CN103938184A - Device for preparing tubular part inner hole coating - Google Patents

Device for preparing tubular part inner hole coating Download PDF

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Publication number
CN103938184A
CN103938184A CN201310020147.2A CN201310020147A CN103938184A CN 103938184 A CN103938184 A CN 103938184A CN 201310020147 A CN201310020147 A CN 201310020147A CN 103938184 A CN103938184 A CN 103938184A
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China
Prior art keywords
container
storing liquid
tubular member
ticl4
clamping fixture
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CN201310020147.2A
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Chinese (zh)
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CN103938184B (en
Inventor
吴护林
孙彩云
张隆平
何庆兵
陈海涛
罗明波
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Southwest Institute of Technology and Engineering of China South Industries Group
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No 59 Research Institute of China Ordnance Industry
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Abstract

The invention relates to a device for preparing a tubular part inner hole coating. The device comprises a clamping fixture, an auxiliary electrode and a TiCl4 liquid storage tank. The clamping fixture is fixed in the center of a vacuum chamber. The TiCl4 liquid storage tank is connected with the vacuum chamber through a connecting pipe. The clamping fixture is composed of a tubular support supported by three supporting rods, the tubular support is connected with the negative electrode of a direct current pulsed bias power source, and the auxiliary electrode is arranged on the axis line of the clamping fixture and connected with the positive electrode of the direct current pulsed bias power source. Due to the fact that the positive electrode of the direct current pulsed bias power source is connected to the auxiliary electrode in the tubular center and the electric potential is suspended, glow discharging is limited to a tubular part inner hole, the problems that due to limit space, sheaths are overlapped, the ion energy is low and the coating binding force is not good are solved, the problems that entering plasmas from external diffusion are exhausted, the density of the plasmas is low, and the plasmas are distributed unevenly in the axial direction are solved, the density and evenness of the plasmas in a tube are improved, and efficient and axial even deposition is achieved.

Description

A kind of device of preparing tubular member internal coating
Technical field
The present invention relates to a kind of coating preparation facilities, particularly a kind of device of preparing the wear-resisting compound coating of tubular member bore surface
Background technology
The abrasion-resistant coating material and the coating technology thereof that under the hot conditions of various countries' primary study, use in recent years, comprise Ta, Mo, W, Re, Nb, the refractory metals such as Hf and alloy thereof and TiB2, the ceramic body coatings such as ZrO2, coating structure is to multi-layer multi future development, its technology of preparing comprises coating produced by laser cladding, plasma flame applies, the spraying of high speed oxygen-fuel heat, wire explosion spraying and plasma strengthen vapour deposition etc., wherein vapour deposition is owing to realizing infusibility, fire-retardant, the reliable deposition of anti-ablator, and used in a large number, vapour deposition is a kind of by physical processes such as chemical reaction or thermal evaporations, produce the gas atom of deposition material, molecule, ion or aggregate form the method for solid rete at matrix, be divided into physical vapor deposition (PVD) and chemical vapour deposition (CVD), CVD technology has around plurality of advantages such as plating property are good, but depositing temperature is higher, greatly limit its range of application.
The plasma reinforced chemical vapour deposition technology (PECVD) of plasma body being introduced to the formation of CVD technology has greatly activated reaction system, can make pyroreaction realize low temperature synthetic, reach object prepared by coating low temperature, this is because plasma temperature and energy density are high, can make reactant gas molecules generation ionization or activation, can reduce the potential barrier of compound decomposition or chemical combination, temperature of reaction improves speed of reaction when reduction, and plasma body can improve the bonding strength of coating and matrix to the activation of matrix surface in addition.
But, elongated tubular product part is prepared in TiB2/TiN coating procedure at PECVD, because limited space causes sheath ply, ion energy is low, and the outside plasma body diffusing into exhausts fast, energy density is low, and axially inhomogeneous, causes plasma application difficulty in the dark endoporus of slender member.
The existing preparation technology of TiB2/TiN compound coating is as higher in the preparation temperature of the methods such as coating produced by laser cladding, plasma flame coating, the spraying of high speed oxygen-fuel heat, wire explosion spraying, very easily cause matrix oxidation, the high temperature in coating preparation process also can affect the mechanical property of thin-walled tubular member etc. simultaneously.And plasma reinforced chemical vapour deposition technology can make reactant gas molecules generation ionization or activation, can reduce the potential barrier of compound decomposition or chemical combination, realize low temperature depositing, but elongated tubular product part is prepared in TiB2/TiN coating procedure at PECVD, striking difficulty, is difficult to the homogeneity that ensures prepared by coating.
Summary of the invention
The object of the present invention is to provide a kind of device of evenly preparing the wear-resistant coating using under hot conditions at tubular member bore surface.This device has solved an inwall striking difficult problem in the elongated tubular product part PECVD process of big L/D ratio, has realized the even preparation of the wear-resisting compound coating using under tubular member inwall hot conditions.
The object of the invention is to realize by such technical scheme, a kind of device of preparing tubular member internal coating, is characterized in that: comprise clamping fixture, supporting electrode and TiCl 4container for storing liquid, described clamping fixture is fixed on the central position of vacuum chamber, described TiCl 4container for storing liquid is connected with vacuum chamber by pipe connecting;
For pipe fitting part can unsettledly be placed, guarantee the realization of glow discharge, and tubular member is neither contacted with center supporting electrode, prevent short circuit, also do not contact with vacuum-chamber wall, prevent from that vacuum chamber is charged to hurt sb.'s feelings.The tubular bracket that wherein said clamping fixture is held up by three support bars forms, described tubular bracket tube wall upper end is evenly equipped with plural fixed orifices, between described support bar and described tubular bracket by the ceramic body connection of insulating, described tubular bracket is connected with the negative electrode of DC pulse grid bias power supply, and described supporting electrode is arranged on the axial line of described clamping fixture and is fixedly connected with DC pulse grid bias power supply anode.
For reactant gases being delivered directly to tubular member inside, make it have air delivery function concurrently, described supporting electrode is tubulose, comprises that termination is the transition conduit of flat cone mouth shape and the upper induction pipe being fixedly connected with it, and plural gas port is laid in the tube wall end of described upper induction pipe.
For TiCl4 gas is provided, described TiCl4 container for storing liquid comprises tank body, be fastened with the upper cover that sealing-ring is housed at the oral area of described tank body, outside the pipe connecting around tank body and between connection TiCl4 container for storing liquid and vacuum chamber, uniform winding has heating zone, described tank body is connected by pipe connecting with vacuum chamber, on the pipe connecting between described tank body and vacuum chamber, be provided with two stopping valve, described stopping valve is connected with upper cover, and wherein said pipe connecting adopts stainless steel tube effective.
In order to realize the gasification of TiCl4 under assigned temperature, reach the required TiCl4 flow of deposition, can observe pressure and the content of gas in tank body simultaneously, described stopping valve output terminal is provided with pressure vacuum meter, and two pressure vacuum meter the other ends connect respectively nitrogen N 2 output terminals and vacuum chamber input terminus by pipe connecting; In order to measure in real time the Heating temperature of heating zone to tank body, between described heating zone and tank body, be provided with thermopair, and the end of described thermocouple temperature sensitive is placed between heating zone and tank body.
In order to observe at any time the temperature of described container for storing liquid, ensure TiCl4 tank body to carry out thermostatically heating, described pressure vacuum meter and thermopair are all connected on thermostatically heating instrument.
In order to ensure that TiCl4 can not overflow, upper cover and described tank body screw fastening.
In order to assist TiCl4 building-up reactions under safe and reliable Working environment to form settled layer, described TiCl4 container for storing liquid is also connected with hydrogen H2 container for storing liquid, boron trichloride BCl3 container for storing liquid and nitrogen N 2 container for storing liquids, described TiCl4 container for storing liquid and hydrogen H2 container for storing liquid, nitrogen N 2 container for storing liquids connect into gas channels, and described TiCl4 container for storing liquid and hydrogen H2 container for storing liquid also connect into another gas channels with boron trichloride BCl3 container for storing liquid.
For guaranteeing that TiCl4 does not block air delivering pipeline, on described TiCl4 container for storing liquid, be also parallel with argon Ar container for storing liquid, described argon Ar container for storing liquid one end is connected between hydrogen H2 container for storing liquid and nitrogen N 2 container for storing liquid air delivering pipelines, the other end is connected between described TiCl4 container for storing liquid and boron trichloride BCl3 container for storing liquid air delivering pipeline, so that starting stage and ending phase in coating deposition are rinsed air delivering pipeline, prevent that TiCl4 is residual in air delivering pipeline.
Owing to having adopted technique scheme, the present invention has advantages of as follows:
1, the present invention is by being connected on tubular center's supporting electrode and electric potential floating by the anode of grid bias power supply, thereby glow discharge is tied to tubular member endoporus, solve limited space and cause sheath ply, ion energy is low, coating binding force is bad problem, make potential difference clamper added negative bias values on tube wall of tubular axis line and tube wall, guarantee ion fully to accelerate and arrive surface, in realizing deposition, improving bonding force; By perforate on tubular center's supporting electrode, make it have air delivery function concurrently, reactant gases is delivered directly to tubular member inside, solving the outside plasma body diffusing into exhausts fast, density is low, axially inhomogeneous problem, improves density and the homogeneity of managing interior plasma body, realizes efficient and axial uniform deposition.
2, the present invention heats by heating zone and temperature control system control realizes TiCl 4gasification under assigned temperature, reaches the required TiCl of deposition 4flow, monitors the vacuum tightness in tank by pressure vacuum meter, ensures TiCl 4do not contact the TiO that prevents forming poisonous HCl and easily stop up air delivering pipeline with atmosphere 2powder; Two hand stop valves are opened in the situation that gas circuit vacuumizes or fill Ar, control respectively and carry H 2input and gaseous state TiCl 4output, prevent TiCl 4contact with air residual in gas circuit.TiCl to container for storing liquid to vacuum chamber 4air delivering pipeline, not only all adopts heating zone to heat, and has manufactured specially Ar flushing pipeline, in starting stage and the ending phase of deposition, it is rinsed, and prevents TiCl 4residual in air delivering pipeline, guarantee TiCl 4do not block air delivering pipeline.Realize TiCl 4vacuum storage, controlled gasification and transport smoothly.
3, the inventive method can be 35 mm at inner thorax diameter, length-to-diameter ratio is 4.4 bushing pipe inside, adopt plasma reinforced chemical vapour deposition technology to realize uniform deposition, ununiformity is controlled at ± 5% in, with respect to the naked pipe that does not do coating, improved more than 2.3 times the work-ing life that cycling hot is impacted more than 2000 DEG C.
Brief description of the drawings
Fig. 1 is the connection diagram of the embodiment of the present invention;
Fig. 2 is the structural representation of embodiment of the present invention supporting electrode;
Fig. 3 is the clamping tubular member connection diagram of the embodiment of the present invention;
Fig. 4 is the vertical view of Fig. 3;
Fig. 5 is embodiment of the present invention TiCl 4the connection diagram of container for storing liquid.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail, but invention is not limited to present embodiment, any improvement on the present embodiment essence spirit or substitute, still belongs to the claims in the present invention scope required for protection.
Embodiment 1, referring to Fig. 1,3,4: a kind of device of preparing tubular member internal coating, comprises clamping fixture 1, supporting electrode 2 and TiCl 4container for storing liquid 3, described clamping fixture 1 is fixed on the central position of vacuum chamber 4, described TiCl 4container for storing liquid 3 is connected with vacuum chamber 4 by stainless steel tube;
The tubular bracket 12 that wherein said clamping fixture 1 is held up by three support bars 11 forms, described tubular bracket 12 tube wall upper ends are evenly equipped with four fixed orificess 13, by fixed orifices 13, tubular member 6 is fixed on described tubular bracket 12 with screw, between described support bar 11 and described tubular bracket 12, insulate by ceramic body 14, described tubular bracket 12 is connected with the negative electrode of DC pulse grid bias power supply 5, described supporting electrode 2 be arranged on the axial line of described clamping fixture 1 and with DC pulse grid bias power supply 5 anodic bondings.
Described support bar 11 is contained on the base 41 of being located in described vacuum chamber, and described base 41 is supported by foot pad 42, base 41 center drilling mounting kits 43, and center supporting electrode 2 is fixedly connected with DC pulse grid bias power supply 5 anodes by external member 43.
With further reference to Fig. 2: described supporting electrode 2 comprises that termination is the transition conduit 21 of flat cone mouth shape and the upper induction pipe 22 being fixedly connected with it; Four gas ports 23 are laid in the tube wall end of described upper induction pipe 22.
With further reference to Fig. 1,5: described TiCl 4container for storing liquid 3 comprises stainless tank body 31, be fastened with upper cover 32 at the oral area of described stainless steel tank body 31, outside the stainless steel tube around stainless steel tank body 31 and between connection stainless steel tank body 31 and vacuum chamber 4, uniform winding has glass fibre heat tape, between described stainless steel tank body 31 and vacuum chamber 4, on stainless steel tube, be provided with two hand stop valves 33, described hand stop valve 33 is connected with upper cover 32.
Described hand stop valve 33 output terminals are provided with pressure vacuum meter 34, between described heating zone and stainless steel tank body 31, are provided with thermopair.
Described pressure vacuum meter 34 and thermopair are all connected on thermostatically heating instrument.
With further reference to Fig. 1: described TiCl4 container for storing liquid 3 is also connected with hydrogen H2 container for storing liquid, boron trichloride BCl3 container for storing liquid and nitrogen N 2 container for storing liquids, described TiCl4 container for storing liquid and hydrogen H2 container for storing liquid, nitrogen N 2 container for storing liquids connect into gas channels, and described TiCl4 container for storing liquid and hydrogen H2 container for storing liquid also connect into another gas channels with boron trichloride BCl3 container for storing liquid.
On described TiCl4 container for storing liquid, be also parallel with argon Ar container for storing liquid, described argon Ar container for storing liquid one end is connected between hydrogen H2 container for storing liquid and nitrogen N 2 container for storing liquid air delivering pipelines, and the other end is connected between described TiCl4 container for storing liquid and boron trichloride BCl3 container for storing liquid air delivering pipeline.

Claims (9)

1. a device of preparing tubular member internal coating, is characterized in that: comprise clamping fixture (1), supporting electrode (2) and TiCl 4container for storing liquid (3), described clamping fixture (1) is fixed on the central position of vacuum chamber (4), described TiCl 4container for storing liquid (3) is connected with vacuum chamber (4) by pipe connecting,
The tubular bracket (12) that wherein said clamping fixture (1) is held up by three support bars (11) forms, described tubular bracket (12) tube wall upper end is evenly equipped with plural fixed orifices (13), between described support bar (11) and described tubular bracket (12), connect by ceramic body (14) insulation, described tubular bracket (12) is connected with the negative electrode of DC pulse grid bias power supply (5), described supporting electrode (2) be arranged on the axial line of described clamping fixture (1) and with DC pulse grid bias power supply (5) anodic bonding.
2. the device of preparing tubular member internal coating as claimed in claim 1, it is characterized in that: described support bar (11) is contained on the base (41) of being located in described vacuum chamber, described base (41) is supported by foot pad (42), base (41) center drilling mounting kit (43), center supporting electrode (2) is fixedly connected with DC pulse grid bias power supply (5) anode by external member (43).
3. the device of preparing tubular member internal coating as claimed in claim 1 or 2, is characterized in that: described supporting electrode (2) comprises that termination is the transition conduit (21) of flat cone mouth shape and the upper induction pipe (22) being fixedly connected with it.
4. the device of preparing tubular member internal coating as claimed in claim 3, is characterized in that: plural gas port (23) is laid in the tube wall end of described upper induction pipe (22).
5. the device of preparing tubular member internal coating as claimed in claim 1, is characterized in that: described TiCl 4container for storing liquid (3) comprises tank body (31), be fastened with upper cover (32) at the oral area of described tank body (31), outside the pipe connecting around tank body (31) and between connection tank body (31) and vacuum chamber (4), uniform winding has heating zone, on pipe connecting between described tank body (31) and vacuum chamber (4), be provided with two stopping valve (33), described stopping valve (33) is connected with upper cover (32).
6. the device of preparing tubular member internal coating as claimed in claim 5, is characterized in that: described stopping valve (33) output terminal is provided with pressure vacuum meter (34), between described heating zone and tank body (31), is provided with thermopair.
7. the device of preparing tubular member internal coating as claimed in claim 6, is characterized in that: described pressure vacuum meter (34) and described thermopair are all connected on thermostatically heating instrument.
8. the device of preparing tubular member internal coating as described in claim 5 or 6 or 7, it is characterized in that: described TiCl4 container for storing liquid (3) is also connected with hydrogen H2 container for storing liquid, boron trichloride BCl3 container for storing liquid and nitrogen N 2 container for storing liquids, described TiCl4 container for storing liquid and hydrogen H2 container for storing liquid, nitrogen N 2 container for storing liquids connect into gas channels, and described TiCl4 container for storing liquid and hydrogen H2 container for storing liquid also connect into another gas channels with boron trichloride BCl3 container for storing liquid.
9. the device of preparing tubular member internal coating as claimed in claim 8, it is characterized in that: on described TiCl4 container for storing liquid, be also parallel with argon Ar container for storing liquid, described argon Ar container for storing liquid one end is connected between hydrogen H2 container for storing liquid and nitrogen N 2 container for storing liquid air delivering pipelines, and the other end is connected between described TiCl4 container for storing liquid and boron trichloride BCl3 container for storing liquid air delivering pipeline.
CN201310020147.2A 2013-01-21 2013-01-21 A kind of device preparing tubular member internal coating Active CN103938184B (en)

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Application Number Priority Date Filing Date Title
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CN103938184B CN103938184B (en) 2016-03-23

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1851045A (en) * 2006-05-31 2006-10-25 大连理工大学 Slender metal pipe inner wall diamond-film-like deposition method using DC glow discharge
KR20070071506A (en) * 2005-12-30 2007-07-04 삼성전자주식회사 Electrode of plasma enhanced chemical vapor deposition apparatus
EP2251452A2 (en) * 2009-05-13 2010-11-17 CV Holdings, LLC. Vessel processing

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20070071506A (en) * 2005-12-30 2007-07-04 삼성전자주식회사 Electrode of plasma enhanced chemical vapor deposition apparatus
CN1851045A (en) * 2006-05-31 2006-10-25 大连理工大学 Slender metal pipe inner wall diamond-film-like deposition method using DC glow discharge
EP2251452A2 (en) * 2009-05-13 2010-11-17 CV Holdings, LLC. Vessel processing

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
韩永超,等: ""管状工件内表面真空镀膜方法的研究进展"", 《真空》, vol. 49, no. 1, 31 January 2012 (2012-01-31), pages 39 - 44 *

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Effective date of registration: 20240715

Address after: 400039 Chongqing Jiulongpo Yuzhou Road No. 33

Patentee after: Southwest Institute of technology and engineering of China Ordnance Equipment Group

Country or region after: China

Address before: 400039 Chongqing Jiulongpo Shiqiaopu Yuzhou Road No. 33

Patentee before: NO 59 Research Institute OF CHINA ORDNACE INDUSTRY

Country or region before: China