9, wherein the pressure in the process chamber is 0.12Torr during the high temperature processing.
12. The method as claimed in claim 9, wherein the treatment temperature of the high temperature treatment is 750-1200 ℃; and/or
The treatment time of the high-temperature treatment at the treatment temperature is 1-240 min.
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