CN1263953A - Industrial pulse or DC plasma and chemical gas-phase deposition equipment for strenthening surface of tool or mould - Google Patents
Industrial pulse or DC plasma and chemical gas-phase deposition equipment for strenthening surface of tool or mould Download PDFInfo
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- CN1263953A CN1263953A CN 99115959 CN99115959A CN1263953A CN 1263953 A CN1263953 A CN 1263953A CN 99115959 CN99115959 CN 99115959 CN 99115959 A CN99115959 A CN 99115959A CN 1263953 A CN1263953 A CN 1263953A
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Abstract
A plasma chemical gas-phase deposition equipment for strengthening the surface of cutter, tool and mould is composed of furnace body, vacuum system, heating and temp control systm, plasma power supply system, and gas supply and control system. Said vacuum furnace body is a bell structure with heating elements on internal surface and shielding hood to prevent the interference between the electric fields of heater and plasma. One or more layers of hand ceramic film can be plated to increase the antiwear, anticorrosion and anti-oxidizing nature and the resistance to thermal fatigue, resulting in longer service life and productivity.
Description
The present invention relates to a kind ofly have high rigidity, strong bonding force, anti-oxidant, corrosion resistant ganoine thin film and with the equipment of stove ion nitriding and carbonitriding, particularly a kind of industrial production type pulse or DC plasma and chemical gas-phase deposition equipment for strenthening surface of tool or mould at the tool and mould surface deposition.
At present, the relevant both at home and abroad method for preparing ganoine thin film mainly contains three kinds, i.e. chemical vapor deposition (CVD), physical vapor deposition (PVD) and plasma auxiliary chemical vapor deposition (PCVD).The CVD method is come out early, be applicable to the reinforcement of Wimet type component, still keeping now certain advantage, but the principle of its technological process mainly is an elevated temperature heat activation vapor deposition reaction, usually reach about 1000 ℃, surpassed the tempering temperature of general steel tool and mould, the tempering of must quenching again behind the plated film, easily produce distortion even cracking, limited its application to a certain extent; In addition, in the inserted tool application facet, the CVD method is also answered careful use, and at first the hydrogen chloride gas of technological process generation may corrode cobalt wedding agent in the Wimet, causes tool surface loose, increases stress raiser; Secondly the easy decarburization of carbide surface reduces cutter intensity.The PVD method mainly heats in the ion bombardment mode, and working temperature has only 200-300 ℃, far below the tempering temperature of speedy steel cutting-tool, has overcome the too high deficiency of CVD method temperature, obtains widespread use aspect the speedy steel cutting-tool film preparation.But because ion low-pricedly penetrates, evaporates and limited by rectilinearity, poor around plating property, be difficult to obtain even plated film at positions such as slit, groove, apertures; Mainly between film and the matrix in addition combine by physics and chemisorption, film-substrate cohesion a little less than, film quality descends.The PCVD method has been avoided the shortcoming of the too high and PVD method technology of CVD method technological temperature around plating property difference, its technological temperature generally is controlled between 500 to 550 ℃, can in same equipment, realize simultaneously the Combined Processing of continuous plasma nitriding, carbonitriding and plated film, be not only applicable to the tool and mould of unlike material, and be specially adapted to the surface strengthening of complex-shaped class mould, thereby since the eighties, extremely paid attention to.At present, press the introducing and the production method of plasma body, the PCVD technology can further be subdivided into radio frequency PCVD, microwave PCVD, direct current PCVD and pulse direct current PCVD.But radio frequency PCVD energy is difficult for concentrating, and watt consumption is bigger; Microwave PCVD is difficult to realize plated film in industrial body of heater owing to the limitation of technology self; And the fatal shortcoming of traditional direct current PCVD is to be prone to hollow cathode effect and to produce arc discharge at positions such as slit, groove, apertures, and the scaling loss workpiece surface is difficult to the tool and mould of complicated shape is realized high-quality even plating.Pulse direct current PCVD technology is introduced pulse direct current glow discharge in the chemical vapour deposition reaction, appropriate modulation by pulse duty factor, overcome the arc discharge problem preferably, thereby fundamentally solved the technical barrier that the tool and mould of complicated shape is carried out surface strengthening, showing favorable industrial application prospect, is the main developing direction of PCVD technology now.Yet existing both at home and abroad pulse direct current PCVD equipment still has the following disadvantages: (1) early stage PCVD surface-strengthening equipment adopts the direct current plasma power supply, heats in the bombardment mode, is called cold wall type equipment.Under the bombardment heating, the furnace space temperature is far below workpiece surface temperature, and plasma chemical reaction can not fully carry out, film quality is descended, and heat in the coating process, the galvanic process parameter pins down mutually, and the separating controlling that differs is difficult to form the process system of standard.For improving the spatial temperature distribution in the body of heater, after this PCVD equipment of exploitation adopts the external-heat heating system at body of heater externally heated oven cover, is called external-heat, but rate of heating is slow and energy consumption is bigger.(2) pulse power is chopped mode in the present PCVD technology, and its shortcoming is that frequency is lower, and immobilizes, and working order is subject to forceful electric power and disturbs, and the efficient of power supply is lower.And be difficult to realize the negative pulse supply, influence the process optimization of preparation with the different coating preparations of the bad coating of electroconductibility.(3) because the restriction of subject plasma field distribution homogeneity, the existing PCVD vacuum furnace body useful space all shows less both at home and abroad, be difficult to that big-and-middle-sized mould is carried out surface coating and strengthen, cause the industrialization promotion of pulse direct current PCVD technology obviously to lag behind the market potential demand.
Purpose of the present invention is all overcoming above-mentioned deficiency; develop a kind of industrial pulse direct current PCVD reinforcing mould surface equipment; adopt big furnace binding, internal heat type heating system; has strong arc extinguishing function; the contravariant pulsed DC power system of short circuit, overload protection and can prepare the working gas supply control system that single film, multicomponent membrane, multilayer film and ion ooze; can satisfy need of industrial production, have the characteristics energy-conservation, that processing performance is stable.
Utilize the present invention can prepare TiN, TiC, (Ti, Si) N, (Ti, Si) C, (Ti, Si) single film, multicomponent membrane and multilayer films such as CN, Ti (CN), TiN/TiC/TiN, its sedimentation rate per hour 0.5 μ m to 2.0 μ m, the densification of film microtexture, crystal grain tiny (several micron), the surface evenly, have metalluster, its film and basal body binding force are strong, and Hv0.05 is at 2000-3000Kg/mm for the rete microhardness
2Between, and have good erosion resistance.
Accompanying drawing 1 is a structural representation of the present invention.
Accompanying drawing 2 is structure iron of well heater (3).
Accompanying drawing 3 is schemas of gas supply control system (12).
Accompanying drawing 4 is schematic diagrams of pulse dc power (10).
Accompanying drawing 5 is schematic circuit of pulse dc power (10).
Accompanying drawing 6 is schematic circuit of controller (34).
Accompanying drawing 7 is IGBT power switch circuit (33) figure.
Below in conjunction with accompanying drawing and example the present invention is further described.
With reference to Fig. 1, the reaction chamber that the present invention has a bell-jar body of heater (1) that is promoted by hydraulic gear to define, reaction chamber rely on body of heater from resealing, and body of heater (1) is anode and ground connection.The inwall of body of heater (1) is uniform-distribution with strip heater (3), is pending workpiece (5) heating, and strip heater (3) is introduced electrode (6) by passing a bridge and is connected with heating and temperature control system (11), to obtain the required three phase worker power of heating.The thermopair (13) of configuration enters reaction chamber and contacts with workpiece (5) is flexible from body of heater (1) bottom, observed temperature is passed to heating and Controlling System (11), changes heating rate in view of the above, or carries out thermostatic control.In reaction chamber, adopt shielding case structure (2) to realize the internal heat type heating with thermal radiation and shielding dual function.There is a slideway shielding case (2) inboard, disposes a supplementary anode (14) on the slideway, according to the shape of workpiece and the relative position of size adjustment supplementary anode (14), to strengthen the homogeneity of different sites geseous discharge in the stove, keeps uniform plasma field.Workpiece (5) is placed on the cathode disc (7), cathode disc (7) is placed on the double shield negative electrode (8) of using the casting mica ceramic making, negative electrode is both to the workpiece load-bearing, again by shielding of little gap and anodized insulation, and link to each other with contravariant pulse dc power (10), between negative and positive the two poles of the earth,, excite glow discharge by high-frequency pulse voltage, set up plasma field, and the discharge physics parameter is regulated and controlled.Working gas is entered in the reaction chamber by ventpipe (4), ventpipe (4) is arranged in the center of reaction chamber according to the big I of reaction chamber and workpiece, also can be arranged in the periphery place of reaction chamber, or the two haves both at the same time, and be communicated with gas supply control system (12), carry out the weight feed of gas.Vacuum system (9) is connected by the lower end of pipeline with bell-jar body of heater (1), and it is vacuumized, and a small amount of obnoxious flavour that gives off condenses in cold-trap.
With reference to Fig. 2, well heater of the present invention (3) is installed on bell-jar body of heater (1) inside, well heater (3) and thermoscreen (16) and the conjuncted installation of bell-jar body of heater (1), the shielding case (2) that has thermal radiation and shielding dual function one of well heater (3) installed inside.This kind internal heat type heating system is enhanced about more than once than the rate of heating of external-heat heating system, and current consumption reduces by more than 50, and weight saving is more than 80%.
With reference to Fig. 3, in the gas supply control system of the present invention (12), comprise and gas circuit (24,25,26,27) electromagnetic valve switch that is connected (17) and evaporating pot (28,29), the other end of electromagnetic valve switch (17) and mass flowmeter (18) are connected, mass flowmeter (18) mixes gas tank (22) with one-level and is connected, evaporating pot (28,29) be connected with suspended body flowmeter (21), suspended body flowmeter (21) and one-level are mixed gas tank (22) and all are connected with the mixed gas tank (23) of secondary, and evaporating pot (28) is connected with the suspended body flowmeter (21) of gas circuit (27) by pipeline.CH in the working gas gas circuit (24,25,26,27)
4, N
2, Ar, H
2With the H in the carrier band gas circuit (27)
2At first opened by connected electromagnetic valve switch (17), their flow size is by mass flowmeter (18) control of configuration, CH
4, N
2, Ar and H
2At first enter the mixed gas tank (22) of one-level and mix TiCl
4Be by carrier band gas H
2Open by manual switch (19) and electromagnetic valve switch (17) and to enter TiCl
4Evaporating pot (28) is taken TiCl out of
4Enter secondary and mix gas tank (23), with the CH that from the mixed gas tank (22) of one-level, mixes
4, N
2, Ar, H
2Gas thorough mixing in the mixed gas tank (23) of secondary is even.SiCl
4Then open SiCl by manual switch (19)
4Evaporating pot (29) is regulated magnetic valve (20) control SiCl
4Flow and show SiCl by suspended body flowmeter (21)
4Flux values, SiCl
4Directly enter secondary and mix gas tank (23), with the CH that from the mixed gas tank (22) of one-level, mixes
4, N
2, Ar, H
2Gas thorough mixing in the mixed gas tank (23) of secondary is even.After the mixed gas tank (23) of secondary mixed, all working gas was entered in the bell-jar body of heater (1) by electromagnetic valve switch (17) control.What particularly point out is, the present invention has developed the indirect flow precision Control Technology, and its principle is in a vapo(u)rization system, when temperature one regularly, TiCl
4The output flow of gas (steam output) is proportional with the flow of carrier gas, so as long as make TiCl
4Evaporating pot (28) keeps constant temperature, just can be by control carrier band gas H
2Flow realize TiCl
4The control of output flow.TiCl among the present invention
4Vapo(u)rization system has adopted the intelligent temperature control principle, and temperature control precision reaches ± and 0.5 ℃.TiCl
4Vapo(u)rization system adopts manual switch (19) and the dual control of electromagnetic valve switch (17).At carrier band gas H
2Pipeline on be provided with one-way cock (30), prevent to close H
2After, TiCl
4Gas backstreaming and corrode mass flowmeter (17).
With reference to Fig. 4, in the contravariant pulse dc power of the present invention (10), three phase worker power is adjusted to big or small continuously adjustable three-phase alternating voltage through AC voltage regulator (31), is the continuously adjustable direct supply of voltage through three-phase rectifier (32) rectification again, to change output amplitude.Direct supply is reverse into pulse power supply through IGBT power switch circuit (33), offers PCVD equipment (38) by DC pulse umformer (35) output pulse.Utilize peak value and average detection circuit (36) from pulse transducer (35) output terminal acquired signal, be fed back into controller (34) again, when out-put supply peak value or mean value transfinite; cut off output; both protected power unit, effective again arc extinguishing is avoided burned work-surface.By the frequency and the dutycycle of controller (34) control output pulse, two-ray oscillographs (37) direct viewing and metering that the waveform of output voltage, electric current can be provided for oneself by power supply.
With reference to Fig. 5, among this embodiment of contravariant pulse dc power (10), three phase worker power is adjusted to big or small continuously adjustable three-phase alternating voltage through AC voltage regulator (31), through three-phase rectifier (32) rectification is the continuously adjustable direct supply of voltage, direct supply is reverse into pulse power supply through IGBT power switch circuit (33), offers PCVD equipment (38) by DC pulse umformer (35) output pulse.Utilize peak value and average detection circuit (36) from pulse transducer (35) output terminal acquired signal, be fed back into controller (34) again, when out-put supply peak value or mean value transfinite, cut off output.
With reference to Fig. 6, in the circuit of controller (34), when peak value and average detection circuit (36) after DC pulse umformer (35) output terminal acquired signal, deliver to unicircuit TL3846 (39), it has 16 pins, utilize the dual pulse in this circuit to suppress end points (4 pin and 5 pin), can reach the output of low level voltage control highpowerpulse, change the value of the potentiometer R39 that is connected in the 9th pin, the time constant of electrical condenser C1, the C2 composition that links to each other with 8 pin is changed, reach the frequency that changes the output pulse.Control the variation that a pulse suppresses end (5 pin) level, reach and regulate the output duty of ratio.When the mean value of high-power output or peak value overrate, its detected another pulse that feeds back to unicircuit TL3846 (39) that overflows suppresses end (4 pin), cuts off the driving voltage of IGBT, makes power be output as zero, reaches the purpose of circuit protection.
With reference to Fig. 7, IGBT power switch circuit (33) is made up of the bridge-type output circuit among the present invention, has four groups of mutual isolated drive (40).Be that example illustrates its principle of work now: as high-frequency pulse transformer T with one group
1When (41) secondary winding was exported high level, actuate signal was through diode D
5, D
9Output is by potentiostat Z
1Limit value is in 15V; When actuate signal was reverse, the high level of g end made triode TR
1Fully conducting makes g, e terminal voltage will make the IGBT reliable turn-off for zero rapidly.As long as the contravariant pulse dc power is to design rational controller than the superior part of chopped mode circuit among the present invention, control the IGBT high power switch in real time, just can obtain the highpowerpulse signal, boost through a rated transformation ratio, reach the requirement of PCVD technology.
It is as follows now to be with preparation TiN that example is set forth the principle of work of present device: pending workpiece (5) is inserted in the bell-jar body of heater (1), open vacuum system (9) bell-jar body of heater (1) is evacuated to 10Pa when following, begin to open the H in the gas supply control system (12)
2, Ar gas, by high-energy ion bombardment workpiece (5) surface in the plasma field of contravariant pulse dc power (10) generation, to reach the effect of clean, after postheating and Controlling System (11) begin to be heated to certain temperature constant temperature maintenance certain hour, under the air pressure conditions that requires, feed working gas H by suitable proportion
2, N
2, Ar and TiCl
4, and by contravariant pulse dc power (10) for suitable high-frequency impulse sparking voltage is provided between two electrodes, this moment, high-energy electron produced glow discharge with the gas molecule collision ionization, formation has chemically active Ti
+, N
+Ion and free radical.These ions and free radical react on workpiece (5) surface and are deposited as the TiN film.Behind the deposition certain hour, at first close gas supply control system (12), then turn off contravariant pulse dc power (10) and heating and Controlling System (11), stop vacuum system (9) work at last, finish coating film treatment, and to charging into H in the bell-jar body of heater (1)
2, N
2Protective atmosphere is cooled to below 100 ℃ and comes out of the stove.
Description of drawings: (1) bell-jar body of heater; (2) radome; (3) heater; (4) breather pipe; (5) worker Part; (6) gap bridge is introduced electrode; (7) cathode disc; (8) double shield simple or compound vowel of a Chinese syllable negative electrode; (9) true Do-nothing system; (10) contravariant pulse dc power; (11) heating and control system; (12) The gas supply control system; (13) thermocouple; (14) impressed current anode; (15) observation window (16) heat screen (17) electromagnetic valve switch; (18) mass flowmenter; (19) manual switch; (20) electromagnetic valve for adjusting; (21) suspended body flowmeter; (22) the mixed gas tank of one-level; (23) two The mixed gas tank of level; (24) CH4Gas circuit; (25) N2Gas circuit; (26) Ar gas circuit; (27) H2Gas circuit, carrier band gas H2Gas circuit; (28) TiCl4Evaporator; (29) SiCl4Evaporator; (30) One-way cock (31) AC voltage regulator; (32) three-phase rectifier; (33) IGBT power is opened Close circuit; (34) controller; (35) DC pulse converter; (36) peak value and mean value Testing circuit; (37) double oscillograph; (38) PCVD equipment; (39) integrated circuit TL3846; (40) drive circuit; (41) high-frequency pulse transformer T1
Claims (8)
1. industrial pulse direct current plasma chemical vapor deposition equipment, the bell-jar body of heater (1) that comprises a ground connection, dispose heating member (3) in the reaction chamber that body of heater (1) defines, the thermopair (13) that is connected with heating and Controlling System (11), with gas supply system (12) ventpipe (4) that is connected and the vacuum system (9) that is connected with body of heater (1) lower end.Feature of the present invention is, the inwall of body of heater (1) is evenly distributed with banded heating member (3), banded heating member (3) is introduced electrode (6) by passing a bridge and is connected with heating and Controlling System (11), the shielding case (2) that the inboard configuration one of banded heating member (3) has thermal radiation and shielding dual function, cathode disc (7) is supported by double shield negative electrode (8) in the reaction chamber bottom of body of heater (1), cathode disc (7) is connected with pulse dc power (10), the ventpipe (4) that the center of said reaction chamber or circumferential arrangement one are connected with gas supply control system (12).
2. equipment according to claim 1 is characterized in that, said shielding case (2) disposed inboard has slideway, and disposing in the slideway can be along the supplementary anode (14) of its slip.
3. equipment according to claim 1 is characterized in that, said well heater (3)
4. with thermoscreen (16) and the conjuncted installation of body of heater (1), has the shielding case (2) of thermal radiation and shielding dual function one of well heater (3) installed inside.
5. equipment according to claim 1, it is characterized in that, said gas supply control system (12) comprises and gas circuit (24,25,26,27) electromagnetic valve switch that is connected (17) and evaporating pot (28,29), the other end of electromagnetic valve switch (17) and mass flowmeter (18) are connected, mass flowmeter (18) mixes gas tank (22) with one-level and is connected, evaporating pot (28,29) be connected with suspended body flowmeter (21), suspended body flowmeter (21) and one-level are mixed gas tank (22) and all are connected with the mixed gas tank (23) of secondary, and evaporating pot (28) is connected with the suspended body flowmeter (21) of gas circuit (27) by pipeline.
6. equipment according to claim 1, it is characterized in that, said contravariant pulse dc power (10) comprises an AC voltage regulator (31), three phase worker power is adjusted to big or small continuously adjustable three-phase alternating voltage through AC voltage regulator (31), be the continuously adjustable direct supply of voltage through three-phase rectifier (32) rectification again, direct supply is reverse into pulse power supply through IGBT power switch circuit (33), offers PCVD equipment (38) by DC pulse umformer (35) output pulse.Utilize peak value and average detection circuit (36) from pulse transducer (35) output terminal acquired signal, be fed back into controller (34) again.
7, equipment according to claim 1, it is characterized in that, said controller (34) comprises a testing circuit (36), when peak value and average detection circuit (36) after DC pulse umformer (35) output terminal acquired signal, deliver to unicircuit TL3846 (39), utilize the dual pulse in this circuit to suppress end points (4 pin and 5 pin), can reach the output of low level voltage control highpowerpulse, change the value of the potentiometer R39 that is connected in the 9th pin, make the electrical condenser C1 that links to each other with 8 pin, the time constant that C2 forms changes, reach the frequency that changes the output pulse, control the variation that a pulse suppresses end (5 pin) level, reach and regulate the output duty of ratio, when the mean value of high-power output or peak value overrate, its detected another pulse that feeds back to unicircuit TL3846 (39) that overflows suppresses end (4 pin), cuts off the driving voltage of IGBT, makes power be output as zero.
8, equipment according to claim 1 is characterized in that, said power switch circuit (33) is made up of the bridge-type output circuit, has four groups of mutual isolated drive (40).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99115959A CN1082100C (en) | 1999-12-29 | 1999-12-29 | Industrial pulse or DC plasma and chemical gas-phase deposition equipment for strenthening surface of tool or mould |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99115959A CN1082100C (en) | 1999-12-29 | 1999-12-29 | Industrial pulse or DC plasma and chemical gas-phase deposition equipment for strenthening surface of tool or mould |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1263953A true CN1263953A (en) | 2000-08-23 |
| CN1082100C CN1082100C (en) | 2002-04-03 |
Family
ID=5278845
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99115959A Expired - Fee Related CN1082100C (en) | 1999-12-29 | 1999-12-29 | Industrial pulse or DC plasma and chemical gas-phase deposition equipment for strenthening surface of tool or mould |
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| Country | Link |
|---|---|
| CN (1) | CN1082100C (en) |
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| CN100439563C (en) * | 2005-06-06 | 2008-12-03 | 贵研铂业股份有限公司 | Chemical vapor deposition equipment |
| CN1648282B (en) * | 2004-01-27 | 2010-06-16 | 三星电子株式会社 | Plasma enhanced semicondutor deposition apparatus |
| CN101555593B (en) * | 2008-04-09 | 2011-07-20 | 福建钧石能源有限公司 | Method and system for preparing functional films in asynchronous pulse mode |
| CN102127755A (en) * | 2011-02-17 | 2011-07-20 | 中国科学技术大学 | Direct current glow plasma device and preparation method of diamond chip |
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| CN100439563C (en) * | 2005-06-06 | 2008-12-03 | 贵研铂业股份有限公司 | Chemical vapor deposition equipment |
| CN101555593B (en) * | 2008-04-09 | 2011-07-20 | 福建钧石能源有限公司 | Method and system for preparing functional films in asynchronous pulse mode |
| CN102127755A (en) * | 2011-02-17 | 2011-07-20 | 中国科学技术大学 | Direct current glow plasma device and preparation method of diamond chip |
| CN102127755B (en) * | 2011-02-17 | 2014-04-30 | 中国科学技术大学 | Direct current glow plasma device and preparation method of diamond chip |
| CN104789946A (en) * | 2014-01-21 | 2015-07-22 | 上海理想万里晖薄膜设备有限公司 | Heat insulation and electricity conduction apparatus for PECVD reaction chamber, and application thereof |
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