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CN-122013323-A - Preparation method and application of doped graphite

CN122013323ACN 122013323 ACN122013323 ACN 122013323ACN-122013323-A

Abstract

The invention discloses a preparation method and application of doped graphite, and belongs to the technical field of doped graphite. The method comprises the steps of vacuum annealing a monocrystalline metal substrate adsorbed with a doping element compound to obtain a monocrystalline metal substrate embedded with the doping element, bonding the monocrystalline metal substrate embedded with the doping element with a graphite base material, preserving heat for 1-3h at 1000-1500 ℃ in a non-oxidizing atmosphere, preserving heat for 4-12h at 700-900 ℃ and cooling to obtain the doped graphite. According to the invention, the doping elements are embedded into the monocrystalline metal substrate, the doped graphite is grown at a variable temperature, so that the doping uniformity and controllability are ensured, and meanwhile, the ultra-slip performance is maintained, and the method is more suitable for being applied to electronic devices needing to maintain the ultra-slip characteristic.

Inventors

  • CHEN YUNXIAN
  • MIAO RUI
  • Request for anonymity
  • HAN YU
  • XIANG XIAOJIAN
  • PAN XUJIE
  • TANG MINGJIE
  • NIE JINHUI

Assignees

  • 深圳清力技术有限公司
  • 深圳清华大学研究院

Dates

Publication Date
20260512
Application Date
20251128

Claims (10)

  1. 1. The preparation method of the doped graphite is characterized by comprising the following steps of: (1) Vacuum annealing the monocrystalline metal substrate adsorbed with the doping element compound to obtain a monocrystalline metal substrate embedded with the doping element; (2) And (3) attaching the monocrystalline metal substrate embedded with the doping element to a graphite base material, preserving heat for 1-3 hours at 1000-1500 ℃ in a non-oxidizing atmosphere, preserving heat for 4-12 hours at 700-900 ℃, and cooling to obtain the doped graphite.
  2. 2. The method of claim 1, wherein the material of the single crystal metal substrate in step (1) is one of single crystal nickel, single crystal iron, single crystal cobalt, single crystal platinum, single crystal palladium, single crystal nickel-based alloy, single crystal iron-based alloy, single crystal cobalt-based alloy; The graphite base material in the step (1) is graphite paper; The doping element compound in the step (1) is a nitrogen-containing compound which can be decomposed by vacuum annealing, or the doping element compound in the step (1) is one or more of melamine, urea and dicyandiamide.
  3. 3. The method of manufacturing a single crystal metal substrate having a dopant element compound adsorbed thereto according to claim 1, wherein the method of manufacturing a single crystal metal substrate having a dopant element compound adsorbed thereto according to step (1) comprises immersing the single crystal metal substrate in a solution of the dopant element compound, taking out and drying the single crystal metal substrate to obtain the single crystal metal substrate having the dopant element compound adsorbed thereto.
  4. 4. A method of preparation according to claim 3, wherein the soaking time is 3-20 minutes; the concentration of the solution of the doping element compound is 0.1-1 mg/ml.
  5. 5. The method of claim 1, wherein the vacuum annealing in step (1) is performed at a temperature of 1000-1500 ℃ for a period of 3-10 minutes.
  6. 6. The method of claim 1, wherein the non-oxidizing atmosphere of step (2) is a non-oxidizing gas stream; the non-oxidizing atmosphere in the step (2) is a reducing atmosphere; The reducing atmosphere is a mixed gas of inert gas and hydrogen; The volume ratio of the inert gas to the hydrogen is 10 (0.1-3).
  7. 7. The method according to claim 1, wherein the graphite-doped single-crystal metal substrate obtained in step (2) is peeled off; The method for stripping the graphite-doped monocrystalline metal substrate comprises etching and stripping with ferric chloride solution; The method for stripping the doped graphite single crystal metal substrate comprises the steps of immersing the doped graphite obtained in the step (2) in ferric trichloride solution, taking out to remove nickel plates, washing and drying to obtain the doped graphite for stripping the single crystal metal substrate.
  8. 8. The method according to claim 7, wherein the concentration of the ferric trichloride solution is 0.01 to 0.2 mg/ml; The soaking time is 12-72h; And (3) attaching the graphite surface of the doped graphite obtained in the step (2) to a silicon wafer or a glass sheet, and then soaking the silicon wafer or the glass sheet in a ferric trichloride solution.
  9. 9. Doped graphite prepared by the method of any one of claims 1-8.
  10. 10. Use of the doped graphite of claim 9 for the preparation of an ultra-smooth micro-electric generator, an ultra-smooth relay or a nano-switch.

Description

Preparation method and application of doped graphite Technical Field The invention belongs to the technical field of doped graphite, and particularly relates to a preparation method and application of doped graphite. Background The graphite is formed by stacking sp 2 hybridized carbon atom layers through Van der Waals force, and when two atomically smooth graphite surfaces are stacked at a certain rotation angle, the interface of the two atomically smooth graphite surfaces can realize a structure super-slip state with near zero friction and zero abrasion. The structural super-slip interface is typically dominated by van der Waals forces (vdW) and is in a non-metric contact state (as shown in FIG. 32). The advent and development of structural ultra-slip provides a revolutionary solution to the friction and wear problems in the fields of microelectromechanical systems, precision manufacturing, etc., and prototype devices such as micro-generators, electrostatic drives, etc., developed based on this feature have demonstrated breakthrough performance in recent years. The graphite is used as a base material of the structural super-slip technology, and has important significance for improving the performance of related devices based on the structural super-slip through regulating and controlling the electrical performance of the structural super-slip technology. For example, a semiconductor direct current micro generator based on the structure super-slip technology is composed of graphite and semiconductor materials. After the two materials are contacted, a depletion layer is formed between the materials in order to establish electrostatic balance due to the difference of work functions. When the two materials slide relatively, unbalanced electric fields are generated by the establishment and destruction of the depletion layer, and electrons are driven to drift and form direct current. The application of the ultra-smooth structure effectively solves the service life problem of the micro-generator caused by friction and abrasion in the mechanical energy collection process. However, although the output current density can reach about 21mA/cm 2 and the output power density is about 0.7mW/cm 2, the power supply requirement of the low-power micro-nano electronic device can not be met. In order to solve the problem, impurity atoms are continuously introduced in the growth process of graphite to obtain doped graphite so as to form substitutional doping to change an electronic structure between graphite layers, and then a built-in electric field between work function control materials is adjusted to improve the power generation efficiency. The electromechanical conversion efficiency of the semiconductor direct-current micro-generator based on the structure super-slip is effectively improved, and the practical process of the micro-generator in the application field is promoted. Opens up new research directions and technical approaches for the research of the performance improvement of related electronic devices based on the structural super-slip. The existing preparation methods of doped graphite mainly comprise ion implantation, plasma treatment, gas phase chemical doping, liquid phase stripping-recombination method and the like, but have the following problems. Ion implantation or plasma treatment, doping atoms can be introduced into the graphite layer, but a large number of defects and lattice damage are often caused, and the interlayer super-slip characteristic is destroyed. Gas phase chemical doping by introducing gaseous doping precursors (e.g., ammonia, diborane) in a CVD atmosphere. However, this method is difficult to ensure doping uniformity, and has a limited doping depth, which is difficult to be applied to a multi-layered graphite structure. According to the liquid phase stripping-recombination method, recombination of the graphite or graphene layer is realized through liquid phase doping, but the process is complex, the doping position is uncontrollable, and the requirement of device-level application is difficult to meet. Therefore, there is a need for a method of preparing doped graphite that is uniformly doped, controllable, and avoids damage to the graphite lattice. Disclosure of Invention In order to overcome the defects in the prior art, the invention provides a preparation method and application of doped graphite. The method adopts an embedded pretreatment and growth synchronous doping mode, ensures doping uniformity and controllability, avoids damaging graphite lattices, and is more suitable for being applied to electronic devices needing to keep super-slip characteristics. The technical scheme adopted for solving the technical problems is as follows: The invention provides a preparation method of doped graphite, which comprises the following steps: (1) Vacuum annealing the monocrystalline metal substrate adsorbed with the doping element compound to obtain a monocrystalline metal substrate embedded wi