CN102409292A - Method and device for continuously synthesizing diamond membrane by radiating carbon nanotube with strong laser - Google Patents
Method and device for continuously synthesizing diamond membrane by radiating carbon nanotube with strong laser Download PDFInfo
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- CN102409292A CN102409292A CN2011103672882A CN201110367288A CN102409292A CN 102409292 A CN102409292 A CN 102409292A CN 2011103672882 A CN2011103672882 A CN 2011103672882A CN 201110367288 A CN201110367288 A CN 201110367288A CN 102409292 A CN102409292 A CN 102409292A
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Abstract
The invention relates to a method and device for continuously synthesizing a diamond membrane by radiating a carbon nanotube with strong laser. The device for continuously synthesizing the diamond membrane is characterized by consisting of a laser generating system, a working system and an auxiliary system. Laser emitted by a high-power pulse laser device is reflected and split by a spectroscope to generate a laser beam G1 and a laser beam G2, the laser beam G1 is focused at an appropriate position over the upper surface of a substrate, and carbon nanotube powder in a solution is gasified and ionized momentarily by absorbing laser energy to generate a large quantity of high-speed plasmas; and meanwhile, a momentary high-temperature and high-pressure micro-zone is formed on the surface of the substrate under the compounding action of laser G2, and the high-speed plasmas bombard the surface of the substrate to form the diamond membrane. According to the method and the device, the problems of low synthesis efficiency, special reaction condition, difficulty in operating equipment and high equipment price are solved, continuous synthesis of the diamond membrane at the macroscopically normal temperature and under the macroscopically normal pressure is realized innovatively, and a large-thickness high-purity diamond membrane is obtained.
Description
Technical field
The present invention relates to the artificial diamond thin field of making, refer in particular to the method and apparatus that a kind of Irradiation of High carbon nanotube prepares diamond thin continuously.
Background technology
Nano diamond has caused people's extensive concern because of it has excellent machinery, calorifics, optics and chemical property.Along with going deep into of understanding, Nano diamond has obtained practical application in fields such as metal plating, lubricating oil, magnetic recording system and medical science.Because laser can make material heating, fusing, gasification or undergo phase transition in the extremely short time, carrying out the research of laser method synthesizing nano diamond both at home and abroad.Ogale in 1992 etc. are applied to diamond with strong laser induced liquid-solid interfacial reaction method and synthesize, and promptly utilize ruby laser irradiation to be immersed in the graphite target in the benzene, have found the diamond phase in the product.Since GE in 1955 first since the diamond synthesis, adamantine artificial synthesis has had very big development with technology.At present; The mankind have grasped multiple adamantine compound method; Divide by its principle, can be divided into two types basically: one type be under high-temperature and high-pressure conditions in the diamond stable region non-diamond carbon to adamantine transformation, like static pressure catalyst method, shock-synthesis technique; Another kind of be under the low pressure condition in the diamond meta district activated carbon-based group reassemble and form diamond, like chemical Vapor deposition process etc.
Wang Jin is refined in recent years also successfully synthesizes diamond with the graphite target of use Irradiation of High in water or acetone such as Yang Guowei.They all adopt the ps pulsed laser and ns pulsed laser device, though its power density surpasses 10
9W/cm
2, but being limited under the HTHP, and only making the product that splashes of time spent and obtain the Nano diamond particle through collecting fixedly graphite target in laser and the liquid medium, combined coefficient is low, is mainly used in theoretical investigation.(publication number is the patent of invention of " method of a clock combination laser chemistry for gas phase depositing diamond film " by name of people such as Feng Zhongchao application: CN1221806A); Its method be under vacuum condition with the XeCl PRK as laser source compound infrared laser irradiation simultaneously, deposit diamond thin at substrate surface, this method great advantage is need not heat to substrate; Depositing temperature is low; Rete purity is high, but shortcoming is that sedimentary diamond thin is thinner, because this device will carry out under vacuum condition; This operation to device brings certain difficulty; Feeding the flow proportional of the hydrocarbon reaction gas that can absorb optical maser wavelength and hydrogen to the reaction chamber of vacuum simultaneously should strict control, so realize the complex equipments of this method, the cost height.
Summary of the invention
The objective of the invention is deficiency to above technology; A kind of method of the carbon nanotube of Irradiation of High at normal temperatures and pressures synthesis of diamond film is provided, and this method combined coefficient is high, and technology is simple; Equipment cost is low, can synthesize and obtain high-quality diamond thin continuously.
The concrete grammar of the continuous synthesis of diamond film of Irradiation of High carbon nanotube is: feed an amount of water in the reaction vessel; Carbon nanotube powder is suspended in water; Make its homodisperse with the electromagnetic shock stirring, the aqueous solution is circulated with certain speed through electric pump and flow rate control device.The high power pulsed laser device sends intense laser beam, and reflection becomes laser beam G1 and laser beam G2 with beam split through spectroscope; Laser beam G1 directly focuses on apart from the appropriate location of substrate surface top through laser processing condenser lens and protective glass in front; Carbon nanotube powder in the aqueous solution absorbs laser energy moment gasification, ionization; Produce a large amount of high speed plasma bodys; Laser beam G2 reflexes on the total reflective mirror that is installed on the swinging strut through 45 ° of total reflective mirrors, and on the substrate surface under total reflective mirror is radiated laser beam G1 focus point, the compound action of laser beam G1 and laser beam G2 is at the microcell of substrate surface formation moment HTHP; Laser beam G1 inductive high speed plasma bombardment substrate surface forms high-quality diamond thin at substrate surface.Water medium carries carbon nanotube powder and circulates, and laser different carbon nanotube powders at different time irradiation, thereby realizes diamond thin continuous synthesizing at normal temperatures and pressures.
The inventive system comprises three systems: laser generating system, workpiece system and subsystem.Described laser generating system comprises: computingmachine, high power pulsed laser device, spectroscope, laser Machining head, 45 ° of total reflective mirrors, total reflective mirror and swinging struts; Computer control high power pulsed laser device; 45 ° of total reflective mirrors be positioned at total reflective mirror directly over, total reflective mirror is fixed on the swinging strut, regulates the reflection direction of laser beam G2 through the rotation swinging strut; Described laser Machining head comprises condenser lens and protective glass, and condenser lens is above protective glass; Described workpiece system comprises: worktable, anchor clamps and substrate, described substrate are nickel-base alloy.On worktable, the computer control worktable is regulated the movement locus of substrate through clamps in substrate; Described subsystem comprises: flow regulation device, liquid-storing box and electric pump.Electric pump one end links to each other with the water outlet of water tank bottom, and an end links to each other with liquid-storing box.Flow regulation device one end links to each other with the water inlet on the water tank left side, and an end links to each other with liquid-storing box.Through electric pump solution circulated is flowed, flow regulation device is used to control the velocity of flow of the aqueous solution.
Practical implementation step of the present invention is following:
A. the surface finish polishing is carried out in substrate, uses acetone, alcohol wash then, and steps up to be fixed on the worktable with anchor clamps;
B. feed an amount of water in the reaction vessel, carbon nanotube powder is suspended in water, electromagnetic shock stirs and makes its homodisperse;
C. open the electric pump power supply aqueous solution is circulated, regulate flow rate control device, make solution circulated speed between 0.3～0.6ml/s;
D. open the high power pulsed laser device, by the computer installation parameter, PW is 10ns～20ns, and pulse-repetition is 20Hz, and power density is 10
8W/cm
2~ 10
9W/cm
2The laser 7 that the high power pulsed laser device sends is through spectroscope reflection and beam split; Laser beam G1 directly reflection focuses on 2mm～4mm place directly over the substrate surface through laser Machining head; Laser beam G2 reflexes on the total reflective mirror that is installed on the swinging strut through 45 ° of total reflective mirrors simultaneously; On the substrate surface under total reflective mirror is radiated laser beam G1 focus point; Laser beam G1 irradiation is dispersed in the carbon nanotube powder in the water, and induces high speed plasma bombardment substrate surface, forms high-quality diamond thin at substrate surface;
E. traverser makes substrate be in different positions.After question response is intact, close all power supplys, take off substrate.
The innovation of the present invention's technology; It is low to be to have overcome the prior art combined coefficient; Reaction conditions special and device operational difficulty and the expensive problem of equipment have realized diamond thin synthesizing continuously under macroscopical normal temperature and pressure, have obtained the thicker high purity diamond thin of thickness.Two laser beam G1 that utilize that laser that the high power pulsed laser device sends produces after spectroscope reflection and beam split and G2; Laser beam G1 focuses on the appropriate location directly over the upper surface of substrate; Carbon nanometer powder pipe in the solution absorbs laser energy moment gasification, ionization, produces a large amount of high speed plasma bodys, simultaneously under laser G2 compound action; Produce the high-temperature high-pressure microdmain of moment at substrate surface, high speed plasma bombardment substrate surface forms diamond thin.The mobile water medium carries carbon nanotube powder, makes the laser can Circulation, realizes the synthetic continuously of diamond thin.Because flowing of the aqueous solution, the microcell HTHP position that laser is produced is brought in constant renewal in, and for the generation of diamond thin provides favourable space environment, has improved the utilization ratio of carbon nanotube powder simultaneously.Through traverser, laser beam can obtain large-area diamond thin in the scanning of substrate surface different positions.After question response is accomplished, only need the aqueous solution is stored in the liquid-storing box, new substrate is installed, the aqueous solution is circulated, repeat other operation stepss, realize producing in batches.
The present invention has following advantage: can obtain highly purified diamond thin at normal temperatures and pressures, and the thin film layer thicker, be evenly distributed.Because it is synthetic that this method can realize continuously, so combined coefficient is high.In addition, the inventive method technology is simple, and reaction process safety is controlled, installs easy to operately, and equipment cost is low.
Description of drawings
Fig. 1: the schematic diagram of device of the continuous synthesis of diamond film of Irradiation of High carbon nanotube.
Label in the accompanying drawing: 1. electric pump; 2. liquid-storing box; 3. flow rate control device; 4. water-in; 5. computingmachine; 6. high power pulsed laser device; 7. laser; 8. laser beam G1; 9. laser Machining head; 10. condenser lens; 11. protective glass; 12. anchor clamps; 13. substrate; 14. spectroscope; 15. laser beam G2; 16. diamond thin; 17.45 ° total reflective mirror; 18. reaction vessel; 19. total reflective mirror; 20. swinging strut; 21. the aqueous solution; 22. worktable; 23. water outlet.
Embodiment
Specify the working condition of the method and apparatus that the present invention proposes below in conjunction with accompanying drawing and use-case, but be not used for limiting the present invention.
Specific embodiment 1
Nickel-base alloy is carried out the surface finish polishing; Use acetone, alcohol wash then, and step up to be fixed on the worktable 22, feed an amount of water then in the reaction vessel 18 with anchor clamps 12; Carbon nanotube powder is suspended in water, stir with electromagnetic shock and make its homodisperse.Open electric pump 1 power supply the aqueous solution is circulated, regulate flow rate control device 3, making aqueous solution speed of circulation is 0.45ml/s.Open high power pulsed laser device 6, by computingmachine 5 parameter is set, PW is 10ns～20ns, and pulse-repetition is 20Hz, and power density is 10
8W/cm
2The laser 7 that high power pulsed laser device 6 sends is through spectroscope reflection and beam split; Laser beam G18 directly reflection focuses on 3mm place directly over the nickel-base alloy surface through laser Machining head 9; 45 ° of total reflective mirror 17 reflected illumination of laser beam G215 warp are to the total reflective mirror 19 that is installed on the swinging strut 20 simultaneously; Be radiated on the nickel-base alloy through total reflective mirror 19, regulate swinging strut 20 laser beam G215 is radiated on the nickel-base alloy surface under the laser beam G18 focus point.The microcell of the compound action of laser beam G18 and laser beam G215 formation moment HTHP on the nickel-base alloy surface, laser beam G18 inductive high speed plasma bombardment nickel-base alloy surface forms high-quality diamond thin 16 on the nickel-base alloy surface.After band has reacted, close all power supplys, take off nickel-base alloy.
Claims (4)
1. an Irradiation of High carbon nanotube synthesizes the method for preparing diamond thin continuously, it is characterized in that the practical implementation step is:
A. the surface finish polishing is carried out in substrate (13), uses acetone, alcohol wash then, and steps up to be fixed on (22) on the worktable with anchor clamps (12);
B. feed water in the reaction vessel (18), carbon nanotube powder is suspended in water, electromagnetic shock stirs and makes the carbon nanotube powder homodisperse;
C. open electric pump (1) power supply and make the aqueous solution (21) circulation, regulate flow rate control device (3), make the aqueous solution (21) speed of circulation between 0.3～0.6ml/s;
D. open the high power pulsed laser device, by computingmachine (5) parameter is set, PW is 10ns～20ns, and pulse-repetition is 20Hz, and power density is 10
8W/cm
2~ 10
9W/cm
2The laser that high power pulsed laser device (6) sends is through spectroscope (14) reflection and beam split; Laser beam G1 (8) directly reflection focuses on 2mm～4mm place directly over substrate (13) surface through laser Machining head (9); Laser beam G2 (15) reflexes on the total reflective mirror (19) that is installed on the swinging strut (20) through 45 ° of total reflective mirrors (17) simultaneously; On the substrate surface under total reflective mirror (19) is radiated laser beam G1 (8) focus point; Laser beam G1 (8) irradiation is dispersed in the carbon nanotube powder in the water; And induce high speed plasma bombardment substrate (13) surface, form high-quality diamond thin (16) on substrate (13) surface;
E. traverser (22) makes substrate (13) be in different positions, after question response is intact, closes all power supplys, takes off substrate (13).
2. the method for the continuous synthesis of diamond film of a kind of Irradiation of High carbon nanotube according to claim 1 is characterized in that described substrate is a nickel-base alloy; Described laser Machining head is below liquid level, and described carbon nanotube powder granularity is 10nm～20nm.
3. implement the device of the method for the described a kind of Irradiation of High carbon nanotube synthesis of diamond film of claim 1, it is characterized in that said device is made up of laser generating system, workpiece system and subsystem;
Said laser generating system comprises computingmachine (5), high power pulsed laser device (6), spectroscope (14), laser Machining head (9), 45 ° of total reflective mirrors (17), total reflective mirror (19) and swinging strut (20); Computingmachine (5) control high power pulsed laser device (6); 45 ° of total reflective mirrors (17) be positioned at total reflective mirror (19) directly over; Total reflective mirror (19) is fixed on the swinging strut (20); Described laser Machining head (9) comprises condenser lens (10) and protective glass (11), and condenser lens (10) is in the top of protective glass (11); Workpiece system comprises worktable (22), anchor clamps (12) and substrate (13), and substrate (13) is fixed on the worktable (22) through anchor clamps (12), and computer control worktable (22) is regulated the movement locus of substrate (13); Subsystem comprises flow regulation device (13), liquid-storing box (13) and electric pump (13); Electric pump (13) one ends link to each other with the water outlet of water tank bottom; One end links to each other with liquid-storing box, and flow regulation device one end links to each other with the water inlet on the water tank left side, and an end links to each other with liquid-storing box; Through electric pump (13) solution circulated is flowed, flow regulation device is used to control the velocity of flow of the aqueous solution.
4. according to the device of the method for implementing the described a kind of Irradiation of High carbon nanotube synthesis of diamond film of claim 3, it is characterized in that described substrate is a nickel-base alloy.
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| CN2011103672882A CN102409292A (en) | 2011-11-18 | 2011-11-18 | Method and device for continuously synthesizing diamond membrane by radiating carbon nanotube with strong laser |
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|---|---|---|---|
| CN2011103672882A CN102409292A (en) | 2011-11-18 | 2011-11-18 | Method and device for continuously synthesizing diamond membrane by radiating carbon nanotube with strong laser |
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Cited By (7)
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|---|---|---|---|---|
| CN103408005A (en) * | 2013-07-29 | 2013-11-27 | 江苏大学 | Device and method for improving preparation efficiency of diamonds |
| CN106082206A (en) * | 2016-06-16 | 2016-11-09 | 江苏大学 | A kind of method and apparatus improving Nano diamond combined coefficient |
| CN107414322A (en) * | 2017-08-10 | 2017-12-01 | 江苏大学 | One kind reduces re cast layer device and method caused by laser micropore processing |
| WO2018045605A1 (en) * | 2016-09-12 | 2018-03-15 | 江苏大学 | Cryogenic laser shock strengthening method and apparatus based on laser-induced high temperature plasma technology |
| CN110143021A (en) * | 2019-05-29 | 2019-08-20 | 梁家昌 | A kind of high quality diamond composite sheet and preparation method thereof |
| CN112710191A (en) * | 2020-12-30 | 2021-04-27 | 北京机电工程研究所 | Gas ejection system |
| WO2022052334A1 (en) * | 2020-09-11 | 2022-03-17 | 江苏大学 | Room-temperature nitriding process based on thermal-mechanical effects of laser, and processing device |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408005A (en) * | 2013-07-29 | 2013-11-27 | 江苏大学 | Device and method for improving preparation efficiency of diamonds |
| CN103408005B (en) * | 2013-07-29 | 2015-07-08 | 江苏大学 | Device and method for improving preparation efficiency of diamonds |
| CN106082206A (en) * | 2016-06-16 | 2016-11-09 | 江苏大学 | A kind of method and apparatus improving Nano diamond combined coefficient |
| CN106082206B (en) * | 2016-06-16 | 2019-02-05 | 江苏大学 | A kind of method and apparatus improving Nano diamond combined coefficient |
| WO2018045605A1 (en) * | 2016-09-12 | 2018-03-15 | 江苏大学 | Cryogenic laser shock strengthening method and apparatus based on laser-induced high temperature plasma technology |
| CN107414322A (en) * | 2017-08-10 | 2017-12-01 | 江苏大学 | One kind reduces re cast layer device and method caused by laser micropore processing |
| CN110143021A (en) * | 2019-05-29 | 2019-08-20 | 梁家昌 | A kind of high quality diamond composite sheet and preparation method thereof |
| WO2022052334A1 (en) * | 2020-09-11 | 2022-03-17 | 江苏大学 | Room-temperature nitriding process based on thermal-mechanical effects of laser, and processing device |
| GB2614984A (en) * | 2020-09-11 | 2023-07-26 | Univ Jiangsu | Room-temperature nitriding process based on thermal-mechanical effects of laser, and processing device |
| GB2614984B (en) * | 2020-09-11 | 2024-02-14 | Univ Jiangsu | Room-temperature nitriding process based on thermal-mechanical effects of laser, and processing device |
| CN112710191A (en) * | 2020-12-30 | 2021-04-27 | 北京机电工程研究所 | Gas ejection system |
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Application publication date: 20120411 |