CN1137284C - Method for modifying inner surface of tubular workpiece - Google Patents
Method for modifying inner surface of tubular workpiece Download PDFInfo
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- CN1137284C CN1137284C CNB01115523XA CN01115523A CN1137284C CN 1137284 C CN1137284 C CN 1137284C CN B01115523X A CNB01115523X A CN B01115523XA CN 01115523 A CN01115523 A CN 01115523A CN 1137284 C CN1137284 C CN 1137284C
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- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000005468 ion implantation Methods 0.000 claims abstract description 7
- 239000010406 cathode material Substances 0.000 claims abstract description 5
- 238000004544 sputter deposition Methods 0.000 claims abstract description 5
- 150000002500 ions Chemical class 0.000 claims description 24
- 238000009792 diffusion process Methods 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 230000001133 acceleration Effects 0.000 claims description 6
- 229960005419 nitrogen Drugs 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 4
- 230000005684 electric field Effects 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 3
- 230000007246 mechanism Effects 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 238000012986 modification Methods 0.000 abstract description 7
- 230000004048 modification Effects 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 4
- 229910021645 metal ion Inorganic materials 0.000 abstract description 4
- 238000002347 injection Methods 0.000 abstract description 3
- 239000007924 injection Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 1
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- 230000002708 enhancing effect Effects 0.000 abstract 1
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- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 3
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000004453 electron probe microanalysis Methods 0.000 description 2
- 238000002513 implantation Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention belongs to the field of plasma material surface modification. The invention provides a method for enhancing inner surface modification of a grid, which comprises the following steps that a three-electrode system is formed by a cathode, a grid electrode and a sample, and the uniformity of dose and the uniform ion implantation are realized by applying radio frequency power and pulse negative high voltage; through cathode sputtering, particles of cathode materials are introduced into radio frequency plasma to realize inner surface coating and inner surface metal ion injection, so that modification means are more abundant. The invention improves the stability and accelerating voltage of the plasma by introducing the grid.
Description
The invention belongs to plasma material surface modification field.
Plasma source ion implantation (PSII) (document 1, J.R.Conrad, J.L.Radtke, R.A.Dodd, F.J.Worzala, N.C.Tran, J.Appl.Phys.
62(1987) 4591) be a kind of new material surface ion implantation technique, be particularly suitable for injecting sample with complicated shape.In this technology, by the magnetic multipole THE FILAMENT DISCHARGE AND, in a big vacuum chamber, produce a homogeneous plasma, the sample that injects is immersed in this plasma body fully, on sample, apply the negative high voltage pulse, like this, at impulse duration, the ion in the plasma body will be accelerated the upper layer that is injected into sample.
The PSII technology provides the possibility of ion implantation sample internal surface, but directly injects the very serious problem of internal surface existence of tubular specimen, the i.e. ununiformity of dosage and accelerating field with the PSII technology.For addressing this problem, we once proposed a kind of method based on PSII technology modifying inner surface (document 2, M.Sun, S.Z.Yang, Bing Li, J.Vac.Sci.Technol.,
A14, (1996) 367), caused domestic and international research and engineering technical personnel's interest (document 3, A.G.Liu, X.F.Wang, B.Y.Tang, P.K.Chu, J.Appl.Phys.
84(1998) 1859.4.T.E.Sheridan, T.K.Kwok, P.K.Chu, Appl.Phys.Lett.
72(1998) 1826).The main thought of this method is, as shown in Figure 1, Figure 1A is the schematic perspective view of modifying inner surface principle, Figure 1B is its sectional view, and a supplementary anode 3 is inserted tubular specimen 4 inside, and supplementary anode is connected with ground 13, sample is connected with a negative high voltage pulse power 2, like this, the negative high voltage impulse duration will be set up uniform electric field between supplementary anode and sample internal surface.When handling sample, in vacuum chamber, produce a plasma body by THE FILAMENT DISCHARGE AND, sample is placed in this plasma body.Plasma body can be by diffusing into the inner diffusion plasma body 1 that forms of tubular specimen, and wherein positive ion quickens to be injected into the sample internal surface under the accelerating field effect.In addition, because supplementary anode is to the booster action of electronics, more primary electron (primary electron is by filament emission and the high-energy electron that quickens through the cathode sheath layer) enters sample interior and strengthens the ionization of neutral gas, has improved plasma body 1 density and homogeneity thereof.But the weak point of this method is: outer plasma body forms by diffusion because the plasma body of sample interior mainly is a sample, therefore certainly exist diffusion gradient, plasma distribution is uneven vertically, the heterogeneity that has caused implantation dosage thus, for elongated tubular (fineness ratio is less than 0.6), pipe middle part dosage is very little especially; Secondly, can not inject metal ion and deposit film.
The objective of the invention is to improve the deficiency of present modifying inner surface method, propose the method that a kind of grid strengthens modifying inner surface.This method is formed three-electrode system by negative electrode, grid electrode and sample, produces an axial equally distributed radio-frequency plasma by add radio frequency power between negative electrode and grid electrode, thereby has solved the inhomogeneity problem of dosage; Between sample and grid electrode, apply the pulse negative high voltage and set up the uniform electric field that quickens positive ion, thereby realize the uniform ion injection; By anticathode radio-frequency sputtering, can in radio-frequency plasma, introduce the ion or the atom of metal or other solid matters, can realize that internal surface plated film and internal surface metal ion inject.
The object of the present invention is achieved like this:
Fig. 2 is a core technology schematic diagram of the present invention, and wherein Fig. 2 A is a schematic perspective view, Fig. 2 B is a schematic cross-section, has also illustrated the ceramic jacket 10 in the sample outside in Fig. 2 B.The three-electrode system that the core component of the technology of the present invention is made up of cylindrical cathode 8, tubulose grid electrode 9 and tubular specimen 4.The concrete steps that realize are as follows:
(1) by shown in Figure 2, negative electrode 8 and tubulose grid electrode 9 are inserted sample 4 coaxially
Inside, three electrodes are coaxial, fixing.Negative electrode 8 and grid 9 are by sealing together
Shaft adapter is connected with vacuum chamber radio-frequency power supply 5 outward; Wherein negative electrode 8 is by every directly
And ground 13 connects.
(2) by shown in Figure 3, above-mentioned three-electrode system is placed vacuum chamber 11, vacuum chamber
Be connected with the vacuum system of forming by diffusion pump and mechanical pump 12.Working gas is by argon
Gas cylinder 14 and nitrogengas cylinder 15 provide, and it is gentle to change air pressure by fine setting needle-valve 7
The size of flow.For ease of the fine analysis of rete, at sample internal surface coordination not
Monocrystal silicon substrate is put in storing, like this by characterizing the silicon base surface characteristic, and can be indirect
Obtain some characteristics of sample internal surface rete.
(3) be evacuated to 10
-3Pa.
(4) charge into working gas to 0.1～1Pa, by radio-frequency power supply 5 output radio frequency powers, at the moon
Produce a uniform vertically stable state radio frequency plasma between the utmost point 8 and the grid 9
Body, and by radio-frequency sputtering mechanism cathode material atom and ion introducing etc. from
Daughter.This plasma body can expand to the tubular specimen internal surface by grid mesh
Loose, thereby between grid and sample internal surface, formed diffusion plasma body 1.
The diffusion plasma body is uniformly vertically, and this has just guaranteed to incide table in the sample
The dosage of face is uniform.
(5) sample 4 joins with pulse negative high voltage power source 2, at negative high voltage impulse duration, grid
And promptly form even radial electric field between the sample internal surface to acceleration of ions, enter
To be accelerated to the positive ion between grid and the sample internal surface and to be injected into table in the sample
Face.
(6) when negative high voltage is added on the sample, shape between sample internal surface and diffusion plasma body
Become plasma sheath.In the time scale of plasma electron frequency inverse,
Near the sample internal surface electronics at first is in the sample repulsion of negative potential and leaves
The sample internal surface forms a positive ion sheath to the motion of grid direction; At plasma body
In the time scale of ion frequency inverse, ion begins to be accelerated to the sample internal surface
Motion also is injected into internal surface, subtracts owing to the ion implantation space charge that causes simultaneously
Little, and then cause and further repulsion to electronics make the sheath edge to grid 9 sides
To motion, and finally terminate in grid, near grid, form stable plasma body
Emitting surface.In this case, the generation of plasma body and acceleration of ions are limited
In two zones, promptly negative electrode 8 and grid 9 produce plasma body, grid 9 and sample
The classical ion source that chamber and extraction system are formed.
(7) high-voltage pulse finishes, and plasma body recovers standard state.
(8) handle after one hour, close high-voltage power supply and radio frequency source, stop high vacuum, take out sample
Product.
If do not need the modification outside surface, then can be at sample outside cover one ceramic jacket 10 (shown in Fig. 2 B).
Show that by the measurement of langmuir type probe plasma density vertically is very even really, has reached desired result near the plasma body axial distribution sample internal surface.
By the material surface analytical technology, the chemical ingredients of the sample internal surface after the characterization process, result show, have deposited metallic diaphragm at the sample internal surface, and rete is also relatively more even vertically.
The present invention is owing to excite radio-frequency plasma between negative electrode and grid, plasma body density distribution vertically is even, the plasma density height, and plasma distribution does not vertically change with discharge air pressure, the isoparametric variation of sample fineness ratio, has fundamentally solved the problem of implantation dose uniformity.The present invention is by cathode sputtering mechanism, and the particle of cathode material can be incorporated into radio-frequency plasma, when cathode material is metal, can realize that metal ion injects or thin film deposition, makes modified method abundanter, can comprehensively improve the internal surface performance.Because the existence of grid, can finally be fixed on the sheath layer edge of dynamic change near the grid, ion is produced the district distinguish with acceleration of ions, reduced greatly on the one hand that negative high voltage pulse article on plasma soma is disturbed and the unstable that produces; On the other hand, can further improve acceleration voltage.
The present invention is described in detail below in conjunction with drawings and Examples:
Fig. 1 is the modifying inner surface technical schematic diagram.Wherein Figure 1A is a stereographic map, and Figure 1B is a sectional view.
Fig. 2 is that grid strengthens the modifying inner surface technical schematic diagram.Wherein Fig. 2 A is a stereographic map, and Fig. 2 B is a sectional view.
Fig. 3 is that grid strengthens internal surface technological system block diagram.
Fig. 4 is a plasma density axial distribution in the cylinder.
Fig. 5 is the different axial positions silicon face thin film compositions with the electron probe micro-analysis commercial measurement.Wherein Fig. 5 A is that silicon chip is placed synoptic diagram at cylinder face; Fig. 5 B is measured surface composition figure.
Fig. 6 is the x-ray photoelectron spectroscopy figure of Ti2p and N1s.Wherein Fig. 6 A is the x-ray photoelectron spectroscopy figure at the Ti2p of different film depth surveys; Fig. 6 B is N1sX photoelectron spectrum figure, and can illustrate has the titanium nitride composition in the film.
Wherein: 1. spread plasma body; 2. the negative high voltage pulse power; 3. supplementary anode; 4. tubular specimen; 5. radio-frequency power supply; 6. electric capacity; 7. fine setting needle-valve; 8. negative electrode; 9. grid electrode; 10. ceramic jacket; 11. vacuum chamber; 12. vacuum system; 13. ground; 14. argon bottle; 15. nitrogengas cylinder.
Embodiment 1:
By shown in Figure 3, the horizontal stainless steel of 5 millimeters of one long 40 centimetres, wall thickness is made vacuum chamber 11, it is some to which is provided with windows such as being used for observation, monitoring.One automobile cylinder is as tubular specimen 4 to be processed, be processed into cylindric negative electrode 8 with a titanium rod, be processed into cylindric grid 9 with a stainless steel aperture plate, coaxial fixing negative electrode and grid, and, make the coaxial fixed in position of negative electrode, grid and cylinder along the coaxial insertion of cylinder axis.Negative electrode is connected by the well-designed sealing coaxial fitting radio-frequency power supply 5 outer with being in vacuum chamber with grid, and wherein negative electrode is connected with the power utmost point of radio-frequency power supply by a stopping condenser 6, and grid is connected with ground 13.Between grid and negative electrode, set up radio frequency discharge, produce a uniform vertically plasma body.Negative bias is connected with injection tubular specimen 4 through the sealed window at vacuum chamber 11 tops.For the ease of carrying out various fine analyses, placed silicon single crystal vertically as substrate at the cylinder face different positions, can be by the analysis of silicon base being characterized indirectly the effect of modifying inner surface.
Wherein negative electrode 8 is processed by 99.9% metal titanium; Grid 9 is processed by the stainless steel aperture plate; Automobile cylinder as sample is of a size of φ 120mm (internal diameter) * 200mm.The air pressure of working gas nitrogen maintains 0.3Pa.Radio frequency power is 10 watts, for strengthening sputter, adds volts DS simultaneously on negative electrode, and direct-current discharge voltage maintains 1800 volts, and discharging current maintains 200 milliamperes.On sample, add 1000 volts of dc negative bias voltages.
With Langmuir probe the axial distribution of plasma density in the sample is measured, Fig. 4 is a plasma density axial distribution in the cylinder.For the ease of comparative effectiveness, the result of other two kinds of currently known methodss also is shown among this figure.The longitudinal axis be normalization method plasma density, transverse axis is represented axial location, initial point is selected in sample middle part.Last triangle is represented the axial distribution of plasma density of the present invention; Plasma body axial distribution in the original modifying inner surface technology of round dot symbolic representation; Circle represents to be immersed in the axial distribution of the interior plasma body of cylinder in the plasma body.Find out that through contrast sample interior plasma density homogeneity has improved greatly.Because in the previous method, the plasma body of sample interior is from the diffusion of sample outside, so density reduces density minimum in the middle part of pipe towards the pipe middle part; And plasma body of the present invention produces in inside, so internal density is even substantially, and maximum value is at the middle part.Because diffusion loss slightly reduces in two end plasma densitys of sample.
In order to confirm that the present invention can realize the homogeneity of ion implantation and deposition of metallic plasma and dosage really, composition analysis is carried out with the electron probe micro-analysis technology in monocrystal silicon sample surface after handling, Fig. 5 A represents silicon chip placement synoptic diagram, Fig. 5 B is the composition analysis result, represents with atomic percent.As can be seen from the figure contain two kinds of compositions of titanium and nitrogen in the film, about 2: 1 of titanium nitrogen ratio illustrate that the present invention has realized deposit metal films, and the composition axial distribution is even substantially.
With x-ray photoelectron spectroscopy the film valence state is analyzed, Fig. 6 is an analytical results.Presentation of results the formation of titanium nitride phase, simultaneously film is oxidized as can be seen.
From above experiment and analytical proof: grid strengthens the even modification that the modifying inner surface technology can realize the tubular specimen internal surface.In fact, this technology provides a kind of thinking of modifying inner surface, and whatsoever the sample of shape as long as can process grid and the negative electrode that meets the demands, just can be realized the modification of internal surface.The present invention is an example with the tubular specimen modifying inner surface only; other complicated shape sample modifying inner surface all can be solved by the three electrode configuration thoughts that the present invention proposes; therefore, everyly utilize three electrode configuration thoughts proposed by the invention, all should belong to the protection domain of this patent.
Claims (1)
1. the method for a modifying inner surface of tubular workpiece, it is characterized in that: may further comprise the steps: (1) inserts the tubulose sample interior coaxially to cylindrical cathode and tubulose grid electrode, will be coaxial by three electrodes that negative electrode, grid, sample are formed, fixing, negative electrode is connected by the outer radio-frequency power supply of sealing coaxial fitting and vacuum chamber with grid, wherein negative electrode is connected with the radio-frequency power supply power utmost point by stopping condenser, and grid is connected with radio-frequency power supply ground electrode and ground; (2) above-mentioned three-electrode system is placed vacuum chamber, vacuum chamber is connected with the vacuum system of being made up of diffusion pump and mechanical pump, working gas is provided by argon bottle and nitrogengas cylinder, by the size of fine setting needle-valve change air pressure and airshed, place monocrystal silicon substrate at sample internal surface different positions; (3) be evacuated to 10
-3Pa; (4) charge into working gas to 0.1～1Pa, by radio-frequency power supply output radio frequency power, between negative electrode and grid, produce a uniform vertically stable state radio-frequency plasma, and cathode material atom and ion are introduced plasma body by radio-frequency sputtering mechanism, this plasma body to the diffusion of tubular specimen internal surface, vertically uniformly spreads plasma body thereby form by grid mesh between grid and sample internal surface; (5) sample and pulse negative high voltage power source join, and at the negative high voltage impulse duration, form the even radial electric field to acceleration of ions between grid and sample internal surface, enter into positive ion between grid and sample internal surface and are accelerated and are injected into the sample internal surface; (6) when negative high voltage is added on the sample, form plasma sheath between sample internal surface and diffusion plasma body, in the time scale of plasma electron frequency inverse, near the sample internal surface electronics at first is in the sample repulsion of negative potential and leaves the sample internal surface and move to the grid direction, form a positive ion sheath, in the time scale of plasma ion frequency inverse, ion begins to be accelerated to the sample inner surface movement and is injected into internal surface, reduce owing to the ion implantation space charge that causes simultaneously, and then cause further repulsion to electronics, make the sheath edge move to the grid direction, and finally terminate in grid, near grid, form stable plasma emission face, in this case, the generation of plasma body and acceleration of ions are limited in two zones, and promptly negative electrode and grid produce plasma body, and grid and sample internal surface are drawn and speeding-up ion; (7) high-voltage pulse finishes, and plasma body recovers standard state; (8) handle after one hour, close high-voltage power supply and radio frequency source, stop high vacuum, take out sample.
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| CNB01115523XA CN1137284C (en) | 2001-04-27 | 2001-04-27 | Method for modifying inner surface of tubular workpiece |
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| CNB01115523XA CN1137284C (en) | 2001-04-27 | 2001-04-27 | Method for modifying inner surface of tubular workpiece |
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| CN1137284C true CN1137284C (en) | 2004-02-04 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1209491C (en) * | 2003-03-04 | 2005-07-06 | 中国科学院物理研究所 | Method and special apparatus for modifying inner surface of tubular workpiece |
| CN100368590C (en) * | 2003-12-26 | 2008-02-13 | 中国科学院物理研究所 | Apparatus for inner surface modification by plasma source ion implantation |
| US7851367B2 (en) * | 2006-08-31 | 2010-12-14 | Kabushiki Kaisha Toshiba | Method for plasma processing a substrate |
| CN101876065A (en) * | 2010-05-25 | 2010-11-03 | 大连理工大学 | Method for modifying inner surface of slender insulating tube by utilizing plasma discharge under normal pressure |
| CN102383115B (en) * | 2011-11-09 | 2013-04-10 | 南昌航空大学 | Method for preparing functionally gradient composite coating in osmosis plating |
| CN102400114B (en) * | 2011-11-09 | 2013-05-01 | 南昌航空大学 | Method for strengthening inner wall of tubular work piece through permeating electroless plating |
| US20160322198A1 (en) * | 2015-04-30 | 2016-11-03 | Infineon Technologies Ag | Ion Source for Metal Implantation and Methods Thereof |
| CN104831519A (en) * | 2015-05-21 | 2015-08-12 | 嘉兴市产品质量检验检测院 | Plasma system for continuously processing yarn materials |
| CN105163476B (en) * | 2015-08-21 | 2017-05-03 | 厦门大学 | Plasma discharge device |
| JP6744694B1 (en) * | 2019-12-03 | 2020-08-19 | 株式会社ソディック | Surface modifying device and surface modifying method |
| CN114657527A (en) * | 2022-03-25 | 2022-06-24 | 哈尔滨工业大学 | Method for improving injection uniformity of surface of outer raceway of bearing inner ring and verification method |
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