CN103938184B - A kind of device preparing tubular member internal coating - Google Patents
A kind of device preparing tubular member internal coating Download PDFInfo
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- CN103938184B CN103938184B CN201310020147.2A CN201310020147A CN103938184B CN 103938184 B CN103938184 B CN 103938184B CN 201310020147 A CN201310020147 A CN 201310020147A CN 103938184 B CN103938184 B CN 103938184B
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- container
- storing liquid
- tubular member
- ticl
- internal coating
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Abstract
The present invention relates to a kind of device preparing tubular member internal coating, 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, the tubular bracket that wherein said clamping fixture is held up by three support bars is formed, described tubular bracket is connected with the negative electrode of DC pulse grid bias power supply, and the axial line that described supporting electrode is arranged on described clamping fixture is connected with DC pulse grid bias power supply anode.The present invention is by being connected on the anode of grid bias power supply on tubular center's supporting electrode and electric potential floating, thus glow discharge has been tied to tubular member endoporus, solve limited space and cause the problem that sheath ply, ion energy are low, coating binding force is bad, solve the outside plasma body diffused into exhaust fast, density is low, axially uneven problem, improves density and the homogeneity of plasma body in pipe, realizes efficient and axial uniform deposition.
Description
Technical field
The present invention relates to a kind of coating preparation facilities, particularly a kind of device preparing the wear-resisting compound coating of tubular member bore surface
Background technology
The abrasion-resistant coating material used under the hot conditions of various countries' primary study in recent years and coating technology thereof, 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, high velocity oxygen-fuel thermospray, wire explosion spraying and plasma enhanced chemical vapor deposition etc., wherein vapour deposition is owing to realizing 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, 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, strongly limit its range of application.
The PECVD (PECVD) plasma body being introduced CVD technology formation greatly have activated reaction system, pyroreaction can be made to realize low temperature synthesis, reach the object of coating low-temperature growth, this is because plasma temperature and energy density high, reactant gas molecules generation ionization or activation can be made, the potential barrier of compound decomposition or chemical combination can be reduced, improve speed of reaction while temperature of reaction reduces, 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 plasma body that outside diffuses into exhausts fast, energy density is low, and axially uneven, causes plasma application difficulty in the dark endoporus of slender member.
The preparation temperature of the existing preparation technology of TiB2/TiN compound coating as methods such as coating produced by laser cladding, plasma flame coating, high velocity oxygen-fuel thermospray, wire explosion sprayings is higher, very easily cause matrix to be oxidized, the high temperature simultaneously in coating preparation process also can affect the mechanical property of thin-walled tubular part etc.And PECVD can make reactant gas molecules generation ionization or activation, the potential barrier of compound decomposition or chemical combination can be reduced, 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 ensureing prepared by coating.
Summary of the invention
The object of the present invention is to provide a kind of device of the wear-resistant coating used under tubular member bore surface evenly prepares hot conditions.Which solves an inwall striking difficult problem in the elongated tubular product part PECVD process of big L/D ratio, the even preparation of the wear-resisting compound coating used under achieving tubular member inwall hot conditions.
The object of the invention is by such technical scheme realize, a kind of device 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;
In order to make pipe fitting part unsettledly place, 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 that vacuum chamber is charged hurts sb.'s feelings.The tubular bracket that wherein said clamping fixture is held up by three support bars is formed, described tubular bracket tube wall upper end is evenly equipped with plural fixed orifices, connected by ceramic body insulation between described support bar and described tubular bracket, described tubular bracket is connected with the negative electrode of DC pulse grid bias power supply, and the axial line that described supporting electrode is arranged on described clamping fixture is fixedly connected with DC pulse grid bias power supply anode.
In order to reactant gases is delivered directly to tubular member inside, it is made to have air delivery function concurrently, described supporting electrode is tubulose, and comprising termination is the transition conduit of flat cone mouth shape and the upper induction pipe be fixedly connected with it, and plural gas port is laid in the tube wall end of described upper induction pipe.
In order to provide TiCl4 gas, described TiCl4 container for storing liquid comprises tank body, the upper cover that sealing-ring is housed is fastened with at the oral area of described tank body, the outer uniform winding of pipe connecting around tank body and between connection TiCl4 container for storing liquid and vacuum chamber has heating zone, described tank body is connected by pipe connecting with vacuum chamber, pipe connecting between described tank body and vacuum chamber is 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 TiCl4 flow needed for 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 nitrogen N 2 output terminal and vacuum chamber input terminus respectively by pipe connecting; In order to measure the Heating temperature of heating zone to tank body in real time, 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 the temperature of described container for storing liquid at any time, ensure to carry out thermostatically heating to TiCl4 tank body, 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.
Settled layer is formed in order to TiCl4 building-up reactions under safe and reliable Working environment can be assisted, 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 liquid, described TiCl4 container for storing liquid and hydrogen H2 container for storing liquid, nitrogen N 2 container for storing liquid 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, described TiCl4 container for storing liquid is 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 pipeline, the other end is connected between described TiCl4 container for storing liquid and boron trichloride BCl3 container for storing liquid air delivering pipeline, to rinse air delivering pipeline in the starting stage that coating deposits and ending phase, prevent TiCl4 residual in air delivering pipeline.
Owing to have employed technique scheme, the present invention has following advantage:
1, the present invention is by being connected on the anode of grid bias power supply on tubular center's supporting electrode and electric potential floating, thus glow discharge has been tied to tubular member endoporus, solve limited space and cause the problem that sheath ply, ion energy are low, coating binding force is bad, make the negative bias values that the potential difference clamper of tubular axis line and tube wall is added on tube wall, guarantee that ion fully can accelerate and arrive surface, while realization deposition, improve bonding force; By perforate on tubular center's supporting electrode, it is made to have air delivery function concurrently, reactant gases is delivered directly to tubular member inside, solve the outside plasma body diffused into exhaust fast, density is low, axially uneven problem, improves density and the homogeneity of plasma body in pipe, realizes efficient and axial uniform deposition.
2, the present invention is heated by heating zone and temperature control system control realization TiCl
4gasification under assigned temperature, reaches the TiCl needed for deposition
4flow, monitors the vacuum tightness in tank by pressure vacuum meter, ensure TiCl
4not with atmosphere, prevent the TiO forming poisonous HCl and easily block air delivering pipeline
2powder; Two hand stop valves are opened when gas circuit vacuumizes or fill Ar, control respectively to carry H
2input and gaseous state TiCl
4output, prevent TiCl
4contact with air residual in gas circuit.To container for storing liquid to the TiCl of vacuum chamber
4air delivering pipeline, not only all adopts heating zone to heat, and has manufactured Ar flushing pipeline specially, rinse, prevent TiCl in the starting stage deposited and ending phase to it
4residual in air delivering pipeline, guarantee TiCl
4do not block air delivering pipeline.Achieve TiCl
4vacuum store, controlled gasification and transporting smoothly.
3, the inventive method can be 35mm at inner thorax diameter, length-to-diameter ratio is the bushing pipe inside of 4.4, PECVD is adopted to realize uniform deposition, ununiformity controls within ± 5%, relative to the naked pipe not doing coating, the work-ing life that cycling hot is impacted more than 2000 DEG C improves more than 2.3 times.
Accompanying drawing explanation
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
Be described in further detail the specific embodiment of the present invention below in conjunction with accompanying drawing, but invention is not limited to present embodiment, any improvement or alternative on the present embodiment essence spirit, still belongs to the claims in the present invention scope required for protection.
Embodiment 1, see Fig. 1,3,4: a kind of device 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 is formed, described tubular bracket 12 tube wall upper end is evenly equipped with four fixed orificess 13, by fixed orifices 13, tubular member 6 is fixed on described tubular bracket 12 with screw, insulated by ceramic body 14 between described support bar 11 and described tubular bracket 12, described tubular bracket 12 is connected with the negative electrode of DC pulse grid bias power supply 5, and the axial line that described supporting electrode 2 is arranged on described clamping fixture 1 is connected with DC pulse grid bias power supply 5 anode.
Described support bar 11 is contained on the base 41 be located in described vacuum chamber, and described base 41 is supported by foot pad 42, and 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.
With further reference to Fig. 2: it is the transition conduit 21 of flat cone mouth shape and the upper induction pipe 22 be fixedly connected with it that described supporting electrode 2 comprises termination; 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, upper cover 32 is fastened with at the oral area of described stainless steel tank body 31, the outer uniform winding of stainless steel tube around stainless steel tank body 31 and between connection stainless steel tank body 31 and vacuum chamber 4 has glass fibre heat tape, between described stainless steel tank body 31 and vacuum chamber 4, stainless steel tube is provided with two hand stop valves 33, described hand stop valve 33 is connected with upper cover 32.
Described hand stop valve 33 output terminal is provided with pressure vacuum meter 34, between described heating zone and stainless steel tank body 31, be 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 liquid, described TiCl4 container for storing liquid and hydrogen H2 container for storing liquid, nitrogen N 2 container for storing liquid 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.
Described TiCl4 container for storing liquid is 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 pipeline, 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. prepare a device for tubular member internal coating, it 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) is formed, described tubular bracket (12) tube wall upper end is evenly equipped with plural fixed orifices (13), connected by ceramic body (14) insulation between described support bar (11) and described tubular bracket (12), described tubular bracket (12) is connected with the negative electrode of DC pulse grid bias power supply (5), the axial line that described supporting electrode (2) is arranged on described clamping fixture (1) is connected with DC pulse grid bias power supply (5) anode.
2. prepare the device of tubular member internal coating as claimed in claim 1, it is characterized in that: described support bar (11) is contained on the base (41) be 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. prepare the device of tubular member internal coating as claimed in claim 1 or 2, it is characterized in that: it is the transition conduit (21) of flat cone mouth shape and the upper induction pipe (22) be fixedly connected with it that described supporting electrode (2) comprises termination.
4. prepare the device of tubular member internal coating as claimed in claim 3, it is characterized in that: plural gas port (23) is laid in the tube wall end of described upper induction pipe (22).
5. prepare the device of tubular member internal coating as claimed in claim 1, it is characterized in that: described TiCl
4container for storing liquid (3) comprises tank body (31), upper cover (32) is fastened with at the oral area of described tank body (31), the outer uniform winding of pipe connecting around tank body (31) and between connection tank body (31) and vacuum chamber (4) has heating zone, pipe connecting between described tank body (31) and vacuum chamber (4) is provided with two stopping valve (33), described stopping valve (33) is connected with upper cover (32).
6. prepare the device of tubular member internal coating as claimed in claim 5, it 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), be provided with thermopair.
7. prepare the device of tubular member internal coating as claimed in claim 6, it is characterized in that: described pressure vacuum meter (34) and described thermopair are all connected on thermostatically heating instrument.
8. the device preparing tubular member internal coating as described in claim 5 or 6 or 7, is characterized in that: described TiCl
4 container for storing liquid (3) is also connected with hydrogen H
2container for storing liquid, boron trichloride BCl
3container for storing liquid and nitrogen N
2container for storing liquid, described TiCl
4container for storing liquid and hydrogen H
2container for storing liquid, nitrogen N
2container for storing liquid connects into gas channels, described TiCl
4container for storing liquid and hydrogen H
2container for storing liquid also with boron trichloride BCl
3container for storing liquid connects into another gas channels.
9. prepare the device of tubular member internal coating as claimed in claim 8, it is characterized in that: described TiCl
4container for storing liquid is also parallel with argon Ar container for storing liquid, and described argon Ar container for storing liquid one end is connected to hydrogen H
2container for storing liquid and nitrogen N
2between container for storing liquid air delivering pipeline, the other end is connected to described TiCl
4container for storing liquid and boron trichloride BCl
3between container for storing liquid air delivering pipeline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310020147.2A CN103938184B (en) | 2013-01-21 | 2013-01-21 | A kind of device preparing tubular member internal coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310020147.2A CN103938184B (en) | 2013-01-21 | 2013-01-21 | A kind of device preparing tubular member internal coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103938184A CN103938184A (en) | 2014-07-23 |
| CN103938184B true CN103938184B (en) | 2016-03-23 |
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ID=51186045
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310020147.2A Active CN103938184B (en) | 2013-01-21 | 2013-01-21 | A kind of device preparing tubular member internal coating |
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| Country | Link |
|---|---|
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Citations (3)
| 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 |
-
2013
- 2013-01-21 CN CN201310020147.2A patent/CN103938184B/en active Active
Patent Citations (3)
| 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)
| Title |
|---|
| "管状工件内表面真空镀膜方法的研究进展";韩永超，等;《真空》;20120131;第49卷(第1期);第39-44页 * |
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|---|---|
| CN103938184A (en) | 2014-07-23 |
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