CN101713065B - Microwave plasma-based low-energy ion implantation device on the inner surface of a small-diameter metal circular tube - Google Patents
Microwave plasma-based low-energy ion implantation device on the inner surface of a small-diameter metal circular tube Download PDFInfo
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Abstract
A microwave plasma-based low-energy ion implantation device for the inner surface of a small-caliber metal round pipe comprises a vacuum chamber (7) and a low-energy ion implantation power supply (10), and belongs to the technical field of material surface engineering. It is characterized in that: the linear ECR microwave plasma source is formed by a microwave source (1), a microwave coaxial waveguide inner conductor (2), a microwave coaxial waveguide outer conductor (3), a microwave coaxial waveguide short-circuit piston (5) and an external magnetic field coil (9), high-density ECR microwave plasmas which are uniformly distributed in the circumferential direction and the axial direction are formed along the central axis of a metal pipe fitting (11) to be processed under the excitation of an external magnetic field by utilizing the excitation and ionization action of a microwave slot radiation antenna (4), and the low-pulse negative bias applied by a low-energy ion implantation power supply (10) and an auxiliary external heat source (8) which is coaxially arranged are combined to complete plasma-based low-energy ion implantation on the inner surface of the metal pipe. The advantages are that: the cost is low; the plasma-based low-energy ion implantation of the inner surface of the metal round pipe with small pipe diameter and large length-diameter ratio can be realized.
Description
Technical field
The present invention relates to a kind of microwave plasma based low-energy ion implantation on internal surface of metal round pipe with small pipe diameter device; Especially adopt linear electron cyclotron resonance (ECR) microwave plasma source to carry out the modification technology that nonmetallic ions such as low energy nitrogen, carbon, boron inject the metal round pipe with small pipe diameter internal surface, belong to the material surface engineering field.
Technical background
The little caliber of round metal pipe fitting, particularly internal diameter 10～30mm, wearing and tearing, corrosion and the fatigue failure of big L/D ratio pipe spare have become a bottleneck problem of using in engineering fields such as petrochemical complex, mechanical power, marine ships.For example, the oil recovery machiner in oil field, pipe laying, the valve of chemical industry, pipeline, and powerdriven component or the like, demand carrying out the wear-resisting erosion resistance antifatigue modification processing of internal surface urgently.Industry is at present gone up wet chemical methods such as mainly adopting plating and is carried out this type component surface treatment, but the coating density that forms is limited, and combines not firm with the pipe fitting substrate; The trade waste pollution on the environment has also limited the application of these methods simultaneously.Therefore, the new technology of various environmental protections more begins to attempt being used for substituting traditional round metal pipe fitting inner surface treatment technology.
Matson in 1992 etc. publish thesis at Journal of Vacuum Science and Technology A, have reported the plasma-deposited thin film technique of a kind of triode sputtering.At internal diameter 25mm, the AISI4340 steel pipe internal-surface of long 213mm, high speed deposition the body-centered cubic structure metal tantalum coating of thick 35～130 μ m.Place the diameter 9.65mm column tantalum cathode target on the steel pipe central axis; And the tantalum wire auxiliary heat negative electrode of steel pipe one end; And discharge forms plasma body between the steel pipe anode that is processed; Utilize the booster action of tantalum wire hot-cathode, improve bar-shaped tantalum cathode sputtering yield effectively, in AISI4340 steel pipe internal-surface sputtering sedimentation tantalum coating.Because the auxiliary heat negative electrode only can be settled at pipe fitting end, causes the inhomogeneous of steel duct plasma distribution, causes the pipe fitting of the inhomogeneous sputter, particularly littler internal diameter of pipe fitting coated inside, the ununiformity of deposited coatings is more serious.
Hytry etc. are in the tenth plasma chemistry international symposium; Reported and utilized electron cyclotron resonace (Electron Cyclotron Resonance-ECR) microwave plasma; The rectangular metal waveguide is carried out the coating on inner surface deposition; And, formally delivered the correlative study result at Journal of Vacuum Science and Technology A in 1993.Microwave adds the toroidal magnetic field through moving in quartz window is coupled to metallic waveguide, in waveguide, produce the ECR microwave plasma, at the noncrystal carbon coating of waveguide internal surface plasma enhanced chemical vapor deposition of long 2m.Because microwave is along the cutoff wavelength restriction of waveguide transmission; The metal wave-guide fixed size that can be used for the plasma enhanced chemical vapor deposition coating; The modifying inner surface that can't be used for the small sized metallic pipe fitting is handled; And the ECR zone that in waveguide, forms is less, causes microwave plasma inhomogeneous, causes coating on inner surface to get lack of homogeneity, sedimentation effect is low.
Nineteen ninety-five; Ensinger is on Review of Scientific Instruments; Reported the ion beam sputter depositing that adopts conventional ion source technology, through the sputtering target that moves on the central axis, at pipe fitting internal surface depositing metal films around the central axis rotation with pitch angle.Adopt energy 2keV ar-ion beam splash-proofing sputtering metal silver target; Low alloy steel pipe fitting internal surface depositing silver film at internal diameter 6mm, long 60mm; Adopt energy 50keV polonium ion beam sputtering metal polonium target, at the metal tantalum pipe fitting internal surface deposition polonium film of internal diameter 10mm, long 120mm.In order to overcome beam line sputter lack of homogeneity, shortcoming that sputter rate is low; 2000; Using plasmas such as Ensinger are fallen into oblivion ion implantation (Plasma Immersion IonImplantation-PIII) technology and are carried out sputtering sedimentation; Substitute existing beam line sputter, respectively at stainless steel and the metal tantalum pipe fitting internal surface of internal diameter 15mm, long 150mm, sputtering sedimentation metal and compound film.Because the restriction of small size pipe fitting internal space, the sputter effect of sputtering target is still limited, and reverse sputtering effect simultaneously is difficult to suppress, and the sputter deposition rate of internal surface upper film is lower, and process efficiency is poor.The employing of plasma Immersion ion implantation technique, though mf is extended to compound film, and the bonding properties of film and substrate makes moderate progress, but still can not overcome the low shortcoming of sputtering yield.
1996; Yang Size etc. have reported that the using plasma source ion injects (Plasma Source IonImplantation-PSII) technology; Carry out the RP of ion implantation Inner Surface of Metal Pipe, relevant improvement technology has been applied for Chinese invention patent (ZL01115523.X, ZL03105058.1; ZL200310113092.6, ZL200380110083.X).The plasma source ion implantation technique that is adopted; Invented (US4764394) in 1987 by Conrad at first; Subsequently; Tendys etc. published thesis on Applied Physics Letters " Plasma immersion ion implantation using plasmas generated by radiofrequency technologies " in 1988, had reported plasma Immersion ion implantation (PIII) technology.Be collectively referred to as plasma based ion after two kinds of technology and inject (Plasma-Based Ion Implantation-PBII) technology.The plasma based ion implantttion technique is directly to be immersed in processed workpiece in the plasma body; Workpiece injects power supply with energetic ion and directly links to each other, and workpiece is applied successive high impulse negative bias, under each negative high voltage pulse action; Form the ion sheath layer around the workpiece; Ion then is accelerated through sheath layer electric field potential drop, from the vertical simultaneously bombardment workpiece surface of all directions, realizes omnibearing ion implantation.This technology has been eliminated " sight line processing " restriction that the conventional ion bunch injects, and does not need workpiece motion s system or ion beam scanning systems, and the surface-treated of special-shaped workpiece is achieved.Therefore, the plasma based ion implantttion technique for the surface-treated that realizes being similar to special-shaped workpiece such as Inner Surface of Metal Pipe provides from principle maybe.Yang Size etc. are at first through introducing coaxial ground-electrode on the central axis of metal tube; Metal tube applies the high impulse negative bias; Between pipe fitting inside center electrode and inwall, set up the uniform electric field of circumferential and axial, effectively improved ion implantation modified effect.But; Because the plasma body in the pipe fitting mainly relies on the pipe fitting two-port to transport to internal divergence; The plasma density of pipe fitting inside is skewness property vertically, and pipe fitting modifying inner surface poor further attempts utilizing the externally-applied magnetic field confining plasma; Increase pipe fitting inner plasma density and homogeneity, still can not satisfy the requirement of even modification.
Calendar year 2001, Yang Size etc. have proposed the uniform plasma source ion injection method of a kind of long metal pipe spare internal surface-grid again and have strengthened plasma source ion implantation (Grid Enhanced PSII) method.On keeping the metal tube axis former introduced coaxial electrode in; Increase the coaxial grid electrode of a ground connection between central electrode and pipe fitting inner wall; Produce plasma body through radio frequency discharge between central electrode and grid; Under the high impulse negative bias effect that metal tube applies, see through grid and be diffused into the ion in the plasma body between grid and pipe fitting inner wall, be injected into the pipe fitting internal surface from all directions.In order to overcome the ion implantation uneven problem that the aperture plate shade influence causes; Through grid electrode relatively move and in the pipe fitting outside or central electrode inside apply magnetic field; Improve the homogeneity of plasma body, increase the sputtering raste of central electrode, effectively improve the radio frequency plasma volume density.Although grid strengthens the plasma source ion implantation technique; In the metal tube set inside equally distributed direct current of plasma body circumferential and axial or radio frequency plasma body source, improve pipe fitting inner plasma density and homogeneity, improved the modified effect of long metal pipe spare internal surface; Yet; Based on the Inner Surface of Metal Pipe method of modifying of plasma based ion implantttion technique, still exist following three main drawbacks: (one) improves the quality of modified layer in order to guarantee enough ion implantation modification layer depth; Must adopt and be higher than 10kV high impulse negative bias; Because the pulse negative high voltage with workpiece directly links to each other causes ion sheath layer variation range very big, in order to reach uniform injection effect; Must keep enough distances between plasma source and workpiece, thereby the Inner Surface of Metal Pipe that causes handling internal diameter 10～50mm is still limited; (2) plasma based ion is injected small-caliber metal tubes spare internal surface, in order to obtain the effective modified layer degree of depth, needs plasma density to be higher than 10
10Cm
-3High-density plasma source, at present grid enhanced direct current or radio-frequency plasma source plasma density are on the low side, can not meet the demands; (3) secondary electron emission of using the high impulse negative bias to produce causes the huge waste of rating of set, and secondary electron also brings intensive x x radiation x simultaneously.These drawbacks limit the application of the Inner Surface of Metal Pipe modification technology that injects based on plasma based ion.
In order to further develop the plasma based low-energy ion implantation technique; Overcome its existing technical disadvantages; Nineteen ninety-five; Lei Mingkai etc. publish thesis " Plasma source ion nitriding:a new low-temperature, low-pressure nitridingapproach " at Journal of Vacuum Science and Technology A, have reported plasma based low-energy ion implantation (Plasma-Based Low Energy IonImplantation-PBLEII) technology; The high impulse negative bias that plasma based ion is injected is reduced to below the 3kV, and this technology becomes the typical case of existing low energy ion implantttion technique.The research and development thinking of plasma based low-energy ion implantation technique is: " low energy " advantage of utilizing the low energy ion bunch implantttion technique that Byeli in 1992 and Williamson in 1994 etc. report respectively on Wear and Surface and Coatings Technology; Combine with " comprehensive " advantage of plasma based ion implantttion technique; Adopt the ECR microwave plasma of higher ion volume density, high electronic temp and high ionization level; In conjunction with applying low pulsed negative bias and auxiliary outer thermal source; Inject combination diffusion synchronously through low energy ion, be implemented in the surface treatment of high mass transfer efficiency under 200 ℃ of ultralow technological temperatures.Compare with the plasma based ion implantttion technique, the plasma based low-energy ion implantation technique has significantly increased the modified layer degree of depth and homogeneity, and the surface-treated effect significantly improves, and has saved apparatus cost and tooling cost simultaneously greatly.Therefore; The plasma based low-energy ion implantation technique is used for the Inner Surface of Metal Pipe modification; Can overcome shortcoming () and (three) effectively based on the modifying inner surface method existence of plasma based ion implantttion technique; But owing to lack the linear plasma source of the high-density with unidimensional scale that is applicable to inner surface treatment, the restriction of shortcoming (two) still exists.
2005; Glukhoy etc. publish thesis at Surface and Coatings Technology " Characterization of a high-density plasma immersion ion implanter with scaleableECR large-area plasma source "; Big area, the high-density ECR microwave plasma source of the integrated designs of new ideas have been reported; It is made up of m ECR microwave plasma cell array, and each ECR microwave plasma cell array is made up of n ECR microwave plasma body unit, and each ECR microwave plasma unit comprises microwave coaxial Waveguide slot radiating antenna and permanent-magnet; The gap radiation antenna is employed in the slit design that oriented parallel is offered on the coaxial waveguide outer conductor; Circumferential subtended angle θ=120 °, for microwave frequency 2.45GHz, the slit spacing is λ/4=30.4mm; Two permanent-magnets are separately fixed at the both sides, slit, and slit surrounding magnetic field intensity reaches the magneticstrength 0.0875T of ECR.Satisfy the high-density plasma source of the diameter 200mm of 8 inches silicon chip processing requirements of diameter; Need m=4 ECR microwave plasma cell array; 2.5 inches of array pitch, each ECR microwave plasma source array then has n=9 ECR microwave plasma body unit; Satisfy the high-density plasma source of the diameter 300mm of 12 inches silicon chip treatment requirement of diameter, then need n * m=15 * 6=90 ECR microwave plasma body unit.Because the purpose of this research is development big area, highdensity plasma source; The ECR microwave plasma cell array of report only is suitable for producing unidirectional plasma body; There is not to form the equally distributed plasma body of circumferential and axial with unidimensional scale; Still can't satisfy the demand of the ion implantation Inner Surface of Metal Pipe of plasma based low-energy, therefore, demand developing highdensity linear plasma source urgently the linear plasma source of high-density.
Summary of the invention
The object of the invention and task are that the Inner Surface of Metal Pipe method of modifying that will overcome based on the plasma based ion implantttion technique exists: (one) is in order to guarantee enough ion implantation modification layer depth; Improve the quality of modified layer; Must adopt and be higher than 10kV high impulse negative bias; Because the pulse negative high voltage with workpiece directly links to each other causes ion sheath layer variation range very big, in order to reach uniform injection effect; Must keep enough distances between plasma source and workpiece, thereby the Inner Surface of Metal Pipe that causes handling internal diameter 10～50mm is still limited; (2) plasma based ion is injected small-caliber metal tubes spare internal surface, in order to obtain the effective modified layer degree of depth, needs plasma density to be higher than 10
10Cm
-3High-density plasma source, at present grid enhanced direct current or radio-frequency plasma source plasma density are on the low side, can not meet the demands; (3) secondary electron emission of using the high impulse negative bias to produce; Cause the huge waste of rating of set; Secondary electron also brings the shortcoming of intensive x x radiation x simultaneously; A kind of linear ECR microwave plasma source that on the metal tube central axis, produces high density plasma is provided, replaces low-density direct current or radio frequency plasma body source, in conjunction with the plasma based low-energy ion implantation on internal surface of metal round pipe with small pipe diameter device that applies low pulsed negative bias and auxiliary outer thermal source.
The technical scheme that the present invention adopted is: a kind of microwave plasma based low-energy ion implantation on internal surface of metal round pipe with small pipe diameter device; It mainly comprises: the Vakuumkammer that the ceramic disrance sleeve of metal to be treated pipe fitting inner coaxial setting with it and both side ends flange constitute; The low energy ion that links to each other with the metal to be treated fitting to fitting injects power supply; It also comprises: outside Vakuumkammer; Place the linear electron cyclotron resonance microwave plasma source on the metal to be treated pipe fitting central axis, the boosting source that metal to be treated pipe fitting outer, coaxial is provided with, its special character is:
(a) said linear electron cyclotron resonance microwave plasma source; On metal to be treated pipe fitting central axis, form high-density ECR microwave plasma with unidimensional scale; Thereby low-density direct current or radio frequency plasma body source have been replaced; Inject the low pulsed negative bias that power supply applies and the auxiliary outer thermal source of coaxial setting in conjunction with low energy ion; It is ion implantation to accomplish plasma based low-energy at the metal circular tube internal surface, realizes that the modifying inner surface of internal diameter 10～50mm, long 200～500mm metal circular tube is handled;
(b) said linear electron cyclotron resonance microwave plasma source is to be made up of microwave source, microwave coaxial waveguide inner wire, microwave coaxial waveguide outer conductor, microwave coaxial waveguide short piston and externally-applied magnetic field coil; Through microwave gap radiation aerial radiation microwave energy; Excite the working gas indoor with electric vacuum; Magneticstrength adding the magneticfield coil generation satisfies under the condition of ECR, forms the equally distributed high-density ECR microwave plasma of circumferential and axial along metal to be treated pipe fitting central axis;
(c) outside at said metal to be treated pipe fitting; The boosting source of coaxial setting is with metal to be treated pipe fitting circumferential and axial even heating; Under low-energy ion bombardment and boosting acting in conjunction; The temperature of metal to be treated pipe fitting evenly rises to technological temperature, guarantees that pipe fitting internal surface low energy ion injects the mass transfer process of following synchronous diffusion.
Microwave plasma based low-energy ion implantation on internal surface of metal round pipe with small pipe diameter device proposed by the invention; Its further special character is: the external diameter of said microwave coaxial waveguide inner wire compares b/a=2.303 with the internal diameter of microwave coaxial waveguide outer conductor; Adopt the internal diameter b=7～16mm of standard coaxial waveguide outer conductor; Nk the gap radiation antenna that the spiral-line rule is offered in coaxial waveguide outer conductor upper edge, wavelength width of a slit is 0.2～0.3mm, circumferential subtended angle θ=30～120 °.
Microwave plasma based low-energy ion implantation on internal surface of metal round pipe with small pipe diameter device proposed by the invention; The magneticstrength that ECR takes place should be satisfied in the magnetic field that said externally-applied magnetic field coil produces in Vakuumkammer; For microwave frequency 2.45GHz; The axial magnetic field intensity that the externally-applied magnetic field coil produces is 0.0875T, is adding under the action of a magnetic field along the gap radiation antenna of spiral-line regular distribution, forms the equally distributed high-density ECR microwave plasma of circumferential and axial with unidimensional scale.
Adopt the guiding theory of technique scheme to be: on the ion implantation metal surface modification device basic of existing plasma based low-energy; Be employed in the linear ECR microwave plasma source that produces high density plasma on the metal tube central axis; Replace low-density direct current or radio frequency plasma body source; In conjunction with the auxiliary outer thermal source that applies low pulsed negative bias and coaxial setting; Inner Surface of Metal Pipe at internal diameter 10～50mm, long 200～500mm realizes that low energy ion injects the mass transfer process of following synchronous diffusion, carries out the ion implantation Inner Surface of Metal Pipe of ECR microwave plasma based low-energy and handles.
Advantage of the present invention is: one, owing to adopt the linear ECR microwave plasma source of high-density; Inject power supply and boosting source in conjunction with low energy ion; Synchronous diffusion is followed in the low energy ion injection that has guaranteed Inner Surface of Metal Pipe, has realized the ion implantation Inner Surface of Metal Pipe modification processing of plasma based low-energy; Two, utilize exciting and ionizing event of microwave gap radiation antenna; Adding under the magnetic excitation; Form the equally distributed high-density ECR microwave plasma of circumferential and axial along the metal tube central axis, can satisfy the industrial requirement of little caliber, the processing of big L/D ratio Inner Surface of Metal Pipe; Three, owing to adopt low energy ion to inject power supply and boosting source; The ion implantation Inner Surface of Metal Pipe treatment unit of plasma based low-energy; Omit the energetic ion that involves great expense and injected power supply; The cost of device significantly reduces, has no adverse effects for environment, and be a kind of eco-friendly surface engineering technology.
Description of drawings
Fig. 1 is the structural profile synoptic diagram of microwave plasma based low-energy ion implantation on internal surface of metal round pipe with small pipe diameter device.1. microwave source, 2. microwave coaxial waveguide inner wire, 3. microwave coaxial waveguide outer conductor, 4. gap radiation antenna; 5. microwave coaxial waveguide short piston, 6. ceramic disrance sleeve, 7. Vakuumkammer, 8. boosting source; 9. externally-applied magnetic field coil, 10. low energy ion injects power supply, 11. metal to be treated pipe fittings; 12. end flange, 13. inlet mouths, 14. bleeding points.
Among Fig. 1, solid arrow is Vakuumkammer 7 airintake directions, and dotted arrow is Vakuumkammer 7 direction of bleeding.Coaxial waveguide outer conductor 3 outer wall upper edge spiral-linees are evenly offered gap radiation antenna 4, and the pitch of its spiral-line is λ/4, and λ is a microwave wavelength, and in each distribution spiral-line cycle, circumferentially central position ± θ/2=0 ° of subtended angle θ is respectively α
0, α
1..., α
i..., α
k, α wherein
i=i (360 °/k), (i=1,2,3 ..., k).
Fig. 2, Fig. 3 and Fig. 4 are the cross sectional representation that the gap radiation antenna of linear ECR microwave plasma source changes a distribution period inner structure, and wherein: Fig. 2 is the α among Fig. 1
oXsect, Fig. 3 are α among Fig. 1
iXsect, Fig. 4 are α among Fig. 1
kXsect.
In Fig. 2～4, a. microwave coaxial waveguide inner conductor outer diameter, b. coaxial waveguide outer conductor internal diameter, d
1. ceramic disrance sleeve internal diameter, d
2. ceramic disrance sleeve external diameter, d
3. metal to be treated pipe fitting internal diameter, d
4. metal to be treated pipe fitting external diameter.Circumferentially the central position of subtended angle θ is α
0And α
kThe circumferential position of gap radiation antenna 4 overlap.
Embodiment
Compare with the ion implantation Metal Surface Modification Technique of existing plasma based low-energy; Microwave plasma based low-energy ion implantation on internal surface of metal round pipe with small pipe diameter modification technology; Can produce the linear ECR microwave plasma of high-density, high electronic temp and high ionization level that circumferential and axial with unidimensional scale all are evenly distributed; Follow synchronous diffusion in nonmetallic ion injections such as the inner low energy nitrogen of metal tube, carbon, boron; Reach enough modified layer degree of depth, thereby have extensive industrialized application prospect in the material surface engineering field.Below in conjunction with specific embodiment, further specify details of the present invention.
Fig. 1 is the structural profile synoptic diagram of microwave plasma based low-energy ion implantation on internal surface of metal round pipe with small pipe diameter device.
Fig. 2, Fig. 3 and Fig. 4 are the cross sectional representation that the gap radiation antenna of linear ECR microwave plasma source changes a distribution period inner structure.
The typical process parameter of microwave plasma based low-energy ion implantation on internal surface of metal round pipe with small pipe diameter device proposed by the invention is: metal to be treated round tube inside diameter 10～50mm, long 200～500mm, outside dimension does not have particular restriction.Microwave source frequency 2.45GHz, power 500～5000W, the uniform magnetic field intensity 0.0875T that the externally-applied magnetic field coil produces, ECR microwave plasma volume density 10
10～10
11Cm
-3, electronic temp 3～7eV, ionization level～10%, operating air pressure (1～10) * 10
-2Pa, DC pulse negative bias-0.5～-3kV, 200～700 ℃ of technological temperatures, treatment time 4～10hr.Microwave plasma based low-energy ion implantation on internal surface of metal round pipe with small pipe diameter device proposed by the invention is 0.2～0.3mm in wavelength width of a slit, and when Nk=15～50 a gap radiation antenna stabilization was worked, required microwave source power was 500～5000W; Operating air pressure (1～10) * 10
-2Pa guarantees ion implantation typical air pressure; Under this high vacuum condition; The ionic free path is long, DC pulse negative bias-0.5～-the 3kV effect under, the energy barrier that the ion that arrives the metal tube surface can overcome the pipe fitting surface gets into the surface; The realization low energy ion injects; Technological temperature is the ion implantation typical process temperature of plasma based low-energy for 200～700 ℃, corresponds respectively to the ceiling temperature of conventional ion beamline ion implanters injection and the lower limit temperature that the plasma heat chemical diffusion is handled, and enough treatment time 4～10hr assurance low energy ions inject follows synchronous diffusion; Reach enough modified layer degree of depth, guarantee to obtain plasma based low-energy ion implantation modification surface.
The operation steps of microwave plasma based low-energy ion implantation on internal surface of metal round pipe with small pipe diameter device proposed by the invention is:
The first step, the installation workpiece also vacuumizes
Metal to be treated pipe fitting 11 and ceramic disrance sleeve 6 are assembled into Vakuumkammer 7 with both side ends flange 12, and the inspection stopping property is opened bleeding point 14 and is vacuumized, and keeps vacuum tightness to be higher than 8 * 10
-4Pa;
Second step, transportation work gas and heated parts
Open inlet mouth 13, charge into working gas and make the operating air pressure of Vakuumkammer 7 keep running balance, reach (1～10) * 10 until operating air pressure
-2Pa, with the 8 energising work of boosting source, the temperature of metal to be treated pipe fitting 11 is heated to and is lower than 30～80 ℃ of technological temperatures;
In the 3rd step, produce homogeneous plasma
With the 9 energising work of externally-applied magnetic field coil; The axial magnetic field of ECR condition is satisfied in generation; Microwave source 1 is started, and microwave transmits along coaxial waveguide, and by gap radiation antenna 4 circumferential and axial homogeneous radiations; Under the action of a magnetic field, in Vakuumkammer, produce the ECR microwave plasma that circumferential and axial all are uniform state;
In the 4th step, apply pulsed negative bias and begin treatment process
Start low energy ion injection power supply 10 and apply pulsed negative bias to metal to be treated pipe fitting 11; Utilize the ECR microwave plasma that forms in the Vakuumkammer 7; Make the temperature of metal to be treated pipe fitting 11 reach 200～700 ℃ of technological temperatures, carry out the ion implantation Inner Surface of Metal Pipe of plasma based low-energy and handle;
The 5th step, shutdown inspection
After the ion implantation treatment time 4～10hr of plasma based low-energy finished, the metal tube 11 that was processed was taken off in shutdown, and the thickness and the homogeneity of check modified layer can be for use after qualified.
Embodiment 1:
Certain machine works requires to make microwave plasma based low-energy ion implantation on internal surface of metal round pipe with small pipe diameter device; To internal diameter is 10mm; Wall thickness 1mm, the austenitic stainless steel pipe spare internal surface of long 200mm carries out the ion implantation processing of plasma based low-energy nitrogen, and its concrete processing parameter is following:
Microwave source power 2000W, microwave coaxial waveguide inner wire 2 external diameters of linear ECR microwave plasma source are 3mm, and coaxial waveguide outer conductor 3 internal diameters are 7mm, have Nk=13 gap radiation antenna, and wavelength width of a slit is 0.2mm, circumferential subtended angle θ=30 °.
The nitrogen operating air pressure of Vakuumkammer 7 reaches 1 * 10
-2Pa applies pulsed negative bias-0.5kV to austenitic stainless steel pipe spare, and the temperature of austenitic stainless steel pipe spare reaches 400 ℃ of technological temperatures, carries out the ion implantation pipe fitting inner surface treatment of plasma based low-energy; After treatment time 4hr finishes, shutdown; Through detecting, it is 5 μ m that austenitic stainless steel pipe spare injects modified layer thickness, and surface nitrogen concentration reaches 30at%, and is up-to-standard, and product performance satisfy user's requirement.
Embodiment 2:
Certain steel mill requires to make microwave plasma based low-energy ion implantation on internal surface of metal round pipe with small pipe diameter device; To internal diameter is 20mm; Wall thickness 1mm, the titanium alloy pipe fitting internal surface of long 300mm carries out the ion implantation processing of plasma based low-energy nitrogen, and its concrete processing parameter is following:
Microwave source power 3000W, microwave coaxial waveguide inner wire 2 external diameters of linear ECR microwave plasma source are 3mm, and coaxial waveguide outer conductor 3 internal diameters are 7mm, have Nk=28 gap radiation antenna, and wavelength width of a slit is 0.2mm, circumferential subtended angle θ=60 °.
The nitrogen operating air pressure of Vakuumkammer 7 reaches 5 * 10
-2Pa applies pulsed negative bias-3kV to the titanium alloy pipe fitting, and the temperature that is processed the titanium alloy pipe fitting reaches 650 ℃ of technological temperatures, carries out the ion implantation pipe fitting inner surface treatment of plasma based low-energy; After treatment time 8hr finishes, shutdown; Through detecting, it is 10 μ m that the titanium alloy pipe fitting injects modified layer thickness, and surface nitrogen concentration reaches 50at%, and is up-to-standard, and product performance satisfy user's requirement.
Embodiment 3:
Certain machine tool plant requires to make microwave plasma based low-energy ion implantation on internal surface of metal round pipe with small pipe diameter device; To internal diameter is 50mm; Wall thickness 5mm, the Martensite Stainless Steel pipe fitting internal surface of long 500mm carries out the ion implantation processing of plasma based low-energy nitrogen, and its concrete processing parameter is following:
Microwave source power 5000W, microwave coaxial waveguide inner wire 2 external diameters of linear ECR microwave plasma source are 7mm, and coaxial waveguide outer conductor 3 internal diameters are 16mm, have Nk=46 gap radiation antenna, and wavelength width of a slit is 0.3mm, circumferential subtended angle θ=120 °.
The nitrogen operating air pressure of Vakuumkammer 7 reaches 3 * 10
-2Pa applies pulsed negative bias-2kV to the Martensite Stainless Steel pipe fitting, makes the temperature of Martensite Stainless Steel pipe fitting reach 200 ℃ of technological temperatures, carries out the ion implantation pipe fitting inner surface treatment of plasma based low-energy; After treatment time 10hr finishes, shutdown; Through detecting, it is 15 μ m that the Martensite Stainless Steel pipe fitting injects modified layer thickness, and surface nitrogen concentration reaches 20at%, and is up-to-standard, and product performance satisfy user's requirement.
Embodiment 4:
Certain machine works requires to make microwave plasma based low-energy ion implantation on internal surface of metal round pipe with small pipe diameter device; To internal diameter is 30mm; Wall thickness 6mm; The austenite-ferrite duplex stainless steel pipe fitting internal surface of long 300mm carries out the plasma based low-energy carbon ion and injects processing, and its concrete processing parameter is following:
Microwave source power 3000W, microwave coaxial waveguide inner wire 2 external diameters of linear ECR microwave plasma source are 7mm, and coaxial waveguide outer conductor 3 internal diameters are 16mm, have Nk=28 gap radiation antenna, and wavelength width of a slit is 0.2mm, circumferential subtended angle θ=120 °.
The methane operating air pressure of Vakuumkammer 7 reaches 1 * 10
-1Pa applies pulsed negative bias-2kV to austenite-ferrite duplex stainless steel pipe fitting, and the temperature of austenite-ferrite duplex stainless steel pipe fitting reaches 560 ℃ of technological temperatures, carries out the ion implantation pipe fitting inner surface treatment of plasma based low-energy; After treatment time 4hr finishes, shutdown; Through detecting, it is 20 μ m that austenite-ferrite duplex stainless steel pipe fitting injects modified layer thickness, and surface carbon concentration reaches 20at%, and is up-to-standard, and product performance satisfy user's requirement.
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| CN102413627B (en) * | 2011-07-22 | 2013-03-20 | 中国科学院空间科学与应用研究中心 | Method for changing parameter of plasma |
| CN103114278B (en) * | 2013-02-06 | 2014-12-24 | 上海君威新能源装备有限公司 | Planar magnetic control ECR-PECVD (Electron Cyclotron Resonance Plasma-Enhanced Chemical Vapor Deposition) plasma source device |
| CN105134340A (en) * | 2015-09-24 | 2015-12-09 | 重庆市科学技术研究院 | Titanium pipe electric purification device for automobile exhaust gas |
| KR101858867B1 (en) * | 2016-12-23 | 2018-05-16 | 한국기초과학지원연구원 | Plasma processing apparatus for generating a plasma by emitting a microwave in a chamber |
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| CN115978785B (en) * | 2022-12-19 | 2024-03-19 | 四川大学 | A coaxial slotted radiator, continuous flow liquid heating system and heating method |
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