CN101597750B - Arc ion plating method for inner walls of deep holes - Google Patents
Arc ion plating method for inner walls of deep holes Download PDFInfo
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- CN101597750B CN101597750B CN2009103039337A CN200910303933A CN101597750B CN 101597750 B CN101597750 B CN 101597750B CN 2009103039337 A CN2009103039337 A CN 2009103039337A CN 200910303933 A CN200910303933 A CN 200910303933A CN 101597750 B CN101597750 B CN 101597750B
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- ion plating
- arc ion
- inner walls
- permanent magnet
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- 238000007733 ion plating Methods 0.000 title claims abstract description 27
- 230000006698 induction Effects 0.000 claims abstract description 11
- 239000011148 porous material Substances 0.000 claims description 27
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 15
- 238000000151 deposition Methods 0.000 abstract description 8
- 238000007747 plating Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- 230000005672 electromagnetic field Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 33
- 150000002500 ions Chemical class 0.000 description 10
- BGPVFRJUHWVFKM-UHFFFAOYSA-N N1=C2C=CC=CC2=[N+]([O-])C1(CC1)CCC21N=C1C=CC=CC1=[N+]2[O-] Chemical compound N1=C2C=CC=CC2=[N+]([O-])C1(CC1)CCC21N=C1C=CC=CC1=[N+]2[O-] BGPVFRJUHWVFKM-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- 230000008021 deposition Effects 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000003245 working effect Effects 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 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
- 230000001133 acceleration Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 239000007888 film coating Substances 0.000 description 2
- 238000009501 film coating Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000010349 pulsation Effects 0.000 description 1
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Abstract
The invention discloses an arc ion plating method for inner walls of deep holes, which belongs to the technical field of materials science and engineering. The invention relates to a method for depositing films on the inner walls of molds and pipes which have deep-hole structures by arc ion plating. The method is characterized in that a non-uniform magnetic field around a workpiece and the pulsed biasing are synchronously used during the plating, and the interaction between the electromagnetic field and a plasma is utilized to achieve the aim of deep plating. The magnetic induction intensity of a used magnet is between 500 and 8,000GS, and the length is between 20 and 150mm, and the distances from the magnet to the inner wall of a hole and the end surface of the hole of the workpiece and the magnetic induction intensity are directly proportional, and satisfy the relation that L is equal to (B+/-500)/40(mm); and the amplitude of the used pulsed biasing is between 200 and 800V, the frequency is between 5 and 40kHz, and the duty factor is between 5 and 40 percent. The method has the advantage that the depth of the plating is two times greater than an aperture when the inner wall of a workpiece with a pipe-hole structure is plated. The method is widely used for plating of inner surfaces of parts and molds which have inner-hole structures in the field of mechanical manufacturing.
Description
Technical field
The invention belongs to the Materials Science and Engineering technical field, relate to a kind of with the method for arc ion plating (aip) at mould with deep-hole structures and the deposition modified film of tube wall.
Background technology
The ion plating modified film technology of material surface as at instrument, piece surface plating TiN ganoine thin film, as far back as the just successful commercialization eighties in last century, and is being brought into play more and more important effect in industrial production.But the more and more significant that also becomes of a problem is arranged, and nearly all exactly report all is the plated film research at outside surface.And in fact, the workpiece that with the internal surface is working face in production practice also occupies very big ratio, as cylinder barrel, transport pipeline, various tubular vessel, ion accelerating tube, gun barrel and the gun barrel etc. of some press tools, drawing die, engine, these workpiece are often destroyed because of forms such as inner wall abrasion, corrosion.Therefore exploitation deposits technology and method wear-resisting, anti-corrosion, resistant to elevated temperatures modified film on the inwall of pore structure workpiece, is more and more urgent problem of ion plating technique field.
The endoporus deposition of film is more much more difficult than outside deposition.In ion plating, whole workpiece is immersed in the plasma environment, plasma sheath centers on the outside surface of workpiece and forms, under the negative bias effect of electric field, ion is accelerated in the sheath layer and arrives workpiece surface, ion can also be come from plasma body in diffusion continuously after the deposition film forming, so can both be well controlled in the thickness and the quality of outside deposition film; But for inner walls of deep holes, especially only the blind hole inwall plated film of an end opening, owing to be subjected to the shielding effect of cavernous structure, plasma body can only spread inwards by only place's opening, along with the continuous consumption of ion in film process, plasma density will constantly descend with the degree of depth, determine past more depths to obtain film difficulty all the more.In general,, adopt the common process the same, also can only obtain the plated film degree of depth the same, promptly 1: 1 plated film aspect ratio with pore diameter with outside surface even use the highest arc ions electroplating method of ionization level.Up-to-date studies show that, adopts pulsed negative bias in the arc ion plating membrane process, can increase the plated film degree of depth 1.4 times to dark pipe diameter
[1], promptly obtain 1.4: 1 plated film aspect ratio.But only use pulsed bias but can't obtain the darker plated film degree of depth, thereby cause those pore depth ratio diameters in production practice all can't adopt this method to realize that plated film improves its work-ing life greater than 1.4 times most parts and mould.
Reference
[1] Shi Changlun, Zhang Min, woods Guoqiang., pulsed bias is to the influence of the dark inside pipe wall depositing TiN thin film of arc ion plating. and vacuum science and technology journal, 2007,27 (6): 517-521.
Summary of the invention
The purpose of this invention is to provide and a kind ofly have the workpiece inwall deposit film of deep-hole structures with the electric arc ion plating, the plated film degree of depth reaches more than 2 times of pore diameter, and promptly the plated film aspect ratio reaches 2.0: 1 above deep hole film coating method.
Technical conceive of the present invention is, in the arc ion plating process, use pulsed bias and workpiece non-uniform magnetic field on every side simultaneously, utilize the complementary interaction of electric field, magnetic field and plasma body, cause plasma body in charged particle local orientation flow, and the vibration of the plasma sheath of pore inside is drawn the purpose of back at the depths deposit film to strengthen the diffusion of plasma body in pore thereby reach in the plasma body.Its ultimate principle is: if place a non-uniform magnetic field in plasma body, then charged particle under the effect in magnetic field, do the translational motion that Larmor perpendicular to the magnetic line of force direction rotatablely moves (its rotation radius is r=mv/qB) and do along magnetic field gradient directions (the gradient magnetic directed force F=-μ dB/dx, wherein μ is a magnetic moment), therefore, distribution when the choose reasonable non-uniform magnetic field, when position and size, thereby just might cause charged particle in the plasma body to flow towards certain azimuthal orientation and form the region clustering of charged particle in the part, if this directed flow zone is chosen in the pore place of deep hole workpiece just, then plasma body can produce and draws tendency in certain under the effect in magnetic field.In addition, pulsed bias makes plasma sheath fluctuation with the pulsation of bias voltage, the thickness d of plasma sheath
s=[(2 ε
0U)/(en
i)]
1/2(ε wherein
0Be permittivity of vacuum, U is the bias voltage amplitude, and e is an electron charge, n
iDensity for plasma body) variation along with bias voltage changes, when being in " accounting for " at bias voltage, the sheath layer is thicker, the acceleration of ions energy is big, coating quality is good, but when the blocked up yardstick to the pore radius of sheath layer, ion can be outside and can not enter inside pipe wall plated film can not be carried out at pore by the shielding of sheath layer; When being in " sky " at bias voltage, the sheath layer is thinner, the acceleration of ions energy is little, coating quality is bad, but little can not formation at the mouth of pipe shields ionic sheath layer yardstick this moment, ion can be diffused into pore inside than the depths, when plasma body directed flow that non-uniform magnetic field causes, this diffusion meeting strengthens more.Therefore the ratio of choose reasonable pulsed bias " accounting for ", " sky " can be taken into account the ion deposition of film and to two processes of internal diffusion, when having non-uniform magnetic field to cause the part of plasma body to assemble simultaneously, this effect of taking into account can be more obvious.
Technical solution of the present invention is, be to have the vacuum chamber of putting into arc ion plating after the workpiece cleaning drying of pore structure, through vacuumizing, logical argon gas, open arc, add negative bias, sputter clean, logical reactant gases, plated film, stop arc, outage and stove take out workpiece after the cold stage, it is characterized in that: use pulsed bias at workpiece arranged around permanent magnet with in the plated film stage with pore structure, the magnetic induction density of the permanent magnet of arranging is 500～8000 Gausses, length is 20～100mm, width and highly be 5～40mm, the magnet geometric center point is directly proportional with the magnetic induction density B of magnet to the distance L of workpiece 3 and hole 6 end faces, and meet L=B/40 ± 50 relation, wherein the unit of B is Gauss, and the unit of L is a millimeter; The pulsed bias that uses be amplitude 200～800V, frequency 5～40kHz, dutycycle 5～40%.
Having the workpiece arranged around permanent magnet of pore structure, is that the side at workpiece 3 becomes 0～45 to arrange a main permanent magnet 4 with the hole direction of principal axis of workpiece.
Having the workpiece arranged around permanent magnet of pore structure, is to become main permanent magnet 4 of 0～45 symmetric arrangement and an auxilliary permanent magnet 5 with the hole direction of principal axis of workpiece in the both sides of workpiece 3.
Has the workpiece arranged around permanent magnet of pore structure, be to be arranged vertically a magnet set that constitutes by first magnet 7 and second magnet 8 in a side of workpiece 3 and the hole direction of principal axis of workpiece, the S utmost point of first magnet 7 is towards workpiece and be positioned at and close on arc source one side, the N utmost point of second magnet 8 is towards workpiece and be positioned at away from arc source one side, the two keeping parallelism and spacing d are directly proportional with magnetic induction density B, meet d=B/80 ± 20 relations, wherein the unit of d is a millimeter, and the unit of B is Gauss; The nearly work end line central point of first magnet 7 and second magnet 8 also is directly proportional with the magnetic induction density B of magnet to the distance L of workpiece 3 and hole 6 end faces, and meets L=B/40 ± 50 relations, and wherein the unit of L is a millimeter, and the unit of B is Gauss.
Workpiece with pore structure is that length is 20～150mm, and diameter is 20～100mm, width and highly be the metal die with inner hole structure of 20～100mm.
Workpiece with pore structure is that diameter is that Φ 10～100mm, length are that 50～400mm, thickness are the metal pipe of 1～10mm.
Workpiece with pore structure is that length is 20～150mm, and diameter is 20～100mm, width and highly be the metal parts with inner hole structure of 20～100mm.
Effect of the present invention and benefit are, solved with the technical barrier of arc ion plating (aip) at workpiece inwall depths deposit film with deep-hole structures, compare with the coating process that adopts routine, the plated film degree of depth can be brought up to more than 2 times to pore diameter from original 1 times, be that the plated film aspect ratio can reach more than 2.0, be particularly suitable for film-coating modification, increase substantially its work-ing life based on the workpiece of internal surface military service.
Description of drawings
Fig. 1 is that the relative position of magnet, workpiece and the cathode arc source when workpiece one side arranges that a main permanent magnet carries out workpiece inwall arc ion plating of the present invention is put synoptic diagram.
Fig. 2 is that the relative position of magnet, workpiece and cathode arc source when a main permanent magnet and an auxilliary permanent magnet carry out workpiece inwall arc ion plating of arranging in the workpiece both sides of the present invention is put synoptic diagram.
Fig. 3 is that the relative position of magnet set, workpiece and the cathode arc source when workpiece one side is arranged the workpiece inwall arc ion plating that magnet set that first magnet and second magnet constitute carries out having the pore structure in the workpiece of the present invention is put synoptic diagram.
Among the figure: the 1st, cathode arc source, the 2nd, plasma body, the 3rd, workpiece, the 4th, main permanent magnet, the 5th, auxilliary permanent magnet, the 6th, the workpiece endoporus, 7 is first magnet, 8 is second magnet.
Embodiment
The present invention is further illustrated below in conjunction with accompanying drawing.
The sintered-carbide die with Φ 10 * 20mm endoporus 3 of Φ 50 * 30mm is cleaned, puts on the work stage of arc ion plating apparatus vacuum chamber after the oven dry, as shown in Figure 1, the opening direction of mould 3 is aimed at the source direction of the plasma body 2 of cathode arc source 1, becoming 0 ° of angle with the hole direction of principal axis of mould in a side of mould 3 is that 4000 Gausses, length are the main permanent magnet 4 of 50mm with magnetic induction density B of insulating material fixed placement, and magnet 4 geometric center point are 100mm to the distance of mould 3 and endoporus 6 end faces; Vacuum is evacuated to 10
-2Pa; logical argon gas is to 0.5Pa; open the titanium arc; arc stream is 60A, and adding negative bias is 800V * 20kHz * 50%, carries out sputter clean 5 minutes; then negative bias drops to 500V * 20kHz * 30%; improve the titanium arc stream and begin plated film, stop arc after 60 minutes, stop the supple of gas or steam, outage, stove be after cold 30 minutes, bleeds off vacuum taking-up mould to 80A, logical nitrogen 100sccm.
Present embodiment can all deposit fine and close TiN film in the depths of mould inner wall 20mm, and its nano hardness 〉=20GPa can improve the anti-corrosion and wear resisting property of mould inner wall and then the work-ing life of improving mould.
The stainless steel pipe with Φ 40 * 100mm endoporus 3 of Φ 50 * 100mm is cleaned, put into after the oven dry on the work stage of arc ion plating apparatus vacuum chamber, as shown in Figure 2, the opening direction of pipe 3 is aimed at the source direction of the plasma body 2 of cathode arc source 1, parallel with the hole direction of principal axis of pipe in pipe 3 left and right sides with insulating material difference 1 main permanent magnet 4 of fixed placement and 1 auxilliary permanent magnet 5, their magnetic induction density B is 8000 Gausses, length is 60mm, the S utmost point of magnet is towards arc source 1 direction, and magnet all is 200mm to the distance of pipe 3 and pipe endoporus 6 end faces; Vacuum is evacuated to 10
-2Pa; logical argon gas is to 0.5Pa; open the titanium arc; arc stream is 60A, and adding negative bias is 800V * 20kHz * 50%, carries out sputter clean 5 minutes; then negative bias drops to 500V * 20kHz * 40%; improve the titanium arc stream and begin plated film, stop arc after 60 minutes, stop the supple of gas or steam, outage, stove be after cold 30 minutes, bleeds off vacuum taking-up pipe to 80A, logical nitrogen 100sccm.
Present embodiment can be at stainless steel pipe inwall until all deposit fine and close TiN film greater than the depths of 80mm, its nano hardness 〉=20GPa can improve the anti-corrosion and wear resisting property of tube wall and then the work-ing life of improving pipe.
The pipe 3 of stainless steel one end closure with Φ 40 * 80mm endoporus of Φ 50 * 100mm is cleaned, put into after the oven dry on the work stage of arc ion plating apparatus vacuum chamber, as shown in Figure 3, opening one end of pipe 3 is aimed at the source direction of the plasma body 2 of cathode arc source 1, above pipe 3 with the vertical magnet set that constitutes by first magnet 7 and second magnet 8 with the insulating material fixed placement of hole direction of principal axis of pipe, their magnetic induction density B is 8000 Gausses, length is 60mm, the S utmost point of first magnet 7 down and be positioned at and close on arc source one side, the N utmost point of second magnet 8 down and be positioned at away from arc source one side, the two in the vertical direction keeping parallelism and spacing are 100 millimeters, and the lower end line central point of magnet 7 and magnet 8 all is 200 millimeters to the distance of pipe 3 and hole 6 end faces; Vacuum is evacuated to 10
-2Pa; logical argon gas is to 0.5Pa; open the titanium arc; arc stream is 60A, and adding negative bias is 800V * 20kHz * 50%, carries out sputter clean 5 minutes; then negative bias drops to 500V * 20kHz * 40%; improve the titanium arc stream and begin plated film, stop arc after 60 minutes, stop the supple of gas or steam, outage, stove be after cold 30 minutes, bleeds off vacuum taking-up pipe to 80A, logical nitrogen 100sccm.
Present embodiment can be at stainless steel pipe inwall until all deposit fine and close TiN film greater than the depths of 80mm, its nano hardness 〉=20GPa can improve the anti-corrosion and wear resisting property of tube wall and then the work-ing life of improving pipe.
Claims (6)
1. arc ion plating method for inner walls of deep holes, be to have the vacuum chamber of putting into arc ion plating after the workpiece cleaning drying of pore structure, through vacuumizing, logical argon gas, open arc, add negative bias, sputter clean, logical reactant gases, plated film, stop arc, outage and stove take out workpiece after the cold stage, it is characterized in that: use pulsed bias at workpiece arranged around permanent magnet with in the plated film stage with pore structure, the magnetic induction density of the permanent magnet of arranging is 500～8000 Gausses, length is 20～100mm, the magnet geometric center point is directly proportional with the magnetic induction density B of magnet to the distance L of workpiece (3) and hole (6) end face, and meet L=B/40 ± 50 relation, wherein the unit of B is Gauss, and the unit of L is a millimeter; The amplitude of the pulsed bias that uses is 200～800V, and frequency is 5～40kHz, and dutycycle is 5～40%.
2. according to the described arc ion plating method for inner walls of deep holes of claim 1, it is characterized in that: described have the workpiece arranged around permanent magnet of pore structure, is to become 0～45 to arrange a main permanent magnet (4) with the hole direction of principal axis of workpiece in workpiece (3) one sides.
3. according to the described arc ion plating method for inner walls of deep holes of claim 1, it is characterized in that: described have the workpiece arranged around permanent magnet of pore structure, is to become a main permanent magnet of 0～45 symmetric arrangement (4) and an auxilliary permanent magnet (5) with the hole direction of principal axis of workpiece in the both sides of workpiece (3).
4. according to the described arc ion plating method for inner walls of deep holes of claim 1, it is characterized in that: described workpiece with pore structure is that length is 20～150mm, diameter is 20～100mm, width and highly be the metal die with inner hole structure of 20～100mm.
5. according to the described arc ion plating method for inner walls of deep holes of claim 1, it is characterized in that: described workpiece with pore structure is that diameter is that Φ 10～100mm, length are that 50～400mm, thickness are the metal pipe of 1～10mm.
6. according to the described arc ion plating method for inner walls of deep holes of claim 1, it is characterized in that: described workpiece with pore structure is that length is 20～150mm, diameter is 20～100mm, width and highly be the metal parts with inner hole structure of 20～100mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009103039337A CN101597750B (en) | 2009-07-02 | 2009-07-02 | Arc ion plating method for inner walls of deep holes |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009103039337A CN101597750B (en) | 2009-07-02 | 2009-07-02 | Arc ion plating method for inner walls of deep holes |
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| CN101597750A CN101597750A (en) | 2009-12-09 |
| CN101597750B true CN101597750B (en) | 2011-11-16 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101838791B (en) * | 2010-04-16 | 2011-06-08 | 南京理工大学 | Method for depositing amorphous carbon film by modifying surface of magnesium alloy |
| CN103814153B (en) | 2011-09-22 | 2015-11-25 | 学校法人芝浦工业大学 | Film forming method, film forming device, the treated object being formed with overlay film, mould and instrument |
| CN104451562B (en) * | 2014-12-08 | 2017-02-22 | 沈阳工业大学 | Arc ion plating device for coating of inner wall of long pipe |
| CN108277456A (en) * | 2018-01-31 | 2018-07-13 | 天津涂冠科技有限公司 | A method of PVD tube type work piece plated film aspect ratios are improved by externally-applied magnetic field |
| CN111636050B (en) * | 2020-06-05 | 2022-08-09 | 合肥工业大学 | Manufacturing method of micropore inner wall conducting layer |
| 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 |
| CN114574829B (en) * | 2022-03-08 | 2023-10-27 | 松山湖材料实验室 | Micro deep hole inner coating process and coating device |
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