CN111926288B - Lanthanum hexaboride composite carbon film on surface of valve sealing body and high-binding-force deposition method thereof - Google Patents
Lanthanum hexaboride composite carbon film on surface of valve sealing body and high-binding-force deposition method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of vacuum coating and chlor-alkali chemical industry, in particular to a lanthanum hexaboride composite carbon film on the surface of a valve sealing body and a high-binding force deposition method thereof. The method adopts titanium, titanium silicon and lanthanum hexaboride as target materials, methane or acetylene as a carbon source, and deposits the lanthanum hexaboride composite carbon film; due to the high ionization rate of the high-binding-force high-power pulse magnetron sputtering and the high hardness and toughness of the silicon-titanium metal, the obtained film not only has high binding force on the valve sealing surface substrate, but also can resist frequent opening impact, and simultaneously ensures the wear resistance and corrosion resistance.
Description
Technical Field
The invention relates to the technical field of vacuum coating and chlor-alkali chemical industry, in particular to a lanthanum hexaboride composite carbon film on the surface of a valve sealing body and a high-binding force deposition method thereof.
Background
The chemical valve is an important accessory for controlling fluid on an industrial pipeline, and in practical application, a valve sealing member is required to be long in service life, and the valve can be prevented from being damaged within one overhaul period (generally 1-2 years) at least so as to ensure the safe and normal operation of the whole system. Traditionally, the valve sealing surface is subjected to Hastelloy surfacing and polishing treatment to meet the requirements of wear resistance and corrosion resistance of the valve sealing surface, or polytetrafluoroethylene is adopted.
In the prior art, the invention patent (CN200910182061) provides a surfacing nickel-chromium alloy for improving the wear resistance and corrosion resistance of a sealing surface of a nuclear power valve, and the invention patent (CN20091023295) further provides a cobalt-free nickel-based alloy for a strengthening coating of the sealing surface of the nuclear power valve.
However, under the conditions of high temperature and high acid, the valve sealing body made of the alloy is easy to generate abrasive chemical reaction, so that the corrosion and the abrasion are accelerated, and accidents can be caused in severe cases. In view of the above, patent ZL201310477578 discloses a composite coating on the surface of a valve sealing element and a preparation method thereof, which utilizes the wear resistance of arc ion plating chromium nitride to further improve the wear resistance of the sealing surface of the valve. However, chromium nitride has a high coefficient of friction (μ -0.4) and wear rate, and the arc deposited coating has a high porosity, providing a channel for corrosive fluids.
Disclosure of Invention
Aiming at the problems, the invention provides a lanthanum hexaboride composite carbon film on the surface of a valve sealing body and a high-binding-force deposition method thereof, which are used for wear resistance and corrosion resistance of valve devices in chlor-alkali chemical industry, hydraulic sealing, nuclear industry and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a lanthanum hexaboride composite carbon film on the surface of a valve sealing body takes the surface of the valve sealing body as a substrate and sequentially comprises a substrate nitride layer, a titanium bonding layer, a titanium silicon nitride layer, a lanthanum hexaboride layer and a lanthanum hexaboride composite carbon film from bottom to top.
Preferably, the thickness of the titanium bonding layer is 200-300 nm, the thickness of the titanium silicon layer is 300-500 nm, the thickness of the titanium silicon nitride layer is 1000-1500 nm, the thickness of the lanthanum hexaboride layer is 300-500 nm, and the thickness of the lanthanum hexaboride composite carbon film is 2000-2500 nm.
The invention also provides a high-bonding-force deposition method of the lanthanum hexaboride composite carbon film on the surface of the valve sealing body, which comprises the following steps:
the method comprises the following steps: nitriding the surface of the substrate nitride layer before depositing the film;
step two: depositing a titanium bonding layer;
step three: depositing a titanium silicon layer;
step four: depositing a titanium nitride silicon layer;
step five: depositing a lanthanum hexaboride layer;
step six: depositing the lanthanum hexaboride composite carbon film.
Preferably, in the step (one), a narrow pulse power supply with voltage of 3000-.
Preferably, in the step (two), a high-power micro-pulse power supply is adopted, the voltage is set to be 500-750V, the single-pulse length is 100 microseconds, the duty ratio is 30-40%, and the single period is 2000 microseconds; the bias power supply is set at 650 and 750V, DC power supply.
Preferably, in the step (III), a high-power micro-pulse power supply is adopted, the voltage is set to be 500-750V, the single-pulse length is 100 microseconds, the duty ratio is 30-40%, and the single period is 2000 microseconds; bias power supply setting 100-.
Preferably, in the step (four), a high-power micro-pulse power supply is adopted, the voltage is set to be 500-750V, the single-pulse length is 150 microseconds, the duty ratio is 30-40%, and the single period is 1500 microseconds; bias power supply setting 100-.
Preferably, in the step (five), a medium frequency pulse power supply is adopted, the voltage is set to be 500-650V, the frequency is 20-40KHz, and the duty ratio is 60%; bias power supply setting 150-.
Preferably, in the step (six), a medium-frequency pulse power supply is adopted, the voltage is set to be 500-650V, the frequency is 20-40KHz, and the duty ratio is 60%; bias power supply setting 650-750V, narrow pulse power supply.
Preferably, the carbon source is a gas, and the gas is any one of methane, ethylene and acetylene.
The invention designs the film on the surface of the valve sealing member substrate into a substrate nitride layer, a titanium bonding layer, a titanium silicon nitride layer, a lanthanum hexaboride layer and a lanthanum hexaboride composite carbon film, and compared with the prior art, the invention has the following beneficial effects:
1. because a high-power micro-pulse technology is introduced, compared with arc ion plating, a more compact film result can be obtained, and the gap transmission of ions is effectively inhibited;
2. the high strength of titanium metal and the high hardness of silicon are combined, so that the toughness of a combined layer is improved, and the hardness and the bearing performance of the combined layer are improved;
3. through the design of a multilayer component change structure, a multilayer interface structure is introduced, so that the interface transmission of strong corrosive ions is further inhibited, and the crack propagation of repeated frequent opening impact can be further prevented;
4. the introduction of the rare earth compound can form an amorphous nanocrystalline composite structure, improve the wear resistance and the bearing performance, and can form boron carbide to improve the corrosion resistance;
5. the lanthanum element is compounded into the carbon-based film, so that the friction coefficient can be further reduced, and is as low as 0.1 and below.
Drawings
FIG. 1 is a schematic structural view of a lanthanum hexaboride composite carbon film of the present invention;
in the figure: 1-substrate nitride layer, 2-titanium bonding layer, 3-titanium silicon layer, 4-titanium nitride silicon layer, 5-lanthanum hexaboride layer and 6-lanthanum hexaboride composite carbon film.
Detailed Description
The technical solution of the present invention is described below with reference to the accompanying drawings and examples.
The first embodiment is as follows:
referring to fig. 1, the lanthanum hexaboride composite carbon film on the surface of the valve sealing body takes the surface of the valve sealing body as a substrate, and sequentially comprises a substrate nitride layer 1, a titanium bonding layer 2, a titanium silicon layer 3, a titanium silicon nitride layer 4, a lanthanum hexaboride layer 5 and a lanthanum hexaboride composite carbon film 6 from bottom to top.
A high-bonding-force deposition method of a lanthanum hexaboride composite carbon film on the surface of a valve sealing body comprises the following steps:
firstly, selecting a 316L stainless steel ball valve, and carrying out hydrocarbon cleaning on a plated valve body to remove oil stains, rust spots and the like; and (3) loading the ball valve into a special fixture and keeping the ball valve capable of rotating 360 degrees in the coating process.
The method comprises the following steps: nitriding treatment is carried out on the surface of the substrate before the film is deposited so as to improve the hardness and the corrosion resistance of the substrate; a narrow pulse power supply with a voltage of 3000V and a treatment time of 30 minutes was used, and argon gas was kept at 50 Pa.
Step two: the deposited titanium bonding layer is 200 nanometers, a high-power micro-pulse power supply is adopted, the voltage is set to be 500V, the single-pulse length is 100 microseconds, the duty ratio is 30%, and the single period is 2000 microseconds. The bias power supply was set at 750V, and the DC power supply was set to keep argon gas at 1 Pa.
Step three: the thickness of the deposited titanium silicon layer is 500 nanometers, a high-power micro-pulse power supply is adopted, the voltage is set to be 500-V, the single pulse length is 100 microseconds, the duty ratio is 40%, and the single period is 2000 microseconds. Bias power supply set 100V, dc power supply. Argon gas was kept at 1 Pa.
Step four: the thickness of the deposited titanium silicon nitride layer is 1000 nanometers, a high-power micro-pulse power supply is adopted, the voltage is set to be 500V, the single-pulse length is 150 microseconds, the duty ratio is 40%, the single period is 1500 microseconds, the bias power supply is set to be 100V, and the direct-current power supply keeps 2Pa of argon.
Step five: the thickness of the deposited lanthanum hexaboride is 500 nanometers, an intermediate frequency pulse power supply is adopted, the voltage is set to be 500V, the frequency is 40KHz, the duty ratio is 60%, a bias power supply is set to be 150V, and a direct current power supply keeps 1Pa of argon.
Step six: the thickness of the deposited lanthanum hexaboride composite carbon film is 2000 nanometers, a medium-frequency pulse power supply is adopted, the voltage is set to be 650V, the frequency is 40KHz, and the duty ratio is 60%. Bias power supply set 750V, narrow pulse power supply; the methane and argon gas were in a ratio of 2:1.5, and the pressure was maintained at 2 Pa.
And finally, closing the power supply and the gas, naturally cooling for 40 minutes, flushing nitrogen to atmospheric pressure, and taking out the valve sealing element.
By the method, the thickness of the prepared lanthanum hexaboride composite carbon film is about 4 microns, and due to multilayer compounding and amorphous nanocrystalline dispersion strengthening, a liquid flow channel of a single film is broken, so that the possibility that porous coating liquid easily penetrates through a pore channel to corrode an interface is prevented.
On the other hand, the combination of toughness and high hardness of the double elements can also play a role in impact resistance, and the service life of the sealing valve is greatly prolonged.
Example two:
referring to fig. 1, the lanthanum hexaboride composite carbon film on the surface of the valve sealing body takes the surface of the valve sealing body as a substrate, and sequentially comprises a substrate nitride layer 1, a titanium bonding layer 2, a titanium silicon layer 3, a titanium silicon nitride layer 4, a lanthanum hexaboride layer 5 and a lanthanum hexaboride composite carbon film 6 from bottom to top.
A high-bonding-force deposition method of a lanthanum hexaboride composite carbon film on the surface of a valve sealing body comprises the following steps:
firstly, selecting a gate valve body, and carrying out hydrocarbon cleaning on the plated valve body to remove oil stains, rust spots and the like.
The method comprises the following steps: the surface of the substrate is nitrided before the film is deposited, so that the hardness and the corrosion resistance of the substrate are improved. A narrow pulse power supply with voltage of 5000V and treatment time of 30 minutes is used, and nitrogen gas is kept at 30 Pa.
Step two: the deposited titanium bonding layer is 300 nanometers, a high-power micro-pulse power supply is adopted, the voltage is set to be 500V, the single-pulse length is 100 microseconds, the duty ratio is 40%, the single period is 2000 microseconds, the bias power supply is set to be 650V, and the direct-current power supply keeps 1Pa of argon.
Step three: the thickness of the deposited titanium silicon layer is 300 nanometers, a high-power micro-pulse power supply is adopted, the voltage is set to be 750V, the single-pulse length is 100 microseconds, the duty ratio is 40%, the single period is 2000 microseconds long, the bias power supply is set to be 100V, and the direct-current power supply keeps 1Pa of argon.
Step four: the thickness of the deposited titanium silicon nitride layer is 1500 nanometers, a high-power micro-pulse power supply is adopted, the voltage is set to be 500V, the single-pulse length is 150 microseconds, the duty ratio is 40%, and the single period is 1500 microseconds; the bias power supply was set at 150V, and the DC power supply was set to maintain 1Pa of argon gas.
Step five: the thickness of the deposited lanthanum hexaboride is 300 nanometers, an intermediate frequency pulse power supply is adopted, the voltage is set to be 650V, the frequency is 20KHz, and the duty ratio is 60 percent; the bias power supply was set at 200V, and the DC power supply was set to maintain 1Pa of argon gas.
Step six: the thickness of the deposited lanthanum hexaboride composite carbon film is 2500 nanometers, and the ratio of methane to argon is 1:1, the air pressure is 3Pa, an intermediate frequency pulse power supply is adopted, the voltage is set to be 650V, the frequency is 20KHz, and the duty ratio is 60 percent; bias power supply set 750V, narrow pulse power supply.
And finally, closing the power supply and the gas, naturally cooling for 40 minutes, flushing nitrogen to atmospheric pressure, and taking out the valve sealing element.
Through the steps, the gradient multilayer structure is obtained by utilizing the air pressure and voltage alternation in the deposition process, the obdurability of the film is favorably improved, the impact resistance of frequent opening is improved, and the service life of the valve body is prolonged.
Example three:
referring to fig. 1, the lanthanum hexaboride composite carbon film on the surface of the valve sealing body takes the surface of the valve sealing body as a substrate, and sequentially comprises a substrate nitride layer 1, a titanium bonding layer 2, a titanium silicon layer 3, a titanium silicon nitride layer 4, a lanthanum hexaboride layer 5 and a lanthanum hexaboride composite carbon film 6 from bottom to top.
A high-bonding-force deposition method of a lanthanum hexaboride composite carbon film on the surface of a valve sealing body comprises the following steps:
firstly, selecting a cast iron check valve, and carrying out hydrocarbon cleaning on a plated valve body to remove oil stains, rusts and the like.
The method comprises the following steps: nitriding treatment is carried out on the surface of the substrate before the film is deposited so as to improve the hardness and the corrosion resistance of the substrate; a narrow pulse power supply with a voltage of 4000V and a treatment time of 30 minutes was used, and argon gas was kept at 20 Pa.
Step two: the deposited titanium bonding layer is 250 nanometers, a high-power micro-pulse power supply is adopted, the voltage is set to be 600V, the single-pulse length is 100 microseconds, the duty ratio is 35%, and the single period is 2000 microseconds long; the bias power supply was set at 700V, and the DC power supply was set to maintain 1Pa of argon gas.
Step three: the thickness of the deposited titanium silicon layer is 400 nanometers, a high-power micro-pulse power supply is adopted, the voltage is set to be 600V, the single-pulse length is 100 microseconds, the duty ratio is 30%, and the single period is 2000 microseconds long; the bias power supply was set at 150V, and the DC power supply was set to maintain 1Pa of argon gas.
Step four: the thickness of the deposited titanium silicon nitride layer is 1000 nanometers, a high-power micro-pulse power supply is adopted, the voltage is set to be 600V, the single-pulse length is 150 microseconds, the duty ratio is 30%, and the single period is 1500 microseconds; the bias power supply was set at 150V, and the DC power supply was set to maintain 1Pa of argon gas.
Step five: the thickness of the deposited lanthanum hexaboride is 400 nanometers, an intermediate frequency pulse power supply is adopted, the voltage is set to be 650V, the frequency is 30KHz, and the duty ratio is 60 percent; the bias power supply was set at 200V, and the DC power supply was set to maintain 1Pa of argon gas.
Step six: the thickness of the deposited lanthanum hexaboride composite carbon film is 2500 nanometers, a medium-frequency pulse power supply is adopted, the voltage is set to be 600V, the frequency is 30KHz, and the duty ratio is 60 percent; the bias power supply was set at 750V, the narrow pulse power supply, the methane to argon ratio 1:1.5, and argon 2Pa was maintained.
And finally, closing the power supply and the gas, naturally cooling for 40 minutes, flushing nitrogen to atmospheric pressure, and taking out the valve sealing element.
Through the steps, the gradient multilayer structure is obtained by utilizing the incremental increase of carbon source airflow and the alternation of sputtering current in the deposition process, the toughness of the film is favorably improved, the impact resistance of frequent opening is improved, and the service life of the valve body is prolonged.
Example four:
referring to fig. 1, the lanthanum hexaboride composite carbon film on the surface of the valve sealing body takes the surface of the valve sealing body as a substrate, and sequentially comprises a substrate nitride layer 1, a titanium bonding layer 2, a titanium silicon layer 3, a titanium silicon nitride layer 4, a lanthanum hexaboride layer 5 and a lanthanum hexaboride composite carbon film 6 from bottom to top.
A high-bonding-force deposition method of a lanthanum hexaboride composite carbon film on the surface of a valve sealing body comprises the following steps:
firstly, selecting a bearing steel stop valve, and carrying out hydrocarbon cleaning on a plated valve body to remove oil stains, rust spots and the like.
The method comprises the following steps: the surface of the substrate is nitrided before the film is deposited, so that the hardness and the corrosion resistance of the substrate are improved. A narrow pulse power supply is used, the voltage is 5000V, the treatment time is 30 minutes, and the argon gas is kept at 30 Pa.
Step two: the deposited titanium bonding layer is 300 nanometers, a high-power micro-pulse power supply is adopted, the voltage is set to be 750V, the single-pulse length is 100 microseconds, the duty ratio is 30%, and the single period is 2000 microseconds long; the bias power supply is set to 700V, and the DC power supply keeps 2Pa of argon.
Step three: the thickness of the deposited titanium silicon layer is 500 nanometers, a high-power micro-pulse power supply is adopted, the voltage is set to be 650V, the single-pulse length is 100 microseconds, the duty ratio is 35%, and the single period is 2000 microseconds long; the bias power supply was set at 150V, and the DC power supply was set to maintain 2Pa of argon gas.
Step four: the thickness of the deposited titanium silicon nitride layer is 1500 nanometers, a high-power micro-pulse power supply is adopted, the voltage is set to be 550V, the single-pulse length is 150 microseconds, the duty ratio is 38%, and the single period is 1500 microseconds; the bias power supply was set at 150V, and the DC power supply was set to maintain 2Pa of argon gas.
Step five: the thickness of the deposited lanthanum hexaboride is 500 nanometers, an intermediate frequency pulse power supply is adopted, the voltage is set to be 650V, the frequency is 40KHz, and the duty ratio is 60 percent; the bias power supply was set to 250V, and the DC power supply was set to maintain 1Pa of argon gas.
Step six: the thickness of the deposited lanthanum hexaboride composite carbon film is 2500 nanometers, an intermediate frequency pulse power supply is adopted, the voltage is set to be 650V, the frequency is 37KHz, and the duty ratio is 60 percent; the bias power supply was set at 750V, the narrow pulse power supply, the methane to argon ratio 1:1.5, and the gas pressure was maintained at 1.5 Pa.
And finally, closing the power supply and the gas, naturally cooling for 40 minutes, flushing nitrogen to atmospheric pressure, and taking out the valve sealing element.
Through the steps, the gradient multilayer structure is obtained by utilizing the incremental carbon source airflow, the bias voltage and the alternating sputtering current in the deposition process, so that the toughness of the film is improved, the impact resistance of frequent opening is improved, and the service life of the valve body is prolonged.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (1)
1. A high-bonding-force deposition method of a lanthanum hexaboride composite carbon film on the surface of a valve sealing body is characterized by comprising the following steps: the surface of a valve sealing body is taken as a substrate, and the valve sealing body sequentially comprises a substrate nitride layer (1), a titanium bonding layer (2), a titanium silicon layer (3), a titanium silicon nitride layer (4), a lanthanum hexaboride layer (5) and a lanthanum hexaboride composite carbon film (6) from bottom to top;
the thickness of the titanium bonding layer (2) is 200-300 nm, the thickness of the titanium silicon layer (3) is 300-500 nm, the thickness of the titanium silicon nitride layer (4) is 1000-1500 nm, the thickness of the lanthanum hexaboride layer (5) is 300-500 nm, and the thickness of the lanthanum hexaboride composite carbon film (6) is 2000-2500 nm;
the method comprises the following steps:
the method comprises the following steps: nitriding the surface of the substrate before depositing the film so as to form a substrate nitride layer;
step two: depositing a titanium bonding layer;
step three: depositing a titanium silicon layer;
step four: depositing a titanium nitride silicon layer;
step five: depositing a lanthanum hexaboride layer;
step six: depositing a lanthanum hexaboride composite carbon film;
in the first step, a narrow pulse power supply is adopted, the voltage is 3000-;
in the second step, a high-power micro-pulse power supply is adopted, the voltage is set to be 500-750V, the single pulse length is 100 microseconds, the duty ratio is 30-40%, and the single period is 2000 microseconds; bias power supply setting 650-;
in the third step, a high-power micro-pulse power supply is adopted, the voltage is set to be 500-750V, the single pulse length is 100 microseconds, the duty ratio is 30-40%, and the single period is 2000 microseconds; bias power supply setting 100-;
in the fourth step, a high-power micro-pulse power supply is adopted, the voltage is set to be 500-750V, the single pulse length is 150 microseconds, the duty ratio is 30-40%, and the single period is 1500 microseconds; bias power supply setting 100-;
in the fifth step, a medium-frequency pulse power supply is adopted, the voltage is set to be 500-650V, the frequency is 20-40KHz, and the duty ratio is 60 percent; bias power supply setting 150-;
in the sixth step, a medium-frequency pulse power supply is adopted, the voltage is set to be 500-650V, the frequency is 20-40KHz, and the duty ratio is 60 percent; bias power supply setting 650 and 750V, narrow pulse power supply;
the carbon source is used as gas, and the gas is any one of methane, ethylene and acetylene.
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