CN1335420A - Method of preparing metastable nanometer crystal through pulse laser induced liquid-solid interface reaction - Google Patents
Method of preparing metastable nanometer crystal through pulse laser induced liquid-solid interface reaction Download PDFInfo
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- CN1335420A CN1335420A CN 00126686 CN00126686A CN1335420A CN 1335420 A CN1335420 A CN 1335420A CN 00126686 CN00126686 CN 00126686 CN 00126686 A CN00126686 A CN 00126686A CN 1335420 A CN1335420 A CN 1335420A
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Abstract
The present invention is one artificial composition of metastable nanometer crystal. Inside one liquid solid reactor, solid material including chemical pure graphite and cubic boron nitride or boron carbide as well as organic or inorganic hydrocarbon solution or secondary distilled water are set with the liquid level being 1-2 mm higher than the solid material surface to form one liquid-solid interface. Laser beam focused by one lens and reflected by one reflector is led to the reactor and acted to the liquid-solid interface for 30-60 min. Powder collected from the reactor is heated in a potassium permanganate at 180-222 deg.c to obtain purified metastable nanometer crystal. The present invention has low material cost, simple preparation condition and other advantages.
Description
The utility model relates to a kind of synthetic metastable state preparation of nano crystal.
Metastable state is nanocrystalline, all is the superhard material the most widely of research at present as cubic boron nitride, diamond and NANO CRYSTALLINE CARBON NITRIDES.Carbon nitride material is that C0hen and Liu come out according to Theoretical Calculation and Si
3N
4A kind of novel superhard material of structural similitude, β-C
3N
4Hardness may with diamond hardness quite or be higher than diamond.Tetert and Hemly point out to exist five kinds of C in theory recently
3N
4: graphite phase, α phase, β phase, pseudo-cube phase with cube mutually.Since the peculiar property of this type material of carbonitride and tempting application prospect, therefore, from experimentally synthesizing the research emphasis that this type material of carbonitride just becomes the investigation of materials worker.If who is earlier from synthetic this material experimentally, just will be in breakthrough progress aspect the carbon nitride material research, and obtain perch.Natural diamond is very rare, and cubic boron nitride also is a kind of superhard material of synthetic.At present, people to have only under some extreme conditions (as High Temperature High Pressure) could synthesize these metastable states nanocrystalline.But the apparatus expensive of these methods, creating conditions requires height, thereby has limited the applied research to them.Particularly carbon nitride material is not also prepared compellent monocrystalline crystal at present.Explosion method once was used to diamond synthesis and cubic boron nitride is nanocrystalline, but a little method is dangerous big, and the synthetic sample quality is not high, and the purification procedures complexity.
The object of the present invention is to provide a kind of nanocrystalline method of metastable state for preparing at normal temperatures and pressures.
The objective of the invention is to realize: a kind of pulse laser induced liquid-nanocrystalline method of liquid/solid interface prepared in reaction metastable state by following approach, with chemical pure graphite, cubic boron nitride or norbide solid material place liquid-solid reactor, in reactor, add organic or inorganic hydrocarbon solution or redistilled water to exceeding chemical pure graphite, cubic boron nitride or norbide solid material 1-2mm, form a liquid-solid interface, the laser that laser apparatus sends is by after the convex lens focus, in the reflection guiding liquid-solid reactor by reflective mirror, in the liquid-solid interface effect after 30-60 minute, collect the powder in the reactor, powder is placed on is heated to 180-222 degree centigrade in the strong potassium permanganate solution, the purification metastable state is nanocrystalline.Laser energy is 10
6～10
10W/cm
2, optical maser wavelength can be from the visible light to the infrared band, and the pulsewidth of pulsed laser is 1-20 nanosecond.
Characteristics of the present invention are that the prices of raw and semifnished materials are cheap, only need normal temperature and pressure, and required equipment is simple, and cost is low, and Working environment does not have danger, and is simple to operate, safe and reliable, has great application prospect.
The invention will be further described below in conjunction with drawings and Examples:
Fig. 1 is a process unit schema of the present invention;
Embodiment 1; As shown in Figure 1, used instrument of the present invention and material are: the Nd:YAG solid statelaser, bandpass filter 1, optical male lens 2, reflective mirror 3, liquid-solid reactor 4, at first with chemical pure graphite, cubic boron nitride or norbide clean, place liquid-solid reactor 4 as laser target then, in liquid-solid reactor 4, slowly inject the chemical pure acetone soln, make the acetone soln liquid level exceed laser target 1-2mm, start the YAG pulsed laser, make laser pass through bandpass filter 1 laser target in reflective mirror 3 guiding liquid-solid reactors 4 again after optical male lens 2 focus on, regulate laser output power, the power density that lasing is acted on the laser target reaches 10
10W/cm
2When pulsed laser action during in liquid-solid interface, the corrode laser target also produces atom, molecule and the active group of carbon and a large amount of ion, electron plasma plumage on its surface.In a pulse, plasma plume absorbs laser energy, becomes the plasmoid that is in High Temperature High Pressure high-density rapid expansion.Acetone soln was vaporized, is decomposed near this plasmoid made its contact interface again, and ionization is atom, molecule, active group and ion.Like this, because the rapid expansion of plasmoid makes various active particles and the active particle in the near interface acetone soln in the plasma body react, generate nanocrystalline.End along with pulse, the quick cancellation of plasmoid, the active particle reaction stops, nanocrystallinely also stop growing, so just in liquid, synthesized to have and pressed the nanocrystalline of steady structure, after practicing shooting through segment length's time, the sample seasoning, collect powder and be placed in the strong potassium permanganate solution and be heated to about 200 degrees centigrade, Graphite Powder 99 is corroded and remaining diamond powder.Analyze being placed on after the remaining powdered sample drying under H800 transmission electron microscope and the high explanation of the EM420 electron microscope, show and contain lonsdaleite and cubic diamond in the powdered sample of preparing.
Embodiment 2; As shown in Figure 1, used instrument of the present invention and material are: the Nd:YAG solid statelaser, bandpass filter 1, optical male lens 2, reflective mirror 3, liquid-solid reactor 4, at first with chemical pure graphite, cubic boron nitride or norbide clean, place liquid-solid reactor 4 as laser target then, in liquid-solid reactor 4, slowly inject liquid ammonia solution, make the liquid ammonia solution liquid level exceed laser target 1-2mm, start the YAG pulsed laser, make laser pass through bandpass filter 1 laser target in reflective mirror 3 guiding liquid-solid reactors 4 again after optical male lens 2 focus on, regulate laser output power, the power density that lasing is acted on the laser target reaches 10
10W/cm
2When pulsed laser action during in liquid-solid interface, the corrode laser target also produces atom, molecule and the active group of carbon and ion body feathers that a large amount of ion, electronics etc. are formed on its surface.In a pulse, plasma plume absorbs laser energy, becomes the plasmoid that is in High Temperature High Pressure high-density rapid expansion.Liquid ammonia solution was vaporized, is decomposed near this plasmoid made its contact interface again, and ionization is atom, molecule, active group and ion.Like this, because the rapid expansion of plasmoid makes various active particles and the active particle in the near interface liquid ammonia solution in the plasma body react, generate the azotized carbon nano nucleus, and owing to there are the various particles of a large amount of carbon particless and nitrogen to provide, the carbonitride nucleus is just grown up slowly.End along with pulse, the quick cancellation of plasmoid, the active particle reaction stops, nanocrystallinely also stop growing, so just in liquid, synthesized to have and pressed the nanocrystalline of steady structure, after practicing shooting through segment length's time, the sample seasoning, collect powder and be placed in the strong potassium permanganate solution and be heated to about 200 degrees centigrade, Graphite Powder 99 is corroded and remaining carbonitride powder.Analyze being placed on behind the remaining powder sample drying under H800 transmission electron microscope and the high explanation of the EM420 electron microscope, have graphite phase, α phase, β mutually with cube mutually azotized carbon nano crystal.
Claims (2)
1. pulse laser induced liquid-nanocrystalline method of liquid/solid interface prepared in reaction metastable state, it is characterized in that: with chemical pure graphite, cubic boron nitride or norbide solid material place liquid-solid reactor, in reactor, add organic or inorganic hydrocarbon solution or redistilled water to exceeding chemical pure graphite, cubic boron nitride or norbide solid material 1-2mm, form a liquid-solid interface, the laser that laser apparatus sends is by after the convex lens focus, in the reflection guiding liquid-solid reactor by reflective mirror, in the liquid-solid interface effect after 30-60 minute, collect the powder in the reactor, powder is placed on is heated to 180-222 degree centigrade in the strong potassium permanganate solution, the purification metastable state is nanocrystalline.
2. pulse laser induced liquid-nanocrystalline method of liquid/solid interface prepared in reaction metastable state according to claim 1, it is characterized in that: laser energy is 10
6～10
10W/cm
2, optical maser wavelength can be from the visible light to the infrared band, and the pulsewidth of pulsed laser is 1-20 nanosecond.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 00126686 CN1335420A (en) | 2000-11-15 | 2000-11-15 | Method of preparing metastable nanometer crystal through pulse laser induced liquid-solid interface reaction |
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| CN 00126686 CN1335420A (en) | 2000-11-15 | 2000-11-15 | Method of preparing metastable nanometer crystal through pulse laser induced liquid-solid interface reaction |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101239391B (en) * | 2008-02-27 | 2010-06-02 | 天津大学 | Method for coating metal nano granule by laser synthesizing carbon |
| CN105149602A (en) * | 2015-08-16 | 2015-12-16 | 河北工业大学 | Method for preparing amorphous nanometer soft magnetism powder and special collection device of amorphous nanometer soft magnetism powder |
| WO2021197471A1 (en) * | 2020-04-03 | 2021-10-07 | 燕山大学 | Diamond composite phase material and preparation method therefor |
-
2000
- 2000-11-15 CN CN 00126686 patent/CN1335420A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101239391B (en) * | 2008-02-27 | 2010-06-02 | 天津大学 | Method for coating metal nano granule by laser synthesizing carbon |
| CN105149602A (en) * | 2015-08-16 | 2015-12-16 | 河北工业大学 | Method for preparing amorphous nanometer soft magnetism powder and special collection device of amorphous nanometer soft magnetism powder |
| CN105149602B (en) * | 2015-08-16 | 2017-03-08 | 河北工业大学 | A kind of amorphous nano soft magnetism raw powder's production technology and its collection special purpose device |
| WO2021197471A1 (en) * | 2020-04-03 | 2021-10-07 | 燕山大学 | Diamond composite phase material and preparation method therefor |
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