CN105543736B - Plate ruthenium molybdenum sheet plasma surface treatment method - Google Patents

Plate ruthenium molybdenum sheet plasma surface treatment method Download PDF

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Publication number
CN105543736B
CN105543736B CN201610035707.5A CN201610035707A CN105543736B CN 105543736 B CN105543736 B CN 105543736B CN 201610035707 A CN201610035707 A CN 201610035707A CN 105543736 B CN105543736 B CN 105543736B
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Prior art keywords
molybdenum sheet
ruthenium
vacuum cavity
plasma
discharge
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CN201610035707.5A
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CN105543736A (en
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俞叶
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YIXING KEXING ALLOY MATERIAL CO Ltd
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YIXING KEXING ALLOY MATERIAL CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58After-treatment
    • C23C14/5826Treatment with charged particles
    • C23C14/5833Ion beam bombardment
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601Process or apparatus
    • C23C18/1633Process of electroless plating
    • C23C18/1689After-treatment
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48After-treatment of electroplated surfaces

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The present invention relates to a kind of molybdenum sheet surface processing method, specially plate ruthenium molybdenum sheet plasma surface treatment method, the plating ruthenium film surface of molybdenum sheet is handled with plasma bombardment, need to molybdenum sheet to be processed be placed in vacuum cavity, plate anode of the ruthenium film surface to plasma discharge, processed molybdenum sheet as electric discharge negative electrode.The plating ruthenium molybdenum sheet plasma surface treatment method that the present invention is provided, improve production efficiency, process simplification, improve the yields of product, and this method energy-saving safe, cleaning, process stabilizing is simple to operate, i.e., with high-purity Ar gas be working gas in vacuum cavity, its ionization is set to form glow discharge, the Ar of ionization+The surface that molybdenum sheet plates ruthenium is bombarded, the film layer of ruthenium obtains energy, so as to reach the effect of plating ruthenium film surface processing, and because under vacuum conditions, electric discharge working gas is high-purity argon gas, molybdenum sheet is plated ruthenium surface plasma treated, it will not be secondary polluted, ruthenium film layer uniformity is good after processing.

Description

Plate ruthenium molybdenum sheet plasma surface treatment method
Technical field
The present invention relates to a kind of molybdenum sheet surface processing method, ruthenium molybdenum sheet plasma surface treatment side is specially plated Method.
Background technology
Thermal compensation molybdenum sheet, the supporting plate as monocrystalline silicon piece plays radiating, maintains protection chip normal work, improves brilliant The effect of the service life of brake tube, is to manufacture one of critical component of super high power IGCT.The usual table of current thermal compensation molybdenum sheet Face needs rhodanizing, the metallic diaphragm of ruthenium, and the molybdenum sheet of plating ruthenium film applies more and more, gradually the trend of substituted rhodanizing, with plating ruthenium The process of film has the methods such as electrochemical plating, chemical plating, physical vapor deposition, but adhesive force, the densification of generally existing ruthenium film The problem of in terms of property or membranous layer stability.The subsequent technique that the processing of one or many annealing in hydrogen atmospheres is usually taken goes to solve this to ask Topic, so that production efficiency is reduced, process procedure increases, and product yield declines, while this technique consumes energy, taken, simultaneously There is certain risk.
The content of the invention
For above-mentioned technical problem, a kind of process energy consumption of present invention offer is low, quick and safe plating ruthenium molybdenum sheet surface treatment Method, concrete technical scheme is:
Ruthenium molybdenum sheet plasma surface treatment method is plated, is comprised the following steps:
(1)The molybdenum sheet for having plated ruthenium film is arranged on the vacuum cavity inner cathode plate of plasma discharge apparatus, place is needed The ruthenium film of reason upward, at a distance of 5-10cm between the anode of plasma discharge, cathode-anode plate;
(2)Vacuum cavity is closed, vavuum pump is opened and vacuum cavity is vacuumized, make its vacuum 2 × 10-1Pa to 5 × 10-2Pa;
(3)Ar air valves are filled in unlatching, and high-strength Ar gas is filled with to vacuum cavity by the control of vacuum flowmeter, makes vacuum cavity Vacuum in the range of 1-10Pa;
(4)Open discharge power supply, make Ar pneumoelectrics between vacuum cavity cathode-anode plate from, form stable glow discharge, The different substrate setting of discharge power correspondence is different, and start recording, and power 100W to 3000W, the time is set in 5-30 minutes;
(5)After setting time of discharging reaches, discharge power supply is closed, Ar air valves are filled in closing, and continuation is evacuated with vavuum pump 5-10 minutes;
(6)Vavuum pump is closed down, vent valve is opened, vacuum cavity is deflated, and opens vacuum cavity door, taking-up is processed Plating ruthenium molybdenum sheet.
The plating ruthenium film surface of molybdenum sheet is handled with plasma bombardment, it would be desirable to which the molybdenum sheet of processing is placed in vacuum cavity, Anode of the ruthenium film surface to plasma discharge is plated, and the molybdenum sheet being processed is more than negative electrode as the negative electrode of electric discharge, and annode area, i.e., Electric discharge device is loaded high-frequency ac voltage, can also form a bias, it is ensured that Ar+It is overall to fly to processed molybdenum sheet direction OK, high direct voltage, pulse voltage can make Ar+It is continuously molybdenum sheet flight bombardment, Ar towards negative electrode+Kinetic energy touching Bump against on molybdenum sheet and transfer energy in plating ruthenium film layer, migrate ruthenium metallic atom and its micromeritics, further crystallization, which reaches, disappears Except the inherent strain of ruthenium film layer, meanwhile, the thickness that ruthenium film layer is plated to different molybdenum sheet size thickness and thereon is accordingly taken The time of different glow discharge and discharge power and to high frequency, pulse, the selection of direct-current discharge, reach corresponding substrates of different Plating ruthenium film layer can eliminate its inherent strain, make the film adhesion of plating ruthenium strengthen, consistency improve, robustness improve.
The plating ruthenium molybdenum sheet plasma surface treatment method that the present invention is provided, improves production efficiency, and process simplification is carried The yields of high product, and this method energy-saving safe, cleaning, process stabilizing are simple to operate, i.e., with high-purity in vacuum cavity Ar gas is working gas, its ionization is formed glow discharge, the Ar of ionization+The surface that molybdenum sheet plates ruthenium is bombarded, the film layer of ruthenium is obtained Energy, so that the effect of plating ruthenium film surface processing is reached, and because under vacuum conditions, electric discharge working gas is high-purity argon gas, Make molybdenum sheet plating ruthenium surface plasma treated, will not be secondary polluted, ruthenium film layer uniformity is good after processing.
Embodiment
It is described in conjunction with the embodiments the embodiment of the present invention.
Ruthenium molybdenum sheet plasma surface treatment method is plated, is comprised the following steps:
(1)The molybdenum sheet for having plated ruthenium film is arranged on the vacuum cavity inner cathode plate of plasma discharge apparatus, place is needed The ruthenium film of reason upward, at a distance of 5-10cm between the anode of plasma discharge, cathode-anode plate;
(2)Vacuum cavity is closed, vavuum pump is opened and vacuum cavity is vacuumized, make its vacuum 2 × 10-1Pa to 5 × 10-2Pa;
(3)Ar air valves are filled in unlatching, and high-strength Ar gas is filled with to vacuum cavity by the control of vacuum flowmeter, makes vacuum cavity Vacuum in the range of 1-10Pa;
(4)Open discharge power supply, make Ar pneumoelectrics between vacuum cavity cathode-anode plate from, form stable glow discharge, The different substrate setting of discharge power correspondence is different, and start recording, and power 100W to 3000W, the time is set in 5-30 minutes;
Because processed molybdenum sheet is to be emitted on supporting plate and be placed in ion plasma to handle, the diameter or length and width chi of molybdenum sheet The very little influential effect to processing less, therefore only considers molybdenum sheet thickness.Specifically:
Plasma discharge apparatus processing specification:As thickness≤0.5mm that molybdenum is justified, the power setting of plasma treatment is 800W, 6 minutes;
When the thickness that molybdenum is justified is more than 0.5mm, less than or equal to 1mm, plasma treatment power is 900W, 10 minutes;
When molybdenum circle thickness is more than 1mm, less than or equal to 2mm, plasma treatment power is 1200w, 10 minutes time;
When molybdenum sheet thickness is more than 2mm, less than 3mm, plasma treatment power is 1500w, 15 minutes;
When molybdenum sheet thickness is more than 3mm, less than 4mm, plasma treatment power 2000w, 20 minutes time;
When molybdenum sheet thickness is more than 4mm, plasma treatment power is 2500w, 30 minutes.
(5)After setting time of discharging reaches, discharge power supply is closed, Ar air valves are filled in closing, and continuation is evacuated with vavuum pump 5-10 minutes;
(6)Vavuum pump is closed down, vent valve is opened, vacuum cavity is deflated, and opens vacuum cavity door, taking-up is processed Plating ruthenium molybdenum sheet.

Claims (1)

1. plate ruthenium molybdenum sheet plasma surface treatment method, it is characterised in that comprise the following steps:
(1)The molybdenum sheet for having plated ruthenium film is arranged on the vacuum cavity inner cathode plate of plasma discharge apparatus, need to be handled Ruthenium film upward, at a distance of 5-10cm between the anode of plasma discharge, cathode-anode plate;
(2)Vacuum cavity is closed, vavuum pump is opened and vacuum cavity is vacuumized, make its vacuum 2 × 10-1Pa to 5 × 10-2Pa;
(3)Ar air valves are filled in unlatching, and high-strength Ar gas is filled with to vacuum cavity by the control of vacuum flowmeter, makes the true of vacuum cavity Reciprocal of duty cycle is in the range of 1-10Pa;
(4)Discharge power supply is opened, makes the Ar pneumoelectrics between vacuum cavity cathode-anode plate from the stable glow discharge of formation, electric discharge The different substrate setting of power correspondence is different, and start recording, and power 100W to 3000W, the time is set in 5-30 minutes;
(5)After setting time of discharging reaches, discharge power supply is closed, Ar air valves are filled in closing, and continuation is evacuated 5-10 with vavuum pump Minute;
(6)Vavuum pump is closed down, vent valve is opened, vacuum cavity is deflated, and opens vacuum cavity door, the plating being processed is taken out Ruthenium molybdenum sheet.
CN201610035707.5A 2016-01-20 2016-01-20 Plate ruthenium molybdenum sheet plasma surface treatment method Active CN105543736B (en)

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CN105543736B true CN105543736B (en) 2017-08-08

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106148896B (en) * 2016-07-29 2019-10-15 泉州市宕存工业设计有限公司 A kind of method that molybdenum base piece plates thick ruthenium
CN112317564A (en) * 2020-10-15 2021-02-05 富甲电子(昆山)有限公司 Thermal shaping clean production process method of light alloy die casting and product

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