CN101045989B - Low energy ion implanter based on great area DC pulse plasma - Google Patents
Low energy ion implanter based on great area DC pulse plasma Download PDFInfo
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- CN101045989B CN101045989B CN2007101015875A CN200710101587A CN101045989B CN 101045989 B CN101045989 B CN 101045989B CN 2007101015875 A CN2007101015875 A CN 2007101015875A CN 200710101587 A CN200710101587 A CN 200710101587A CN 101045989 B CN101045989 B CN 101045989B
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Abstract
The present invention relates to material surface engineering, and is especially one low energy ion implanter based on great area DC pulse plasma. The ion implanter includes one metal vacuum chamber, one low energy ion implanting power source and one vacuum system, and features that one meshed metal sleeve set inside the vacuum chamber is applied with negative DC pulse bias with the a plasma power source the form plasma between the furnace inner wall and the meshed metal sleeve, and that the DC pulse plasma source and the low energy ion implanting device are combined inside the vacuum chamber and negative DC pulse bias is applied alternately on the meshed metal sleeve and the sample stage so as to generate plasma and implant low energy ion alternately. The present invention has the advantages of low cost and capacity of realizing great area ion implantation.
Description
Technical field
The present invention relates to the great area DC pulse plasma source and carry out the technology that nonmetallic ions such as plasma based low-energy nitrogen, carbon, boron inject, belong to the material surface engineering field.
Technical background
Ion implantation technique relates to multi-disciplinary a kind of infant industry technology such as physics, electrician, material.Ion implantation begin to be used for material surface modifying the seventies in 20th century, makes the wear-resisting, against corrosion, high temperature resistant of material, and functional performance such as light, electricity, superconduction be improved significantly.Ion implantation technique has the energy of injection and dosage is accurately controlled, advantages such as alloying rule limits such as the modified layer that forms is not balanced each other, be widely used in high-tech sectors such as information technology, advanced manufacturing and biomedical engineering, and promoted development of technologies greatly.Yet, the surface modification of a large amount of special-shaped component, must adopt technologies such as scanning of bundle spot or workpiece rotation to be achieved because of the vertical incidence of ion beam line, some positions, dead angle then are difficult to handle, promptly have so-called " sight line processing " limitation, simultaneously, the high energy ion beam beam spot size that the conventional ion bunch injects is less, modified technique efficient is on the low side, has restricted the wider application of technology.In order to overcome the defective of conventional ion bunch implantttion technique, the patent of invention US4764394 of J.R.Conrad in 1987 has proposed plasma source ion implantation (Plasma Source Ion Implantation-PSII) technology, 1988, the paper " Plasma immersion ionimplantation using plasmas generated by radio frequency technologies " on Applied Physics Letters such as J.Tendys was reported plasma Immersion ion implantation (Plasma Immersion Ion Implantation-PIII) technology.Be collectively referred to as plasma based ion after two kinds and inject the technology of (Plasma Based Ion Implantation-PBII), all be directly to be immersed in processed workpiece in the plasma body, workpiece is applied the pulse of successive negative high voltage, under each negative high voltage pulse action, form the ion sheath layer around the workpiece, ion then is accelerated by sheath layer potential drop, from the vertical simultaneously bombardment workpiece surface of all directions, thereby realizes omnibearing ion implantation.The plasma based ion implantttion technique 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 can realize that large-area ionic injects, and is achieved the surface modification of special-shaped workpiece.The plasma based ion implantttion technique is through after the development in nearly ten years, the problem of its existence also exposes gradually, mainly show: 1. owing to adopt the high impulse negative bias that directly puts on workpiece, secondary electron emission has caused the huge waste of rating of set, and secondary electron also brings the intensive X-radiation simultaneously; Although 2. omitted special ion source, powerful high-voltage pulse power source involves great expense equally, has increased the technology cost; 3. the homogeneity that the ion sheath layer influence surface that variation range is bigger is injected makes complex-shaped workpieces, and is still limited as the processing of aperture.These problems have been limited to the plasma based ion implantttion technique equally in industrial applications.
In order to further develop the plasma based ion implantttion technique, overcome its existing technical disadvantages, nineteen ninety-five, article " Plasmasource ion nitriding:a new low-temperature on Journal of Vacuum Science and Technology A such as Lei Mingkai, low-pressure nitriding approach " report plasma based low-energy ion implantation technique, 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 on the one hand the low energy ion bunch implantttion technique that A.V.Byeli in 1992 and D.L.Williamson in 1994 etc. report respectively on Wear and Surface and Coatings Technology, on the other hand in conjunction with " comprehensive " advantage of the plasma based ion implantttion technique of report such as J.R.Conrad and J.Tendys, adopt high-density, the plasma body of high electronic temp and high ionization level, in conjunction with applying pulsed negative bias and auxiliary outer thermal source, low energy ion by 0.4～3keV injects in conjunction with diffusion synchronously, is implemented in the surface treatment of high mass transfer efficiency under 200 ℃ of ultralow technological temperatures.The plasma based low-energy ion implantation technique has been improved the homogeneity of comprehensive ion implantation modification layer, reduce apparatus cost and tooling cost greatly, the injection ion energy of Jiang Diing is development great area DC plasma source simultaneously, further realize the large parts processing, and industrialized mass production provides the assurance on the know-why, but, there is following shortcoming in existing plasma based low-energy ion implantation technique: 1. comprise the direct current hot-cathode, the plasma body area that conventional plasma source such as radio frequency and microwave produces is less, is difficult to satisfy the requirement of large parts or industrialized mass production; 2. high-power (～10kW) the power supply manufacturing process complexity of radio frequency, microwave plasma source, cost is higher, and has the hazards of electromagnetic radiation of power supply concurrently; 3. plasma body is introduced by the plasma source generation back in the external world, and its homogeneity is difficult to guarantee, workpiece surface occurs in the injection process " focus " or superheat region, the surface quality of destruction processed workpiece; Therefore, research and development are applicable to that the large-area high uniformity plasma source that low energy ion injects becomes the main task that realizes plasma based low-energy ion implantation technique industrial applications.
1999, the patent of invention US5989363 of J.Georges etc. has introduced a kind of plasma based ion nitridation technique, its technical characterictic is to increase a metal guard negative electrode at the nitriding internal vacuum chamber, can apply the DC pulse negative bias on the guard, glow discharge takes place between guard and vacuum chamber inboard wall of furnace body, produce DC pulse plasma, in the guard space, be provided for the required homogeneous plasma of nitriding by this DC pulse plasma source, simultaneously, the heat temperature raising effect of discharging current on the guard, with the workpiece surface radiation heating, be provided for the required technological temperature of nitriding easily.The processing parameter of ion implantation technique requires: 1. high vacuum (being lower than 0.1Pa), and with this understanding, the ionic free path is long, and the ion of arrival workpiece surface still has high-energy, thereby has realized injection; 2. high negative bias (being higher than 1000V) will realize discharge under high vacuum, must increase negative bias, otherwise discharge can not take place; But (67Pa～180Pa), voltage is 500～600V to the operating air pressure of the guard that this patent proposes, and is only applicable to ionitriding technology, can not be applied to field ion implantation under rough vacuum.
Summary of the invention
Purpose of the present invention and task will overcome existing plasma based low-energy ion implantation technique and exist: the plasma body area that 1. comprises conventional plasma source generation such as direct current hot-cathode, radio frequency and microwave is less, is difficult to satisfy the requirement of large parts or industrialized mass production; 2. high-power (～10kW) the power supply manufacturing process complexity of radio frequency, microwave plasma source, cost is higher, and has the hazards of electromagnetic radiation of power supply concurrently; 3. plasma body produces the back introducing by the plasma source in the external world, its homogeneity is difficult to guarantee, workpiece surface occurs in the injection process " focus " or superheat region, destroy the deficiency of the surface quality of processed workpiece, and provide a kind of energy to produce cheap, large-area homogeneous plasma, and need not to increase special auxiliary thermal source and provide technology temperature required low energy ion implanter based on great area DC pulse plasma, technical solution of the present invention is proposed hereby.
Basic design of the present invention is: on conventional plasma based low-energy ion implantation apparatus basis, cancel the plasma source of various extraneous inputs, in the body of heater of metal vacuum chamber, increase a metal guard and do negative electrode, vacuum chamber body of heater ground connection is done anode, on guard, apply a direct current pulsed negative bias, make the discharge generation DC pulse plasma takes place between guard and inboard wall of furnace body, the plasma body that forms extends to guard inside, surround the workpiece on the sample table, by being applied to another high impulse negative bias on the sample table, carry out plasma based low-energy in guard inside ion implantation.Guarantee two pulsed negative bias alternating actions, the generation of DC pulse plasma and low energy ion injection process alternative are uninterruptedly carried out.
Low energy ion implanter based on great area DC pulse plasma proposed by the invention, comprise: Qi Bishang is evenly equipped with the cylindrical furnace (2) of a plurality of inlet mouths (4), be equipped with the base (1) of bleeding point (15), under the effect of sealing-ring (12), constitute metal vacuum chamber (5), low energy ion injection power supply (14) is located at the body of heater outside and links to each other with sample table (11), metal guard (6) is located in the body of heater, and it is coaxial with body of heater, hot-cathode filament (9) is located in the zone (7) between inboard wall of furnace body and the guard, and link to each other with the heater supply that is located at the body of heater outside (13), it is characterized in that:
(a) metal vacuum chamber (5) comprise the zone (7) between inboard wall of furnace body and the guard and the zone (10) of guard inside, two zones are communicated with by the mesh on the guard, in zone (7), produce great area DC pulse plasma, and can evenly spread and be transported to zone (10), it is ion implantation to finish plasma based low-energy in zone (10), thereby cancelled the independent plasma source that transports plasma body by the external world, great area DC pulse plasma source and low energy ion implanter are combined in the metal vacuum chamber (5), have realized low cost, large-area homogeneous plasma base low energy ion injects;
(b) large area plasma source is by constituting as anodic body of heater [2] with as the guard [6] of negative electrode, and plasma body source current [8] is located at the body of heater outside, applies the DC pulse negative bias to guard, feeds working gas, is 1～5 * 10 in vacuum tightness
-2Under the Pa condition, glow discharge taking place in zone [7], forms plasma body; Perhaps in this large area plasma source, increase the hot-cathode filament [9] that the discharge booster action is provided, at this moment, can reduce the DC pulse negative bias that is applied on the guard, form plasma body;
(c) plasma body source current (8) apply the DC pulse negative bias to guard and be-0.5～-3kV, frequency is 100～1000Hz, dutycycle is 1: 3～1: 10, low energy ion injects power supply (14) and applies the DC pulse negative bias to sample table and be-3～-5kV, frequency is 100～1000kHz, dutycycle is 1: 3～1: 10, two negative biass alternately take place, and the latter is than the former 0.3～8 μ s that lags behind, and guarantees that great area DC pulse plasma produces and alternately uninterruptedly the carrying out of low energy ion injection.
Low energy ion implanter based on great area DC pulse plasma proposed by the invention, it further is characterized as: metal guard (6) is for cup-shaped, uniform a plurality of mesh on it, the single hole area is 100～120mm
2, the total area in hole accounts for 1/2～4/5 of guard surface-area, has 50%～80% permeability, and guard is 80～100mm with the distance of inboard wall of furnace body radially, and axial height is 400～1800mm, and thickness is 5～8mm; Hot-cathode filament (9) diameter is 1～3mm, and total length is 3～15m, and filament applies volts DS 20～30V, current density 20～30A/mm
2When not adopting the booster action of hot-cathode filament, the DC pulse negative bias that plasma body source current (8) applies to guard (6) is-1.5～-3kV, when adopting the booster action of hot-cathode filament,
Cylindrical, its axis is vertical with base (1), highly is 500～2000mm, and the vacuum chamber volume is 0.4～4m
3, body of heater can upwards rise; Big 80～the 100mm of external diameter of base edge radius ratio body of heater; Circular sample table (11) is housed on base, and sample table is placed in the middle coaxial with base, and diameter insulate apart from base 80～100mm and with base less than guard (6) diameter 150～200mm; Bleeding point on the base (15) links to each other with vaccum-pumping equipment (as molecular pump or diffusion pump and mechanical pump unit), can make the vacuum tightness of vacuum chamber reach 5 * 10
-3More than the Pa; The quantity of inlet mouth (4) is 5～10, should guarantee that total sectional area is 1/5～1/10 of a bleeding point area; Body of heater and base are at the auxiliary formation vacuum chamber (5) down of sealing-ring (12), and vacuum chamber is made of two zones, is respectively: the zone (10) of the zone between inboard wall of furnace body and the guard (7) and guard inside, two zones are communicated with by the mesh on the guard.
Plasma body source current (8) is located at the vacuum chamber outside, links to each other with guard (6), and exportable DC pulse negative bias is-0.5～-3kV, frequency is 100～1000Hz, dutycycle is 1: 3～1: 10.The pulsed negative bias that is proposed for-0.5kV is under the booster action of hot-cathode filament, the lower voltage limit of discharge takes place between inboard wall of furnace body and the guard, when negative bias be lower than-during 0.5kV, sparking voltage is lower than voltage breakdown, discharge can not take place, and negative bias-3kV is under the booster action that does not have the hot-cathode filament, and the upper voltage limit of discharge takes place between inboard wall of furnace body and the guard, when negative bias is higher than 3kV, then need the DC pulse negative bias power supply of high cost; The pulsed negative bias lower frequency limit that is proposed is 100Hz, be for enough power output, keep the successional lower frequency limit of plasma body, the pulsed negative bias upper limiting frequency that is proposed is 1000Hz, is in order to satisfy the manufacturing requirement of low cost DC pulse negative bias power supply; The dutycycle that is proposed 1: 3rd, plasma body are not subjected to the lower limit of guard surface sputtering corrasion, when dutycycle during greater than 1: 3, can cause a large amount of sputters on guard surface long discharge time, pollute plasma body, influence the activity of plasma body, dutycycle 1: 10th keeps plasma body to keep the high active upper limit, when dutycycle during less than 1: 10, can cause the active decline of plasma body long time of persistence even buries in oblivion.
Low energy ion injects power supply (14) and is located at the vacuum chamber outside, links to each other with sample table (11), and exportable DC pulse negative bias is-3～-5kV, frequency is 100～1000kHz, dutycycle is 1: 3～1: 10.Voltage-the 3kV that is proposed is a lower voltage limit of realizing that low energy ion injects, be lower than-input horizon is shallow during 3kV, and modified effect is relatively poor, proposed-5kV is the upper voltage limit that low energy ion injects, be higher than-during 5kV, ion energy is higher, has exceeded the processing range that low energy ion injects; Frequency 100～the 1000Hz that is proposed is for the pulsed negative bias that is applied on the guard being equated with pulsed negative bias frequency on being applied to sample table, having guaranteed alternately taking place of two DC pulse negative biass; Dutycycle 1: 3rd, plasma body are not subjected to the lower limit of workpiece surface ise effect, when dutycycle during greater than 1: 3, a large amount of sputters of workpiece surface have been caused long discharge time, pollute plasma body, influence the activity of plasma body, dutycycle 1: 10th guarantees the upper limit of low energy ion injection efficiency, when dutycycle less than 1: 10, the time that low energy ion injects is short partially, and injection efficiency is on the low side.
Be positioned at zone (7) hot-cathode filament (9) and apply volts DS 20～30V, current density 20～30A/mm
2, the 20～30V that is proposed, 20～30A/mm
2, be filament remain valid power bound, be lower than 20V, 20A/mm
2The time, filament wattage is low excessively, is unfavorable for the generation of discharging being higher than 20V, 30A/mm
2The time, filament wattage is too high, blows easily.
The typical process parameter of low energy ion implanter based on great area DC pulse plasma proposed by the invention is: 200～570 ℃ of temperature, operating air pressure (1～5) * 10
-2Pa, injection length 4～12h.The low energy ion implanter based on great area DC pulse plasma that is used for proposed by the invention, need not increase special auxiliary thermal source just can provide technology temperature required, guard is under the heat temperature raising effect of discharging current, with the workpiece surface radiation heating, be provided for the technological temperature that low energy ion injects easily.Temperature is the ion implantation typical process temperature of plasma based low-energy for 200～570 ℃, correspond respectively to the ceiling temperature of conventional ion bunch injection and the lower limit temperature of thermochemistry diffusion, low energy ion injects follows synchronous thermochemistry diffusion, guarantees the degree of depth of ion implantation modification layer; Operating air pressure 1～5 * 10
-2Pa is ion implantation exemplary operation air pressure, and under this high vacuum condition, the ionic free path is long, and the ion that arrives workpiece surface still has high-energy, can overcome the potential barrier of workpiece surface and enters workpiece inside.
The operation steps of low energy ion implanter based on great area DC pulse plasma proposed by the invention is:
The first step, the dress workpiece also vacuumizes
The body of heater (2) of slinging, open vacuum chamber, after placing workpiece on the sample table (11), the resistance to air loss of closing vacuum chamber (5) and inspection units, check whether ground connection of body of heater and base (1), guarantee insulation between body of heater and the guard (6), open bleeding point (15) subsequently and vacuumize, guarantee that vacuum tightness is higher than 1 * 10
-3Pa;
In second step, supply gas
Open inlet mouth (4), charge into working gas and make the pressure in the vacuum chamber keep running balance, reach (1～5) * 10 until operating air pressure
-2Pa;
The 3rd step applied pulsed negative bias respectively, and it is ion implantation to carry out plasma based low-energy
Open plasma source current (8) and low energy ion inject power supply (14) simultaneously, two pulse powers alternating voltage output under the effect of timer, plasma body source current plasma body when the guard output voltage produces in zone (7), subsequently, low energy ion injects power supply on sample table during output voltage, the plasma body that produces is introduced zone (10) surround workpiece, realize that comprehensive low energy ion injects.
The 4th step, shutdown inspection
Vacuum chamber is opened in shutdown, the workpiece after take out handling, and the thickness and the homogeneity of check modified layer can be stand-by after qualified.
Advantage of the present invention is: 1. owing to adopted the plasma based low-energy of big area uniform DC pulsed plasma realization cheaply ion implantation, can satisfy large parts or industrialized mass production requirement; 2. because therefore the device that has adopted the based on great area DC pulse plasma low energy ion to inject need not to increase special auxiliary outer thermal source heat or supplementary heating are provided, device is further simplified; 3. because the device that has adopted the based on great area DC pulse plasma low energy ion to inject, great area DC pulse plasma source and low energy ion implanter are combined in the vacuum chamber, having overcome conventional plasma based low-energy ion implantation technique ionic medium body transports by the independent plasma source in the external world, the unmanageable disadvantage of its homogeneity has realized that low-cost, large-area homogeneous plasma base low energy ion injects.
Description of drawings
The present invention's design is totally two accompanying drawings, and Fig. 1 is the semi-section structural representation of low energy ion implanter based on great area DC pulse plasma; Fig. 2 is applied to the DC pulse negative bias sequence of operation on guard and the sample table and concerns synoptic diagram action time.
Below by the description of the drawings, further illustrate details of the present invention.
Fig. 1 is the semi-section structural representation of low energy ion implanter based on great area DC pulse plasma
Show among the figure, the body of heater of this device (2) and base (1) formation vacuum chamber (5) under the effect of sealing ring (12), vacuum chamber is made up of two parts, respectively zone (7) between inboard wall of furnace body and the guard and the zone (10) of guard inside, be equipped with bleeding point (15) on the base, be equipped with a plurality of air inlets (4) on the body of heater, body of heater and base ground connection, metal net mask (6) as negative electrode is housed in body of heater inside, at base circular sample stage (11) is housed, sample stage and base insulation, be equipped with workpiece (3) on the sample stage, hot cathode filament (9) is located in the zone (7), and link to each other with the filament supply that is located at the body of heater outside (13), plasma source current (8) can be exported the direct current pulsed negative bias to guard, and low energy ion injects power supply (14) can export the direct current pulsed negative bias to sample stage. Solid arrow is airintake direction among the figure, and dotted arrow represents outgassing direction.
Fig. 2 is applied to the direct current pulsed negative bias sequence of operation on guard and the sample stage and concerns schematic diagram action time
As shown in FIG., abscissa is time (t), and ordinate is voltage (U), and fine line represents that the plasma source current is to the direct current pulsed negative bias of guard output, wherein V1Be voltage, t1Be the cycle, t2Be the action time of direct current pulsed negative bias, t2∶t
1Be dutycycle; Dotted line represents that low energy ion injects power supply to the direct current pulsed negative bias of sample stage output, wherein V2Be voltage, T1Be the cycle, T2Be the action time of direct current pulsed negative bias, T2∶T
1Be dutycycle; T0For the back bias voltage on the sample stage lags behind time of the back bias voltage on the guard, the pass of two pulsed negative bias is: alternately take place, namely plasma source current and low energy ion inject not output voltage simultaneously of power supply.
Embodiment
Below in conjunction with specific embodiment, further specify details of the present invention:
Compare with conventional plasma based low-energy ion implantation technique, based on great area DC pulse plasma low energy ion implantttion technique can produce large-area homogeneous plasma, and low energy ion injects in conjunction with diffusion synchronously, increase the degree of depth of modified layer, thereby have extensive industrialized application prospect in the material surface engineering field.
Embodiment 1:
Certain machine works requires manufacturing plasma based low-energy ion implantation apparatus that the workpiece of the austenitic stainless steel of size 400mm * 400mm * 300mm is carried out the ion implantation processing of plasma based low-energy nitrogen, because the volume of workpiece is bigger, be difficult to satisfy its requirement with conventional plasma based low-energy ion implantation apparatus, the based on great area DC pulse plasma low energy ion implantttion technique that now adopts the present invention to propose is achieved, and its concrete parameter is as follows:
The cylindrical furnace of vacuum chamber (2) highly is 700mm, and internal diameter is 800mm; Base (1) is coaxial with body of heater, and it highly is 300mm, and internal diameter is 800mm; Guard (6) is coaxial with body of heater, and it highly is 400mm, and diameter is 700mm, and thickness is 5mm, and area of uniform mesh is 100mm on it
2, the total area in hole accounts for 1/2 of guard total surface area, and permeability is 50%; Sample table (11) is coaxial apart from base 100mm with guard, highly is 300mm, and radius is 500mm; Bleeding point (15) links to each other with a molecular pump, can make the vacuum tightness of vacuum chamber reach 5 * 10
-3More than the Pa; Five inlet mouths (4) are evenly distributed on the furnace body wall, account for 1/10 of bleeding point total sectional area.
Under the situation that satisfies above-mentioned installation design requirements:
The first step, the dress workpiece also vacuumizes
The body of heater of slinging is opened vacuum chamber (5), and workpiece is placed the resistance to air loss of rear enclosed vacuum chamber on the sample table and inspection units, checks whether ground connection of body of heater and base, guarantees to insulate between body of heater and the guard, opens bleeding point subsequently and is evacuated to 5 * 10
-3Pa closes then;
In second step, supply gas
Opening inlet mouth charges into nitrogen and reaches 5 * 10 until air pressure
-2Behind the Pa, the flow of opening bleeding point and regulating inlet mouth makes the pressure in the vacuum chamber keep running balance;
In the 3rd step, add negative bias and carry out ion implantation
Plasma body source current (8) applies DC pulse negative bias-3kV to guard, frequency is 100Hz, dutycycle is 1: 10, low energy ion injects power supply (14) and applies DC pulse negative bias-5kV to sample table, and frequency is 100Hz, and dutycycle is 1: 10, under the effect of timer, the latter is than the former the 8 μ s that lag behind, and technological temperature is 300 ℃, and injection length is 6h.
The 4th step, shutdown inspection
Vacuum chamber is opened in shutdown, takes out workpiece, after testing, adopting the workpiece nitriding modified layer thickness after the low energy ion implanter based on great area DC pulse plasma technical finesse of the present invention is 20 μ m, and the highest face temperature nitrogen concentration reaches 30at%, up-to-standard, product performance satisfy user's requirement.
Embodiment 2:
Certain steel mill requires to make the plasma based low-energy ion implantation apparatus and carries out the carbon ion injection to being of a size of Φ 500mm * 700mm 20CrMn steel workpiece, because the workpiece volume is bigger, be difficult to satisfy its requirement with conventional plasma based low-energy ion implantation apparatus, the based on great area DC pulse plasma low energy ion implantttion technique that now adopts the present invention to propose is achieved, and its concrete parameter is as follows:
The height of the body of heater of cylindrical vacuum chamber (2) is 1300mm, internal diameter 1100mm; Base (1) is coaxial with the body of heater axis, and it highly is 300mm, and internal diameter is 1100mm; Guard (6) is coaxial with the body of heater axis, and it highly is 1000mm, and diameter is 1000mm, and thickness is 6mm, and single hole area of uniform mesh is 110mm on it
2, the total area in hole accounts for 3/5 of guard surface-area, and permeability is 60%; Sample table (11) is coaxial apart from base 100mm with guard, highly is 300mm, and radius is 800mm.Bleeding point (15) links to each other with a mechanical pump unit with a diffusion pump, can make the vacuum tightness of vacuum chamber reach 5.5 * 10
-3More than the Pa; Eight inlet mouths (4) are evenly distributed on the furnace body wall, account for 1/7 of bleeding point total sectional area; Filament (9) total length is 3m, applies voltage 20V, electric current 20A.
Under the situation that satisfies above-mentioned installation design requirements:
The first step, the dress workpiece also vacuumizes
The body of heater of slinging is opened vacuum chamber (5), and workpiece is placed the resistance to air loss of rear enclosed vacuum chamber on the sample table and inspection units, opens bleeding point subsequently and is evacuated to 5 * 10
-3Pa closes then;
In second step, supply gas
Open that inlet mouth charges into methane and hydrogen mixed gas (ratio is 10: 90) reaches 3 * 10 until air pressure
-2Behind the Pa, the flow of opening bleeding point and regulating inlet mouth makes the pressure in the vacuum chamber keep running balance;
In the 3rd step, add negative bias and carry out ion implantation
Plasma body source current (8) applies DC pulse negative bias-1kV to guard, frequency is 500kHz, dutycycle is 1: 7, low energy ion injects power supply (15) and applies DC pulse negative bias-4kV to sample table, and frequency is 500kHz, and dutycycle is 1: 7, under the effect of timer, the latter is than the former the 1.5 μ s that lag behind, and technological temperature is 400 ℃, and injection length is 8h.
The 4th step, shutdown inspection
Vacuum chamber is opened in shutdown, takes out workpiece, after testing, adopting the workpiece carbonization modified layer thickness after the low energy ion implanter based on great area DC pulse plasma technical finesse of the present invention is 25 μ m, and the average carbon content in surface is 35at%, up-to-standard, product performance satisfy user's requirement.
Embodiment 3:
Certain machine tool plant requires to make plasma based low-energy ion implantation apparatus, and that 45 steel workpieces of 600mm * 600mm * 800mm are carried out boron is ion implantation, because the workpiece volume is bigger, be difficult to satisfy its requirement with conventional plasma based low-energy ion implantation apparatus, the based on great area DC pulse plasma low energy ion implantttion technique that now adopts the present invention to propose is achieved, and its concrete parameter is as follows:
The height of cylindrical vacuum chamber body of heater (2) is 1900mm, and internal diameter is 1200mm; Base (1) is coaxial with the body of heater axis, and it highly is 300mm, and internal diameter is 1200mm; Guard (6) is coaxial with the body of heater axis, and it highly is 1800mm, and diameter is 1100mm, and thickness is 8mm, and area of uniform mesh is 120mm on it
2, the total area in hole accounts for 4/5 of guard surface-area, and permeability is 80%; Sample table (11) is coaxial apart from base 100mm with guard, highly is 300mm, and radius is 900mm.Bleeding point (15) links to each other with a molecular pump, can make the vacuum tightness of vacuum chamber reach 5 * 10
-3More than the Pa; Ten inlet mouths (4) are evenly distributed on the furnace body wall, account for 1/5 of bleeding point total sectional area; Filament (9) total length is 15m, and voltage is 30V, and electric current is 30A.
Under the situation that satisfies above-mentioned installation design requirements:
The first step, the dress workpiece also vacuumizes
The body of heater of slinging is opened vacuum chamber (5), and workpiece is placed the resistance to air loss of rear enclosed vacuum chamber on the sample table and inspection units, opens bleeding point subsequently and is evacuated to 5 * 10
-3Pa closes then;
In second step, supply gas
Open the gas mixture (ratio is 5: 95) that inlet mouth charges into boron trichloride and hydrogen and reach 1 * 10 until air pressure
-2Behind the Pa, the flow of opening bleeding point and regulating inlet mouth makes the pressure in the vacuum chamber keep running balance;
In the 3rd step, add negative bias and carry out ion implantation
Plasma body source current (8) applies DC pulse negative bias-0.5kV to guard, frequency is 1000Hz, dutycycle is 1: 3, low energy ion injects power supply (14) and applies DC pulse negative bias-5kV to sample table, and frequency is 1000Hz, and dutycycle is 1: 3, under the effect of timer, the latter is than the former the 0.3 μ s that lags behind, and technological temperature is 500 ℃, and injection length is 10h.
The 4th step, shutdown inspection
Shutdown is opened vacuum chamber and is taken out workpiece, after testing, adopting the workpiece boronising modified layer thickness after the low energy ion implanter based on great area DC pulse plasma technical finesse of the present invention is 30 μ m, highest face temperature boron content is 30at%, and is up-to-standard, and product performance satisfy user's requirement.
Claims (3)
1. low energy ion implanter based on great area DC pulse plasma, comprise: Qi Bishang is evenly equipped with the cylindrical furnace [2] of a plurality of inlet mouths [4], be equipped with the base [1] of bleeding point [15], under the effect of sealing-ring [12], constitute metal vacuum chamber [5], low energy ion injection power supply [14] is located at the body of heater outside and links to each other with sample table [11], metal guard [6] is located in the body of heater, and it is coaxial with body of heater, hot-cathode filament [9] is located in the zone [7] between inboard wall of furnace body and the guard, and link to each other with the heater supply that is located at the body of heater outside [13], it is characterized in that:
(a), metal vacuum chamber [5], comprise the zone [7] between inboard wall of furnace body and the guard and the zone [10] of guard inside, two zones are communicated with by the mesh on the guard, produce great area DC pulse plasma in the zone between inboard wall of furnace body and guard [7], and can evenly spread the zone [10] that is transported to guard inside, it is ion implantation to finish plasma based low-energy in the zone [10] of guard inside, thereby cancelled the independent plasma source that transports plasma body by the external world, great area DC pulse plasma source and low energy ion implanter are combined in the metal vacuum chamber [5], have realized low cost, large-area homogeneous plasma base low energy ion injects;
(b), large area plasma source is by constituting as anodic cylindrical furnace [2] with as the metal guard [6] of negative electrode, plasma body source current [8] is located at the body of heater outside, applying the DC pulse negative bias to guard, feed working gas, is 1～5 * 10 in vacuum tightness
-2Under the Pa condition, glow discharge taking place in the zone between inboard wall of furnace body and guard [7], forms plasma body; Perhaps in this large area plasma source, increase the hot-cathode filament [9] that the discharge booster action is provided, at this moment, can reduce the DC pulse negative bias that is applied on the guard, form plasma body;
(c), plasma body source current [8] apply the DC pulse negative bias to guard and be-0.5～-3kV, frequency is 100～1000Hz, dutycycle is 1: 3～1: 10, low energy ion injects power supply [14] and applies the DC pulse negative bias to sample table and be-3～-5kV, frequency is 100～1000kHz, dutycycle is 1: 3～1: 10, two negative biass alternately take place, and the latter is than the former 0.3～8 μ s that lags behind, and guarantees that great area DC pulse plasma produces and alternately uninterruptedly the carrying out of low energy ion injection.
2. low energy ion implanter based on great area DC pulse plasma according to claim 1, it is characterized in that: metal guard [6] is for cup-shaped, uniform a plurality of mesh on it, the single hole area is 100～120mm2, the total area in hole accounts for 1/2～4/5 of guard surface-area, has 50%～80% permeability, and guard is 80～100mm with the distance of inboard wall of furnace body radially, axial height is 400～1800mm, and thickness is 5～8mm.
3. low energy ion implanter based on great area DC pulse plasma according to claim 1 is characterized in that: hot-cathode filament [9] diameter is 1～3mm, and total length is 3～15m, and filament applies volts DS 20～30V, current density 20～30A/mm
2
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| CN102024658B (en) * | 2009-09-22 | 2012-09-05 | 北京北方微电子基地设备工艺研究中心有限责任公司 | Plasma processing equipment and method |
| CN101845616B (en) * | 2010-05-25 | 2012-06-13 | 大连理工大学 | Conductor electric exploding plasma-based low-energy metal ion implantation (PBLEMII) device |
| CN110749645B (en) * | 2018-07-24 | 2021-10-01 | 中国科学院上海硅酸盐研究所 | Cage-shaped sample introduction device for glow discharge mass spectrometry and sample testing method |
| CN109830419B (en) * | 2019-01-24 | 2020-05-19 | 中国原子能科学研究院 | Miniature penning ion source |
| CN113463037B (en) * | 2021-07-19 | 2022-10-11 | 秦皇岛本征晶体科技有限公司 | Method for coating reflecting film on outer surface of fluoride special-shaped light guide rod |
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| US4897579A (en) * | 1987-04-13 | 1990-01-30 | The United States Of America As Represented By The United States Department Of Energy | Method of processing materials using an inductively coupled plasma |
| CN2195551Y (en) * | 1994-08-15 | 1995-04-26 | 核工业西南物理研究院 | Multi-function omnibearing reinforcing gravity pouring ion-filling machine |
| US5989363A (en) * | 1997-04-18 | 1999-11-23 | Plasma Metal Sa | Nitriding process and nitriding furnace therefor |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4897579A (en) * | 1987-04-13 | 1990-01-30 | The United States Of America As Represented By The United States Department Of Energy | Method of processing materials using an inductively coupled plasma |
| CN2195551Y (en) * | 1994-08-15 | 1995-04-26 | 核工业西南物理研究院 | Multi-function omnibearing reinforcing gravity pouring ion-filling machine |
| US5989363A (en) * | 1997-04-18 | 1999-11-23 | Plasma Metal Sa | Nitriding process and nitriding furnace therefor |
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