CN100500934C - Method and device for plating diamond like film on inner-outer wall of quartz round tube - Google Patents
Method and device for plating diamond like film on inner-outer wall of quartz round tube Download PDFInfo
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- CN100500934C CN100500934C CNB2007100518330A CN200710051833A CN100500934C CN 100500934 C CN100500934 C CN 100500934C CN B2007100518330 A CNB2007100518330 A CN B2007100518330A CN 200710051833 A CN200710051833 A CN 200710051833A CN 100500934 C CN100500934 C CN 100500934C
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Abstract
The invention provides a method and apparatus for plating diamond or fake-diamond membrane on the inner and outer wall of quartz circular tubes. The method includes: firstly cylindraceous plasma is produced between both coaxial quartz circular tubes microwave-excited working-gas-discharge, then plating diamond or fake-diamond membrane on the outer wall of inner quartz circular tube or on the inner wall of outer quartz circular tube using plasma activated chemical vapour deposition arts, in which the plated membrane is compact and uniform with good adhesive strenght. The apparatus comprises microwave source (1), microwave match (2), waveguide coupling plasma reactor (3) and vanuum system. The structure of said waveguide coupling plasma reactor is: flange and air-in and off-gas passage at both ends; metal water-cooled jacket (7) and inner and outer quartz circular tubes in intermediate section, provided with copper tube (15) in inner quartz circular tube (11); the cavity between both quartz circular tubes is vacuum chamber (12). The apparatus can plate membrane on different-sized quartz circular tubes walls.
Description
Technical field
The present invention relates to plasma technique and diamond, quasi-diamond superhard material Application Areas, particularly a kind of plasma chemical vapor deposition technique that utilizes is at the inwall of quartz round tube or the method and the device of gold-plated hard rock of outer wall or diamond like carbon film.
Background technology
Diamond and quasi-diamond have the highest hardness, high heat conductance and chemical stability, and good light transmittance, therefore are widely used in machining, optics, microelectronics and military field.Particularly diamond and quasi-diamond have good acidproof, alkaline-resisting characteristic, can use under the environment of very severe during therefore as supercoat.Silica glass owing to have good light transmittance, thermostability, resistance to acids and bases is widely used in the liquid level observation of boiler preferably.But because the glassware for drinking water of boiler has weakly alkaline, the long-time inside and outside wall of back silica tube that uses weathers influence observation.For increasing the service life, need plate layer protecting film at the inside and outside wall of silica tube.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of at the inwall of quartz round tube or the method and apparatus of gold-plated hard rock of outer wall or diamond like carbon film, this method and device can utilize plasma chemical vapor deposition in quartz round tube inwall or gold-plated hard rock of outside surface or diamond like carbon film, thereby reach wear-resistant, erosion-resisting purpose, to prolong the work-ing life of quartz round tube.
The technical solution adopted in the present invention is as follows:
The invention provides and a kind ofly utilize plasma activated chemical vapour deposition to be in the method for quartz round tube inwall or gold-plated hard rock of outer wall or diamond-film-like: at first utilize the discharge of microwave excitation working gas between the quartz round tube of two coaxial placements, to produce plasma body cylindraceous, utilize again plasma chemical vapor deposition technique the outer wall of interior silica tube or outside the gold-plated hard rock of inwall or the diamond like carbon film of silica tube.This method may further comprise the steps:
A. feed working gas in vacuum chamber, utilize the discharge of microwave excitation working gas, make it to produce plasma body, the operating air pressure of vacuum chamber is 1～6kPa.
B. when outer wall plated film that need be at interior silica tube, at first utilize the outer wall of the internal silica tube of diadust (particle diameter 0.1～2 μ m) to polish uniformly, it is smooth that the inwall of outer silica tube keeps, the temperature of quartzy tube wall is at 400～800 ℃ in making by the temperature of controlling the copper pipe in the interior silica tube again, and the outer metal water jacket of outer silica tube feeds water coolant.
C. at needs outside during the inwall plated film of silica tube, at first utilize the inwall of the external silica tube of diadust (particle diameter 0.1～2 μ m) to polish uniformly, it is smooth that the outer wall of interior silica tube keeps, in copper pipe, feed water coolant, and not feeding water coolant in the metal water jacket outside the outer silica tube, the temperature that makes outer quartzy tube wall is at 400～800 ℃.
The invention provides a kind of device that can realize aforesaid method, it comprises microwave source, microwave matching, waveguide-coupled plasma reactor and vacuum system.The structure of described waveguide-coupled plasma reactor is: respectively there is flange at its two ends, and two flanges are respectively equipped with induction trunk and the bleed-off passage with vacuum chamber; The interior silica tube that its middle part is provided with the metal water jacket that interlocks successively, outer silica tube and communicates with atmosphere is provided with copper pipe in the middle of the interior silica tube, and the outer wall of copper pipe closely contacts with the inwall of interior silica tube during plated film; Two silica tubes are provided with vaccum seal ring between its two ends and flange, and the cavity between it is a vacuum chamber, and its axis is consistent with the power line of microwave field in the waveguide, and microwave is set up strong axial electric field; At the inner chamber of rectangular waveguide, be provided with the short-circuit plunger of regulating the distribution situation of this axial electric field between quartz round tube.
The invention has the beneficial effects as follows: can be as required optionally at the gold-plated hard rock of interior or outer wall or the quasi-diamond protective membrane of silica tube, the protective membrane densification of being plated, evenly, adhesion strength is good, has good acid-and base-resisting corrosive characteristic.Device provided by the invention can according to the needs of industrial application external diameter of pipe less than 100mm, bore greater than the quartzy tube wall of the different size specification of 5mm on plated film.
Description of drawings
Fig. 1 is first kind of structural representation of the present invention.
Fig. 2 is second kind of structural representation of the present invention.
Fig. 3 is the structural representation of the present invention when being used for the quartz round tube outer wall plated film of end sealing.
Embodiment
The invention provides and a kind ofly utilize plasma activated chemical vapour deposition in quartz round tube or the method for gold-plated hard rock of outer wall or diamond-film-like, this method is: at first utilize microwave excitation working gas discharge between the quartz round tube of two coaxial placements, to produce plasma body cylindraceous, utilize again plasma chemical vapor deposition technique the outer wall of interior silica tube or outside the inwall depositing diamond or the diamond like carbon film of silica tube.This method may further comprise the steps:
A. feed working gas in vacuum chamber 12, utilize the discharge of microwave excitation working gas, make it to produce plasma body, the operating air pressure of vacuum chamber is 1～6kPa.
B. when outer wall plated film that need be at interior silica tube 11, at first utilize the outer wall of the internal silica tube of diadust (particle diameter 0.1～2 μ m) to polish uniformly, it is smooth that the inwall of outer silica tube 10 keeps, the temperature of quartzy tube wall is at 400～800 ℃ in making by the temperature of controlling the copper pipe 15 in the interior silica tube again, and the outer metal water jacket 7 of outer silica tube feeds water coolants.
C. at needs outside during the inwall plated film of silica tube 10, at first utilize the inwall of the external silica tube of diadust (particle diameter 0.1～2 μ m) to polish uniformly, it is smooth that the outer wall of interior silica tube 11 keeps, in copper pipe 15, feed water coolant, and not feeding water coolant in the metal water jacket 7 outside the outer silica tube, the temperature that makes outer quartzy tube wall is at 400～800 ℃.
The present invention also provides a kind of device that can realize aforesaid method.
Below in conjunction with specific embodiment and accompanying drawing described device is described further, but does not limit the present invention.
Embodiment 1.
As shown in Figure 1 utilize plasma activated chemical vapour deposition at the inwall of quartz round tube or the device of outer wall depositing diamond or diamond like carbon film, its structure is: comprise microwave source 1, microwave matching 2, waveguide-coupled plasma reactor 3 and vacuum system, microwave matching 2 is made up of circulator, water load and three screw impedance tuners.Wherein, the structure of waveguide-coupled plasma reactor 3 is: its two ends have upper flange 8, lower flange 9, two flanges to be respectively equipped with induction trunk 13 and bleed-off passage 14 with vacuum chamber respectively; Its middle part is provided with metal water jacket 7, outer silica tube 10 that interlocks successively and the interior silica tube 11 that communicates with atmosphere, is provided with copper pipe 15 in the middle of the interior silica tube, and the outer wall of copper pipe closely contacts with the inwall of interior silica tube during plated film; Two silica tubes are provided with the vaccum seal ring 4 of rubber material between its two ends and flange, the cavity between it is a vacuum chamber 12, and its axis is consistent with the power line of microwave field in the waveguide, and microwave is set up strong axial electric field; The inner chamber of rectangular waveguide 5 is provided with short-circuit plunger 6, is used to regulate the distribution of axial electric field between quartz round tube.
Above-mentioned microwave source 1, the frequency of the microwave of its generation are 2.45GHz, or 915MHz; According to the size situation of the silica tube of actual needs plated film and decide.
When outer wall plated film that need be at interior silica tube 11, at first utilize the outer wall of the internal silica tube of diadust (particle diameter 0.1～2 μ m) to polish uniformly, it is smooth that the inwall of outer silica tube keeps, the temperature of quartzy tube wall is at 400～800 ℃ in making by the temperature of controlling the copper pipe 15 in the interior silica tube again, and the outer metal water jacket of outer silica tube feeds water coolant.
At needs outside during the inwall plated film of silica tube 10, at first utilize the inwall of the external silica tube of diadust (particle diameter 0.1～2 μ m) to polish uniformly, it is smooth that the outer wall of interior silica tube keeps, in copper pipe 15, feed water coolant, and not feeding water coolant in the metal water jacket outside the outer silica tube, the temperature that makes outer quartzy tube wall is at 400～800 ℃.
During plated film, plasma body is that vacuum chamber 12 produces between two silica tubes, and plasma body becomes to cylindric because of the restriction that is subjected to quartzy tube wall.Vacuum chamber 12 is a reaction chamber, and its operating air pressure can be 1～6kPa.Working gas can adopt: methane and hydrogen, methyl alcohol and hydrogen, ethanol and hydrogen or acetone and hydrogen etc.
This device has a waveguide-coupled plasma reactor, and itself and microwave source 1, microwave matching 2 constitute a film coating unit.
The present invention can be according to the difference of the silica tube length of requirement plated film, adopts the use that is together in series of two or more a plurality of film coating unit, thereby derive following examples on the basis of embodiment 1.
Embodiment 2.
As shown in Figure 2 utilize plasma activated chemical vapour deposition at the inwall of quartz round tube or the device of gold-plated hard rock of outer wall or diamond like carbon film, its film coating unit has two, their uses that is together in series.Other is with the structure of embodiment 1.
Embodiment 3.
The gold-plated hard rock of outer wall that utilizes the quartz round tube 16 that plasma activated chemical vapour deposition at one end seals as shown in Figure 3 or the device of diamond like carbon film, its film coating unit has two, their uses that is together in series.The upper flange 17 of device is a blind flange, and other is with the structure of embodiment 1.
Among the present invention, the quantity of film coating unit is mainly by the length decision of the plasma body of needs.Increase the quantity of film coating unit, can increase the length of cylindric plasma body.
The present invention can be at external diameter of pipe less than 100mm, bore gold-plated hard rock of interior or outer wall or the diamond like carbon film greater than the quartz round tube of the different size specification of 5mm.
Working process of the present invention is: the microwave that microwave source 1 produces is gone into waveguide coupled plasma reactor 3 through microwave matching 2 is laggard, excite the thin working gas discharge generation plasma body between two silica tubes, by to the surface treatment of quartzy tube wall and the temperature of control silica tube, can deposit diamond or diamond like carbon film on the outer wall of the inwall of silica tube 10 or interior silica tube 11 outside respectively.During plated film, the quartz round tube wall that needs plated film is through the bortz powder milled processed, and the copper pipe 15 in the internal respectively as required silica tube carries out the water flowing cooling or energising is heated, and makes coating temperature be controlled at 400-800 ℃.
Working gas is fed by the induction trunk on the upper flange 8 13, has bleed-off passage 14 simultaneously on lower flange 9, is connected with vacuum pump by valve, and the operating air pressure in vacuumometer Indicator Reaction chamber is housed.
Claims (9)
- One kind in quartz round tube or the method for gold-plated hard rock of outer wall or diamond like carbon film, it is characterized in that the using plasma chemical gaseous phase depositing process, promptly at first utilize microwave excitation working gas discharge between the quartz round tube of two coaxial placements, to produce plasma body cylindraceous, utilize again the plasma activated chemical vapour deposition method the outer wall of interior silica tube or outside the inwall depositing diamond or the diamond like carbon film of silica tube; This method may further comprise the steps:A. feed working gas in vacuum chamber (12), utilize the discharge of microwave excitation working gas, make it to produce plasma body, the operating air pressure of vacuum chamber is 1～6kPa;B. need be when the outer wall plated film of interior silica tube (11), at first utilizing particle diameter is that the outer wall of the internal silica tube of diadust of 0.1～2 μ m carries out uniform grinding process, it is smooth that the inwall of outer silica tube (10) keeps, the temperature of quartzy tube wall is at 400～800 ℃ in making by the temperature of controlling the copper pipe (15) in the interior silica tube again, and the outer metal water jacket (7) of outer silica tube feeds water coolant;When c. needing the inwall plated film of silica tube (10) outside, at first utilizing particle diameter is that the inwall of the external silica tube of diadust of 0.1～2 μ m carries out uniform grinding process, it is smooth that the outer wall of interior silica tube (11) keeps, in copper pipe (15), feed water coolant, and not feeding water coolant in the metal water jacket (7) outside the outer silica tube, the temperature that makes outer quartzy tube wall is at 400～800 ℃.
- 2. the method for gold-plated hard rock according to claim 1 or diamond like carbon film is characterized in that used working gas adopts the mixed gas of methane and hydrogen, methyl alcohol and hydrogen, ethanol and hydrogen or acetone and hydrogen.
- 3. the method for gold-plated hard rock according to claim 2 or diamond like carbon film, when it is characterized in that used working gas is methane and hydrogen, the shared volume ratio of methane is 0.5～2%.
- 4. the method for gold-plated hard rock according to claim 2 or diamond like carbon film, when it is characterized in that used working gas adopts methyl alcohol and hydrogen, ethanol and hydrogen or acetone and hydrogen, the mole ratio of methyl alcohol, ethanol or acetone and hydrogen is 10～30%.
- 5. one kind at the inwall of quartz round tube or the device of gold-plated hard rock of outer wall or diamond like carbon film, comprise microwave source (1), microwave matching (2), waveguide-coupled plasma reactor (3) and vacuum system, it is characterized in that a kind ofly utilizing plasma activated chemical vapour deposition at the inwall of quartz round tube or the device of gold-plated hard rock of outer wall or diamond like carbon film, wherein, the structure of waveguide-coupled plasma reactor (3) is: respectively there is flange at its two ends, and two flanges are respectively equipped with induction trunk (13) and the bleed-off passage (14) that is communicated with vacuum chamber (12); The interior silica tube (11) that its middle part is provided with the metal water jacket (7) that interlocks successively, outer silica tube (10) and communicates with atmosphere is provided with copper pipe (15) in the middle of the interior silica tube, and the outer wall of copper pipe during plated film (15) closely contacts with the inwall of interior silica tube (11); Two silica tubes are provided with vaccum seal ring (4) between its two ends and flange, the cavity between it is vacuum chamber (12), and its axis is consistent with the power line of microwave field in the waveguide, and microwave is set up strong axial electric field; Inner chamber in rectangular waveguide (5) is provided with the short-circuit plunger (6) of regulating the distribution situation of axial electric field between quartz round tube.
- 6. device according to claim 5 is characterized in that: the waveguide-coupled plasma reactor has one at least, constitutes a film coating unit with microwave source (1), microwave matching (2); A plurality of film coating unit adopt series system to link to each other.
- 7. device according to claim 5 is characterized in that: the frequency of the microwave that used microwave source (1) produces is 2.45GHz, and corresponding waveguide specification is BJ-22 or BJ-26; Or 915MHz, corresponding waveguide specification is BJ-9.
- 8. device according to claim 5 is characterized in that: the operating air pressure of vacuum chamber (12) is 1～6kPa.
- 9. device according to claim 5 is characterized in that: need be when the outer wall plated film of silica tube, and this silica tube uses as the interior silica tube (11) of device; Need be when the inwall plated film of silica tube, this silica tube uses as the outer silica tube (10) of device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100518330A CN100500934C (en) | 2007-04-10 | 2007-04-10 | Method and device for plating diamond like film on inner-outer wall of quartz round tube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100518330A CN100500934C (en) | 2007-04-10 | 2007-04-10 | Method and device for plating diamond like film on inner-outer wall of quartz round tube |
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| CN101037768A CN101037768A (en) | 2007-09-19 |
| CN100500934C true CN100500934C (en) | 2009-06-17 |
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| CNB2007100518330A Expired - Fee Related CN100500934C (en) | 2007-04-10 | 2007-04-10 | Method and device for plating diamond like film on inner-outer wall of quartz round tube |
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Families Citing this family (14)
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| JP5073545B2 (en) * | 2008-03-26 | 2012-11-14 | 東京エレクトロン株式会社 | Plasma processing apparatus and plasma processing method |
| CN101734642B (en) * | 2008-11-05 | 2013-01-16 | 新疆天业（集团）有限公司 | Plasma high temperature carbon conversion gas film reactor |
| CN103074594A (en) * | 2011-10-25 | 2013-05-01 | 浚鑫科技股份有限公司 | Quartz tube used in tablet PECVD equipment and installation method thereof |
| CN102794146B (en) * | 2012-08-17 | 2013-12-11 | 清华大学 | Microwave plasma reaction device for preparing nano-material |
| CN103526187A (en) * | 2013-10-12 | 2014-01-22 | 武汉工程大学 | Large-area microwave plasma chemical vapor deposition system |
| CN104561931B (en) * | 2015-01-25 | 2017-12-26 | 渤海大学 | Metal organic chemical vapor deposition device |
| CN106282973A (en) * | 2015-06-26 | 2017-01-04 | 核工业西南物理研究院 | Device and method for inside pipe wall plated film |
| CN105417962A (en) * | 2015-12-04 | 2016-03-23 | 太仓市建兴石英玻璃厂 | Quartz glass tube with corrosion-resistant film on surface |
| CN105970166A (en) * | 2016-05-20 | 2016-09-28 | 广东蒙泰纺织纤维有限公司 | Production method of polypropylene fiber wire |
| CN108615667B (en) * | 2016-12-09 | 2020-04-14 | 韩国三重核心株式会社 | Low-pressure plasma reactor with improved ignition performance |
| CN108385082A (en) * | 2016-12-21 | 2018-08-10 | 中国航空制造技术研究院 | A method of depositing DLC protection films in accessory inner surface |
| CN108277474A (en) * | 2018-03-21 | 2018-07-13 | 北京沅瀚环境科技有限公司 | A method of in tubular workpiece inner wall deposition of high-quality diamond coatings |
| CN110418486A (en) * | 2019-07-19 | 2019-11-05 | 武汉光盛通设备咨询有限公司 | A kind of double plasma resonator |
| CN114759333B (en) * | 2022-06-14 | 2022-09-02 | 成都纽曼和瑞微波技术有限公司 | Microwave transmission device and microwave plasma equipment |
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2007
- 2007-04-10 CN CNB2007100518330A patent/CN100500934C/en not_active Expired - Fee Related
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Assignee: Hubei E-Xin Diamond Material Co., Ltd. Assignor: Wuhan Institute of Technology Contract record no.: 2010420000188 Denomination of invention: Method and device for plating diamond like film on inner-outer wall of quartz round tube Granted publication date: 20090617 License type: Exclusive License Open date: 20070919 Record date: 20101221 |
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