CN103408005A - Device and method for improving preparation efficiency of diamonds - Google Patents

Device and method for improving preparation efficiency of diamonds Download PDF

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CN103408005A
CN103408005A CN201310319625XA CN201310319625A CN103408005A CN 103408005 A CN103408005 A CN 103408005A CN 201310319625X A CN201310319625X A CN 201310319625XA CN 201310319625 A CN201310319625 A CN 201310319625A CN 103408005 A CN103408005 A CN 103408005A
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diamond
target
laser
target container
splashproof cover
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CN103408005B (en
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任旭东
唐少雄
杨慧敏
郑腊梅
占秋波
随赛
刘帆帆
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Jiangsu University
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Jiangsu University
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Abstract

The invention relates to a device and method for improving the preparation efficiency of diamonds. The device mainly comprises a laser generating system, a target material system and a purification system. The method comprises the following steps: during the preparation process of nanodiamonds, a high-energy intensive laser beam is used for acting on a graphite powder target material in the target material system so as to prepare a diamond solution; then, diamond nano-particles are extracted from the diamond solution through the purification system. According to the device and method, the graphite powder target material, on which the laser beam acts, is efficiently prevented from splashing out, and the laser beam circularly acts on the graphite powder target material, so as to increase the conversion rate of the nanodiamonds. Therefore, the utilization ratio of the graphite powder target material and the quality of the prepared nanodiamonds are improved. Besides, a target material container is made of transparent toughened glass with high impact strength, so that not only can the condition that the laser beam acts on the graphite powder target material in the target material container be observed conveniently but also the security during the preparation process is improved.

Description

A kind of apparatus and method that improve the diamond preparation efficiency
Technical field
The present invention relates to manually manufacture the Nano diamond field, particularly a kind of apparatus and method that improve the diamond preparation efficiency.
Background technology
In recent years, the successful preparation of Nano diamond has caused the upsurge of a global fundamental research and applied research.The application of Nano diamond is confined to do the grinding tool abrasive material fields such as glomerocryst, rumbling compound in the past.Along with the in-depth of people to Nano diamond character understanding, the discovery of the characteristics such as small-size effect, surface effects and macro quanta tunnel effect, Nano diamond has started to obtain application in fields such as metal plating, lubricating oil, magnetic recording system, medical science, demonstrated the unique effect of nano diamond structure material, and Application Areas is also in continuous expansion, and the industrialized development that production that makes Nano diamond and products thereof is developed becomes trend.
But the technology of preparing of artificial Nano diamond is also immature.The tradition preparation method mainly contains static pressure diamond synthesis, impact of dynamic pressure diamond synthesis and detonation synthesizing nanometer diamond crystalline substance.But these method synthesis conditions are all very strict, and cost is very high, and exist impurity level large, and especially the detonation diamond synthesis also contains a small amount of metal or metal oxide impurities, and transformation efficiency is low, and the diamond transformation efficiency only has 8% left and right.
In recent years, along with the rise of laser optics, the related researcher has proposed the lasing synthesizing nano diamond.The method of the laser that Fedoseev and Derjaguin propose direct irradiation carbon black diamond synthesis in gaseous media.They think, the material of bulk is difficult to obtain sufficiently high rate of cooling, and minimum particulate material is due to very large specific surface area being arranged, thereby are easy to obtain high rate of cooling.Due to laser energy, in the short period of time, obtain high temperature at the utmost point, if with laser, carry out the carbon black pellet of irradiation nanometer scale, just can obtain very high rate of cooling, thus the generation of induced transformation.Fedoseev and Derjaguin are used the continuous infrared laser of 10.6 μ m as irradiation source, and carbon black powder acts at the focus place by vibrator and laser.Carbon black powder is heated rapidly then cooling rapidly in the laser spot zone, reacting residing gaseous media has respectively air, carbonic acid gas and nitrogen.Collect reacted powder circulation for several times, last product is removed to unconverted carbon black with pickling oxidation and plasma gas oxidation, product after purification has all been observed the cubic diamond phase in TEM and XRD analysis, but has also observed graphite, two kinds of products of Zhao Shimo (chaoite).It is synthetic that the people such as Ogale are applied to diamond by induced with laser liquid-solid interfacial reaction method, and the graphite target of namely utilizing ruby laser irradiation to be immersed in benzene has been synthesized diamond.The people such as the Wang Jinbin of China and Yang Guowei use respectively again induced with laser liquid-solid interface method to synthesize diamond in water and acetone in recent years.The people such as Pearce have further expanded the work of Wang Jinbin, and they have verified the experiment in water, and have also obtained diamond in hexanaphthene.Although utilize the laser diamond synthesis to reduce conversion condition, never have special-purpose Preparation equipment, implementation and operation is still very complicated, and its effect neither be clearly, and transformation efficiency is still very low, is unfavorable for putting into production.And when lasing prepared Nano diamond, laser was and the graphite target direct effect, because laser energy is large, graphite target splashed, pollute and prepare platform, even laser head is caused to certain damage, the work-ing life of impact preparation precision and laser head.
Summary of the invention
The object of the invention is to overcome above-mentioned difficulties, solve the diamond preparation efficiency low, pollute and the problem such as damage apparatus for preparation, provide that a kind of intensity is high, the apparatus and method of sealing splashproof and safe and reliable raising diamond preparation efficiency, these apparatus and method can improve the diamond combined coefficient, technique is simple, equipment cost is low, can synthesize continuously and obtain high-quality Nano diamond.
A kind of device that improves the diamond preparation efficiency, comprise laser generating system, target system and purification system, described laser generating system comprises computer, the high energy beam impulse laser unit, 45 ° of total reflective mirrors, laser Machining head, condenser lens and protective glass, described purification system comprises heating unit, reactor, strong acid container and exhaust gas cleaner, described target system is positioned on worktable, described target system is comprised of target container and Splashproof cover, described target container inner wall top is provided with internal thread, the internal thread below is provided with the annular slope bearing, described annular slope bearing upper surface is plane, described Splashproof cover is hollow cylinder, its outer wall is provided with outside screw, inside is the supine hollow centrum in the end, the top of described hollow centrum has sharp incident light hole, internal thread on described target container and the outside screw on described Splashproof cover have formed threaded connection pair, the upper transverse plane laminating of the lower end wall of described Splashproof cover and described annular slope bearing.
In such scheme, between the lower end wall of described Splashproof cover and the upper transverse plane of described annular slope bearing, seal washer is housed.Due to the effect that seal washer is arranged, the Splashproof cover after tightening and target container are in closed state.
In such scheme, the rim of a cup of described target container is provided with a drainage mouth.
In such scheme, described target container and described Splashproof cover are made by the high impact strength transparent toughened glass.
The present invention also provides a kind of method that improves the diamond preparation efficiency, comprises following steps.
A, add suitable quantity of water to the target container, add quantitative graphite powder target to suspend in water in 0.02 g/ml ratio, stir and make it dispersed with electromagnetic shock.
B, seal washer is placed on the inclined-plane bearing; Splashproof cover is screwed in the target container, the target system is placed on worktable, adjust its position to suitably locating, swash incident light hole so that laser Machining head is aimed at.
C, open the high energy beam impulse laser unit, by computer control, laser beam directly focuses in the target container by laser processing condenser lens and protective glass in front through 45 ° of total reflective mirror reflections, and bombardment is dispersed in the powdered graphite target in water, during preparation is synthetic because the graphite mixed solution spattered is outward blocked by Splashproof cover, can again flow back in the target container, the circulation that the powdered graphite target will be accepted laser constantly acts on, make graphite that ionization occur and form carbon plasma, by graphite-phase, change and generate the diamond phase, end to be prepared, close all power supplys, take off the target system.
D, back out Splashproof cover, take out seal washer, by the drainage of drainage mouth, the Nano diamond mixed solution be prepared in the target container is poured out, moved in the reactor of purification system, open heating unit, diamond is purified, after to be purified completing, take out the diamond in reactor.
The present invention has following technological merit and positively effect: can obtain at normal temperatures and pressures the high quality Nano diamond, and prepare in the Nano diamond process in lasing, can prevent that graphite target from spattering outward, and can bear the stress that the high energy beam laser-impact brings, this device can make again graphite target accept the laser Circulation simultaneously, has greatly improved the Nano diamond transformation efficiency.Technique of the present invention is simple, operates easy to loading and unloadingly, has kept preparing the platform cleaning, the target container of being made by the high impact strength transparent toughened glass, not only be convenient to observe the target Stimulated Light effect situation in container, but also the security that has improved preparation process, installation cost is low.
The accompanying drawing explanation
Fig. 1 is a kind of apparatus and method structural representation that improves the diamond preparation efficiency of the present invention.
Fig. 2 is Splashproof cover, seal washer and inclined-plane bearing fit structure schematic diagram partial enlarged drawing.
Fig. 3 is the Splashproof cover three-dimensional structure diagram.
Fig. 4 is gasket structure figure.
Fig. 5 is target container three-dimensional structure diagram.
Fig. 6 is purification apparatus structure schematic diagram.
1. computers in figure, 2. high energy beam impulse laser unit, 3. laser beam, 4. 45 ° of total reflective mirrors; 5. laser Machining head, 6. condenser lens, 7. protective glass; 8. Splashproof cover, 9. swash incident light hole, 10. drainage mouth; 11. threaded connection pair, 12. seal washers, 13. inclined-plane bearings; 14. the target container, 15. worktable, 16. heating units; 17. reactor, 18. strong acid containers, 19. exhaust gas cleaners.
Embodiment
Below in conjunction with accompanying drawing and concrete use-case, the apparatus and method that the present invention proposes are further described in detail.
As can be known by Fig. 1-Fig. 6, a kind of device that improves the diamond preparation efficiency of the present invention is comprised of three parts, is respectively: laser generating system, target system and purification system.Described laser generating system comprises computer 1, high energy beam impulse laser unit 2, 45 ° of total reflective mirrors 4, laser Machining head 5, condenser lens 6 and protective glass 7, described purification system comprises heating unit 16, reactor 17, strong acid container 18 and exhaust gas cleaner 19, described target system is positioned on worktable 15, described target system is comprised of target container 14 and Splashproof cover 8, target container 14 and described Splashproof cover 8 are made by the high impact strength transparent toughened glass, the rim of a cup of target container 14 is provided with a drainage mouth 10, described target container 14 upper inside wall are provided with internal thread, the internal thread below is provided with annular slope bearing 13, described annular slope bearing 13 upper surfaces are plane, described Splashproof cover 8 is hollow cylinder, its outer wall is provided with outside screw, inside is the supine hollow centrum in the end, the top of described hollow centrum has swashs incident light hole 9, internal thread on described target container 14 and the outside screw on described Splashproof cover 8 have formed threaded connection pair 11, between the lower end wall of described Splashproof cover 8 and the upper transverse plane of described annular slope bearing 13, seal washer 12 is housed, the lower end wall of described Splashproof cover 8 and the upper transverse plane of described annular slope bearing 13 fit together by gasket seal 12.
During use, add suitable quantity of water to the target container, add quantitative graphite powder target to suspend in water in 0.02 g/ml ratio, stir and make it dispersed with electromagnetic shock, seal washer is placed on the inclined-plane bearing, Splashproof cover is screwed in the target container, the target system is placed on worktable, adjust its position to suitably locating, swash incident light hole so that laser Machining head is aimed at, open the high energy beam impulse laser unit, by computer control, laser beam directly focuses in the target container by laser processing condenser lens and protective glass in front through 45 ° of total reflective mirror reflections, and bombardment is dispersed in the powdered graphite target in water, during preparation is synthetic because the graphite mixed solution spattered is outward blocked by Splashproof cover, can again flow back in the target container, the circulation that the powdered graphite target will be accepted laser constantly acts on, make graphite that ionization occur and form carbon plasma, by graphite-phase, change and generate the diamond phase, end to be prepared, close all power supplys, take off the target system, back out Splashproof cover, take out seal washer, by the drainage of drainage mouth, the Nano diamond mixed solution be prepared in the target container is poured out, moved in the reactor of purification system, open heating unit, diamond is purified, after to be purified completing, take out the diamond in reactor.

Claims (5)

1. device that improves the diamond preparation efficiency, comprise laser generating system, target system and purification system, described laser generating system comprises computer (1), high energy beam impulse laser unit (2), 45 ° of total reflective mirrors (4), laser Machining head (5), condenser lens (6) and protective glass (7), described purification system comprises heating unit (16), reactor (17), strong acid container (18) and exhaust gas cleaner (19), described target system is positioned on worktable (15), it is characterized in that, described target system is comprised of target container (14) and Splashproof cover (8), described target container (14) upper inside wall is provided with internal thread, the internal thread below is provided with annular slope bearing (13), described annular slope bearing (13) upper surface is plane, described Splashproof cover (8) is hollow cylinder, its outer wall is provided with outside screw, inside is the supine hollow centrum in the end, the top of described hollow centrum has sharp incident light hole (9), outside screw on internal thread on described target container (14) and described Splashproof cover (8) has formed threaded connection pair (11), the upper transverse plane laminating of the lower end wall of described Splashproof cover (8) and described annular slope bearing (13).
2. a kind of device that improves the diamond preparation efficiency according to claim 1, is characterized in that, between the upper transverse plane of the lower end wall of described Splashproof cover (8) and described annular slope bearing (13), seal washer (12) is housed.
3. according to the described a kind of device that improves the diamond preparation efficiency of claims 1 or 2, it is characterized in that, the rim of a cup of described target container (14) is provided with a drainage mouth (10).
4. according to the described a kind of device that improves the method for diamond preparation efficiency of claims 3, it is characterized in that, described target container (14) and described Splashproof cover (8) are made by the high impact strength transparent toughened glass.
5. method that improves the diamond preparation efficiency comprises following steps:
A, add suitable quantity of water to target container (14), add quantitative graphite powder target to suspend in water in 0.02 g/ml ratio, stir and make it dispersed with electromagnetic shock;
B, seal washer (12) is placed on inclined-plane bearing (13); Splashproof cover (8) is screwed in target container (14), and due to the effect that seal washer (12) and inclined-plane bearing (13) are arranged, the Splashproof cover after tightening (8) is in closed state with target container (14); The target system is placed in to worktable (15) upper, adjusts its position to suitably locating, swash incident light hole (9) so that laser Machining head (5) is aimed at;
C, open high energy beam impulse laser unit (2), by computer (1), controlled, laser beam (3) directly focuses in target container (14) by the inner condenser lens (6) of laser Machining head (5) and protective glass (7) through 45 ° of total reflective mirrors (4) reflection, and bombardment is dispersed in the powdered graphite target in water, during preparation is synthetic because the graphite mixed solution spattered is outward blocked by Splashproof cover (8), can again flow back in target container (14), the circulation that the powdered graphite target will be accepted laser constantly acts on, make graphite that ionization occur and form carbon plasma, by graphite-phase, change and generate the diamond phase, end to be prepared, close all power supplys, take off the target system,
D, back out Splashproof cover (8), take out seal washer (12), drainage by drainage mouth (10), the Nano diamond mixed solution be prepared in target container (14) is poured out, move in the reactor (17) of purification system, open heating unit (16), diamond is purified, after to be purified completing, take out the diamond in reactor (17).
CN201310319625.XA 2013-07-29 2013-07-29 Device and method for improving preparation efficiency of diamonds Expired - Fee Related CN103408005B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106082206A (en) * 2016-06-16 2016-11-09 江苏大学 A kind of method and apparatus improving Nano diamond combined coefficient

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5464159A (en) * 1992-05-27 1995-11-07 Wacker-Chemitronic Gesellschaft Fur Elektronik-Grundstoffe Mbh Method for the contamination-free size reduction of semiconductor material, especially silicon
CN102409339A (en) * 2011-11-18 2012-04-11 江苏大学 Method and device for preparing diamond-like carbon coating by cladding fiber laser
CN102409292A (en) * 2011-11-18 2012-04-11 江苏大学 Method and device for continuously synthesizing diamond membrane by radiating carbon nanotube with strong laser
CN102409291A (en) * 2011-11-18 2012-04-11 江苏大学 Method and device for preparing diamond film doped with ultrafine nano-structural metal particles

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5464159A (en) * 1992-05-27 1995-11-07 Wacker-Chemitronic Gesellschaft Fur Elektronik-Grundstoffe Mbh Method for the contamination-free size reduction of semiconductor material, especially silicon
CN102409339A (en) * 2011-11-18 2012-04-11 江苏大学 Method and device for preparing diamond-like carbon coating by cladding fiber laser
CN102409292A (en) * 2011-11-18 2012-04-11 江苏大学 Method and device for continuously synthesizing diamond membrane by radiating carbon nanotube with strong laser
CN102409291A (en) * 2011-11-18 2012-04-11 江苏大学 Method and device for preparing diamond film doped with ultrafine nano-structural metal particles

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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