Apparatus and method for depositing interfacial phase on fiber surface using solid precursor

By designing the low-temperature and high-temperature zones of the reactor and using gaseous precursors to process solid precursors, the deposition of interfacial phases on the fiber surface was achieved, solving the problem that existing technologies cannot process solid precursors and enabling the deposition of diverse thin film materials.

CN118147614BActive Publication Date: 2026-06-19NORTHWESTERN POLYTECHNICAL UNIV

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
NORTHWESTERN POLYTECHNICAL UNIV
Filing Date
2024-03-08
Publication Date
2026-06-19

AI Technical Summary

Technical Problem

Existing CVD equipment and methods cannot directly process solid precursors, resulting in the inability to deposit interfacial phases on fiber surfaces, thus failing to meet the high requirements of composite materials for interface control.

Method used

A reactor was designed, comprising a low-temperature zone and a high-temperature zone. A gaseous precursor is supplied by an inlet system, and the temperature of the chamber is heated and detected by a temperature control component. An outlet system discharges unreacted gas, thereby achieving interfacial phase deposition of the solid precursor on the fiber surface.

🎯Benefits of technology

It breaks through the limitations of traditional CVD devices on gaseous precursors, can process solid precursors, realize the deposition of diverse thin film materials, and meet the high requirements of composite materials for interface phases.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention relates to the field of chemical vapor deposition (CVD) technology, specifically disclosing an apparatus and method for depositing an interfacial phase on a fiber surface using a solid precursor. The apparatus provided by this invention includes an inlet system, a reactor, a temperature control component, a data detection system, and an outlet system. The reactor has two heating zones: the upper heating zone performs the CVD reaction, while the lower zone heats the solid precursor, converting it into a gaseous state. Compared to the gas delivery system and reaction chamber design used in traditional CVD equipment, this invention overcomes the limitation that the precursor in CVD processes is a gaseous compound or element, thus meeting the processing requirements for solid precursors. This invention has a wider range of applications and can perform the deposition of more diverse thin film materials.
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Description

Technical Field

[0001] This invention relates to the field of chemical vapor deposition technology, and in particular to an apparatus and method for depositing an interfacial phase on a fiber surface using a solid precursor. Background Technology

[0002] Chemical vapor deposition (CVD) is a common technique for preparing thin films, coatings, and interface phases on solid substrates or fiber surfaces. It involves converting chemical substances in a gaseous phase into solid substances through gas-phase reactions, forming a thin film on the object's surface. CVD is suitable for preparing conductors, semiconductors, and dielectric materials, such as silicon dioxide films, silicon nitride films, and polycrystalline silicon films. Especially in the preparation of interface phases on fiber surfaces, compared to other processes, CVD can create a more uniform coverage and a more consistent interface phase distribution, resulting in better uniformity and stability of the interface phase on the fiber surface. CVD plays a very important role in the field of fiber interface phase preparation and has broad application prospects and potential.

[0003] To date, most precursors for fiber surface interface phase preparation are gaseous compounds or elements. These gaseous precursors react directly inside the furnace, forming an interface phase on the fiber surface, such as a pyrolytic carbon interface. However, with the development of materials, especially the increasing application of composite materials, the requirements for interface control are gradually increasing. Interfaces require various properties such as oxidation resistance, high temperature resistance, and good thermal compatibility, leading to increasingly stringent requirements for the interface phase composition. This increased requirement for interface phase composition necessitates a wider range of precursor choices, particularly for interface phases with specific properties. However, some of these precursors exist in solid form under standard conditions. Traditional CVD devices and methods primarily consider the technology and processes for handling gaseous precursors in their gas delivery systems and reaction chambers. This results in limitations in current CVD devices and methods when handling solid precursors; that is, solid precursors cannot be directly deposited onto fiber surfaces using CVD devices and methods.

[0004] Therefore, in order to meet the processing requirements of fiber surface interface phase deposition using solid precursors, it is urgent to develop a new CVD device and method that enables solid precursors to meet the conditions required by the CVD process. Summary of the Invention

[0005] The purpose of this invention is to provide an apparatus and method for depositing an interfacial phase on a fiber surface using a solid precursor, so as to solve the problems existing in the prior art.

[0006] To achieve the above objectives, the present invention provides an apparatus for depositing an interfacial phase on a fiber surface using a solid precursor, comprising:

[0007] A reactor, wherein a cavity is provided inside the reactor, a low-temperature zone assembly for placing solid precursors is provided at the bottom of the cavity, and a high-temperature zone assembly for suspending samples is provided at the top of the cavity;

[0008] An air intake system is provided for supplying a gaseous precursor into the cavity, and the port of the air intake system located in the cavity is correspondingly disposed to the low-temperature zone component.

[0009] A temperature control component, which is used to increase the temperature inside the cavity and to detect the temperature inside the cavity;

[0010] A data detection system, wherein the temperature control component is electrically connected to the data detection system, and the data detection system is used to control the temperature inside the cavity and maintain the temperature inside the cavity stable;

[0011] A venting system for discharging gas from the cavity.

[0012] Preferably, the reactor includes a furnace body, and the cavity is disposed within the furnace body; both ends of the furnace body are provided with sealing covers, the sealing covers being divided into a top sealing cover and a bottom sealing cover, both the top sealing cover and the bottom sealing cover being detachably connected to the furnace body via flanges; the low-temperature zone assembly is mounted on the bottom sealing cover, and the high-temperature zone assembly is mounted on the top sealing cover.

[0013] Preferably, the low-temperature zone component includes:

[0014] A graphite column, wherein an air passage is provided inside the graphite column, the air passage being composed of a left air passage, a right air passage and a middle air passage, and the air intake system is connected to the bottom end of the air passage of the graphite column;

[0015] A graphite disk is fitted onto the top of the graphite column. A through hole adapted to the intermediate gas passage is opened in the middle of the graphite disk. The solid precursor is placed on the graphite disk. A protrusion is provided on the top edge of the graphite disk.

[0016] Preferably, the high-temperature zone assembly includes a hanging ring, the top end of which is detachably connected to the top sealing cap via a hook, and the sample is detachably mounted on the bottom end of the hanging ring, with the sample suspended in the heating zone of the cavity via the hanging ring.

[0017] Preferably, the furnace body and the cavity are filled with heat insulation cotton, and the low temperature zone component and the sample are provided with a heat insulation component. Both the heat insulation cotton and the heat insulation component are used to reduce the heat loss of the heating zone of the cavity.

[0018] Preferably, the heat insulation component includes a plurality of supports, which are fixedly installed at equal intervals along the circumference on the top of the low-temperature zone component. A mica column is fixedly installed on the top of the plurality of supports, and a plurality of heat insulation sheets are fixedly sleeved on the mica column. A gap is provided between the heat insulation sheets and the cavity, and a gap is provided between two adjacent heat insulation sheets. A plurality of holes are opened on the heat insulation sheets, and the holes on two adjacent heat insulation sheets are staggered.

[0019] Preferably, the temperature control component includes:

[0020] A resistance wire is wound around the lower outer wall of the cavity, and the resistance wire is used to heat the lower part of the cavity.

[0021] A silicon carbide rod is disposed between the furnace body and the cavity, and the silicon carbide rod is suspended on the top sealing cover. The silicon carbide rod is used to heat the upper part of the cavity.

[0022] Thermocouple, used to measure the temperature of the two heating zones, the resistance wire and the silicon carbide rod, within the cavity;

[0023] The resistance wire, the silicon carbide rod, and the thermocouple are all electrically connected to the data detection system.

[0024] Preferably, the intake system includes:

[0025] A gas cylinder, the gas cylinder being used to supply a gaseous precursor into the cavity;

[0026] An air inlet pipe is provided, through which the gas cylinder is connected to the bottom of the cavity. An air valve and a gas meter are installed on the air inlet pipe.

[0027] Preferably, the air outlet system includes:

[0028] An air outlet pipe is connected to the top of the cavity. A barometer and an air valve are installed on the air outlet pipe. The barometer is used to measure the air pressure inside the cavity.

[0029] A vacuum pump that discharges gas from the cavity through the outlet pipe;

[0030] A recovery device, which is connected to the cavity through the air outlet pipe, is used to restore the air pressure inside the cavity;

[0031] The air valves on the outlet pipe are configured one-to-one with the vacuum pump and the recovery equipment.

[0032] This invention also provides a method for preparing an interface phase on a fiber surface using chemical vapor deposition, specifically including the following steps:

[0033] S1. Place the solid precursor and sample into the cavity and seal the cavity and reactor.

[0034] S2. Vacuum treatment of the cavity is carried out using the exhaust system;

[0035] S3. The cavity is heated by the temperature control component, and the temperature inside the cavity is controlled by the data detection system to reach the set temperature.

[0036] S4. Turn on the air intake system to supply gaseous precursor into the cavity. The gaseous precursor drives the solid precursor to undergo a chemical reaction on the surface of the sample, thereby generating a solid interface phase. During the process, the unreacted gaseous precursor and the generated impurity gas are discharged through the air outlet system.

[0037] S5. After the reaction is complete, turn off the inlet system and wait for the chamber to cool naturally before turning off the outlet system to make the chamber equal in pressure to the external environment. Then, remove the sample.

[0038] Compared with the prior art, the present invention has the following advantages and technical effects:

[0039] The present invention provides an apparatus for depositing an interfacial phase on a fiber surface using a solid precursor. The reactor has two heating zones: the upper heating zone performs chemical vapor deposition, and the lower heating zone heats the solid precursor and converts it into a gaseous state. Compared with the pneumatic conveying system and reaction chamber design used in traditional CVD apparatuses, the present invention overcomes the limitation that the precursor in the CVD process is a gaseous compound or element, and can meet the processing requirements of solid precursors. The present invention has a wider range of applications and can perform more diverse thin film material deposition. Attached Figure Description

[0040] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0041] Figure 1 This is a schematic diagram of the structure of the present invention;

[0042] Figure 2 This is a schematic diagram of the reactor structure;

[0043] Figure 3 Top view of the graphite disk;

[0044] Figure 4 This is a top view of the high-temperature heating zone;

[0045] Figure 5 This is a schematic diagram of the three-dimensional structure of the heat insulation sheet;

[0046] In the diagram: 1. Inlet system; 10. Gas cylinder; 11. Gas valve; 12. Inlet pipe; 13. Gas meter; 2. Reactor; 20. Sealing cap; 200. Flange; 21. High-temperature zone assembly; 210. Hanging ring; 211. Sample; 22. Furnace body; 220. Insulation cotton; 23. Cavity; 230. Insulation sheet; 231. Mica column; 232. Support; 24. Low-temperature zone assembly; 240. Protrusion; 241. Graphite disk; 242. Graphite column; 3. Temperature control assembly; 30. Thermocouple; 31. Silicon carbide rod; 32. Resistance wire; 4. Data detection system; 5. Outlet system; 50. Outlet pipe; 51. Barometer; 52. Vacuum pump; 53. Recovery equipment. Detailed Implementation

[0047] It should be noted that, unless otherwise specified, the embodiments and features described in this invention can be combined with each other. The described embodiments are merely some, not all, of the embodiments of this invention. All other embodiments obtained by those skilled in the art without inventive effort are within the scope of protection of this invention. The invention will now be described in detail with reference to the accompanying drawings and embodiments.

[0048] This invention provides an apparatus for depositing an interfacial phase on a fiber surface using a solid precursor, comprising:

[0049] The reactor 2 has a cavity 23 inside. The bottom of the cavity 23 is provided with a low-temperature zone assembly 24 for placing a solid precursor. The solid precursor is a powder precursor. The top of the cavity 23 is provided with a high-temperature zone assembly 21 for suspending the sample 211.

[0050] The intake system 1 is used to supply gaseous precursors into the cavity 23. The port of the intake system 1 located in the cavity 23 is correspondingly set with the low temperature zone component 24.

[0051] Temperature control component 3 is used to increase the temperature inside the cavity 23 and to detect the temperature inside the cavity 23.

[0052] The data detection system 4 and the temperature control component 3 are electrically connected to the data detection system 4. The data detection system 4 is used to control the temperature inside the cavity 23 and keep the temperature inside the cavity 23 stable.

[0053] The gas exhaust system 5 is used to exhaust the gas inside the cavity 23.

[0054] Furthermore, the reactor 2 includes a furnace body 22, and a cavity 23 is disposed inside the furnace body 22; both ends of the furnace body 22 are provided with sealing covers 20, the sealing covers 20 are divided into a top sealing cover and a bottom sealing cover, and both the top sealing cover and the bottom sealing cover are detachably connected to the furnace body 22 through flanges 200; the low temperature zone assembly 24 is installed on the bottom sealing cover, and the high temperature zone assembly 21 is installed on the top sealing cover.

[0055] Furthermore, the low-temperature zone component 24 includes:

[0056] The graphite column 242 has an internal air passage consisting of a left air passage, a right air passage, and a middle air passage. The air intake system 1 is connected to the bottom of the air passage of the graphite column 242.

[0057] A graphite disk 241 is fitted onto the top of a graphite column 242. A through hole adapted to the intermediate gas passage is opened in the middle of the graphite disk 241. A solid precursor is placed on the graphite disk 241. A protrusion 240 is provided on the top edge of the graphite disk 241.

[0058] The graphite column 242 is fixedly connected to the bottom sealing cover. The graphite column 242 and graphite disk 241 are removed by taking out the bottom sealing cover, and then the powder precursor is replenished on the graphite disk 241. By setting multiple gas paths, the gaseous precursor can flow from bottom to top in the cavity 23, avoiding the retention of some gaseous precursor in the cavity 23, thereby ensuring the continuity of the reaction. The protrusion 240 can ensure that the powder precursor does not leak out in the environment of gaseous precursor flow in the cavity 23.

[0059] Furthermore, the high-temperature zone component 21 includes a hanging ring 210, the top of which is detachably connected to the top sealing cover via a hook, and the sample 211 is detachably mounted on the bottom of the hanging ring 210, with the sample 211 suspended in the heating zone of the cavity 23 via the hanging ring 210.

[0060] The uppermost end of the hanging ring 210 is movably connected to the top sealing cover via a hook, ensuring that the hanging ring 210 can be flexibly removed and installed. The hanging ring 210 suspends the sample 211 in the heating zone. The hanging ring 210 and the sample 211 can be removed by taking out the top sealing cover, thereby allowing the sample 211 to be reassembled.

[0061] Furthermore, heat insulation cotton 220 is filled between the furnace body 22 and the cavity 23, and a heat insulation component is provided between the low temperature zone component 24 and the sample 211. Both the heat insulation cotton 220 and the heat insulation component are used to reduce the heat loss of the heating zone of the cavity 23.

[0062] Furthermore, the heat insulation component includes several supports 232, which are fixedly installed at equal intervals along the circumference on the top of the protrusion 240. A mica column 231 is fixedly installed on the top of the supports 232, and several heat insulation sheets 230 are fixedly sleeved on the mica column 231. There is a gap between the heat insulation sheet 230 and the cavity 23, and there is a gap between two adjacent heat insulation sheets 230. Several holes are opened on the heat insulation sheet 230, and the holes on two adjacent heat insulation sheets 230 are staggered.

[0063] The heat insulation sheets 230 are connected in series via mica pillars 231. Four supports 232 are built below the mica pillars 231 and then fixed to the protrusions 240. The heat insulation sheets 230 are installed in the middle of the cavity 23 and are spaced a certain distance from the cavity 23 to prevent the heat insulation sheets 230 from expanding thermally and colliding with the cavity 23 when the temperature rises. The heat insulation sheets 230 can reduce heat transfer between high-temperature and low-temperature areas. The heat insulation sheets 230 have multiple through holes, and the positions of the through holes of adjacent heat insulation sheets 230 are different. This can ensure that the gaseous precursors can pass smoothly through the heat insulation sheets 230, while different gaseous precursors are fully mixed within the gaps of the heat insulation sheets 230, thereby ensuring the fullness of the chemical reaction of the gaseous precursors.

[0064] Furthermore, the temperature control component 3 includes:

[0065] Resistance wire 32 is wound around the lower outer wall of cavity 23 and is used to heat the lower part of cavity 23.

[0066] Silicon carbide rod 31 is disposed between furnace body 22 and cavity 23 and suspended on top sealing cover. Silicon carbide rod 31 is used to heat the upper part of cavity 23.

[0067] Thermocouple 30 is used to measure the temperature of the two heating zones, resistance wire 32 and silicon carbide rod 31, inside cavity 23.

[0068] Resistance wire 32, silicon carbide rod 31, and thermocouple 30 are all electrically connected to data detection system 4.

[0069] The resistance wire 32 and silicon carbide rod 31 are separated from the cavity 23 by a certain distance to prevent the current in the resistance wire 32 and silicon carbide rod 31 from entering the cavity 23; the thermocouple 30 detects the temperature of the heating zone and transmits the relevant information to the data detection system 4. After processing the relevant information, the data detection system 4 generates heat by supplying current to the resistance wire 32 and silicon carbide rod 31, thereby achieving the effect of controlling the temperature of the two heating zones.

[0070] Furthermore, the intake system 1 includes:

[0071] Gas cylinder 10 is used to supply gaseous precursors into cavity 23;

[0072] The air inlet pipe 12 connects the gas cylinder 10 to the bottom of the cavity 23. An air valve 11 and a gas meter 13 are installed on the air inlet pipe 12.

[0073] Furthermore, the exhaust system 5 includes:

[0074] An air outlet pipe 50 is connected to the top of the cavity 23. A barometer 51 and an air valve 11 are installed on the air outlet pipe 50. The barometer 51 is used to measure the air pressure inside the cavity 23.

[0075] Vacuum pump 52, the vacuum pump 52 discharges the gas in cavity 23 through gas outlet pipe 50;

[0076] The recovery device 53 is connected to the cavity 23 through the air outlet pipe 50. The recovery device 53 is used to restore the air pressure in the cavity 23.

[0077] The gas valve 11 on the gas outlet pipe 50 is set one-to-one with the vacuum pump 52 and the recovery device 53 to ensure that the gaseous precursor does not flow back in the gas path when the vacuum pump 52 and the recovery device 53 stop running.

[0078] This invention also provides a method for preparing an interface phase on a fiber surface using chemical vapor deposition, specifically including the following steps:

[0079] S1. Place the solid precursor and sample 211 into the cavity 23, and seal the cavity 23 and the reaction furnace 2.

[0080] Remove the bottom sealing cap located at the bottom of cavity 23. The graphite column 242 fixed to the bottom sealing cap is removed together with it. Add an appropriate amount of powder precursor to the graphite disk 241 that is sleeved with the graphite column 242. Then restore the bottom sealing cap to the bottom of cavity 23. Remove the top sealing cap located at the top of cavity 23. Connect the sample 211 to the hanging ring 210. The hanging ring 210 is connected to the top sealing cap through a hook. Then restore the top sealing cap to the bottom of cavity 23.

[0081] S2. Vacuum treatment of cavity 23 is performed using the venting system 5.

[0082] Turn on the vacuum pump 52 and related gas valves 11 to evacuate the gaseous precursor in the cavity 23, observe the barometer 51, and reduce the gas pressure to approximately -0.1 MPa.

[0083] S3. The temperature control component 3 heats the inside of the cavity 23 and the data detection system 4 controls the temperature inside the cavity 23 to reach the set temperature.

[0084] The data detection system 4 controls the temperature control component 3. The temperature control component 3 uses silicon carbide rod 31 and resistance wire 32 to raise the temperature of the two heating zones. The temperature information measured by thermocouple 30 is returned to the data detection system 4. The data detection system 4 processes the relevant information and responds, and finally reaches the set temperature and keeps it warm.

[0085] S4. Turn on the air intake system 1 to supply gaseous precursor into the cavity 23. The gaseous precursor drives the solid precursor to undergo a chemical reaction on the surface of the sample 211 to generate a solid interface phase. During the process, the unreacted gaseous precursor and the generated impurity gas are discharged through the air outlet system 5.

[0086] Open the gas cylinder 10 and related gas valves 11, and control the gas flow rate by adjusting the gas meter 13. The gaseous precursor enters the cavity 23 in three paths from the inlet pipe 12, so that the gaseous precursor rises stably from the lower part of the cavity 23 to the upper part of the cavity 23, avoiding backflow of the gaseous precursor in the cavity 23. When the gaseous precursor passes through the heat insulation sheet 230, the different positions of the through holes of the adjacent heat insulation sheets 230 ensure that the gaseous precursor passes through the heat insulation sheet 230 smoothly, while also ensuring that different gaseous precursors are fully mixed within the gaps of the heat insulation sheet 230, thereby ensuring the sufficiency of the chemical reaction of the gaseous precursor. When the gaseous precursor flows to the high temperature zone, it will undergo a chemical reaction on the surface of the sample 211 to generate a solid interface phase. The unreacted gaseous precursor and the generated impurity gas are discharged to the outside of the device through the outlet pipe 50 in the outlet system 5. The vacuum pump 52 runs continuously throughout the process to ensure the accuracy of the gas flow direction.

[0087] S5. After the reaction is complete, shut off the inlet system 1. After the chamber 23 has cooled naturally, shut off the outlet system 5 to make the chamber 23 equal in pressure to the external environment. Then take out the sample 211.

[0088] After the device has finished operating, close the gas cylinder 10 and related gas valves 11. After the temperature of the heating zone drops to a suitable range, close the vacuum pump 52 and related gas valves 11, open the recovery device and related gas valves 11, so that the pressure inside the cavity 23 is equal to that of the external environment. Remove the top sealing cover located on the upper part of the cavity 23, take out the sample 211, and the test is completed.

[0089] The above are merely preferred embodiments of this application, but the scope of protection of this application is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in this application should be included within the scope of protection of this application. Therefore, the scope of protection of this application should be determined by the scope of the claims.

Claims

1. An apparatus for depositing an interfacial phase on a fiber surface using a solid precursor, characterized in that, include: The reactor (2) has a cavity (23) inside. The bottom of the cavity (23) is provided with a low-temperature zone assembly (24) for placing solid precursors, and the top of the cavity (23) is provided with a high-temperature zone assembly (21) for suspending samples (211). An air intake system (1) is used to supply gaseous precursors into the cavity (23). The port of the air intake system (1) located in the cavity (23) is correspondingly arranged with the low temperature zone component (24). Temperature control component (3), the temperature control component (3) is used to increase the temperature inside the cavity (23) and detect the temperature inside the cavity (23); The data detection system (4) is electrically connected to the temperature control component (3). The data detection system (4) is used to control the temperature inside the cavity (23) and keep the temperature inside the cavity (23) stable. An exhaust system (5) is provided for discharging gas from the cavity (23); The low-temperature zone component (24) includes: A graphite column (242) is provided with an air passage inside the graphite column (242), and the air intake system (1) is connected to the bottom end of the air passage of the graphite column (242); A graphite disk (241) is fitted onto the top of the graphite column (242). A through hole adapted to the gas passage is opened in the middle of the graphite disk (241). The solid precursor is placed on the graphite disk (241). A heat insulation component is provided between the low-temperature zone component (24) and the sample (211). The heat insulation component includes a support (232). A mica column (231) is fixedly installed on the top of the support (232). A plurality of heat insulation sheets (230) are fixedly sleeved on the mica column (231). A gap is provided between the heat insulation sheet (230) and the cavity (23), and a gap is provided between two adjacent heat insulation sheets (230). A plurality of holes are opened on the heat insulation sheet (230), and the holes on two adjacent heat insulation sheets (230) are staggered.

2. The apparatus for depositing an interfacial phase on a fiber surface from a solid precursor of claim 1, wherein, The reactor (2) includes a furnace body (22), and the cavity (23) is disposed inside the furnace body (22). Both ends of the furnace body (22) are provided with sealing covers (20). The sealing covers (20) are divided into a top sealing cover and a bottom sealing cover. The top sealing cover and the bottom sealing cover are detachably connected to the furnace body (22) through flanges (200). The low temperature zone component (24) is installed on the bottom sealing cover, and the high temperature zone component (21) is installed on the top sealing cover.

3. The apparatus for depositing an interfacial phase on a fiber surface using a solid precursor according to claim 2, characterized in that, The gas passage consists of a left gas passage, a right gas passage and a middle gas passage. The through hole in the middle of the graphite disk (241) is adapted to the middle gas passage. The top edge of the graphite disk (241) is provided with a protrusion (240).

4. The apparatus for depositing an interfacial phase on a fiber surface using a solid precursor according to claim 2, characterized in that, The high-temperature zone component (21) includes a hanging ring (210), the top of which is detachably connected to the top sealing cover via a hook. The sample (211) is detachably installed at the bottom of the hanging ring (210), and the sample (211) is suspended in the heating zone of the cavity (23) via the hanging ring (210).

5. The apparatus for depositing an interfacial phase on a fiber surface using a solid precursor according to claim 4, characterized in that, The furnace body (22) and the cavity (23) are filled with heat insulation cotton (220), and both the heat insulation cotton (220) and the heat insulation component are used to reduce the heat loss of the heating zone of the cavity (23).

6. The apparatus for depositing an interfacial phase on a fiber surface using a solid precursor according to claim 5, characterized in that, The support (232) is fixedly installed on the top of the low-temperature zone assembly (24) at equal intervals along the circumference.

7. The apparatus for depositing an interfacial phase on a fiber surface using a solid precursor according to claim 2, characterized in that, The temperature control component (3) includes: A resistance wire (32) is wound around the lower outer wall of the cavity (23) and is used to heat the lower part of the cavity (23). Silicon carbide rod (31), the silicon carbide rod (31) is disposed between the furnace body (22) and the cavity (23), and the silicon carbide rod (31) is suspended on the top sealing cover, the silicon carbide rod (31) is used to heat the upper part of the cavity (23); Thermocouple (30) is used to measure the temperature of the two heating zones of the resistance wire (32) and the silicon carbide rod (31) inside the cavity (23); The resistance wire (32), the silicon carbide rod (31), and the thermocouple (30) are all electrically connected to the data detection system (4).

8. The apparatus for depositing an interfacial phase on a fiber surface using a solid precursor according to claim 1, characterized in that, The intake system (1) includes: Gas cylinder (10), the gas cylinder (10) is used to supply gaseous precursor into the cavity (23); An air inlet pipe (12) is provided, through which the gas cylinder (10) is connected to the bottom of the cavity (23). An air valve (11) and a gas meter (13) are installed on the air inlet pipe (12).

9. The apparatus for depositing an interfacial phase on a fiber surface using a solid precursor according to claim 1, characterized in that, The air outlet system (5) includes: An air outlet pipe (50) is connected to the top of the cavity (23). A barometer (51) and an air valve (11) are installed on the air outlet pipe (50). The barometer (51) is used to measure the air pressure inside the cavity (23). A vacuum pump (52) discharges gas from the cavity (23) through the outlet pipe (50); The recovery device (53) is connected to the cavity (23) through the air outlet pipe (50), and the recovery device (53) is used to restore the air pressure in the cavity (23); The air valve (11) on the air outlet pipe (50) is set in a one-to-one correspondence with the vacuum pump (52) and the recovery device (53).

10. A method for preparing an interface phase on a fiber surface using chemical vapor deposition, characterized in that, The apparatus for depositing an interfacial phase on a fiber surface using a solid precursor, as described in any one of claims 1-9, specifically includes the following steps: S1. Place the solid precursor and sample (211) into the cavity (23) and seal the cavity (23) and the reactor (2); S2. Vacuum treatment of cavity (23) is performed using the exhaust system (5); S3. The cavity (23) is heated by the temperature control component (3), and the temperature inside the cavity (23) is controlled to reach the set temperature by the data detection system (4). S4. Turn on the air intake system (1) and supply gaseous precursor into the cavity (23). The gaseous precursor drives the solid precursor and reacts chemically on the surface of the sample (211) to generate a solid interface phase. During the process, the unreacted gaseous precursor and the generated impurity gas are discharged through the air outlet system (5). S5. After the reaction is complete, shut off the inlet system (1), and after the cavity (23) has cooled naturally, shut off the outlet system (5) to make the cavity (23) equal to the external environment and take out the sample (211).

Citation Information

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