CN103641112A - Method for preparing nano-diamond through femtosecond laser - Google Patents
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- CN103641112A CN103641112A CN201310724033.6A CN201310724033A CN103641112A CN 103641112 A CN103641112 A CN 103641112A CN 201310724033 A CN201310724033 A CN 201310724033A CN 103641112 A CN103641112 A CN 103641112A
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Abstract
The invention discloses a method for preparing nano-diamond through femtosecond laser, and provides a method for preparing the nano-diamond by generating shock wave in a diamond solution by using the nonlinear effect of the femtosecond laser, wherein the method is free of pollution, simple in process, safe to use and capable of being repeatedly used. A device used in the method comprises an inverted microscope, wherein a precision displacement platform is arranged on an objective table of the inverted microscope; a sample tank is arranged on the precise displacement platform; the inverted microscope is provided with a main light path and an auxiliary light path in symmetry; a focus objective is arranged on one side of the light main path of the inverted microscope; a collecting lens is arranged on one side of the auxiliary light path of the inverted microscope; the main light path and the auxiliary light path of the inverted microscope are overlapped with each other and focused on the sample tank. The nano-diamond disclosed by the invention is widely applied to fields of electronics, machines, chemicals, medicines and the like.
Description
Technical field
The present invention relates to the preparation of Nano diamond material, specifically, relate to a kind of.Particularly utilize femtosecond laser non-linear effect in the aqueous solution, to produce shockwave and prepare Nano diamond.
Background technology
Femtosecond laser is the new technology that development in recent years is got up.Femtosecond laser is a kind of laser with impulse form running, and the time length is very short, and from several femtoseconds to hundreds of femtosecond (1 femtosecond is exactly negative 15 power seconds of 10), the short pulse that its Billy obtains with electronics method is short several thousand times.Femtosecond laser has very high momentary power.For the laser pulse of 10 femtoseconds, 10 millijoules, its instantaneous power can reach more than 1012 watts.Because femto-second laser pulse has the instantaneous power of superelevation, so often can cause obvious non-linear optical effect.But the difference of the pulse energy level of femtosecond laser, its effect causing is also not quite similar.For relatively low-energy pulse (as receiving below joule), can cause obvious multiphoton-effect; And reach micro-joule even during millijoule when pulse energy, laser pulse often can cause breakdown potential from etc. violent reaction.Femtosecond laser is all widely used in a plurality of fields such as nonlinear optics and nanometer making.
Nano diamond is one of the nano material of tool DEVELOPMENT PROSPECT of 21 century.Nano diamond, except having adamantine general characteristic, also has the characteristic of nano material simultaneously.Nano diamond has the characteristics such as textural defect that specific surface area is large, chemically reactive good, entropy is large and more.
The preparation method of Nano diamond be take oxygen negative explosive as carbon source at present, and under the high temperature and high pressure environment producing at explosive detonation, moment is synthetic.Diamond particle diameter is less than 60nm, shape and epigranular, but due to surface effects, particle exists with reunion state form, and its premium properties as nano-powder cannot be brought into play.The agglomeration traits of particle is not resolved, although Here it is, as far back as the beginning of the nineties in last century, just to have realized Detonation Process technical scale synthetic, the one of the main reasons that Nano diamond application progress still obviously lags behind so far.Therefore, the present invention can realize its stable dispersion, and for promoting, this field applied research and industry development are significant.
The detonation preparation method of Nano diamond powder, belongs to high temperature, high pressure preparation method at present.The shortcoming of Detonation Process is synthesis technique more complicated, have certain danger and contaminative.
In sum, based on femtosecond laser non-linear effect, prepare Nano diamond, can obtain better the diamond nano particle of stable dispersion in the aqueous solution, advance better the development of Nano diamond technology.
Summary of the invention
The object of the invention is to overcome the shortcoming of prior art, provide a kind of pollution-free, technique is simple, uses safety, can reusablely utilize femtosecond laser to fly linear effect and in the diamond aqueous solution, produce the method that shockwave is prepared Nano diamond.
For reaching above-mentioned purpose, a kind of device that utilizes femtosecond laser to prepare Nano diamond of the present invention, adopts following technical scheme:
A kind of device that utilizes femtosecond laser to prepare Nano diamond, comprise inverted microscope, the Stage microscope of inverted microscope is provided with precision displacement platform, precision displacement platform is provided with sample pool, inverted microscope is provided with symmetrical main optical path and auxiliary light path, main optical path one side of inverted microscope is provided with focusing objective len, and auxiliary light path one side of inverted microscope is provided with condensor, and the main optical path of inverted microscope and auxiliary light path overlap each other and focus on sample pool;
The auxiliary optical routing means of illumination of inverted microscope, A lens, condensor form, inverted microscope one side is provided with condensor, condensor is provided with A lens before the opposite side of inverted microscope, A lens opposite side is provided with means of illumination, the fill-in light that means of illumination sends is through A lens lighting to condensor, and fill-in light focuses on sample pool through condensor;
The main optical path of inverted microscope is by femto-second laser, collimation lens set, extender lens group, two-phase look mirror, focusing objective len forms, inverted microscope is provided with focusing objective len away from the opposite side of auxiliary light path condensor, before focusing objective len opposite side, be provided with the two-phase look mirror of a miter angle, two-phase look mirror side and focusing objective len light path vertical direction are provided with femto-second laser, between femto-second laser and two-phase look mirror, be provided with successively collimation lens set, extender lens group, the light path of femto-second laser is through collimation lens set, after extender lens group, by the reflection of two-phase look mirror, arrive focusing objective len, focus on sample pool.
In certain embodiments, the main optical path homonymy of described inverted microscope is provided with imaging device, between imaging device and inverted microscope, be provided with successively photo-sensor, B lens, two-phase look mirror, focusing objective len, photo-sensor connects imaging device, two-phase look mirror is positioned at the opposite side of the auxiliary light path of inverted microscope, at the contrary beam direction of the auxiliary light path of inverted microscope, be provided with the two-phase look mirror of a miter angle, the transmission from sample pool of the auxiliary light path of inverted microscope is come and is passed through focusing objective len light beam out by two-phase look mirror, after B lens, arrive photo-sensor, and in imaging device, complete real time imagery.
In certain embodiments, described condensor is: NA=1.2～1.8; Focusing objective len is: the microcobjective of 10x, 20x, 25x; Extender lens group: the focal length of left lens is 2cm～5cm, the focal length of right lens is 3cm～7cm; Collimation lens set: two focal lengths of lens are 4cm～7cm; B lens: the focal length of lens is 4cm～7cm; A lens: the focal length of lens is 1cm～2cm.
Utilize femtosecond laser to prepare a method for Nano diamond, method is as follows:
Sample preparation: diamond powder is configured to the aqueous solution of 0.5mol/ml～2mol/ml in sample pool with deionized water, and adds 0.1mol/ml～0.5mol/ml ethylene glycol, as the tensio-active agent of particle;
By the ultrasonic 15min of deionized water for the solution configuring, uniform particles is distributed in solution; Then in the environment of air, sample pool is put on the nano level precision displacement platform of inverted microscope Stage microscope, by controlling precision displacement platform, realized the movement of diamond solution on locus in sample pool;
The femtosecond laser of femto-second laser of take is main optical path, and the illumination path that the means of illumination of inverted microscope of take sends is auxiliary light path, adjusts main optical path and auxiliary light path, and both light paths are overlapped each other; Femto-second laser pass through focusing objective len vertical focusing in the diamond solution of sample pool; The lighting source that means of illumination sends, through condensor, makes the diamond solution in sample pool be imaged on photo-sensor through focusing objective len;
First close the femtosecond laser of femto-second laser, make now as long as the illumination path (auxiliary light path) of means of illumination is radiated at the 2um～10um position, distance sample pool bottom in the diamond solution of sample pool, then at the contrary beam direction of illumination path (auxiliary light path), adopt the two-phase look mirror of a miter angle, from the diamond solution of sample pool transmission is come and carry out separated on space through light beam out of focusing objective len and the light beam of main optical path, through B lens, arrive photo-sensor, by imaging device to its collection and real time imagery;
Open the femtosecond laser of femto-second laser, femtosecond laser arrives focusing objective len by the reflection of two-phase look mirror after collimation lens set, extender lens group, focuses in the diamond solution of sample pool; Now by the variation of imaging device observation experiment, and by the control of precision displacement platform, in two dimensional surface, mobile example pond, makes the full and uniform pulverizing of whole diamond in diamond solution;
Femtosecond laser through 15min～60min irradiates, and due to the high pulse energy that femtosecond laser produces, diamond in sample pool is pulverized and is obtained Nano diamond.
In certain embodiments, the laser radiation power regulating range of described femto-second laser is 2w～4w, and laser frequency is 100Hz～1100Hz.
In certain embodiments, the femtosecond laser parameter of described femto-second laser is: frequency 800Hz～1100Hz, and wavelength is 800nm, and pulse width is 35fs～40fs, and laser radiation power is 3w, and polarization direction is linear polarization.
Currently reported Nano diamond manufacture craft,, all there is certain danger and contaminative in Detonation Process for example, and the present invention can provide a kind of safe, pollution-free, Nano diamond preparation method that can reuse.Femtosecond laser of the present invention is a kind of laser with impulse form running, time length is very short, it is 35fs that the present invention uses, the short pulse that its Billy obtains with electronics method wants short several thousand times, can obtain very high momentary power, thereby produce powerful shockwave, pulverize diamond particles, prepare Nano diamond.
Utilize this invention can prepare the diamond nano particle that particle diameter is less, Nano diamond, except having adamantine general characteristic, also has the characteristic of nano material simultaneously.Nano diamond has the characteristics such as textural defect that specific surface area is large, chemically reactive good, entropy is large and more.So Nano diamond has extensive utilization in fields such as electronics, machinery, chemical industry, medical treatment.
Accompanying drawing explanation
Figure 1 shows that the structural representation of the embodiment of the present invention;
Figure 2 shows that the present invention is that scintigram under 10000 times of magnifications of Nano diamond is prepared in 0.5mol/ml pulverizing for 60 minutes in diamond strength of solution;
Figure 3 shows that the present invention is that scintigram under 10000 times of magnifications of Nano diamond is prepared in 1mol/ml pulverizing for 60 minutes in diamond strength of solution;
Figure 4 shows that the present invention is that scintigram under 10000 times of magnifications of Nano diamond is prepared in 2mol/ml pulverizing for 60 minutes in diamond strength of solution;
Figure 5 shows that the present invention is that scintigram under 50000 times of magnifications of Nano diamond is prepared in 2mol/ml pulverizing for 60 minutes in diamond strength of solution;
Description of reference numerals is as follows:
Femto-second laser 101, imaging device 102, means of illumination 103, two-phase look mirror 105, extender lens group 201, collimation lens set 202, B lens 204, A lens 205, inverted microscope 300, condensor 301, focusing objective len 302, sample pool 303, precision displacement platform 304, photo-sensor 305.
Embodiment
For further understanding feature of the present invention, technique means and the specific purposes that reach, function, resolve the advantages and spirit of the present invention, by below in conjunction with accompanying drawing and embodiment, detailed description of the present invention being further understood.
The present invention includes inverted microscope 300, shown in accompanying drawing 1, the Stage microscope of inverted microscope 300 is provided with precision displacement platform 304, precision displacement platform 304 is provided with sample pool 303,303 li of loading diamond solution of sample pool, inverted microscope 300 is provided with symmetrical main optical path and auxiliary light path, main optical path one side of inverted microscope 300 is provided with focusing objective len 302, auxiliary light path one side of inverted microscope 300 is provided with condensor 301, and the main optical path of inverted microscope 300 and auxiliary light path overlap each other and focus in the diamond solution of sample pool 303.
Inverted microscope 300 comprises Stage microscope, condensor 301, focusing objective len 302.
In an embodiment, condensor 301 is therein: NA=1.2, and focusing objective len 302 is: the microcobjective of 10x; Extender lens group 201: in figure, the focal length of left lens is 3cm, the focal length of right lens is 5cm; 202: two focal lengths of lens of collimation lens set are 5cm; B lens 204: the focal length of lens is 5cm; A lens 205: the focal length of lens is 1cm.
The auxiliary optical routing means of illumination 103 of inverted microscope 300, A lens 205, condensor 301 form, inverted microscope 300 1 sides are provided with condensor 301, condensor 301 is provided with A lens 205 before the opposite side of inverted microscope 300, A lens 205 opposite sides are provided with means of illumination 103, the fill-in light that means of illumination 103 sends is irradiated to condensor 301 through A lens 205, and fill-in light focuses in the diamond solution of sample pool 303 through condensor 301.
The main optical path of inverted microscope 300 is by femto-second laser 101, extender lens group 201, collimation lens set 202, two-phase look mirror 105, focusing objective len 302 forms, inverted microscope 300 is away from the auxiliary light path of condensor 301() opposite side be provided with focusing objective len 302, before focusing objective len 302 opposite sides, be provided with the two-phase look mirror 105 of a miter angle, two-phase look mirror 105 sides and focusing objective len 302 light path vertical direction are provided with femto-second laser 101, between femto-second laser 101 and two-phase look mirror 105, be provided with successively extender lens group 201, collimation lens set 202, the light path of femto-second laser 101 is through extender lens group 201, after collimation lens set 202, by 105 reflections of two-phase look mirror, arrive focusing objective len 302, focus in the diamond solution of sample pool 303.
The main optical path homonymy of inverted microscope 300 is provided with imaging device 102, between imaging device 102 and inverted microscope 300, be provided with successively photo-sensor 305, B lens 204, two-phase look mirror 105, focusing objective len 302, photo-sensor 305 connects imaging device 102, two-phase look mirror 105 is positioned at the opposite side of inverted microscope 300 auxiliary light paths, at the contrary beam direction of inverted microscope 300 auxiliary light paths, be provided with the two-phase look mirror 105 of a miter angle, the transmission from the diamond solution of sample pool 303 of the auxiliary light path of inverted microscope 300 is come and is passed through focusing objective len 302 light beam out by two-phase look mirror 105, the rear arrival photo-sensor 305 of B lens 204, and complete real time imagery in imaging device 102.
The Nano diamond method of preparing of the present invention, its technical scheme is as follows:
Sample preparation: diamond powder is configured to the aqueous solution of 0.5mol/ml～2mol/ml in sample pool 303 with deionized water, and adds 0.1mol/ml～0.5mol/ml ethylene glycol, as the tensio-active agent of particle;
By the ultrasonic 15min of deionized water for the solution configuring, uniform particles is distributed in solution; Then in the environment of air, sample pool 303 is put on the nano level precision displacement platform 304 of inverted microscope 300 Stage microscopes, by controlling precision displacement platform 304, realized the movement of diamond solution on locus in sample pool 303;
The femtosecond laser of femto-second laser 101 of take is main optical path, and the illumination path that the means of illumination 103 of inverted microscope 300 of take sends is auxiliary light path, adjusts main optical path and auxiliary light path, and both light paths are overlapped each other; Femto-second laser 101 pass through focusing objective len 302 vertical focusings in the diamond solution of sample pool 303; The lighting source that means of illumination 103 sends, through condensor 301, makes the diamond solution in sample pool 303 be imaged on photo-sensor 305 through focusing objective len 302;
First close the femtosecond laser of femto-second laser 101, make now as long as the illumination path (auxiliary light path) of means of illumination 103 is radiated at the 2um～5um position, distance sample pool bottom in the diamond solution of sample pool 303, be preferably apart from 2um position, sample pool bottom, then at the contrary beam direction of illumination path (auxiliary light path), adopt the two-phase look mirror 105 of a miter angle, from the diamond solution of sample pool 303 transmission is come and carry out separated on space through light beam out of focusing objective len 302 and the light beam of main optical path, through B lens 204, arrive photo-sensor 305, by imaging device 102 to its collection and real time imagery,
Open the femtosecond laser of femto-second laser 101, femtosecond laser arrives focusing objective len 302 by 105 reflections of two-phase look mirror after extender lens group 201, collimation lens set 202, focuses in the diamond solution of sample pool 303; Now by the variation of imaging device 102 observation experiments, and by the control of precision displacement platform 304, in two dimensional surface, mobile example pond 303, makes the full and uniform pulverizing of whole diamond in diamond solution;
Femtosecond laser through 15min～60min irradiates, and due to the high pulse energy that femtosecond laser produces, diamond in sample pool 303 is pulverized and is obtained Nano diamond.
The laser radiation power regulating range of femto-second laser 101 is 2w～4w, and laser frequency is 100Hz～1100Hz.
In an embodiment, the femtosecond laser parameter of femto-second laser 101 is therein: frequency 1kHz, and wavelength is 800nm, and pulse width is 35fs, and laser radiation power is 3w, and polarization direction is linear polarization.
The present invention is that a kind of femtosecond laser non-linear effect of utilizing produces the method that shockwave pulverizing diamond particles is prepared Nano diamond in the aqueous solution, utilize extender lens group 201(to expand light path), collimation lens set 202(collimated light path), two-phase look mirror 105(reflected light path) light path is introduced into the femtosecond laser of femto-second laser 101 in inverted microscope 300, the focusing objective len 302 of recycling inverted microscope 300 focuses on femtosecond laser the diamond solution that is arranged in sample pool 303 on precision displacement platform 304, with the laser direct irradiation diamond solution focusing on, when femtosecond laser focuses on the aqueous solution, the aqueous solution is breakdown, produce a large amount of plasma bodys, and then formation supersonic shock wave, vaporization and jet.Near the focus of laser, can produce very large mechanical pressure therebetween.Utilize this effect, the object particle in solution is pulverized.The irradiation time of laser is 15min～60min, and the power of incident laser is 2w～4w, and frequency is 100Hz～1100Hz, and the concentration of solution is 0.5mol/ml～2mol/ml.Technique of the present invention is simple, pollution-free, can repetitive operation.
Utilize this invention can prepare the diamond nano particle that particle diameter is less.Nano diamond is one of the nano material of tool DEVELOPMENT PROSPECT of 21 century.Nano diamond, except having adamantine general characteristic, also has the characteristic of nano material simultaneously.Nano diamond has the characteristics such as textural defect that specific surface area is large, chemically reactive good, entropy is large and more.So Nano diamond has extensive utilization in fields such as electronics, machinery, chemical industry, medical treatment.
The above embodiment has only expressed part embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as limitation of the scope of the invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with claims.
Claims (6)
1. a device that utilizes femtosecond laser to prepare Nano diamond, comprise inverted microscope (300), it is characterized in that, the Stage microscope of described inverted microscope (300) is provided with precision displacement platform (304), described precision displacement platform (304) is provided with sample pool (303), described inverted microscope (300) is provided with symmetrical main optical path and auxiliary light path, main optical path one side of described inverted microscope (300) is provided with focusing objective len (302), auxiliary light path one side of described inverted microscope (300) is provided with condensor (301), the main optical path of described inverted microscope (300) and auxiliary light path overlap each other and focus on sample pool (303),
The auxiliary optical routing means of illumination (103) of described inverted microscope (300), A lens (205), condensor (301) form, described inverted microscope (300) one sides are provided with condensor (301), described condensor (301) is provided with A lens (205) before the opposite side of inverted microscope (300), described A lens (205) opposite side is provided with means of illumination (103), the fill-in light that described means of illumination (103) sends is irradiated to condensor (301) through A lens (205), through condensor (301), focuses on sample pool (303);
The main optical path of described inverted microscope (300) is by femto-second laser (101), extender lens group (201), collimation lens set (202), two-phase look mirror (105), focusing objective len (302) forms, described inverted microscope (300) is provided with focusing objective len (302) away from the opposite side of auxiliary light path condensor (301), before described focusing objective len (302) opposite side, be provided with the two-phase look mirror (105) of a miter angle, described two-phase look mirror (105) side and focusing objective len (302) light path vertical direction are provided with femto-second laser (101), between described femto-second laser (101) and two-phase look mirror (105), be provided with successively extender lens group (201), collimation lens set (202), the light path of described femto-second laser (101) is through extender lens group (201), after collimation lens set (202), by two-phase look mirror (105) reflection, arrive focusing objective len (302), focus on sample pool (303).
2. a kind of device that utilizes femtosecond laser to prepare Nano diamond according to claim 1, it is characterized in that, the main optical path homonymy of described inverted microscope (300) is provided with imaging device (102), between described imaging device (102) and inverted microscope (300), be provided with successively photo-sensor (305), B lens (204), two-phase look mirror (105), focusing objective len (302), described photo-sensor (305) connects imaging device (102), described two-phase look mirror (105) is positioned at the opposite side of the auxiliary light path of inverted microscope (300), at the contrary beam direction of the auxiliary light path of described inverted microscope (300), be provided with the two-phase look mirror (105) of a miter angle, the transmission from sample pool (303) of the auxiliary light path of described inverted microscope (300) is come and is passed through focusing objective len (302) light beam out by two-phase look mirror (105), after B lens (204), arrive photo-sensor (305), and complete real time imagery in imaging device (102).
3. a kind of device that utilizes femtosecond laser to prepare Nano diamond according to claim 1, is characterized in that, described condensor (301) is: NA=1.2～1.8; Focusing objective len (302) is: the microcobjective of 10x, 20x, 25x; Extender lens group (201): the focal length of left lens is 2cm～5cm, the focal length of right lens is 3cm～7cm; Collimation lens set (202): two focal lengths of lens are 4cm～7cm; B lens (204): the focal length of lens is 4cm～7cm; A lens (205): the focal length of lens is 1cm～2cm.
4. utilize femtosecond laser to prepare a method for Nano diamond, it is characterized in that, method is as follows:
Sample preparation: diamond powder is configured to the aqueous solution of 0.5mol/ml～2mol/ml in sample pool (303) with deionized water, and adds 0.1mol/ml～0.5mol/ml ethylene glycol, as the tensio-active agent of particle;
By the ultrasonic 15min～30min of deionized water for the solution configuring, uniform particles is distributed in solution; Then the nano level precision displacement platform (304) of sample pool (303) being put into inverted microscope (300) Stage microscope in the environment of air is upper, by controlling precision displacement platform (304), realizes the movement on locus to diamond solution in sample pool (303);
The femtosecond laser of femto-second laser (101) of take is main optical path, and the illumination path that the means of illumination (103) of inverted microscope (300) of take sends is auxiliary light path, adjusts main optical path and auxiliary light path, and both light paths are overlapped each other; Femto-second laser (101) pass through focusing objective len (302) vertical focusing in the diamond solution of sample pool (303); The lighting source that means of illumination (103) sends, through condensor (301), makes the diamond solution in sample pool (303) be imaged on photo-sensor (305) through focusing objective len (302);
First close the femtosecond laser of femto-second laser (101), make now as long as the illumination path of the auxiliary light path of means of illumination (103) is radiated at the 2um～10um position, distance sample pool bottom in the diamond solution of sample pool (303), then at the contrary beam direction of illumination path, adopt the two-phase look mirror (105) of a miter angle, from the diamond solution of sample pool (303) transmission is come and carry out separated on space through light beam out of focusing objective len (302) and the light beam of main optical path, through B lens (204), arrive photo-sensor (305), by imaging device (102) to its collection and real time imagery,
Open the femtosecond laser of femto-second laser (101), femtosecond laser arrives focusing objective len (302) by two-phase look mirror (105) reflection after extender lens group (201), collimation lens set (202), focuses in the diamond solution of sample pool (303); Now by the variation of imaging device (102) observation experiment, and by the control of precision displacement platform (304), mobile example pond (303) in two dimensional surface, makes the full and uniform pulverizing of whole diamond in diamond solution;
Femtosecond laser through 15min～60min irradiates, and due to the high pulse energy that femtosecond laser produces, diamond in sample pool (303) is pulverized and is obtained Nano diamond.
5. a kind of method of utilizing femtosecond laser to prepare Nano diamond according to claim 4, is characterized in that, the laser radiation power regulating range of described femto-second laser (101) is 2w～4w, and laser frequency is 100Hz～1100Hz.
6. a kind of method of utilizing femtosecond laser to prepare Nano diamond according to claim 4, it is characterized in that, the femtosecond laser parameter of described femto-second laser (101) is: frequency 800Hz～1100Hz, wavelength is 800nm, pulse width is 35fs～40fs, laser radiation power is 3w, and polarization direction is linear polarization.
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| 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 |
| CN108663387A (en) * | 2018-05-16 | 2018-10-16 | 国家纳米科学中心 | A kind of method that wet etching prepares nano particle TEM sample |
| CN108663387B (en) * | 2018-05-16 | 2021-11-09 | 国家纳米科学中心 | Method for preparing nano-particle TEM sample by wet etching |
| CN109225080A (en) * | 2018-08-24 | 2019-01-18 | 天津大学 | Microballoon controllable preparation and method of operating based on optical tweezer |
| CN109225080B (en) * | 2018-08-24 | 2019-09-13 | 天津大学 | Microballoon controllable preparation and method of operating based on optical tweezer |
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