CN102627413B - Composite fiber preparation method of microwave-assisted diamond-like carbon film covered glass fiber - Google Patents
Composite fiber preparation method of microwave-assisted diamond-like carbon film covered glass fiber Download PDFInfo
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- CN102627413B CN102627413B CN2012101437825A CN201210143782A CN102627413B CN 102627413 B CN102627413 B CN 102627413B CN 2012101437825 A CN2012101437825 A CN 2012101437825A CN 201210143782 A CN201210143782 A CN 201210143782A CN 102627413 B CN102627413 B CN 102627413B
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Abstract
The invention relates to a composite fiber preparation method of microwave-assisted diamond-like carbon film covered glass fibers. The method comprises the following steps of: 1) starting a microwave plastic chemical vapor deposition system and vacuumizing; 2) feeding natural gas into a cylindrical stainless steel vacuum chamber to enable the natural gas to be fully filled in the entire cylindrical stainless steel vacuum chamber; 3) starting a microwave source to enable the microwave source to generate microwaves to excite plasmas in a conical metal roller, so as to fully decompose the natural gas into hydrocarbon groups with activity; 4) adding raw material glass fibers into the conical metal roller; 5) starting a motor to enable the raw materials to be evenly dispersed and centrifugally move, wherein, at the moment, the hydrocarbon groups produced by the decomposed natural gas are deposited on the surfaces of the glass fibers and grow to a diamond-like carbon film, and composite fibers, i.e. the diamond-like carbon film covered glass fibers are formed and are regularly discharged; 6) repeating step 1 to step 5; and 7) after the production is finished, closing all valves and shutting down the microwave and the engine. The composite fiber preparation method of microwave-assisted diamond-like carbon film covered glass fibers provided by the invention has the advantages of low cost, simplicity in implementation and convenience in operation.
Description
Technical field
The present invention relates to diamond like carbon film reinforced composite field, relate in particular to the conjugated fibre preparation method that the microwave-assisted diamond like carbon film coats glass fibre.
Background technology
Along with world's Mineral resources increasingly reduce and industrial production in the increase day by day of materials demand, fibre reinforced composites, all are widely used in all respects such as productive life, military and national defense the significant reinforced effects of the mechanical property of materials due to it.And cheap and rather well received due to its material plant fiber of wood plastic composite, but needing the subject matter solved in the wood plastic composite production process is the wetting property of improving between vegetable fibre and thermoplastics, to strengthen the bonding properties between vegetable fibre and matrix plastic.At present, chemical treatment method commonly used can improve vegetable fibre reinforced composite impact property, bending property, but it is a lot of aspect tensile property, because of weakening of the mechanical strength of vegetable fibre own, to have descended, limited its widespread use in a lot of fields, chemical process inevitably produces environmental pollution simultaneously, does not meet the theory of social enviroment protection development.Therefore, be worth cheap glass fibre as a kind of inorganic environmental friendliness shaped material for carbon fiber, fiberglass plastic matrix material (glass plastic composite materials) gets more and more people's extensive concerning, but the glass plastic composite materials need to solve wettability between fiber and plastics equally to increase the problem of bonding properties between interface.Along with China's glass output improves constantly, glass fiber product must squeeze into the international market, and quality product is the key of competitive power power.The exploitation new product, improve quality and must take the treating compound technology as prerequisite.Because diamond like carbon film possesses excellent mechanical property, good wettability and the bonding force superior with substrate, if it is used for coating glass fibre, will improve significantly mechanical property and the wettability of glass fibre, and then improve the over-all properties of glass plastic composite materials.
In sum, we propose to utilize microwave plasma CVD (MWPECVD), take cheap Sweet natural gas as reactant gases at fiberglass surfacing depositing diamond-like film, with the mechanical property that increases glass fibre with improve its wettability of the surface, and then improve the over-all properties of glass plastic composite materials.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind ofly to be implemented microwave-assisted diamond like carbon film simple, convenient operation and coats the conjugated fibre preparation method of glass fibre.
For addressing the above problem, microwave-assisted diamond like carbon film of the present invention coats the conjugated fibre preparation method of glass fibre, comprises the following steps:
(1) start the microwave plasma CVD system, by extraction valve, by cylindrical stainless-steel vacuum, indoor vacuum is extracted into 10
-3below Pa;
(2) by the intake valve in described microwave plasma CVD system, Sweet natural gas is passed into to described cylindrical Stainless steel chamber, make it evenly be full of whole described cylindrical Stainless steel chamber;
(3) start the microwave source in the microwave plasma CVD system, the microwave that described microwave source is produced enters described cylindrical Stainless steel chamber by waveguide from left quartz window, and activated plasma in the cone-shaped metal cylinder in described microwave plasma CVD system, Sweet natural gas fully is decomposed into to the activated hydrocarbon group of tool;
(4) the raw material glass fibre in storage compartment in described microwave plasma CVD system is added in described cone-shaped metal cylinder by charging valve;
(5) start the electric motor in the microwave plasma CVD system, described motor drive rotating shaft drives the plectrum rotation of described cone-shaped metal cylinder together with its inwall by the flange at quartz window center, right side and the cross frame of bearing and the indoor described cone-shaped metal cylinder right-hand member of described cylindrical stainless-steel vacuum, the raw material that continuously will be gathered in described cone-shaped metal cylinder bottom is transported to top from bottom and falls under the effect of gravity, rotation along with described cone-shaped metal cylinder, make raw material dispersed and centrifugal motion occurs and end motion to the right, meanwhile, Sweet natural gas decomposes the hydrocarbon group produced and deposits and grow into diamond like carbon film at fiberglass surfacing, form conjugated fibre---the glass fibre that quasi-diamond coats, finally from described cone-shaped metal cylinder right-hand member, by bleeder valve, regularly discharge, it is outdoor that the gas that there is no a complete reaction is discharged described cylindrical stainless-steel vacuum by extraction valve,
(6) repeat (1) ~ (5) step;
(7), after producing end, close described intake valve, extraction valve, charging valve, bleeder valve and microwave source and electric motor.
Described microwave plasma CVD system refers to that this system comprises that horizontal positioned and two ends, left and right are respectively equipped with the cylindrical Stainless steel chamber of quartz window, microwave source, cone-shaped metal cylinder and storage compartment; The left side of described cylindrical Stainless steel chamber is provided with described microwave source and waveguide, and its right side is provided with electric motor, is provided with described cone-shaped metal cylinder in it, and its top is provided with described storage compartment and charging valve; The top right side of described cylindrical Stainless steel chamber is provided with intake valve, and its bottom left is provided with extraction valve, and its right side, bottom is provided with bleeder valve; The left end of described cone-shaped metal cylinder is provided with baffle plate, and its inner wall even distribution has several plectrums, and its right-hand member is provided with cross frame; One end of described electric motor is provided with rotating shaft, and this rotating shaft is through being fixed on the described cylindrical Stainless steel chamber supercentral flange of right side quartz window and bearing is connected with the center of described cross frame.
The pipeline that passes on left of described cone-shaped metal cylinder is connected with described storage compartment, and this pipeline is provided with charging valve.
The left side barrel dliameter of described cone-shaped metal cylinder is less than its right side barrel dliameter.
Described charging valve and described bleeder valve be external time switch all.
The present invention compared with prior art has the following advantages:
1, fiberglass surfacing is processed, improving its wettability is the technical difficult points of utilizing the glass plastic composite materials, and chemical treatment method at present used can inevitably be sacrificed its mechanical property when raising is infiltrating.The present invention coats diamond like carbon film at fiberglass surfacing, increases its surface wettability, improves the physical strength of glass fibre simultaneously.In addition, diamond like carbon film, than tensio-active agent, has more stable chemical property, can be on active service at extreme environment, and have longer work-ing life.
2, produce microwave because the present invention uses microwave source, excite highdensity microwave plasma, therefore, diamond like carbon film is in the easy nucleation of substrate surface, and do not need substrate bias auxiliary, thereby simple to operate, is convenient to realize and be dirt cheap.
3, intermediate roll formula reaction unit of the present invention is conducive to dispersed at reaction compartment of raw material to be plated, guarantees the homogeneity coated, and can add raw material how to be plated simultaneously.
4, the design of conical drum in the present invention for self-emptying provides possibility, can be controlled the reaction times of raw material simultaneously by its rotating speed, can produce the product of inhomogeneity thin diamond film thickness, realizes the controllability of coating material thickness.
5, be provided with the charging valve (size of charging valve opening determines feed rate) of storage compartment, time opening adjustable feed rate and the bleeder valve of time opening in the present invention, for continuous high efficiency production in enormous quantities is given security.
6, inlet mouth of the present invention and bleeding point lay respectively at cylindrical Stainless steel chamber upper right and lower-left end, make reactant gases be full of the cone-shaped metal cylinder, realize decomposing fully and fully reaction, have improved raw material availability, have lowered production cost.
7, the present invention is driven the plectrum rotation of cone-shaped metal cylinder and inner wall of rotary drum by electric motor, makes raw material to be plated dispersed in reaction compartment, guarantees to coat the homogeneity of thickness.
8, cone-shaped metal cylinder of the present invention left side is provided with baffle plate, and this baffle plate can prevent overflowing of raw material glass fibre.
9, the present invention utilizes the microwave plasma CVD technology, take cheap Sweet natural gas for being raw material, control good distribution and the self-emptying of glass fibre with the cone-shaped metal cylinder, but be aided with the charging valve of storage compartment, adjustable reinforced break-make and speed and the bleeder valve of time switch, realize that the quasi-diamond of the controlled production cheapness of high-level efficiency in enormous quantities coats the high strength high wettability conjugated fibre of glass fibre.
The accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Fig. 1 is structural representation of the present invention.
In figure: 1-cylindrical Stainless steel chamber 2-quartz window, 3-microwave source, 4-waveguide, 5-cone-shaped metal cylinder 6-electric motor, 7-rotating shaft, 8-flange and bearing 9-cross frame 10-plectrum 11-baffle plate, 12-charging valve 13-storage compartment 14-bleeder valve, 15-intake valve, 16-extraction valve.
Embodiment
The microwave-assisted diamond like carbon film coats the conjugated fibre preparation method of glass fibre, comprises the following steps:
(1) start the microwave plasma CVD system, by extraction valve 16, the vacuum in cylindrical Stainless steel chamber 1 is extracted into to 10
-3below Pa;
(2) by the intake valve 15 in the microwave plasma CVD system, Sweet natural gas is passed into to cylindrical Stainless steel chamber 1, make it evenly be full of whole cylindrical Stainless steel chamber 1;
(3) start the microwave source 3 in the microwave plasma CVD system, the microwave that microwave source 3 is produced enters cylindrical Stainless steel chamber 1 by waveguide 4 from left quartz window 2, and the interior activated plasma of cone-shaped metal cylinder 5 in the microwave plasma CVD system, Sweet natural gas fully is decomposed into to the activated hydrocarbon group of tool;
(4) the raw material glass fibre in storage compartment in the microwave plasma CVD system 13 is added in cone-shaped metal cylinder 5 by charging valve 12;
(5) start the electric motor 6 in the microwave plasma CVD system, electric motor 6 drive shafts 7 drive plectrum 10 rotations of cone-shaped metal cylinder 5 together with its inwall by the flange at right side quartz window 2 centers and the cross frame 9 of bearing 8 and cylindrical Stainless steel chamber 1 inner conical metal roller 5 right-hand members, the raw material that continuously will be gathered in cone-shaped metal cylinder 5 bottoms is transported to top from bottom and falls under the effect of gravity, rotation along with cone-shaped metal cylinder 5, make raw material dispersed and centrifugal motion occurs and end motion to the right, meanwhile, Sweet natural gas decomposes the hydrocarbon group produced and deposits and grow into diamond like carbon film at fiberglass surfacing, form conjugated fibre---the glass fibre that quasi-diamond coats, finally from cone-shaped metal cylinder 5 right-hand members, by bleeder valve 14, regularly discharge, do not have the gas of complete reaction to discharge outside cylindrical Stainless steel chamber 1 by extraction valve 16,
(6) repeat (1) ~ (5) step;
(7), after producing end, close intake valve 15, extraction valve 16, charging valve 12, bleeder valve 14 and microwave source 3 and electric motor 6.
Wherein:
The microwave plasma CVD system refers to that this system comprises that horizontal positioned and two ends, left and right are respectively equipped with the cylindrical Stainless steel chamber 1 of quartz window 2, microwave source 3, cone-shaped metal cylinder 5 and the 13(of storage compartment as shown in Figure 1).The left side of cylindrical Stainless steel chamber 1 is provided with microwave source 3 and waveguide 4, and its right side is provided with electric motor 6, is provided with cone-shaped metal cylinder 5 in it, and its top is provided with storage compartment 13 and charging valve 12; The top right side of cylindrical Stainless steel chamber 1 is provided with intake valve 15, and its bottom left is provided with extraction valve 16, and its right side, bottom is provided with bleeder valve 14; The left end of cone-shaped metal cylinder 5 is provided with baffle plate 11, and its inner wall even distribution has several plectrums 10, and its right-hand member is provided with cross frame 9; One end of electric motor 6 is provided with rotating shaft 7, and this rotating shaft 7 is through being fixed on the cylindrical Stainless steel chamber supercentral flange of 1 right side quartz window 2 and bearing 8 is connected with the center of cross frame 9.
Cylindrical Stainless steel chamber 1 is connected by waveguide 4 with microwave source 3.
The pipeline that passes on left of cone-shaped metal cylinder 5 is connected with storage compartment 13, and this pipeline is provided with charging valve 12.
The left side barrel dliameter of cone-shaped metal cylinder 5 is less than its right side barrel dliameter.
Charging valve 12 and bleeder valve 14 be external time switch all.
Claims (6)
1. the microwave-assisted diamond like carbon film coats the conjugated fibre preparation method of glass fibre, comprises the following steps:
(1) start the microwave plasma CVD system, by extraction valve (16), the vacuum in cylindrical Stainless steel chamber (1) is extracted into to 10
-3below Pa;
(2) by the intake valve (15) in described microwave plasma CVD system, Sweet natural gas is passed into to described cylindrical Stainless steel chamber (1), make it evenly be full of whole described cylindrical Stainless steel chamber (1);
(3) start the microwave source (3) in the microwave plasma CVD system, the microwave that described microwave source (3) is produced enters described cylindrical Stainless steel chamber (1) by waveguide (4) from left quartz window (2), and activated plasma in the cone-shaped metal cylinder (5) in described microwave plasma CVD system, Sweet natural gas fully is decomposed into to the activated hydrocarbon group of tool;
(4) the raw material glass fibre in storage compartment (13) in described microwave plasma CVD system is added in described cone-shaped metal cylinder (5) by charging valve (12);
(5) start the electric motor (6) in the microwave plasma CVD system, described electric motor (6) drive shaft (7) drives plectrum (10) rotation of described cone-shaped metal cylinder (5) together with its inwall by the flange at right side quartz window (2) center and the cross frame (9) of bearing (8) and interior described cone-shaped metal cylinder (5) right-hand member of described cylindrical Stainless steel chamber (1), the raw material that continuously will be gathered in described cone-shaped metal cylinder (5) bottom is transported to top from bottom and falls under the effect of gravity, rotation along with described cone-shaped metal cylinder (5), make raw material dispersed and centrifugal motion occurs and end motion to the right, meanwhile, Sweet natural gas decomposes the hydrocarbon group produced and deposits and grow into diamond like carbon film at fiberglass surfacing, form conjugated fibre---the glass fibre that quasi-diamond coats, finally from described cone-shaped metal cylinder (5) right-hand member, by bleeder valve (14), regularly discharge, do not have the gas of complete reaction to discharge outside described cylindrical Stainless steel chamber (1) by extraction valve (16),
(6) repeat (1) ~ (5) step;
(7), after producing end, close described intake valve (15), extraction valve (16), charging valve (12), bleeder valve (14) and microwave source (3) and electric motor (6).
2. microwave-assisted diamond like carbon film as claimed in claim 1 coats the conjugated fibre preparation method of glass fibre, it is characterized in that: described microwave plasma CVD system refers to that this system comprises that horizontal positioned and two ends, left and right are respectively equipped with the cylindrical Stainless steel chamber (1) of quartz window (2), microwave source (3), cone-shaped metal cylinder (5) and storage compartment (13); The left side of described cylindrical Stainless steel chamber (1) is provided with described microwave source (3) and waveguide (4), its right side is provided with electric motor (6), be provided with described cone-shaped metal cylinder (5) in it, its top is provided with described storage compartment (13) and charging valve (12); The top right side of described cylindrical Stainless steel chamber (1) is provided with intake valve (15), and its bottom left is provided with extraction valve (16), and its right side, bottom is provided with bleeder valve (14); The left end of described cone-shaped metal cylinder (5) is provided with baffle plate (11), and its inner wall even distribution has several plectrums (10), and its right-hand member is provided with cross frame (9); One end of described electric motor (6) is provided with rotating shaft (7), and this rotating shaft (7) is through being fixed on the supercentral flange of described cylindrical Stainless steel chamber (1) right side quartz window (2) and bearing (8) is connected with the center of described cross frame (9).
3. microwave-assisted diamond like carbon film as claimed in claim 2 coats the conjugated fibre preparation method of glass fibre, and it is characterized in that: described cylindrical Stainless steel chamber (1) is connected by waveguide (4) with described microwave source (3).
4. microwave-assisted diamond like carbon film as claimed in claim 2 coats the conjugated fibre preparation method of glass fibre, it is characterized in that: the pipeline that passes on left of described cone-shaped metal cylinder (5) is connected with described storage compartment (13), and this pipeline is provided with charging valve (12).
5. microwave-assisted diamond like carbon film as claimed in claim 2 coats the conjugated fibre preparation method of glass fibre, and it is characterized in that: the left side barrel dliameter of described cone-shaped metal cylinder (5) is less than its right side barrel dliameter.
6. microwave-assisted diamond like carbon film as claimed in claim 2 coats the conjugated fibre preparation method of glass fibre, and it is characterized in that: described charging valve (12) and described bleeder valve (14) be external time switch all.
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| CN1016364B (en) * | 1989-09-19 | 1992-04-22 | 北京市科学技术研究院 | Chemical gaseous deposition process of thin diamond film by means of arc discharge |
| EP0931853B1 (en) * | 1992-11-13 | 2001-12-05 | Energy Conversion Devices, Inc. | Method of depositing barrier coatings by plasma assisted chemical vapour deposition |
| EP0743375B1 (en) * | 1995-03-31 | 2000-07-12 | CeramOptec GmbH | Method of producing diamond-like-carbon coatings |
| CN1389593A (en) * | 2001-11-16 | 2003-01-08 | 刘铁林 | Normal temperature diamond crystal film and its formation |
| JP2005135736A (en) * | 2003-10-30 | 2005-05-26 | Nippon Spindle Mfg Co Ltd | Plasma processing device for particulates |
| CN1931566A (en) * | 2005-09-18 | 2007-03-21 | 邓代维 | Process and apparatus for preparing reinforced plastic directly after on-line plasma treatment of glass fiber |
| US20090120366A1 (en) * | 2007-01-29 | 2009-05-14 | Sumitomo Electric Industries, Ltd. | Microwave plasma cvd device |
| CN202099616U (en) * | 2011-05-06 | 2012-01-04 | 宁波表面工程研究中心 | Film and fiber surface plasma continuous processing device |
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