阅读说明：本技术 一种燃料电池极板金属碳化物涂层的四腔体沉积系统 (Four-cavity deposition system for metal carbide coating of fuel cell pole plate ) 是由 毕飞飞 黎焕明 姜天豪 蓝树槐 彭林法 于 2019-09-30 设计创作，主要内容包括：一种燃料电池极板金属碳化物涂层的四腔体沉积系统,主要包括：依次为进片腔室、过渡层沉积腔室、金属碳化物层沉积腔室和出片腔室；各个腔室的进出口均设有腔室阀门,腔室阀门将两侧的腔室相互隔开；样品传动装置穿过各个腔室内的底部,形成一条闭合回路；样品架设在样品传动装置上,带着样品从左至右依次穿过各个腔室。本发明采用非平衡磁场和平衡磁场的结合,对磁场方式,电源系统和靶基距的匹配优化,提高了金属碳化物涂层的结合性能和稳定性能；采用连续化的小型沉积设备,引入机械手等自动化设备实现对金属碳化物涂层的快速沉积,可降低涂层制备成本。(A four-chamber deposition system for a fuel cell plate metal carbide coating, consisting essentially of: the device comprises a wafer inlet chamber, a transition layer deposition chamber, a metal carbide layer deposition chamber and a wafer outlet chamber in sequence; the inlet and outlet of each chamber are provided with chamber valves which separate the chambers on the two sides from each other; the sample transmission device penetrates through the bottom of each chamber to form a closed loop; the sample is mounted on a sample actuator which carries the sample through the chambers in sequence from left to right. The invention adopts the combination of the unbalanced magnetic field and the balanced magnetic field, optimizes the matching of the magnetic field mode, the power supply system and the target base distance, and improves the combination property and the stability of the metal carbide coating; the continuous small-sized deposition equipment is adopted, and automatic equipment such as a mechanical arm and the like is introduced to realize the rapid deposition of the metal carbide coating, so that the preparation cost of the coating can be reduced.)

1. A four-chamber deposition system for a fuel cell plate metal carbide coating, comprising: the device comprises a wafer inlet chamber (1), a transition layer deposition chamber (2), a metal carbide layer deposition chamber (3) and a wafer outlet chamber (4) in sequence; the inlet and the outlet of each chamber are provided with chamber valves (5) to separate the chambers on the two sides from each other; the sample transmission device (8) penetrates through the bottom of each chamber to form a closed loop; the sample frame (6) is arranged on the sample transmission device (8) and drives the sample (7) to sequentially pass through the chambers from left to right, and the preparation of the coating is finished.

2. The four-cavity deposition system according to claim 1, wherein the wafer inlet chamber (1), the transition layer deposition chamber (2), the metal carbide layer deposition chamber (3) and the wafer outlet chamber (4) are respectively provided with an independent vacuum system, a power supply system and a gas path system.

3. The four-chamber deposition system according to claim 1, wherein 2-20 fuel cell plates can be hung on the sample holder (6).

4. The four-chamber deposition system according to claim 1, wherein a number of heating devices (12) are symmetrically and uniformly arranged on both side wall surfaces of the transition layer deposition chamber (2) and the metal carbide layer deposition chamber (3), respectively.

5. The four-chamber deposition system according to claim 1, wherein a cathode magnetic field (13) is provided on both side walls in the transition layer deposition chamber (2) and the metal carbide layer deposition chamber (3), respectively, spaced from the heating device (12).

6. The four-chamber deposition system according to claim 5, wherein the cathode magnetic field (13) is provided by 5-9 magnets.

7. The four-cavity deposition system according to claim 1, wherein the surface of the cathode magnetic field (13) of the transition layer deposition chamber (2) is provided with a plurality of metal target positions (9) side by side, and magnetic lines of force on each metal target position (9) are closed to each other to form an unbalanced closed magnetic field.

8. The four-chamber deposition system according to claim 7, wherein the number of metal target sites (9) is 1-5, and the distance between two symmetrical target sites is 2-30 cm.

9. the four-chamber deposition system according to claim 7, wherein each metal target (9) is mounted with a pure metal target, which is one of the transition metals.

10. The four-chamber deposition system according to claim 1, wherein the surface of the cathode magnetic field (13) of the metal carbide layer deposition chamber (3) is provided with a plurality of carbide target sites (10) side by side, and the magnetic field at each target site is a balanced magnetic field.

11. The four-chamber deposition system according to claim 10, wherein the number of carbide target sites (10) is 1-5 and the distance between bilaterally symmetrical target sites is 2-20 cm.

12. the four-chamber deposition system according to claim 10, wherein each carbide target (10) is mounted with a pure metal target, a metal carbide target or a multi-component silicon carbon ceramic target; the pure metal target material is one of transition metals, the metal carbide target material is one of transition metal carbides, and the multi-element silicon-carbon ceramic target material is one of transition metals and compounds formed by multiple elements of silicon and carbon.

13. The four-chamber deposition system according to claim 10, wherein the target of the carbide target (10) is a metal carbide target.

14. A four-chamber deposition system according to claim 7 or 10, wherein reducing gas venting tubes (11) are provided on both sides of the metal target site (9) and the carbide target site (10).

Technical Field

The invention belongs to the technical field of fuel cells, and relates to a four-cavity deposition system for a metal carbide coating of a fuel cell polar plate.

background

With the continuous development of society, the reserves of fossil energy such as coal and petroleum are limited, and the bad influence is generated on the ecological environment, so that clean and renewable energy sources are widely applied and are greatly regarded. Among them, the Fuel Cell has been paid attention to by many organizations and people as a power generation device directly generating electric energy through electrochemical reaction, and a Proton Exchange Membrane Fuel Cell (PEMFC for short) using hydrogen as Fuel is widely used, and the application range includes automobiles, unmanned aerial vehicles, stationary power stations, and the like. In addition, in the operation process of the fuel cell, the working temperature of the polar plate can reach 65-85 ℃, and the polar plate is in an acid solution environment with pH =3, has a certain potential, and the potential varies from 0.6-1.6V. Continued operation in this environment without any treatment of the metal plates can result in severe electrochemical corrosion, which can lead to degradation of fuel cell performance and reduced life. The conductivity and corrosion resistance of the fuel cell plate are further improved by carrying out corresponding surface modification on the plate, such as deposition of a coating. In a fuel cell stack, tens of plates and membrane electrodes are stacked together, which also puts higher demands on the consistency and uniformity of the plates to meet the lifetime requirements of thousands of hours of fuel cells.

At present, four types of coatings are mainly used for surface treatment and modification of a fuel cell metal pole plate, namely a precious metal coating, a graphite coating, a conductive polymer coating and a metal ceramic coating. Although the noble metal coating and the graphite coating both have good chemical stability and good electrical conductivity, the noble metal coating is limited to material selection and has high material cost, and the graphite coating has high time cost due to too slow deposition rate, so that the high material cost and time cost are not favorable for large-scale mass production. The chemical properties of the conductive polymer coating are not very stable, and the mechanical properties and bonding properties of the material itself limit its wide application.

For the metal ceramic coating, particularly the metal carbide coating has extremely excellent conductivity and corrosion resistance, and meanwhile, the metal carbide coating has the characteristics of high deposition rate, low production cost and the like, so that the metal carbide coating is widely applied in the actual production process. The carbon atoms and the metal atoms in the metal carbide coating form crystals through strong chemical bonds so as to have high conductivity, but a small amount of metal simple substances still exist in the metal carbide coating under the influence of a deposition environment and a deposition process, and the metal simple substances escape in the service process of the polar plate to cause the reduction of the performance and the service life of the coating.

At present, most of the preparation of the metal carbide coating is focused on the research of monomer equipment, the production efficiency of the monomer equipment is far lower than that of continuous equipment, adjustable parameters are limited, and the preparation of the metal carbide coating is not beneficial to large-batch production. Meanwhile, the conductivity of the metal carbide coating is greatly improved compared with that of a graphite coating and a precious metal coating, so that the formation of metal carbide crystals can be effectively promoted by introducing hydrogen into the deposition process to etch the coating, conductive particles are exposed on the surface of the coating, and the conductivity and the corrosion resistance of the coating are further improved.

Disclosure of Invention

It is an object of the present invention to provide a four-chamber deposition system for metal carbide coatings on fuel cell plates that overcomes the above-mentioned problems of the prior art.

A four-chamber deposition system for a fuel cell plate metal carbide coating, comprising: the device comprises a wafer inlet chamber, a transition layer deposition chamber, a metal carbide layer deposition chamber and a wafer outlet chamber in sequence; the inlet and the outlet of each chamber are provided with chamber valves which separate the chambers on the two sides from each other; the sample transmission device penetrates through the bottom of each chamber to form a closed loop; the sample rack is arranged on the sample transmission device and carries the sample to pass through each chamber from left to right in sequence.

Furthermore, the four-cavity deposition system for the metal carbide coating of the fuel cell pole plate is also provided with an independent vacuum system, a power supply system and an independent gas circuit system in the plate inlet cavity, the transition layer deposition cavity, the metal carbide layer deposition cavity and the plate outlet cavity.

The sample rack can hang 2-20 fuel cell polar plates, and a mechanical arm or other similar automatic devices are adopted to complete the feeding and discharging process of the fuel cell polar plates.

The wafer feeding chamber is used for exhausting air and cleaning a sample, the cleaning mode comprises radio frequency self-bias cleaning, pulse bias cleaning and cleaning of ion sources symmetrically arranged on two sides of the chamber, and meanwhile, hydrogen is introduced into the chamber to etch the oxide on the surface of the sample.

Furthermore, the hydrogen flow rate used in the etching treatment is 5-500 sccm.

A certain number of heating devices are symmetrically and uniformly arranged on two side wall surfaces of the transition layer deposition chamber and the metal carbide layer deposition chamber respectively and used for heating a sample; the deposition temperature of the transition layer deposition chamber is 0-700 ℃, and the deposition temperature of the metal carbide layer deposition chamber is 0-1000 ℃.

Furthermore, cathode magnetic fields are respectively arranged on two side wall surfaces in the transition layer deposition chamber and the metal carbide layer deposition chamber and are arranged at intervals with the heating device; the cathode magnetic field adopts 5-9 magnets, preferably 7 magnets, so as to improve the utilization rate of the target material.

a plurality of metal target positions are arranged on the surface of a cathode magnetic field of the transition layer deposition chamber side by side, and magnetic lines of force on each target position are mutually closed to form an unbalanced closed magnetic field.

Further, the number of the metal target positions is 1-3, and the distance between the symmetrical target positions on the two sides is 2-30 cm, preferably 5-20 cm.

Furthermore, each metal target is provided with a pure metal target, and the pure metal target comprises one of transition metals such as titanium, chromium, niobium, zirconium and the like and is used for depositing a metal transition layer.

The power supply connected with the target position of the transition layer deposition chamber adopts a mode of mutually coupling a high-power pulse magnetron sputtering power supply and a direct-current sputtering power supply, and the high-power pulse magnetron sputtering power supply and the direct-current sputtering power supply are connected through a power matcher, so that the bonding performance and compactness of the transition layer are effectively improved.

The surface of the cathode magnetic field of the metal carbide layer deposition chamber is provided with a plurality of carbide target positions side by side, and the magnetic field on each carbide target position is a balanced magnetic field.

Furthermore, each carbide target position is provided with a pure metal target material, a metal carbide target material or a multi-element silicon carbon ceramic target material; the pure metal target is one of transition metals such as titanium, chromium, niobium, zirconium and the like, the metal carbide target is one of carbides of transition metals such as titanium carbide, chromium carbide, niobium carbide, zirconium carbide and the like, and the multi-element silicon-carbon ceramic target is one of compounds formed by transition metals and multiple elements such as silicon and carbon, for example: titanium silicon carbon, chromium silicon carbon.

Furthermore, the number of the carbide target positions is 1-3, and the distance between the symmetrical target positions on two sides is 2-20 cm, preferably 2-10 cm.

The power supply connected with the target position of the metal carbide layer deposition chamber is a direct current sputtering power supply or a pulse sputtering power supply; when the target material of the target position is a metal carbide target material or a multi-element silicon carbon ceramic target material, the target material can be directly sputtered to complete the preparation of the metal carbide layer; and when the target material of the target position is a pure metal target material, performing reactive sputtering on the pure metal target material by adopting a carbon source gas to complete the preparation of the metal carbide layer.

Further, when a pure metal target is reactively sputtered with a carbon source gas, the carbon source gas includes one of carbon-containing organic gases such as methane, acetylene, benzene, pyridine, and the like.

Furthermore, reducing gas breather pipes are arranged on two sides of the target material position in the metal carbide layer deposition chamber; the reducing gas is hydrogen to promote the formation of metal carbide crystals and improve the conductivity and corrosion performance of the metal carbide coating.

Further, the hydrogen flow rate is controlled to be 2 to 500sccm, preferably 5 to 20 sccm.

Compared with the prior art, the invention has the following characteristics:

(1) The combination of the unbalanced magnetic field and the balanced magnetic field is adopted, the matching optimization of the magnetic field mode, the power supply system and the target base distance is carried out, and the combination performance and the stability of the metal carbide coating are further improved;

(2) Reducing gas hydrogen is introduced in the deposition process of the metal carbide coating to promote the formation of metal carbide crystals and improve the conductivity and corrosion performance of the coating;

(3) The continuous small-sized deposition equipment is adopted, and automatic equipment such as a mechanical arm and the like is introduced to realize the rapid deposition of the metal carbide coating, so that the preparation cost of the coating can be reduced.

Drawings

FIG. 1 is a schematic diagram of a metal carbide coating four-chamber deposition system according to the present invention;

FIG. 2 is a schematic diagram of a power supply and magnetic field for a transition layer deposition chamber;

FIG. 3 is a schematic diagram of a power supply and magnetic field for a metal carbide deposition chamber;

FIG. 4 is a schematic diagram of the output current of the power supply of the deposition chamber for the transition layer;

the notation in the figure is: 1-a chip inlet chamber, 2-a transition layer deposition chamber, 3-a metal carbide layer deposition chamber, 4-a chip outlet chamber, 5-a chamber valve, 6-a sample frame, 7-a sample, 8-a sample transmission device, 9-a metal target position, 10-a carbide target position, 11-a breather pipe, 12-a heating device and 13-a cathode magnetic field.

Detailed Description

The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.