CN102627413A - 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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- CN102627413A CN102627413A CN2012101437825A CN201210143782A CN102627413A CN 102627413 A CN102627413 A CN 102627413A CN 2012101437825 A CN2012101437825 A CN 2012101437825A CN 201210143782 A CN201210143782 A CN 201210143782A CN 102627413 A CN102627413 A CN 102627413A
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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 DLC film reinforced composite field, relate in particular to the conjugated fibre preparation method that the microwave-assisted DLC film coats spun glass.
Background technology
Along with world's Mineral resources reduce day by day with industrial production in the increase day by day of materials demand, fibre reinforced composites are because it to the significant reinforced effects of the mechanical property of materials, has all obtained application widely in all respects such as productive life, military and national defense.And wood plastic composite is because its material plant fiber cheap and rather well received; But the subject matter that needs in the wood plastic composite production process to solve is the wellability of improving between vegetable fibre and the thermoplastics, with the bonding properties between enhancement of plant fiber and the matrix plastic.At present; The common chemical treatment process can improve vegetable fibre reinforced composite impact property, bending property; But it is a lot of aspect tensile property, to have descended because of weakening of the mechanical strength of vegetable fibre own; Limited it in a lot of extensive applications, chemical process produces environmental pollution inevitably simultaneously, does not meet the theory of social enviroment protection development.Therefore; For thomel, be worth cheap spun glass as a kind of inorganic environmental friendliness type material; Fiberglass plastic matrix material (glass plastic composite materials) gets more and more people's extensive concerning, but the glass plastic composite materials need solve wettability between fiber and the plastics equally to increase the problem of bonding properties between the interface.Along with China's glass output improves constantly, the glass product must squeeze into the international market, and quality product is the strong and weak key of competitive power.The exploitation new product, improving the quality to be prerequisite with the treating compound technology.Because DLC film possesses excellent mechanical property, good wettability and the bonding force superior with substrate; If it is used for coating spun glass; Will improve the mechanical property and the wettability of spun glass significantly, and then improve the over-all properties of glass plastic composite materials.
In sum; We propose to utilize microwave plasma CVD (MWPECVD); Sweet natural gas with cheapness is that reactant gases is at fiberglass surfacing depositing diamond-like film; With the mechanical property that increases spun glass with improve its wetting of surfaces property, and then improve the over-all properties of glass plastic composite materials.
Summary of the invention
Technical problem to be solved by this invention provides a kind of conjugated fibre preparation method simple, that microwave-assisted DLC film that be convenient to operate coats spun glass that implements.
For addressing the above problem, microwave-assisted DLC film of the present invention coats the conjugated fibre preparation method of spun glass, may further comprise the steps:
⑴ start the microwave plasma CVD system, and vacuum cylindrical stainless-steel vacuum is indoor through extraction valve is extracted into 10
-3Below the Pa;
⑵ feed said cylindrical stainless-steel vacuum chamber through the intake valve in the said microwave plasma CVD system with Sweet natural gas, makes it evenly be full of whole said cylindrical stainless-steel vacuum chamber;
⑶ start the microwave source in the microwave plasma CVD system; The microwave that said microwave source is produced gets into said cylindrical stainless-steel vacuum chamber through waveguide from left quartz window; And activated plasma in the cone-shaped metal cylinder in said microwave plasma CVD system, Sweet natural gas fully is decomposed into has active hydrocarbon group;
⑷ add the raw material spun glass in the storage compartment in the said microwave plasma CVD system in the said cone-shaped metal cylinder through charging valve;
⑸ start the phonomoter in the microwave plasma CVD system; Said direct motor drive rotating shaft drives the plectrum rotation of said cone-shaped metal cylinder together with its inwall through the flange at quartz window center, right side and the cross frame of bearing and the indoor said cone-shaped metal cylinder right-hand member of said cylindrical stainless-steel vacuum; The raw material that continuously will accumulate in said cone-shaped metal cylinder bottom is transported to the top and under the effect of gravity, falls from the bottom; Rotation along with said cone-shaped metal cylinder; Make the raw material homodisperse and centrifugal motion takes place and end motion to the right; Meanwhile; Sweet natural gas decomposes the hydrocarbon group that produces and deposits and grow into DLC film at fiberglass surfacing, forms conjugated fibre---the spun glass that quasi-diamond coats, finally regularly discharge through bleeder valve from said cone-shaped metal cylinder right-hand member; It is outdoor that the gas that does not have a complete reaction is discharged said cylindrical stainless-steel vacuum through extraction valve;
⑹ repeat ⑴ ~ ⑸ step;
⑺ of production is closed said intake valve, extraction valve, charging valve, bleeder valve and microwave source and phonomoter after finishing.
Said microwave plasma CVD system is meant that this system comprises that horizontal positioned and right ends are respectively equipped with cylindrical stainless-steel vacuum chamber, microwave source, cone-shaped metal cylinder and the storage compartment of quartz window; The left side of said cylindrical stainless-steel vacuum chamber is provided with said microwave source and waveguide, and its right side is provided with phonomoter, is provided with said cone-shaped metal cylinder in it, and its top is provided with said storage compartment and charging valve; The top right side of said cylindrical stainless-steel vacuum chamber is provided with intake valve, and its bottom left is provided with extraction valve, and its bottom, right side is provided with bleeder valve; The left end of said 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 said phonomoter is provided with rotating shaft, and this rotating shaft is passed and is fixed on the said cylindrical stainless-steel vacuum chamber supercentral flange of right side quartz window and bearing links to each other with the center of said cross frame.
Said cone-shaped metal cylinder pass on left pipeline and said storage compartment, this pipeline is provided with charging valve.
The left side barrel dliameter of said cone-shaped metal cylinder is less than its right side barrel dliameter.
The all external time switch of said charging valve and said bleeder valve.
The present invention compared with prior art has the following advantages:
1, fiberglass surfacing is handled, improving its wettability is the technical difficult points of utilizing the glass plastic composite materials, and at present used chemical treatment method can be sacrificed its mechanical property inevitably when raising is infiltrating.The present invention coats DLC film at fiberglass surfacing, increases its surface wettability, improves the physical strength of spun glass simultaneously.In addition, DLC film has stable chemical property more than tensio-active agent, can under extreme environment, be on active service, and have longer work-ing life.
2, because the present invention uses microwave source to produce microwave, excite highdensity microwave plasma, therefore, DLC 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 helps the homodisperse of raw material to be plated at reaction compartment, guarantees cladding uniformity, and can add raw material more how to be plated simultaneously.
4, the design of conical drum among the present invention for self-emptying provides possibility, can be produced the product of inhomogeneity diamond thin thickness through the reaction times of its rotating speed control raw material simultaneously, realizes the controllability of coating material thickness.
5, be provided with the charging valve (the size decision feed rate of charging valve opening) of storage compartment, time opening and adjustable feed rate and the bleeder valve of time opening among the present invention, for successive high efficiency production in enormous quantities is given security.
6, inlet mouth of the present invention and bleeding point lay respectively at upper right and left lower end, cylindrical stainless-steel vacuum chamber, 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 by the rotation of the plectrum of motor drives cone-shaped metal cylinder and inner wall of rotary drum, makes raw material to be plated homodisperse in reaction compartment, guarantees to coat the homogeneity of thickness.
8, be provided with baffle plate on the left of the cone-shaped metal cylinder of the present invention, this baffle plate can prevent overflowing of raw material spun glass.
9, the present invention utilizes the microwave plasma CVD technology; With the Sweet natural gas of cheapness for being raw material; Good distribution and self-emptying with cone-shaped metal cylinder feed glass fiber; 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 cheap quasi-diamond of the controlled production of high-level efficiency in enormous quantities coats the HS high wettability conjugated fibre of spun glass.
Description of drawings
Do further detailed explanation below in conjunction with the accompanying drawing specific embodiments of the invention.
Fig. 1 is a structural representation of the present invention.
Among the figure: 1-cylindrical stainless-steel vacuum chamber, 2-quartz window, 3-microwave source, 4-waveguide, 5-cone-shaped metal cylinder 6-phonomoter, 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 DLC film coats the conjugated fibre preparation method of spun glass, may further comprise the steps:
⑴ start the microwave plasma CVD system, through extraction valve 16 vacuum in the cylindrical stainless-steel vacuum chamber 1 is extracted into 10
-3Below the Pa;
⑵ feed cylindrical stainless-steel vacuum chamber 1 through the intake valve in the microwave plasma CVD system 15 with Sweet natural gas, makes it evenly be full of whole cylindrical stainless-steel vacuum chamber 1;
⑶ start the microwave source 3 in the microwave plasma CVD system; The microwave that microwave source 3 is produced gets into cylindrical stainless-steel vacuum chamber 1 through waveguide 4 from left quartz window 2; And activated plasma in the cone-shaped metal cylinder 5 in the microwave plasma CVD system, Sweet natural gas fully is decomposed into has active hydrocarbon group;
⑷ add the raw material spun glass in the storage compartment in the microwave plasma CVD system 13 in the cone-shaped metal cylinder 5 through charging valve 12;
⑸ start the phonomoter 6 in the microwave plasma CVD system; Phonomoter 6 drives rotating shaft 7 and drives plectrum 10 rotations of cone-shaped metal cylinder 5 together with its inwall through the flange at right side quartz window 2 centers and the cross frame 9 of bearing 8 and cylindrical stainless-steel vacuum chamber 1 inner conical metal roller, 5 right-hand members; The raw material that continuously will accumulate in cone-shaped metal cylinder 5 bottoms is transported to the top and under the effect of gravity, falls from the bottom; Rotation along with cone-shaped metal cylinder 5; Make the raw material homodisperse and centrifugal motion takes place and end motion to the right; Meanwhile; The hydrocarbon group that the Sweet natural gas decomposition produces is in the fiberglass surfacing deposition and grow into DLC film, forms conjugated fibre---and the spun glass that quasi-diamond coats, finally pass through bleeder valve 14 from cone-shaped metal cylinder 5 right-hand members and regularly discharge; There is not the gas of complete reaction to discharge outside the cylindrical stainless-steel vacuum chamber 1 through extraction valve 16;
⑹ repeat ⑴ ~ ⑸ step;
⑺ of production is closed intake valve 15, extraction valve 16, charging valve 12, bleeder valve 14 and microwave source 3 and phonomoter 6 after finishing.
Wherein:
The microwave plasma CVD system is meant that this system comprises that horizontal positioned and right ends are respectively equipped with the cylindrical stainless-steel vacuum chamber 1 of quartz window 2, microwave source 3, cone-shaped metal cylinder 5 and storage compartment 13 (as shown in Figure 1).The left side of cylindrical stainless-steel vacuum chamber 1 is provided with microwave source 3 and waveguide 4, and its right side is provided with phonomoter 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 vacuum chamber 1 is provided with intake valve 15, and its bottom left is provided with extraction valve 16, and its bottom, right side 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 phonomoter 6 is provided with rotating shaft 7, and this rotating shaft 7 is passed and is fixed on cylindrical stainless-steel vacuum chamber 1 right side quartz window, 2 supercentral flanges and bearing 8 links to each other with the center of cross frame 9.
Cylindrical stainless-steel vacuum chamber 1 links to each other through waveguide 4 with microwave source 3.
Cone-shaped metal cylinder 5 pass on left pipeline and storage compartment 13, 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 all external time switch of bleeder valve 14.
Claims (6)
1. the microwave-assisted DLC film coats the conjugated fibre preparation method of spun glass, may further comprise the steps:
⑴ start the microwave plasma CVD system, through extraction valve (16) vacuum in the cylindrical stainless-steel vacuum chamber (1) is extracted into 10
-3Below the Pa;
⑵ feed said cylindrical stainless-steel vacuum chamber (1) through the intake valve (15) in the said microwave plasma CVD system with Sweet natural gas, makes it evenly be full of whole said cylindrical stainless-steel vacuum chamber (1);
⑶ start the microwave source (3) in the microwave plasma CVD system; The microwave that said microwave source (3) is produced gets into said cylindrical stainless-steel vacuum chamber (1) through waveguide (4) from left quartz window (2); And activated plasma in the cone-shaped metal cylinder (5) in said microwave plasma CVD system, Sweet natural gas fully is decomposed into has active hydrocarbon group;
⑷ add the raw material spun glass in the storage compartment (13) in the said microwave plasma CVD system in the said cone-shaped metal cylinder (5) through charging valve (12);
⑸ start the phonomoter (6) in the microwave plasma CVD system; The cross frame (9) that said phonomoter (6) drives said cone-shaped metal cylinder (5) right-hand member in flange and bearing (8) and the said cylindrical stainless-steel vacuum chamber (1) of rotating shaft (7) through right side quartz window (2) center drives plectrum (10) rotation of said cone-shaped metal cylinder (5) together with its inwall; The raw material that continuously will accumulate in said cone-shaped metal cylinder (5) bottom is transported to the top and under the effect of gravity, falls from the bottom; Rotation along with said cone-shaped metal cylinder (5); Make the raw material homodisperse and centrifugal motion takes place and end motion to the right; Meanwhile; Sweet natural gas decomposes the hydrocarbon group that produces and deposits and grow into DLC film at fiberglass surfacing; Form conjugated fibre---the spun glass that quasi-diamond coats, finally regularly discharge through bleeder valve (14) from said cone-shaped metal cylinder (5) right-hand member; There is not the gas of complete reaction to discharge outside the said cylindrical stainless-steel vacuum chamber (1) through extraction valve (16);
⑹ repeat ⑴ ~ ⑸ step;
⑺ of production is closed said intake valve (15), extraction valve (16), charging valve (12), bleeder valve (14) and microwave source (3) and phonomoter (6) after finishing.
2. microwave-assisted DLC film as claimed in claim 1 coats the conjugated fibre preparation method of spun glass, it is characterized in that: said microwave plasma CVD system is meant that this system comprises that horizontal positioned and right ends are respectively equipped with the cylindrical stainless-steel vacuum chamber (1) of quartz window (2), microwave source (3), cone-shaped metal cylinder (5) and storage compartment (13); The left side of said cylindrical stainless-steel vacuum chamber (1) is provided with said microwave source (3) and waveguide (4); Its right side is provided with phonomoter (6); Be provided with said cone-shaped metal cylinder (5) in it, its top is provided with said storage compartment (13) and charging valve (12); The top right side of said cylindrical stainless-steel vacuum chamber (1) is provided with intake valve (15), and its bottom left is provided with extraction valve (16), and its bottom, right side is provided with bleeder valve (14); The left end of said 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 said phonomoter (6) is provided with rotating shaft (7), and this rotating shaft (7) is passed and is fixed on the supercentral flange of said cylindrical stainless-steel vacuum chamber (1) right side quartz window (2) and bearing (8) links to each other with the center of said cross frame (9).
3. microwave-assisted DLC film as claimed in claim 2 coats the conjugated fibre preparation method of spun glass, and it is characterized in that: said cylindrical stainless-steel vacuum chamber (1) links to each other through waveguide (4) with said microwave source (3).
4. microwave-assisted DLC film as claimed in claim 2 coats the conjugated fibre preparation method of spun glass; It is characterized in that: said cone-shaped metal cylinder (5) pass on left pipeline and said storage compartment (13), this pipeline is provided with charging valve (12).
5. microwave-assisted DLC film as claimed in claim 2 coats the conjugated fibre preparation method of spun glass, and it is characterized in that: the left side barrel dliameter of said cone-shaped metal cylinder (5) is less than its right side barrel dliameter.
6. microwave-assisted DLC film as claimed in claim 2 coats the conjugated fibre preparation method of spun glass, it is characterized in that: said charging valve (12) and all external time switch of said bleeder valve (14).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111491437A (en) * | 2019-01-29 | 2020-08-04 | 四川宏图普新机械设备安装服务有限公司 | Non-jet normal-pressure large-volume microwave plasma generation method |
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| CN1041187A (en) * | 1989-09-19 | 1990-04-11 | 北京市科学技术研究院 | The method of arc discharge chemical vapor deposition diamond film |
| US5411591A (en) * | 1992-11-13 | 1995-05-02 | Energy Conversion Devices, Inc. | Apparatus for the simultaneous microwave deposition of thin films in multiple discrete zones |
| EP0743375A2 (en) * | 1995-03-31 | 1996-11-20 | 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 |
| CN101410549A (en) * | 2007-01-29 | 2009-04-15 | 住友电气工业株式会社 | Microwave plasma CVD system |
| 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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2012
- 2012-05-10 CN CN2012101437825A patent/CN102627413B/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1041187A (en) * | 1989-09-19 | 1990-04-11 | 北京市科学技术研究院 | The method of arc discharge chemical vapor deposition diamond film |
| US5411591A (en) * | 1992-11-13 | 1995-05-02 | Energy Conversion Devices, Inc. | Apparatus for the simultaneous microwave deposition of thin films in multiple discrete zones |
| EP0743375A2 (en) * | 1995-03-31 | 1996-11-20 | CeramOptec GmbH | Method of producing diamond-like-carbon coatings |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111491437A (en) * | 2019-01-29 | 2020-08-04 | 四川宏图普新机械设备安装服务有限公司 | Non-jet normal-pressure large-volume microwave plasma generation method |
| CN111491437B (en) * | 2019-01-29 | 2022-06-07 | 四川宏图普新机械设备安装服务有限公司 | Non-jet normal-pressure large-volume microwave plasma generation method |
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