CN1174114C - Bicathode-high frequency glow ion diffusion coating equipment and its process - Google Patents

Bicathode-high frequency glow ion diffusion coating equipment and its process Download PDF

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Publication number
CN1174114C
CN1174114C CNB021101833A CN02110183A CN1174114C CN 1174114 C CN1174114 C CN 1174114C CN B021101833 A CNB021101833 A CN B021101833A CN 02110183 A CN02110183 A CN 02110183A CN 1174114 C CN1174114 C CN 1174114C
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China
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frequency
direct current
power supply
coating apparatus
diffusion coating
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CN1412343A (en
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原 高
高原
徐重
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Taiyuan University of Technology
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Taiyuan University of Technology
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Abstract

The present invention relates to double cathode and high-frequency glow ion plating equipment and a process. A high-frequency induction device is arranged between the cathode and the source electrode of double-layer glow ion diffusion metallizing equipment. The high-frequency induction device is not a sputtering supply source, and is a discharge device without electrodes for generating a glow discharge ionization body. The high-frequency induction device has a help to heat a sputtering material with the source electrode and a workpiece with the anode. A strong magnetic field and an electric field produced by the high-frequency induction device are used to enable glow discharge between the anode and the source electrode to be reinforced and the ionization efficiency is increased, so equipment and a process method for accelerating to form an alloy element diffusion layer, a deposit layer and a combined composite plating layer between the alloy element diffusion layer and the deposit layer on the workpiece surface of a conducting material are provided.

Description

Double cathode-high frequency glow ion diffusion coating apparatus and technology
One, technical field
Double cathode of the present invention-high frequency glow ion diffusion coating apparatus and technology belong to the category of plasma surface metallurgic.Concrete, provided a kind of a kind of equipment that utilizes high-frequency device to strengthen cathode sputtering and glow discharge.And form the single or composite cementation coating of diffusion layer, settled layer or the diffusion layer+settled layer of various elements (comprising metallic element and non-metallic element) on the surface of all electro-conductive materials with this equipment.
Two, background technology
A lot of at various device that utilizes the gas discharge plasma surface metallurgic and processing method, mainly contain as double-layer metallic glow ion cementation equipment and technology, multi sphere ionic diffusion coating apparatus and technology, radio-frequency sputtering ion plating equipment and technology, magnetic controlled sputtering ion plating equipment and technology, direct current diode sputtering and direct current three utmost points or four utmost point sputter coating apparatus and technology etc.And direct current diode sputtering and direct current three utmost points or four utmost point sputter coating apparatus and technology and magnetic controlled sputtering ion plating equipment and technology all are two utmost points or multipolar direct current glow discharge in the above equipment, the effect of each utmost point is by the ion bombardment sputter, desire co-diffusioning alloy element is provided, and can only carries out surface coating and can not carry out the pyritous infiltration.Radio-frequency sputtering ion plating equipment and technology are one pole, multipolar alternating current glow discharge.Radio-frequency pole by the ion bombardment sputter, directly provides alloying element at this, and also can only carry out surface coating and can not carry out the pyritous infiltration.Multi sphere ionic diffusion coating apparatus and technology are one pole or multipolar arc light alternating current discharge, the multi sphere ion diffusion coating utmost point also is by arc discharge at this, and vaporization and ionized metal atom provide alloying element.Double-layer metallic glow ion cementation equipment and technology, the effect of a negative electrode are by the ion bombardment sputter, and desire co-diffusioning alloy element is provided, and the effect of another negative electrode is that heated parts forms surface alloying layer.
The difference of the maximum of the present invention and above equipment and technology is: 1. have in double-layer metallic glow ion cementation equipment in the negative electrode and source electrode of two direct current glow discharges, added the high-frequency induction device, this device is not the sputter supply source, but a device that produces the electrodeless discharge of discharge ionization body.It mainly acts on is to utilize powerful electric field and magnetic field, makes the plasma body in the region of discharge between the negative electrode of two direct current glow discharges and the source electrode, and electronic journey increases, and electron energy increases, and probability of collision increases, and ionization level improves.When producing hollow cathode effect or non-equi-potential hollow cathode effect between the negative electrode of these two direct current glow discharges and the source electrode, this effect will make hollow cathode discharge further strengthen.2. the high-frequency induction device also has the effect of rapid heating magneticsubstance.This moment, the sputtering raste of source electrode increased greatly, workpiece under the heated condition of this powerful electric field, magnetic field and fast cycle in, permeating speed is accelerated, the settled layer bonding force is good.3. the working vacuum degree in the time of can making double-layer metallic glow ion cementation improves 1~2 order of magnitude.
Three, summary of the invention
Double cathode of the present invention-high frequency glow ion diffusion coating apparatus and technology, so its purpose is being provided with the high-frequency induction device between two negative electrodes of double-layer metallic glow ion cementation equipment, utilize the strong magnetic field and the electric field of high-frequency induction that two glow discharges between the negative electrode are strengthened, ionization level increases, thereby a kind of equipment and technology of the composite cementation coating that forms alloying element diffusion layer, settled layer on the electro-conductive material surface and mutually combine between them are provided.
Double cathode of the present invention-high frequency glow ion diffusion coating apparatus, it is characterized in that, be between two negative electrodes of double-layer metallic glow ion cementation equipment, the high-frequency induction device to be set, mainly by the source electrode 1 of desiring the sputter alloying element is provided, the negative electrode 2 of place work piece, workpiece 3, the shell 4 of vacuum vessel, high-frequency induction device 5, auxiliary cathode 6, high voltage direct current shielding power supply 7 and high voltage direct current heating power supply 8, radio-frequency generator 9, pumped vacuum systems 10) inlet system 11 compositions, provide the source electrode 1 of desire sputter alloying element and the negative electrode of high voltage direct current shielding power supply 7 to join, the negative electrode 2 of place work piece joins with the negative electrode of high voltage direct current heating power supply 8, workpiece 3 places in the auxiliary cathode 6 on the negative electrode 2 of place work piece, and the anode of high voltage direct current shielding power supply 7 and high voltage direct current heating power supply 8 all is connected on the shell 4 of vacuum vessel, and high-frequency induction device 5 is arranged on the outside of auxiliary cathode 6, auxiliary cathode 6 is placed on the negative electrode 2 of place work piece, and two utmost points of radio-frequency generator 9 are connected on two of high-frequency induction device 5 respectively and extremely go up.
Above-mentioned double cathode-high frequency glow ion diffusion coating apparatus, high voltage direct current shielding power supply 7 and high voltage direct current heating power supply 8 can be high-voltage pulse power sources, the variable range 0~2000V of voltage.
Above-mentioned double cathode-high frequency glow ion diffusion coating apparatus, the material that the source electrode 1 of desiring the sputter alloying element is provided are the materials of conduction.
Above-mentioned double cathode-high frequency glow ion diffusion coating apparatus, radio-frequency generator 9, its operating frequency range are two sections: the integral multiple of 0.5KHz~400KHz or 13.56MHz.
Above-mentioned double cathode-high frequency glow ion diffusion coating apparatus, workpiece material is all electro-conductive materials.
All hardwares in the above-mentioned double cathode-high frequency glow ion diffusion coating apparatus, the inwall of vacuum vessel and vacuum vessel except that source electrode sputter material and workpiece material, all should be made by austenitic stainless steel or non-magnetic conductive material.
Above-mentioned double cathode-high frequency glow ion diffusion coating apparatus, auxiliary cathode structure are the structures of hollow, and the auxiliary cathode of hollow is can the side of being barrel-shaped, round tank, rectangular barrel-shaped etc., its material or metal or graphite.
Above-mentioned double cathode-high frequency glow ion diffusion coating apparatus, high-frequency induction device can be screw type, flat, circular, ellipse or quadrate, can be that a circle also can be a multiturn.
The technology of double cathode of the present invention-high frequency glow ion diffusion coating apparatus, it is characterized in that, at first workpiece 3, be placed in the auxiliary cathode 6 of hollow, provide the material of the source electrode 1 of desiring the sputter alloying element to select W-Mo as the sputter element, then high-frequency induction device 5 is set, vacuumizes and reach final vacuum 5 * 10 in the outside of auxiliary cathode -4More than the Pa, the fill gas body medium is to the working vacuum degree, add the high frequency anode voltage earlier, adjust tank circuit voltage, again to the workpiece DC heating voltage that adds high pressure, to the source electrode d.c. sputtering voltage that adds high pressure, be raised to working temperature insulation 1 hour, slowly cooling can obtain 60 microns W-Mo diffusion layer and 2 microns W-Mo settled layer, processing parameter is: the high voltage direct current shielding power supply, high voltage direct current heating power supply or pulse direct current high tension voltage-200V~-2000V, anode voltage 3000V~the 13500V of radio-frequency generator, the tank circuit voltage 3000V~10000V of radio-frequency generator, the anodic current 0.2A~4A of radio-frequency generator, the grid current 0.1A~0.7A of radio-frequency generator, 500 ℃~1300 ℃ of working temperatures, final vacuum 5 * 10 -4Pa, working vacuum degree 10 -2Pa~10 3Pa, soaking time is decided on processing requirement, fill gas body medium Ar or N 2Or NH 3Or CH 4Or H 2, can make workpiece surface form nitrogenize, carburizing or carbo-nitridization layer.
Craft technical feature of the present invention is, under the metallic cementation working condition that is in strong glow discharge under hollow cathode effect, the effect of non-equi-potential hollow cathode effect, added the high-frequency induction device again, because strong electric field and the action of a magnetic field that it produced, increase the energy of electronics and flown to the anodic stroke, increased the probability of collision of electronics, ionization level is increased, glow discharge current increases.Hollow cathode effect will further be strengthened.Ionic current sputters out the form of the element in the source electrode with atom, ion or various particles, the effect of auxiliary cathode has two: the one, and heat up, be incubated, produce hollow cathode effect, the 2nd, various elementary particles are strapped in the cavity, form higher infiltration element atmosphere, make the workpiece surface that is adsorbed on that atom is exceedingly fast, diffuse into workpiece inside, form surperficial infiltration layer or settled layer.As this moment working medium contain NH 3Or nitrogen, and carbon-containing atmosphere, then can make workpiece surface form nitrogenize, carburizing or carbo-nitridization layer.
Advantage of the present invention is: the 1. adding of high-frequency induction device, and strong electric field that is produced and the action of a magnetic field have increased the energy of electronics and have flown to the anodic stroke, increased the probability of collision of electronics, ionization level will be increased, and glow discharge current increases, and hollow cathode effect is further strengthened.2. the adding of high-frequency induction device can play rapid heating to source electrode and workpiece.3. the adding of high-frequency induction device can make the discharge operating air pressure reduce by 1~2 order of magnitude than direct-current discharge operating air pressure, has increased the cementation coating bonding force.4. the adding of high-frequency induction device makes the element speed of infiltrating, sedimentation velocity quickening.
Four, description of drawings
Accompanying drawing 1 is the structure scheme of installation of double cathode-high frequency glow ion diffusion coating apparatus and technology
Label in the accompanying drawing 1 is respectively:
The source electrode 1 of sputter alloying element, the negative electrode 2 of place work piece, workpiece 3, the shell of vacuum vessel (anode of ground connection) 4, high-frequency induction device 5, auxiliary cathode 6, high voltage direct current shielding power supply 7 and high voltage direct current heating power supply 8, radio-frequency generator 9, pumped vacuum systems 10, inlet system 11 compositions such as grade.
Accompanying drawing 2 is structure diagrams of accompanying drawing 1 medium-high frequency induction installation 5.
Five, embodiment
Concrete performance as shown in the figure.To be of a size of Ф 40 * 25mm (diameter * height), material is the workpiece 3 of 20 steel, is placed on tubbiness, is of a size of in the auxiliary cathode 6 of Ф 80 * 50mm (diameter * height) hollow, and source electrode 1 material selects W-Mo as the sputter element.The high-frequency induction device 5 of Ф 90 * 7mm (diameter * number of turn) is set in the outside of auxiliary cathode.Vacuumize and reach final vacuum 5 * 10 -4More than the Pa, fill gas body medium Ar is to working vacuum degree 10Pa, adds high frequency anode voltage 10000V earlier, adjusts tank circuit voltage 6000V, anodic current 1A, and grid current 0.2A is again to the workpiece DC heating voltage-400V that adds high pressure.To the source electrode d.c. sputtering voltage-1000V that adds high pressure.Be raised to 1100 ℃ of working temperatures, be incubated 1 hour.Slowly be cooled to below 50 ℃ the taking-up sample of coming out of the stove.Can obtain 60 microns W-Mo diffusion layer and 2 microns W-Mo settled layer.

Claims (9)

1. double cathode of the present invention-high frequency glow ion diffusion coating apparatus, it is characterized in that, between two negative electrodes of double-layer metallic glow ion cementation equipment, the high-frequency induction device is set, mainly by the source electrode (1) of desiring the sputter alloying element is provided, the negative electrode of place work piece (2), workpiece (3), the shell of vacuum vessel (4), high-frequency induction device (5), auxiliary cathode (6), high voltage direct current shielding power supply (7) and high voltage direct current heating power supply (8), radio-frequency generator (9), pumped vacuum systems (10), inlet system (11) is formed, provide the source electrode (1) of desire sputter alloying element and the negative electrode of high voltage direct current shielding power supply (7) to join, the negative electrode of place work piece (2) joins with the negative electrode of high voltage direct current heating power supply (8), workpiece (3) places in the auxiliary cathode (6) on the negative electrode (2) of place work piece, the anode of high voltage direct current shielding power supply (7) and high voltage direct current heating power supply (8) all is connected on the shell (4) of vacuum vessel, high-frequency induction device (5) is arranged on the outside of auxiliary cathode (6), auxiliary cathode (6) is placed on the negative electrode (2) of place work piece, and two utmost points of radio-frequency generator (9) are connected on two of high-frequency induction device (5) respectively and extremely go up.
2. double cathode according to claim 1-high frequency glow ion diffusion coating apparatus, high voltage direct current shielding power supply (7) and high voltage direct current heating power supply (8) can be high-voltage pulse power sources, the variable range 0~2000V of voltage.
3. double cathode according to claim 1-high frequency glow ion diffusion coating apparatus, the material that the source electrode (1) of desiring the sputter alloying element is provided are the materials of conduction.
4. double cathode according to claim 1-high frequency glow ion diffusion coating apparatus, radio-frequency generator (9), its operating frequency range are two sections: the integral multiple of 0.5KHz~400KHz or 13.56MHz.
5. double cathode according to claim 1-high frequency glow ion diffusion coating apparatus, workpiece material is all electro-conductive materials.
6. all hardwares in the double cathode according to claim 1-high frequency glow ion diffusion coating apparatus, the inwall of vacuum vessel and vacuum vessel except that source electrode sputter material and workpiece material, all should be made by austenitic stainless steel or non-magnetic conductive material.
7. double cathode according to claim 1-high frequency glow ion diffusion coating apparatus, auxiliary cathode structure are the structures of hollow, and the auxiliary cathode of hollow can barrel-shaped, the round tank, rectangular barrel-shaped in the side of being, its material or metal or graphite.
8. double cathode according to claim 1-high frequency glow ion diffusion coating apparatus, high-frequency induction device can be screw type, flat, circular, ellipse or quadrate, can be that a circle also can be a multiturn.
9. the technology of double cathode of the present invention-high frequency glow ion diffusion coating apparatus, it is characterized in that, workpiece (3) at first, be placed in the auxiliary cathode (6) of hollow, provide the material of the source electrode (1) of desiring the sputter alloying element to select W-Mo as the sputter element, high-frequency induction device (5) then is set in the outside of auxiliary cathode, vacuumizes and reach final vacuum 5 * 10 -4More than the Pa, the fill gas body medium is to the working vacuum degree, add the high frequency anode voltage earlier, adjust tank circuit voltage, again to the workpiece DC heating voltage that adds high pressure, to the source electrode d.c. sputtering voltage that adds high pressure, be raised to working temperature insulation 1 hour, slowly cooling can obtain 60 microns W-Mo diffusion layer and 2 microns W-Mo settled layer, processing parameter is: the high voltage direct current shielding power supply, high voltage direct current heating power supply or pulse direct current high tension voltage-200V~-2000V, anode voltage 3000V~the 13500V of radio-frequency generator, the tank circuit voltage 3000V~10000V of radio-frequency generator, the anodic current 0.2A~4A of radio-frequency generator, the grid current 0.1A~0.7A of radio-frequency generator, 500 ℃~1300 ℃ of working temperatures, final vacuum 5 * 10 -4Pa, working vacuum degree 10 -2Pa~10 3Pa, soaking time is decided on processing requirement, fill gas body medium Ar or N 2Or NH 3Or CH 4Or H 2, can make workpiece surface form nitrogenize, carburizing or carbo-nitridization layer.
CNB021101833A 2002-03-18 2002-03-18 Bicathode-high frequency glow ion diffusion coating equipment and its process Expired - Fee Related CN1174114C (en)

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CN100532635C (en) * 2007-01-30 2009-08-26 南京航空航天大学 Method for precipitating corrosion-resistant alloy layer using magnesium alloy surface glow plasma
CN102244971A (en) * 2010-05-13 2011-11-16 贵州翔明科技有限责任公司 Atmospheric-pressure direct current arc discharge plasma generator and cathode manufacturing method
CN103361615B (en) * 2013-06-24 2015-09-09 南京航空航天大学 The equipment of diamond surface double cathode plasma deposition nano coating and technique
CN103320772B (en) * 2013-07-04 2015-06-10 大连理工大学 Metal inner surface modification device and method
CN104109830B (en) * 2014-07-22 2017-01-18 桂林电子科技大学 Surface hafnium-infiltrated austenitic stainless steel resistant to high temperature and preparation method thereof
CN104651779A (en) * 2015-02-11 2015-05-27 烟台首钢磁性材料股份有限公司 Coating equipment and coating technology for neodymium-iron-boron magnet
CN105220108A (en) * 2015-10-23 2016-01-06 西华大学 Interactive double cathode ion surface heat treatment furnace
CN106381474B (en) * 2016-08-31 2019-01-22 江苏华力金属材料有限公司 The preparation method of stainless steel surface composite anti-wear coating
CN108411246B (en) * 2018-06-13 2024-03-19 深圳市奥美特纳米科技有限公司 Auxiliary equipment and method for improving ion nitriding efficiency of surface of low-alloy structural steel
CN114481009B (en) * 2022-02-14 2024-04-30 四川中科海科技有限责任公司 Anode high-pressure low-temperature nitriding device

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