CN103320772B - Metal inner surface modification device and method - Google Patents
Metal inner surface modification device and method Download PDFInfo
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- CN103320772B CN103320772B CN201310278344.4A CN201310278344A CN103320772B CN 103320772 B CN103320772 B CN 103320772B CN 201310278344 A CN201310278344 A CN 201310278344A CN 103320772 B CN103320772 B CN 103320772B
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- cathode
- negative electrode
- anode
- surface modification
- metal inner
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- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000012986 modification Methods 0.000 title claims abstract description 16
- 230000004048 modification Effects 0.000 title claims abstract description 16
- 239000002184 metal Substances 0.000 title abstract 5
- 239000007789 gas Substances 0.000 claims abstract description 29
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052786 argon Inorganic materials 0.000 claims abstract description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000000694 effects Effects 0.000 claims abstract description 11
- 229910021385 hard carbon Inorganic materials 0.000 claims abstract description 11
- 238000000151 deposition Methods 0.000 claims abstract description 10
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 7
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000005260 corrosion Methods 0.000 claims abstract description 5
- 230000007797 corrosion Effects 0.000 claims abstract description 5
- 238000005121 nitriding Methods 0.000 claims abstract description 5
- 239000010408 film Substances 0.000 claims description 9
- 239000000376 reactant Substances 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000000427 thin-film deposition Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 230000003213 activating effect Effects 0.000 claims description 2
- 239000010406 cathode material Substances 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000012159 carrier gas Substances 0.000 abstract 2
- 210000002381 plasma Anatomy 0.000 abstract 2
- 239000012495 reaction gas Substances 0.000 abstract 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 229910003460 diamond Inorganic materials 0.000 abstract 1
- 239000010432 diamond Substances 0.000 abstract 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract 1
- 230000008021 deposition Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 238000002513 implantation Methods 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- QFUKUPZJJSMEGE-UHFFFAOYSA-N 5-(hydroxymethyl)-1-(3-methylbutyl)pyrrole-2-carbaldehyde Chemical compound CC(C)CCN1C(CO)=CC=C1C=O QFUKUPZJJSMEGE-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000007772 electroless plating Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000005468 ion implantation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
Landscapes
- Chemical Vapour Deposition (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Abstract
The invention discloses a metal inner surface modification device and method and belongs to the technical field of plasma surface modification. The method is characterized by comprising the following steps: generating plasmas on a metal inner surface by utilizing the principle of hollow-cathode discharge, and nitriding or depositing diamond like carbon, so as to improve the hardness, the wear resistance and the corrosion resistance of the metal inner surface; by taking a treated piece as a cathode, arranging the cathode inside, adjusting the distance and the vacuum degree between a workpiece and the cathode to reach the discharge condition, arranging an anode at the periphery of a cathode cavity, and adding a direct current pulse power supply between the anode and the cathode, wherein reaction gas is nitrogen or ammonia gas and carrier gas is argon gas during the nitriding, and the reaction gas is methane or acetylene and the carrier gas is argon gas in the process of depositing a hard carbon film. The method has the effects and advantages of simple process, low cost and high efficiency and is particularly suitable for treating the metal inner surface and pipe fittings of large draw ratios.
Description
Technical field
The invention belongs to plasma surface modification technology field, relate to the deposition that surface chemistry blends hard carbon films, be related specifically to and chemistry is realized to metallic interior surface ooze or the method for thin film deposition, to improve the physical and chemical performances such as the hardness of metallic interior surface, wear resistance and solidity to corrosion.
Background technology
Internal surface is that the workpiece class of working face is numerous, as the cylinder barrel of engine, transport pipeline, ion accelerating tube, gun barrel, interior punch die and axle sleeve etc., these workpiece are often because the form such as inner wall abrasion, corrosion is destroyed, in order to improve the hardness of workpiece inner wall, wear-resisting resistance to and corrodibility, and then improve its working efficiency and life-span, within it wall chemistry oozes or deposit film is very important technique means.But the relevant report at present about inner wall surface modification is few, technical reserve critical shortage compared with the heavy demand of internal surface military service parts, therefore develops inner wall surface modification technology and have and urgent realistic meaning.Pipe internal surface not only can be confined to the internal surface of tubular workpiece, but can be generalized to concave face on complex part, hole and inner chamber.So pipe internal surface treatment research has great application potential.
At present the main method adopted has plating, laser intensify treatment, physical vapor deposition, plasma enhanced chemical vapor deposition, ion implantation etc.Plating and electroless plating are the preferred method of socket part inner surface treatment, are characterized in that modified effect is good, can process by the pipe fitting very little to internal diameter, and most I reaches several millimeter.But plating and electroless plating cause serious pollution to environment, and the wear resistance of coating is lower, and tack is poor.
Utilize fiber optic conduction laser, thus make pipe internal surface laser quenching not by the restriction of pipe range, the inner surface laser phase transformation strengthening of elongated tubular can be realized, but laser can only be applied to some special occasions; When using plasma is ion implantation, if processed tube internal diameter too carefully, because sheaths is intersected, in pipe, plasma potential will reduce with applying potential difference, and result injection effect may reduce greatly, even may not produce injection effect.There is investigator to propose interior electrode method for this reason, namely in socket, place a ground-electrode.But because majority adopts external ion source, the outer portion of plasma body produces, and diffuses into cylinder interior subsequently, tubular body plasma density must be caused so uneven, also the axis just causing implantation dosage is uneven, and when processing elongated tubular, this phenomenon is comparatively obvious.Generally speaking, interior electrode method improves Implantation Energy, does not provide terms of settlement to the ununiformity of implantation dosage.
Summary of the invention
The invention provides a kind of apparatus and method of metallic interior surface modification, utilize hollow cathode effect, i.e. endoporus cathode glow area overlapping, in overlap, glow current sharply increases, highdensity plasma body is produced in metallic interior surface, realize chemistry ooze or deposit ganoine thin film, solve metallic interior surface modification, improve internal surface hardness, wear resistance and corrosion proof object.
Technical scheme of the present invention is: the device of metallic interior surface modification utilizes hollow cathode effect to produce plasma body in cavity, realizes plasma and oozes or plasma activated chemical vapour deposition.Processed part is negative electrode, according to processed part surface shape, increases negative electrode that is identical with cathode material, profile similarity, forms double cathode.Reactant gases is evenly incorporated in the cavity between negative electrode and negative electrode by negative electrode, and the residual gas after reaction need be extracted out by mechanical pump by cathode inner surface edge surrounding.Negative electrode and meet Pd=0.5 ~ 10Torrcm relation between cathode spacing d and vacuum chamber reaction pressure P, molybdenum anode is positioned at cavity edge surrounding, and negative electrode and positive electrode spacing is 2 ~ 5 times of double cathode spacing.
The method of metallic interior surface modification passes into reactant gases, adds DC pulse bias voltage between anode and cathode, controls the temperature of processed part, carry out chemistry and ooze or thin film deposition.Under the effect of hollow cathode plasma, processed part is heated between 400 ~ 700 ° of C, passes into the mixed gas of nitrogen or ammonia and argon gas, to inner surface of pipe fitting nitriding; During deposition hard carbon thin film, processed workpiece and water-cooled copper electrode contact, make the temperature of processed workpiece control, between 50 ~ 300 ° of C, to pass into the mixed gas of acetylene or methane and argon gas, add pulsed voltage and deposit hard carbon thin film at inner surface of pipe fitting.
Effect of the present invention and benefit are: can process the pipe fitting of big L/D ratio and the internal surface of various complicated shape; Chemistry can be realized ooze, comprise single element and blend multiple permeation, also can carry out thin film deposition, as deposition hard carbon films etc.; Surface modification efficiency is high.
Accompanying drawing explanation
Accompanying drawing 1 is inner surface of pipe fitting reforming apparatus schematic diagram.
Accompanying drawing 2 is device schematic diagram of internal surface deposition hard carbon films.
In figure: 1 power supply; 2 processed pipe fittings; 3 negative electrode air taking ports; 4 negative electrodes; 5 anodes; 6 insulating ceramic pipes; 7 bleeding points; 8 vacuum measurements; 9 seal washers; 10 silica tubes; 11 tongued and grooved flanges.
Embodiment
The specific embodiment of the present invention is described in detail below in conjunction with technical scheme and accompanying drawing.
The specific embodiment of the invention is, first, vacuumizes and makes reaction chamber reach base vacuum ~ 10
-3torr, passes into argon gas and carries out surface cleaning and activating pretreatment 5-20min to 0.05Torr to processed part, pass into reactant gases in proportion afterwards.In nitrogen or ammonia and argon gas mixed gas, nitrogen or ammonia ratio are 20 ~ 80%, regulate vacuum tightness 5 × 10
-2between ~ 5Torr, add pulsed voltage 0 ~ 10kV or electric current 0 ~ 5A between anode and cathode, under the effect of hollow cathode plasma, processed part is heated between 400 ~ 700 ° of C naturally, and nitriding time is 0.5 ~ 4h.
During deposition hard carbon films, reactant gases is changed into acetylene or methane and argon gas mixed gas, acetylene or methane ratio are 5 ~ 40%, and water flowing cooling ensures that workpiece temperature is between 50 ~ 300 ° of C.Regulate vacuum tightness 5 × 10
-2between ~ 5Torr, between anode and cathode, add pulsed voltage 0 ~ 10kV or electric current 0 ~ 5A, hard carbon films depositing time 0.5 ~ 4h.
Embodiment 1:
As shown in Figure 1, adjustment cathode spacing is 5mm, and cathode and anode spacing 20mm, is evacuated to 10
-3torr, passes into argon gas to 0.05Torr, adds DC pulse voltage 2kV, plasma clean sample 10min.Pass into 40% nitrogen, the pressure of adjustment vacuum chamber is 3Torr, and add direct current pulse power source, discharging current maintains 0.3A, and underlayer temperature about 500 ° of C, the reaction times is 2h.
Embodiment 2:
As shown in Figure 2, adjustment cathode spacing is 10mm, and cathode and anode spacing 40mm, is evacuated to 10
-3torr, passes into argon gas to 0.05Torr, and to substrate holder water flowing cooling, underlayer temperature is no more than 300 ° of C.Add DC pulse voltage 2kV, plasma clean sample 10min.Pass into 20% acetylene gas, the pressure of adjustment vacuum chamber is 0.5Torr, and add direct current pulse power source, discharging current maintains 0.2A, and the reaction times is 2h.
Claims (2)
1. the device of a metallic interior surface modification, utilize hollow cathode effect in cavity, produce highdensity plasma body, realize the modification of metallic interior surface, chemistry can be realized ooze, also can deposit hard carbon films, improve the hardness of metallic interior surface, wear resistance and solidity to corrosion physical and chemical performance, it is characterized in that processed part is negative electrode, according to processed part surface shape, increase negative electrode that is identical with cathode material, profile similarity, form double cathode; Reactant gases is evenly incorporated in the cavity between negative electrode and negative electrode by negative electrode, and the residual gas after reaction need be extracted out by mechanical pump by cathode inner surface edge surrounding; Negative electrode and meet Pd=0.5-10Torrcm relation between cathode spacing d and vacuum chamber reaction pressure P, molybdenum anode is positioned at cavity edge surrounding, negative electrode and positive electrode spacing be the 2-5 of double cathode spacing doubly; Pass into reactant gases, between anode and cathode, add DC pulse bias voltage, control the temperature of processed part, carry out chemistry and ooze or thin film deposition.
2. a method for metallic interior surface modification, utilizes the device of a kind of metallic interior surface modification described in claim 1, it is characterized in that:
A) first, vacuumize and make reaction chamber reach base vacuum ~ 10
-3torr, passes into argon gas and carries out surface cleaning and activating pretreatment 5-20min to 0.05Torr to processed part, pass into reactant gases in proportion afterwards; In nitrogen or ammonia and argon gas mixed gas, nitrogen or ammonia ratio are 20 ~ 80%, regulate vacuum tightness 5 × 10
-2between ~ 5Torr, add pulsed voltage 0 ~ 10kV or electric current 0 ~ 5A between anode and cathode, under the effect of hollow cathode plasma, processed part is heated between 400 ~ 700 DEG C naturally, and nitriding time is 0.5 ~ 4h;
When b) depositing hard carbon films, reactant gases is changed into acetylene or methane and argon gas mixed gas, acetylene or methane ratio are 5 ~ 40%, and water flowing cooling ensures that workpiece temperature is between 50 ~ 300 DEG C; Regulate vacuum tightness 5 × 10
-2between ~ 5Torr, between anode and cathode, add pulsed voltage 0 ~ 10kV or electric current 0 ~ 5A, hard carbon films depositing time 0.5 ~ 4h.
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CN201310278344.4A CN103320772B (en) | 2013-07-04 | 2013-07-04 | Metal inner surface modification device and method |
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CN103320772B true CN103320772B (en) | 2015-06-10 |
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CN104313567A (en) * | 2014-09-12 | 2015-01-28 | 湖州鑫隆镀膜科技有限公司 | Metal chromium production technology for replacing electroplating technology |
CN105648424B (en) * | 2016-03-29 | 2018-08-31 | 北京航空航天大学 | A kind of device and method of hollow cathode discharge diameter metal inside pipe wall coating |
CN107217228B (en) * | 2017-05-18 | 2019-11-22 | 清华大学 | Improve the method and bearing of bearing wear-resisting property |
RU2671522C1 (en) * | 2017-08-14 | 2018-11-01 | Российская Федерация, от имени которой выступает Государственная корпорация по атомной энергии "Росатом" | Method of internal cylindrical surface plasma strengthening |
CN107937880B (en) * | 2017-09-20 | 2020-03-10 | 深圳市中科摩方科技有限公司 | Method for modifying surface of metal material, product and application thereof |
CN108342708B (en) * | 2018-03-22 | 2020-08-07 | 深圳大学 | Carbon element injection method and modified cutter and mold thereof |
CN109518121B (en) * | 2018-11-21 | 2021-09-10 | 中国航发哈尔滨东安发动机有限公司 | Method for regulating and controlling deformation of thin-wall titanium alloy part by using hollow cathode effect |
CN109680243B (en) * | 2018-12-05 | 2021-11-09 | 中国航发哈尔滨东安发动机有限公司 | Thin-wall medium-small-size asymmetric rotation type titanium alloy part nitriding deformation control method |
CN109609889B (en) * | 2018-12-05 | 2021-11-09 | 中国航发哈尔滨东安发动机有限公司 | High-temperature nitriding ultra-precision deformation control method for thin-wall double-shell titanium alloy bushing |
CN109518122B (en) * | 2018-12-05 | 2022-01-14 | 中国航发哈尔滨东安发动机有限公司 | Ion nitriding control method for thin-wall large-size asymmetric rotary titanium alloy part |
CN111647879A (en) * | 2020-04-20 | 2020-09-11 | 中国科学技术大学 | Chemical vapor deposition device and method |
CN112025202A (en) * | 2020-08-21 | 2020-12-04 | 广东粤江鸿锐电力科技发展有限公司 | Method for repairing straight gear |
CN113198804B (en) * | 2021-04-30 | 2023-02-03 | 辽宁科技大学 | Method and apparatus for cleaning inner wall of slender pipeline by inert gas ionization |
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