CN103938185B - A kind of preparation method of tubular member internal coating - Google Patents

A kind of preparation method of tubular member internal coating Download PDF

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CN103938185B
CN103938185B CN201310020151.9A CN201310020151A CN103938185B CN 103938185 B CN103938185 B CN 103938185B CN 201310020151 A CN201310020151 A CN 201310020151A CN 103938185 B CN103938185 B CN 103938185B
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tubular member
vacuum
coating
preparation
deposition
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CN103938185A (en
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吴护林
张隆平
孙彩云
何庆兵
陈海涛
罗明波
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No 59 Research Institute of China Ordnance Industry
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No 59 Research Institute of China Ordnance Industry
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Abstract

The present invention relates to the preparation method of a kind of tubular member internal coating, tubular member is installed in the deposition plater including the auxiliary electrode of inducing QI effect, TiCl4 fluid reservoir and tubular member clamping fixture, it is then charged into evacuation in vacuum chamber, it is passed through argon Ar, open grid bias power supply aura and clean tubular member, being passed through hydrogen H2, titanium tetrachloride TiCl4, nitrogen N 2, boron chloride BCl3 reacting gas, alternately switch N2 and BCl3 is passed through the deposition realizing TiN and TiB2;The present invention solves limited space by tubular member deposition plater and causes the problem that sheath ply, ion energy are low, coating binding force is bad, solve the outside plasma diffused into rapidly depleting, density is low, the most uneven problem, improve density and the uniformity of the interior plasma of pipe, it is achieved efficient and axial uniform deposition.

Description

A kind of preparation method of tubular member internal coating
Technical field
The present invention relates to the preparation method of a kind of tubular member internal coating, a kind of elongated tubular product part deep in The preparation method of the wear-resisting composite coating of hole surface.
Background technology
In recent years under the hot conditions of various countries' primary study use abrasion-resistant coating material and coating technology, including Ta, The refractory metals such as Mo, W, Re, Nb, Hf and the ceramic body coating such as alloy and TiB2, ZrO2 thereof, coating structure is to multi-layer multi side To development, its technology of preparing include the coating of coating produced by laser cladding, plasma flame, high velocity oxygen-fuel thermal spraying, wire explosion spraying with And plasma enhanced chemical vapor deposition etc., wherein vapour deposition is owing to can realize infusibility, fire-retardant, the reliable deposition of anti-yaw damper material, And used in a large number, vapour deposition is a kind of by the physical process such as chemical reaction or thermal evaporation, produces the gas of deposition material The method that body atom, molecule, ion or aggregation form solid film layer at matrix, is divided into physical vapour deposition (PVD) (PVD) and chemistry Vapour deposition (CVD), CVD technology has around plurality of advantages such as plating property are good, but depositing temperature is higher, strongly limit its application model Enclose.
The PECVD (PECVD) that plasma introduces CVD technology formation is the most sharp Live reaction system, pyroreaction can have been made to realize low temperature synthesis, reached purpose prepared by coating low temperature, this is because plasma Temperature and energy density are high, it is possible to make reactant gas molecules generation ionization or activation, it is possible to decrease compound decomposes or chemical combination Potential barrier, reaction temperature improves reaction rate while reducing, and additionally the activation of matrix surface can be improved painting by plasma Layer and the bond strength of matrix.
But, elongated tubular product part is in PECVD prepares TiB2/TiN coating procedure, owing to limited space causes sheaths weight Folded, ion energy is low, and the plasma that outside diffuses into is rapidly depleting, and energy density is low, and the most uneven, causes Plasma application difficulty in the deep endoporus of slender member.
The coating of the existing preparation technology of TiB2/TiN composite coating such as coating produced by laser cladding, plasma flame, high velocity oxygen-fuel The preparation temperature of the method such as thermal spraying, wire explosion spraying is higher, easily causes matrix to aoxidize, simultaneously the high temperature in coating preparation process Also the mechanical property of thin-walled tubular part etc. can be affected.And PECVD can make reacting gas divide There is ionization or activation in son, it is possible to decrease compound decomposes or the potential barrier of chemical combination, it is achieved low temperature depositing, but elongated tubular product part exists PECVD prepares in TiB2/TiN coating procedure, striking difficulty, it is difficult to ensure that uniformity prepared by coating.
Summary of the invention
It is an object of the invention to provide and use under hot conditions a kind of uniformly preparation on elongated tubular product inner bore of part surface The method of wear-resistant coating.Propose the preparation method of the wear-resisting composite coating of elongated tubular product part of the present invention, solve big L/D ratio Elongated tubular product part PECVD during an inwall striking difficult problem, it is achieved that under elongated tubular product part inwall hot conditions use The uniform preparation of wear-resisting composite coating.
It is an object of the invention to be realized by such technical scheme, the preparation side of a kind of tubular member internal coating Method, it is characterised in that: make vacuum reach 1.0 × 10-2Pa~2.5 × 10-2Pa, keeps vacuum to maintain, is passed through argon Ar, Vacuum is down to 6 × 10-2Pa ~ 8×10-2Pa, maintains this vacuum, opens grid bias power supply aura cleaning workpiece 5 ~ 10min, Heating, vacuum room temperature is to 300~450 DEG C simultaneously, closes argon and grid bias power supply;Logical nitrogen N 2, hydrogen H2, titanium tetrachloride TiCl4 reacting gas, after vacuum is down to 1000 ~ 1600Pa, maintains this vacuum, opens grid bias power supply, deposit coating TiN 30min~120min, closes grid bias power supply, stops being passed through nitrogen N 2, hydrogen H2, titanium tetrachloride TiCl4 reacting gas, is passed through argon Gas Ar detergent line 5min~10min;It is passed through boron chloride BCl3, hydrogen H2, titanium tetrachloride TiCl4 reacting gas again, opens Grid bias power supply, deposits coating TiB23h~5h.
Described argon Ar, hydrogen H2, boron chloride BCl3, the gas flow of nitrogen N 2 are Ar:80~100 sccm respectively, H2:1400~1600 sccm, BCl3:450~520 sccm, N2:200~300 sccm.
Described direct current pulse power source biases: 700~1000V, electric current: 1~1.2A, dutycycle: 40% ~ 60%, frequency: 40KHz。
Before carrying out depositing coating, need to do following preparation: the tubular member of coating to be prepared is carried out pretreatment, logical Crossing grinding makes tubular member endoporus roughness reach Ra0.8 ~ Ra1.6, uses organic solvent such as ethanol and acetone to carry out clearly successively Washing, and clean 10min~15min in organic solvent is such as acetone with ultrasound wave, tubular member takes out latter 60 DEG C dries 1h.
Installing tubular member evacuation in vacuum chamber, first described vacuum chamber uses mechanical pump forvacuum, very Open diffusion pump when reciprocal of duty cycle is better than 5 ~ 10Pa and vacuum chamber pumping high vacuum, vacuum are better than 6 × 10-2Pa ~ 8×10-2During Pa, By described vacuum chamber temperature 300~450 DEG C of tubular parts and be incubated 20min, continue to be evacuated to vacuum reach 1 × 10-2Pa ~ 2×10-2Pa。
The present invention, by closing diffusion pump, retains mechanical pump and carries out vacuum maintenance.
After deposition coating terminates, stop being passed through TiCl4、BCl3And H2, close grid bias power supply Ar and clean air delivering pipeline 15min~more than 20min, degree for the treatment of is down to 140 DEG C~less than 150 DEG C, is stopped mechanical pump, takes out tubular member.
The painting of tubular member of the present invention is deposited upon in deposition plater and completes, and described deposition plater includes Having the auxiliary electrode of gas port, TiCl4 fluid reservoir and clamping fixture, described clamping fixture is fixed on the base centre bit of vacuum chamber Putting, described fluid reservoir is connected with vacuum chamber by stainless steel tube, and described auxiliary electrode is arranged on the axle center of described clamping fixture It is connected on line and with described DC pulse grid bias power supply anode;
Wherein said clamping fixture includes being held up by three support bars, tube wall has the tubular bracket of four fixing holes, Connected by ceramic body insulation between described support bar and described tubular bracket, described tubular bracket and DC pulse grid bias power supply Negative electrode connect.
In order to be delivered directly to inside tubular member by reacting gas so that it is have air delivery function concurrently, described auxiliary electrode is Tubulose, including the transition conduit that termination is flat cone mouth shape and the upper snorkel of connection fixed thereto, described gas port is at upper snorkel Tube wall end arrange, and this gas port is at least two.
In order to provide TiCl4 gas, described TiCl4 fluid reservoir includes stainless steel tank body, sealing ring, upper cover, thermocouple, adds The torrid zone, pressure vacuum meter and hand stop valve, pour TiCl4 into stainless steel tank body on the workbench having strength exhaust apparatus In, stainless steel tank body oral area set sealing ring, on sealing ring, put lid, upper cover is fastenedly connected with stainless steel tank body, it is ensured that TiCl4 will not overflow, and the connecting tube of upper cover welded top is connected with hand stop valve, and hand stop valve is followed by pressure vacuum meter, Two pressure vacuum meter other ends connect N2 outfan and vacuum chamber input respectively by connecting tube, and heating tape uniformly twines in stainless Cylinder of steel body and gas transmission connecting pipe surface, the end of thermocouple temperature sensitive is put between heating tape and stainless steel tank body, measures in real time and adds The torrid zone heating-up temperature to tank body, the other end of heating tape and thermocouple is all connected on temperature control system, it is ensured that enter TiCl4 tank body Row heated at constant temperature, described connecting tube uses stainless steel tube effect all good.
Described heating tape temperature is opened while described vacuum chamber temperature to 70 DEG C~85 DEG C, in stainless steel tank body heating Gas pressure 1300 Pa~8000 Pa.
In order to ensure that TiCl4 will not overflow, upper cover fastens with stainless steel tank body screw.
In order to be able to assist TiCl4 synthetic reaction under safe and reliable working environment to form sedimentary, described TiCl4 liquid storage Tank is also associated with hydrogen H2 fluid reservoir, boron chloride BCl3 fluid reservoir and nitrogen N 2 fluid reservoir, described TiCl4 fluid reservoir and hydrogen H2 fluid reservoir, nitrogen N 2 fluid reservoir connect into gas channels, and described TiCl4 fluid reservoir and hydrogen H2 fluid reservoir are also and boron chloride BCl3 fluid reservoir connects into another gas channels.
For guaranteeing that TiCl4 does not block air delivering pipeline, described TiCl4 fluid reservoir is also parallel with argon Ar fluid reservoir, described Argon Ar fluid reservoir one end is connected between hydrogen H2 fluid reservoir and nitrogen N 2 fluid reservoir air delivering pipeline, and the other end is connected to described Between TiCl4 fluid reservoir and boron chloride BCl3 fluid reservoir air delivering pipeline, in order on starting stage and the end rank of coating deposition Air delivering pipeline is rinsed by section, prevents TiCl4 from remaining in air delivering pipeline.
Described tubular member clamping fixture is that three support bars hold up, tube wall has the tubular bracket of four fixing holes, Being insulated by ceramic body between support bar and tubular bracket, tubular bracket is connected with the negative electrode of grid bias power supply, and tubular member passes through Four fixing hole fastenings on tubular bracket, it is achieved DC pulse grid bias power supply negative electrode is connected with tubular member, it is ensured that aura is put The realization of electricity, and make tubular member neither contact with center auxiliary electrode, prevent short circuit, do not contact with vacuum-chamber wall, prevent Vacuum chamber is charged hurts sb.'s feelings.Support bar is contained on described vacuum chamber base, and base is supported by callosity, and central opening of the seal installs set Part, center auxiliary electrode is connected by external member and DC pulse grid bias power supply anode are fixing.
Check tubular member and center auxiliary electrode contactless after, close bell.
Owing to have employed technique scheme, present invention have the advantage that:
1, the present invention prepares, at the bore area of tubular member, the TiB2/TiN laminated construction used under a kind of hot conditions Wear-resisting composite coating, be with TiN as the end, prepare TiB2 wear-resisting functions coating in the above, utilize TiB2 high-melting-point, high rigidity The reliability that workpiece uses the most for a long time is ensured etc. characteristic.
2, the present invention is by being connected on the anode of grid bias power supply on tubular center's auxiliary electrode and electric potential floating, thus by brightness Light electric discharge has been tied to tubular member endoporus, solves limited space and causes that sheath ply, ion energy are low, coating binding force is bad Problem, make the negative bias values that the electric potential difference clamper of pipe axis and tube wall is added on tube wall, it is ensured that ion can fully accelerate And arrive surface, while realizing deposition, improve adhesion;By perforate on tubular center's auxiliary electrode so that it is have concurrently defeated Airway dysfunction, is delivered directly to reacting gas inside tubular member, solves the outside plasma diffused into rapidly depleting, close Spend low, the most uneven problem, improve density and the uniformity of the interior plasma of pipe, it is achieved efficient and axial uniform deposition.
3, heated by heating tape and temperature control system realizes TiCl4Gasification under assigned temperature, passes through pressure vacuum meter Monitor the TiCl needed for pressure inside the tank and regulation4Flow, it is ensured that TiCl4Not with atmosphere, prevent from being formed poisonous HCl and Easily block the TiO of air delivering pipeline2Powder;Hand stop valve is opened at gas circuit evacuation or in the case of filling Ar, controls respectively to carry H2 Input and gaseous state TiCl4Output, prevent TiCl4With the air contact of residual in gas circuit.For guaranteeing TiCl4Do not block gas transmission Pipeline, the TiCl to fluid reservoir to vacuum chamber4Air delivering pipeline, the most all uses heating tape to heat, and is specifically manufactured Ar flushing line, it is rinsed by starting stage and ending phase in deposition, prevents TiCl4Remain in air delivering pipeline. By above measure, it is achieved that TiCl4Vacuum storage, controlled gasification and transporting smoothly.
4, the inventive method can be 35 mm at inner thorax diameter, and draw ratio is inside the bushing pipe of 4.4, uses plasma to increase Extensive chemical gas phase deposition technology realizes uniform deposition, and inhomogeneities controls within ± 5%, relative to not doing the naked pipe of coating, More than 2000 DEG C, the service life of cycling hot impact improves more than 2.3 times.
Accompanying drawing explanation
Fig. 1 is the microstructural SEM photograph in embodiment of the present invention 1TiB2/TiN composite coating cross section;
Fig. 2 is the microstructural SEM photograph of coating surface of the embodiment of the present invention 1 to embodiment 4 preparation;
Fig. 3 is the XRD figure spectrum of the coating of the embodiment of the present invention 1 to embodiment 4 preparation;
Fig. 4 is embodiment of the present invention tubular member clamping schematic diagram;
Fig. 5 is the top view of Fig. 4;
Fig. 6 is the structural representation of embodiment of the present invention auxiliary electrode;
Fig. 7 be deposition plater of the present invention respectively form connection diagram;
Fig. 8 is that TiCl4 fluid reservoir of the present invention respectively forms connection diagram.
Detailed description of the invention
Further illustrate the present invention below by the mode of embodiment, the most therefore limit the present invention to described enforcement Within the scope of example.
Embodiment 1: the preparation method of a kind of tubular member internal coating, comprises the following steps:
A. the preparation before deposition coating
Pretreatment before tubular member coating: grind, polish tubular member endoporus and reach Ra0.8 ~ Ra1.6 to roughness, Being carried out 2~3 times with ethanol and acetone successively, then clean 10min~15min with ultrasound wave in acetone, tubular member takes Go out latter 60 DEG C and dry 1h.
Installation tubular member (seeing Fig. 4,5,6,7,8):
By inner thorax diameter be 35 mm, draw ratio be 4.4 unsettled being placed on of tubular member 6 hold up with three support bars 11 Tube wall have on the tubular bracket 12 of four screw holes, between support bar 11 and tubular bracket 12 by insulating ceramics body 14 even Connecing, support bar 11 is contained on the base 41 of described vacuum chamber 4, and base 41 is supported by callosity 42, and base 41 center drilling installs set Part 43, center auxiliary electrode 2 is connected by external member 43 and DC pulse grid bias power supply 5 anode are fixing, described tubular bracket 12 and The negative electrode of DC pulse grid bias power supply 5 connects.
Check tubular member 6 and center auxiliary electrode 2 contactless after, close bell.
Evacuation: first with mechanical pump 7 forvacuum, opens diffusion pump 8 and vacuum chamber is taken out Gao Zhen when vacuum is 5Pa Sky, vacuum is 8 × 10-2During Pa, tubular part to 450 DEG C is also incubated 20min, opens adding of TiCl4 fluid reservoir simultaneously The torrid zone is heated to 85 DEG C, continues to vacuum, vacuum chamber is reached 2 × 10-2Pa。
B. depositing Ti B2/TiN coating (see Fig. 6,7):
Keep vacuum to maintain, be passed through argon Ar, open DC pulse grid bias power supply simultaneously, make bias: 1000V, electric current: 1.2A, dutycycle: 60%, frequency: 40KHz;Aura cleans tubular member 5min~10min;Then pass to reacting gas hydrogen H2、TiCl4、N2, deposit coating TiN 0.5h, stop being passed through reacting gas hydrogen H2, TiCl4, N2, close grid bias power supply, logical Enter argon Ar detergent line 5min~10min;It is passed through boron chloride BCl3, hydrogen H2, titanium tetrachloride TiCl4 reacting gas again, Open grid bias power supply, deposit coating TiB23h;Vacuum is made to be maintained at 1000Pa during deposition.
Described argon Ar, hydrogen H2, BCl3, the gas flow of N2 be Ar:100 sccm respectively, H2:1600 sccm, BCl3:520 sccm, N2:300 sccm.
C. deposition coating terminates
Stop being passed through TiCl4, BCl3 and H2, close grid bias power supply Ar cleaning air delivering pipeline and be more than 15min~20min, Treat that temperature is down to 140 DEG C~150 DEG C, stop mechanical pump, take out tubular member.
Embodiment 2~4 is in addition to parameter listed by table 1, and other parameter and step are with embodiment 1.
Table 1
Table 2 is 35 mm for obtain through embodiment 1~4 preparation method at inner thorax diameter, and draw ratio is the tubulose zero of 4.4 The coating layer thickness resistance to impact of part inside deposition TiB2/TiN coating and the test result of hardness.Enter according to the regulation of national standard The preparation of row coating sample and measurement, the combination property of measured coating is as shown in table 2.
Table 2
Detection project Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Detection method
Coating layer thickness um 15.3 14.5 14.7 15.5 Eddy current thickness measuring
Resistance to sudden heating (1500~1600) The punching of DEG C instantaneous flame Hit 810 times not open Split (1500~1600) The punching of DEG C instantaneous flame Hit 750 times not open Split (1500~1600) DEG C wink Time flame impingement 790 times Do not ftracture (1500~ 1600) DEG C wink Shi Huoyan rushes Hit 800 times not Cracking
Hardness HV0.1 3102 3062 3050 3045 GB/T6739
Knowable to table 2 data analysis, the TiB2/TiN coating obtained by embodiment 1~4, its uniform coating thickness, resistance to punching Hitting property is strong, hardness is high.
Fig. 1 is the TiB obtained by embodiment 1 preparation method2The microstructural SEM photograph of/TiN coating cross sections;From photo Find out TiB2Clear and legible with TiN coating, coating interpenetrates with coating intersection;Fig. 2 is prepared by embodiment 1 to embodiment 4 The microstructural SEM photograph of coating surface, Fig. 3 is the X-ray diffraction analysis XRD of coating of embodiment 1 to embodiment 4 preparation From Fig. 2 and Fig. 3, collection of illustrative plates, finds out that coating surface density and uniformity through embodiment 1 to embodiment 4 preparation are preferable.

Claims (9)

1. the preparation method of a tubular member internal coating, it is characterised in that: evacuation keeps vacuum 1.0 × 10-2Pa~ 2.0×10-2Pa, is passed through argon Ar, adjusts vacuum and maintains 6 × 10-2Pa ~ 8×10-2Pa, opens grid bias power supply aura clear Washing workpiece 5 min ~ 10min, heating, vacuum room temperature is to 300~450 DEG C simultaneously, closes argon and grid bias power supply;It is passed through one group Reacting gas, adjusts vacuum and maintains 1000 ~ 1600Pa, open grid bias power supply, deposit coating TiN 30min~120min, Close grid bias power supply, stop being passed through described one group of reacting gas, be passed through argon Ar detergent line 5min~10min;It is passed through another again One group of reacting gas, opens grid bias power supply, deposits coating TiB2150 min~300 min;
Wherein said one group of reacting gas is nitrogen N2, hydrogen H2, titanium tetrachloride TiCl4, another group reacting gas is boron chloride BCl3, hydrogen H2, titanium tetrachloride TiCl4;Described argon Ar, hydrogen H2, boron chloride BCl3, nitrogen N2Gas flow be respectively Ar:80~100 sccm, H2: 1400~1600 sccm, BCl3: 450~520 sccm, N2: 200~300 sccm;
Direct current pulse power source biases: 700~1000V, electric current: 1~1.2A, dutycycle: 40% ~ 60%, frequency: 40KHz.
2. the preparation method of tubular member internal coating as claimed in claim 1, it is characterised in that: described evacuation is the most logical Cross forvacuum, when making vacuum reach 5 ~ 10Pa, then pumping high vacuum, making vacuum is 6 × 10-2Pa ~ 8×10-2Pa, presses Tubular member is heated and is incubated 20min by temperature described in vacuum chamber, continues to be evacuated to vacuum and reaches 1 × 10-2Pa ~ 2×10-2Pa。
3. the preparation method of tubular member internal coating as claimed in claim 1 or 2, it is characterised in that: described tubular member Painting be deposited upon deposition plater in complete, described deposition plater includes clamping fixture (1), band gas port (23) Auxiliary electrode (2) and TiCl4Fluid reservoir (3), described clamping fixture (1) is fixed on base (41) centre bit of vacuum chamber (4) Put, described TiCl4Fluid reservoir (3) is connected with vacuum chamber (4) by connecting tube, and described auxiliary electrode (2) is arranged on described folder Hold on the axial line of fixture (1) and be connected with DC pulse grid bias power supply (5) anode;
Wherein said clamping fixture (1) includes being held up by three support bars (11), tube wall has the pipe of four fixing holes (13) Shape support (12), is connected by ceramic body (14) insulation between described support bar (11) and described tubular bracket (12), described pipe Shape support (12) is connected with the negative electrode of DC pulse grid bias power supply (5).
4. the preparation method of tubular member internal coating as claimed in claim 3, it is characterised in that: described auxiliary electrode (2) For tubulose, including the transition conduit (21) that termination is flat cone mouth shape and the upper snorkel (22) of connection fixed thereto, described gas port (23) on described, the tube wall end of snorkel (22) arranges two or more.
5. the preparation method of tubular member internal coating as claimed in claim 3, it is characterised in that: described TiCl4Fluid reservoir (3) by stainless steel tank body (31), sealing ring, upper cover (32), thermocouple, heating tape, pressure vacuum meter (33) and hand stop valve (34) composition;Described upper cover (32) is fastened on oral area equipped with on the stainless steel tank body (31) of sealing ring, described hand stop valve (34) being connected with upper cover (32), described hand stop valve (34) connects pressure vacuum meter (33), described pressure vacuum meter below (33) other end accesses described vacuum chamber (4), and described heating tape uniformly twines in stainless steel tank body (31) and is connected with vacuum chamber (4) Stainless steel tube outside, the end of described thermocouple temperature sensitive is placed between heating tape and stainless steel tank body (31), described heating tape and The outfan of thermocouple is connected on heated at constant temperature instrument.
6. the preparation method of tubular member internal coating as claimed in claim 5, it is characterised in that: heating described vacuum chamber Described heating tape temperature is opened to 70 DEG C~85 DEG C, gas pressure 1300 Pa~8000 in stainless steel tank body while temperature Pa。
7. the preparation method of tubular member internal coating as claimed in claim 1 or 2, it is characterised in that: manage before deposition coating The endoporus roughness of shape part is Ra0.8 ~ Ra1.6.
8. the preparation method of tubular member internal coating as claimed in claim 7, it is characterised in that: before deposition coating, use After organic solvent cleans, then cleaning 10min~15min in organic solvent with ultrasound wave, tubular member takes out rear 60 DEG C of drying 1h。
9. the preparation method of tubular member internal coating as claimed in claim 1 or 2, it is characterised in that: after deposition terminates, stop Stop-pass enters TiCl4、BCl3And H2, after regulation pulse voltage and dutycycle are 0, close grid bias power supply, be passed through argon Ar and clean appendix Road 15min~20min, treats that temperature is down to less than 150 DEG C, stops vacuum and maintains.
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CN104264126B (en) * 2014-09-17 2016-08-31 四川大学 Long-range microchannel interior walls TiO2coating chemical vapor deposition unit and painting method
CN105668998B (en) * 2016-01-11 2019-11-05 苏州工业园区纳米产业技术研究院有限公司 A kind of P5000 board BPSG technique improves equipment
CN113136562A (en) * 2021-04-19 2021-07-20 东北大学 High-hardness TiN protective coating capable of being coated on deep-hole part and preparation method thereof
CN113681939A (en) * 2021-07-30 2021-11-23 江西昌河航空工业有限公司 Equivalent substitution method for composite material thermocouple
CN114059040A (en) * 2021-11-24 2022-02-18 四川大学 Deposition method and device for TiN coating on inner surface of pipe network

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4234622A (en) * 1979-04-11 1980-11-18 The United States Of American As Represented By The Secretary Of The Army Vacuum deposition method
CN102154672A (en) * 2008-04-09 2011-08-17 北京航空航天大学 Non-metallic film with high heat conduction efficiency and anti-fouling capability and preparation method thereof
CN102683481A (en) * 2011-03-15 2012-09-19 罗伯特·博世有限公司 Method for operating a vacuum coating device

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4234622A (en) * 1979-04-11 1980-11-18 The United States Of American As Represented By The Secretary Of The Army Vacuum deposition method
CN102154672A (en) * 2008-04-09 2011-08-17 北京航空航天大学 Non-metallic film with high heat conduction efficiency and anti-fouling capability and preparation method thereof
CN102683481A (en) * 2011-03-15 2012-09-19 罗伯特·博世有限公司 Method for operating a vacuum coating device

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