CN106903301A - Nanoparticle size control method and realize device - Google Patents
Nanoparticle size control method and realize device Download PDFInfo
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- CN106903301A CN106903301A CN201710019649.1A CN201710019649A CN106903301A CN 106903301 A CN106903301 A CN 106903301A CN 201710019649 A CN201710019649 A CN 201710019649A CN 106903301 A CN106903301 A CN 106903301A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
Abstract
The present invention relates to a kind of nanoparticle size control method and device is realized, by the subpulse number in the pulse envelope for controlling laser, realize the effectively control on a large scale to nano material size.Nano particle preparation facilities is made up of processing equipment device two parts of the adjustable picosecond pulse laser of umber of pulse and computer controls.Pulse laser multi-parameter is adjustable, including subpulse number, laser power, repetition rate；Machinery processing apparatus multi-parameter is adjustable, including vibration mirror scanning mode, processing linear velocity, process time；So as to the nano material for realizing diversified forms is processed.Based on the method, the invention provides a kind of nano material processing unit (plant), this device processing mode is various, can process target material broad covered area, process green non-pollution, the nano material size that is obtained is controllable, surface is pure, and LASER Light Source is full-optical-fiber laser, long-term processing work stabilization, easily meets practical, convenient, stabilization the requirement of industrial system of processing.
Description
Technical field
The present invention relates to a kind of nanometer technology, more particularly to a kind of nanoparticle size based on multiple pulsed light fibre laser
Control method and realize device.
Background technology
Nano particle typically means the particle that particle diameter is 1~100 nanometer, the volume hundred because size is small, shared by surface
Fraction is big, surface atom number, surface energy and tension force are sharply increased with the decline of particle diameter, therefore nano particle has many uniquenesses
Property.The small-size effect of nano-particle（Also referred to as bulk effect）, make its for the properties such as light absorbs, electromagnetism, chemism with
Compared to great changes will take place, the ferromagnetism particle of such as nanoscale can be made into magnetic credit card to common material, using nano material
Low-melting property can reduce the melting condition of metallurgical industry, and then provide New Metallurgical Technology；For another example the surface of nano-particle
Effect, makes some aphlogistic materials at room temperature, and oxidizing fire just can occur in atmosphere after nano particle is prepared as；Receive
The materials such as rice gold can carry biological antibody or medicine carries out targeting therapy for tumor, also can carry out photo-thermal by the aggregation of nano particle
Treatment；Nanoscale Iron, nickel and gamma-iron oxide mixed sintering body can be instead of noble metals as car tail gas purificant --- receive
A variety of characteristics of rice grain cause it to be different from conventional particle at aspects such as calorifics, electricity, optics and catalytic performances, with wide
Application prospect.
At this stage, the preparation method of different nano particles is divided into Physical and chemical method.Common physical preparation method has
Comminuting method, evaporation/sedimentation and hybrid plasma method etc., the material granule that physics prepares method preparation are often large, and particle diameter
Skewness, therefore range of application is relatively limited.Chemical method is prepared including gas phase reaction and liquid phase reactor method etc..Chemical legal system
Standby nano-grain size is controllable, and particle diameter distribution is relatively uniform.But, conventional nano material can be divided into nothing by composition
Machine, organic and composite nanometer particle, for different nano particles, due to the physical chemical differences of raw material, its chemistry system
Preparation Method is different, so preparation method is also varied, without universality.Additionally, the nanometer prepared by chemical method
Material is frequently accompanied by being mixed with chemical by-product in reaction intermediate or the product prepared in building-up process, and is difficult to point
From.This not only has a certain impact to the purity of nano material, and because some raw materials and activating agent for being related in synthesis, deposit
In certain environmental contamination and bio-toxicity, the batch production and application of nano material are limited significantly.
Laser pyrolysis method is a kind of processing method of nano particle developed in recent years, is acted on by Laser Focusing
The processes such as shock wave, the fuel factor that the surface of solids is produced, make atom depart from the surface of solids and then assemble to form nano particle.It is this
Nano particle prepared by method can accomplish pure surface, size tunable, be distributed homogeneous and can stably preserve.
In processing method, a kind of control that laser pyrolysis method is processed to nano particle, mode is by change laser parameter
To realize.Existing adjustable laser parameter is mainly repetition rate, pulse width and pulse power etc., but its problem is also very bright
It is aobvious：The processing efficiency of the main influence particle of change of repetition rate, it is impossible to realize the effect of control particle size；Pulse width pair
Though in nanoparticle size influence it is verified that, due to the different pulse widths from femtosecond to millisecond processing nanometer
The physical mechanism of particle is completely different, therefore pulse width does not have linear influence to become with the corresponding relation of nanoparticle size
Gesture, it is impossible to as effective particle size control condition；It is particle size controlling party the most frequently used at this stage to change pulse energy
Method, but because the processing of nano particle needs pulse energy to exceed certain threshold value, obtained more by reducing pulse power
Small nano particle has significant limitation, and existing the results show is made in water environment by controlling pulse power
Standby particle is general in ten to tens rans, and the nano particle heterogeneity for preparing, size distribution ranges are very big, its scope
It is small then tens nanometers at most to more than 100 nanometers.For this problem, there is research to it is also proposed other improved procedures, such as to
Nanoparticles solution through preparing carries out the secondary operation particle smaller and homogeneous to obtain Size Distribution, but this process work
Sequence is complicated and time-consuming；Also method proposes that the pulsed light for having certain hour difference using two beams carries out processing simultaneously, it is also possible to will
Particle do it is small do even, however it is necessary that two pulsed lights are carried out into room and time synchronization, its system complexity is also evident from.
Also there are many problems in terms of system of processing device, existing laser pyrolysis are to be radiated at same point using laser
Processing mode target is processed, focal spot can be made depression occur for a long time, so as to not only cause laser easily and target
Defocus, the situation for producing particle size inequality, can also be too high because of local particle concentration, increase laser light scattering, the effective light of reduction
Flux, makes processing efficiency be greatly affected.Additionally, existing laser pyrolysis are used mostly the solid state laser of different crystal doping,
Mostly with high costs, maintenance is complicated, is not suitable for the application in the fields such as industrial production.
The content of the invention
The present invention be directed to the problem that nanoprocessing is present, it is proposed that a kind of nanoparticle size control method and realization dress
Put, using the Parameter adjustable of multiple-pulse psec optical fiber laser, there is provided a kind of method that can control nanoparticle size, and
Propose accordingly it is a kind of can be used as the processing unit (plant) for industrially preparing various nano materials.
The technical scheme is that：A kind of nanoparticle size control method based on multiple pulsed light fibre laser, with
Multiple identical subpulses constitute a pulse envelope, and pulse envelope sends in serial fashion, and adjacent pulse envelope time
The laser at the interval more than adjacent subpulse spaced far is referred to as multi-pulse laser, is received in processing using multi-pulse laser focussing force
On the target material of rice grain, contained subpulse number is come receiving after controlling target material to process in controlling to adjust a pulse envelope
Rice grain diameter.
The controllable nanon size granular materials of the processing, including metal, semiconductor, metal oxide, organic polymer,
In biological tissue any one.
The target material for processing nano particle, including in body material, powder, colloid, solution any one.
The target material processing environment for processing nano particle, including the deionization that target material stable existence can be made
In water, the aqueous solution dissolved with solute molecule, organic solution, gaseous environment any one.
Realize the device of the nanoparticle size control method based on multiple pulsed light fibre laser, multiple-pulse is adjustable psec arteries and veins
Rush the multi-pulse laser that laser sends and export a bundle of pulsed laser in spatial light form after optical fiber and collimation lens, warp can be turned over
Tilting mirror enters beam-expanding system, and laser beam, into the galvanometer pair of step motor control, changes beam direction by after beam-expanding system
Again via lens focus, vertical irradiation enters the shuttle of the target material for being placed with processing nano particle, and shuttle is by adjustable
Section three-dimensional sample platform is supported and controlled.
The adjustable picosecond pulse laser multi-parameter of multiple-pulse is adjustable, and adjustable parameter includes that power output is adjustable, repeats
Frequency-adjustable, subpulse number is adjustable.
The beam-expanding system is made up of coaxial placement before and after two panels condenser lens, light beam diameter increase after beam-expanding system.
The galvanometer, by step motor control, makes the light beam can be along X-direction to being made up of the silver completely reflecting mirror of two panels
Uniform rectilinear's scanning is carried out with Y direction both direction, the face on the basis of processing platform is X-axis with the direction of input parallel light
Direction, the direction vertical with input light is Y direction.
The adjustable three-dimensional sample platform carries out the regulation control of 0.01 millimeter of X/Y/Z axles, 1.5 centimetres of precision range, Z axis
It is defined as the direction vertical with processing platform plane.
The beneficial effects of the present invention are：Nanoparticle size control method of the present invention and device is realized, use all -fiber
Structure ensure the long-term working stability of laser, not only reduce cost, safeguard simple and insensitive to environmental disturbances, it is full
Practical, convenient, stabilization the requirement of the industrial system of processing of foot；One kind is provided and effectively controls nanometer by changing subpulse number
The method of particle size, the nano particle that it is prepared is between 2 nanometers to 80 nanometers, and size controlled range is wide, attainable to receive
Rice grain is smaller, and particle homogeneity is more preferable；Propose a kind of multifunctional nanoparticles system based on multi-pulse laser light source
Standby device, wherein, the multiple parameters such as power output, repetition rate, subpulse number of laser are adjustable, are capable of achieving nano material
Different-grain diameter, shape, structure of composite etc., make whole system of processing feature more powerful；In preparation facilities, galvanometer is added
Scanning machining system, Surface scan processing is carried out to target, processes more careful, uniform, and particle is difficult in localized clusters, processing efficiency
It is higher.Processing is directly controlled by computer software users interface, set according to demand machining area and laser plus
Work parameter, more intuitively, conveniently；The nano material preparation system has universality, the target for processing nano particle
Material and machinable material broad covered area, including but not limited to metal, semiconductor, metal oxide, organic polymer, biological group
Knit, etc..Processing environment is various, including but not limited to deionized water, the aqueous solution dissolved with solute molecule, organic solution, gas
Environment.
Brief description of the drawings
Fig. 1 is the pulse train schematic diagram of multi-pulse laser output；
Fig. 2 realizes nanoparticle size control device structural representation for the present invention；
Fig. 3 is the schematic diagram that scanning machining is carried out on Laser Focusing target material of the present invention；
Fig. 4-1 is under having 4 sub- impulsive conditions in pulse envelope of the present invention, in deionized water environment, processing gold nano grain
Transmission electron microscope photo schematic diagram；
Fig. 4-2 is under having 6 sub- impulsive conditions in pulse envelope of the present invention, in deionized water environment, processing gold nano grain
Transmission electron microscope photo schematic diagram；
Fig. 4-3 is under having 8 sub- impulsive conditions in pulse envelope of the present invention, in deionized water environment, processing gold nano grain
Transmission electron microscope photo schematic diagram；
Fig. 4-4 is under having 8 sub- impulsive conditions in pulse envelope of the present invention, in alcoholic environment, to process the saturating of gold nano grain
The sub- microphotographs of radio；
Fig. 5-1 is under having 4 sub- impulsive conditions in pulse envelope of the present invention, in deionized water environment, the nano particle of processing
The statistical results chart of diameter；
Fig. 5-2 is under having 6 sub- impulsive conditions in pulse envelope of the present invention, in deionized water environment, the nano particle of processing
The statistical results chart of diameter；
Fig. 5-3 is under having 8 sub- impulsive conditions in pulse envelope of the present invention, in deionized water environment, the nano particle of processing
The statistical results chart of diameter；
Fig. 5-4 is under having 8 sub- impulsive conditions in pulse envelope of the present invention, in alcoholic environment, the nano-particle diameter of processing
Statistical results chart.
Specific embodiment
Particle size control method of the invention is：By the subpulse number in the pulse envelope for controlling laser, it is right to realize
The effectively control on a large scale of nano material size.Nano particle preparation facilities of the invention is by the adjustable picosecond pulse laser of umber of pulse
Processing equipment device two parts composition of device and computer controls.Pulse laser multi-parameter is adjustable, including：Subpulse number, laser
Power, repetition rate；Machinery processing apparatus multi-parameter is adjustable, including：Vibration mirror scanning mode, processing linear velocity, process time；From
And realize the nano material processing of diversified forms.
The pulse train schematic diagram of multi-pulse laser output as shown in Figure 1, an arteries and veins is constituted with multiple identical subpulses 1
Envelope 2 is rushed, pulse envelope 2 sends in serial fashion, and the time interval of adjacent pulse envelope 2 is much larger than adjacent subpulse 1
The laser at interval is referred to as multi-pulse laser, multi-pulse laser outgoing from laser.Multi-pulse laser has following parameter, Ru Zimai
The time width of punching 1 is 20 psecs, and time interval between adjacent subpulse was 50 nanoseconds, and the time cycle 3 of pulse envelope is
10 microseconds.
The nanoparticle size control device structural representation of multiple pulsed light fibre laser, multiple-pulse are based on as shown in Figure 2
The multi-pulse laser that adjustable picosecond pulse laser 4 sends exports a beam pulse after optical fiber and collimation lens in spatial light form
Laser, beam-expanding system 5 is entered through may be reversed mirror.After laser beam passes through beam-expanding system 5, into the galvanometer pair of step motor control
6, change beam direction and focused on via lens 7 again, vertical irradiation enters shuttle 8, and shuttle 8 is by can adjust three-dimensional sample
Platform 9 is supported and controlled.
The laser includes but is not limited to multiple-pulse adjustable pulse laser.Laser multi-parameter is adjustable, including output
Power adjustable, repetition rate is adjustable, and subpulse number is adjustable.
The beam-expanding system 5 is made up of coaxial placement before and after two panels condenser lens, and front and rear focal length is respectively 10 millimeters and 80
Millimeter, light beam diameter after beam-expanding system 5 is increased to original 8 times.
The galvanometer is made up of to 6 the silver completely reflecting mirror of two panels, by step motor control, makes the light beam can be along X-axis side
To（The face on the basis of processing platform is defined as, the direction with input parallel light）And Y direction（It is defined as with processing platform as base
Quasi- face, the direction vertical with input light）Both direction carries out uniform rectilinear's scanning.
The condenser lens 7 is spherical focusing lens, and focal length is 160 millimeters.
The adjustable three-dimensional sample platform 9 can carry out X/Y/Z axles（Z axis are defined as the direction vertical with processing platform plane）
The regulation control of 0.01 millimeter of precision, 1.5 centimetres of ranges.
The schematic diagram of scanning machining is carried out on Laser Focusing target material as shown in Figure 3, shuttle is 20 milliliters of hyaloids
Product bottle 8, inside fills 4 milliliters of processing environment solution 11, and the bottom level of shuttle 8 one piece of purity of placement is 99.99% cylinder
Proof gold target 12, body diameter is 6 millimeters, is highly 5 millimeters.The focused spot of laser 13 is in the upper surface of proof gold target 12 and sweeps
Processing is retouched, scan mode includes snake scan 14 and zigzag scan 15.
Have in pulse envelope as shown in Figure 4 under different bar number subpulses and different processing environment solution conditions, process Jenner
The transmission electron microscope photo schematic diagram of rice grain, black gray expandable spheric granules is gold nano grain in figure, and engineer's scale is 20
Nanometer.The subpulse number of pulse envelope is respectively in figure：Fig. 4-1 is 4, and Fig. 4-2 is 6, and Fig. 4-3 and Fig. 4-4 is 8
It is individual.The single pulse energy of laser is 5 micro- Jiao in figure, and the overall pulse number of processing is identical（Can be controlled by controlling process time
Overall pulse number processed）.Processing environment solution is respectively in figure：Fig. 4-1, Fig. 4-2 and Fig. 4-3 are deionized water processing environment, Fig. 4-4
It is ethanol processing environment.
Under the conditions of corresponding diagram 4 as shown in Figure 5, the statistical results chart of the nano-particle diameter of processing, in the experiment bar of Fig. 4-1
Under part, the diameter maximum probability of nano particle is distributed in 30 nms as shown in fig. 5-1, successively decreases to both sides respectively, and particle is straight
Footpath overall distribution is in 10-110 nanometers altogether about 100 nanometers of interval ranges wide；Under the experiment condition of Fig. 4-2, such as Fig. 5-2 institutes
Show that the diameter maximum probability of nano particle is distributed in about 10 nms, successively decrease to both sides respectively, particle diameter overall distribution
In 5-35 nanometers altogether about 30 nanometers of interval ranges wide；Under the experiment condition of Fig. 4-3, the nano particle as shown in Fig. 5-3
Diameter maximum probability is distributed in about 4.5 nms, successively decreases to both sides respectively, particle diameter distribution at 2.5-8.5 nanometers altogether
In about 6 nanometers of regional extents wide；The diameter maximum probability of nano particle as shown in Fig. 5-4 is distributed in about 2.5 nms,
Successively decrease to both sides respectively, particle diameter distribution is in 0.5-6.5 nanometers altogether about 6 nanometers of regional extents wide.
Specific procedure of processing is as follows：
1st, first, multiple pulsed light fibre laser 4 is opened；
2nd, machining area is set for the disc of 5 millimeters of diameter, scan mode are snake scan, scanning by computer control software
Speed is 100 mm/seconds；
3rd, the KHz of laser repetition rate 100, the psec of pulse width 20 are set by computer control software, subpulse number sets
4 are set to, power output is set to 2 watts；
4th, the proof gold target removed after surface film oxide is placed in shuttle bottom centre position；Take 4 ml deionized waters note
Enter shuttle；Then shuttle is positioned on adjustable three-dimensional sample stage；
5th, laser shield is opened, regulation makes Laser Focusing focal plane be overlapped with proof gold target upper surface, and processes 60 minutes；Close
Laser shield；
Preserved in the glass sample bottle of 5 milliliters of the solution immigration that the 6th, will be machined, and surface cleaning shuttle and proof gold target
Material surface；
7th, by computer control software, other settings are constant, and subpulse number is set into 6, and power output is set to 3 watts；
Repeat the above steps 4-6, and wherein process time is 40 minutes.
8th, by computer control software, other settings are constant, and subpulse number is set into 8, and power output is set to 4
Watt；
Repeat the above steps 4-6, and wherein process time is 30 minutes.
9th, by computer control software, set constant, the proof gold target removed after surface film oxide is placed in into sample holds
Device bottom centre position；Take ethanol injection shuttle of 4 milliliters of contents more than 99.6%；Then shuttle is positioned over can
Adjust on three-dimensional sample platform；
Repeat the above steps 5-6, and wherein process time is 30 minutes.
The controllable nanon size granular materials of the processing, including but not limited to metal, semiconductor, metal oxide, have
Machine macromolecule, biological tissue.
The target material for processing nano particle, including but not limited to body material, powder, colloid, solution.
The target material processing environment for processing nano particle, including but not limited to deionized water, dissolved with solute point
The aqueous solution, organic solution, the gaseous environment of son.
In method, instant invention overcomes multiple defects that particle is controlled by other laser parameters, first, different from changing
The particle size prepared during change other specification is bigger than normal and distribution of particles is wider, and we control the particle chi prepared by subpulse quantity
Very little minimum 2 nanometers and distribution are less than 10 nanometers；Secondly, subpulse quantity and prepared nanoparticle size are as a result proved
There is good linear relationship；3rd, before only being realized by laser double excitation or secondary processing process could realize
Grain processing effect, the problems such as it also avoid complicated system, complex operation.It is of the invention by solid state laser in terms of processing unit (plant)
Optical fiber laser is improved to, cost is not only reduced, safeguards that simple and operating environment requirements are not high；Meanwhile, for processing side
The problem that efficiency is low, processing particle size is uneven of formula, we add galvanometer scanning system, and carrying out Surface scan to target adds
Work, also substantially increases particle size uniformity and preparation efficiency.This preparation facilities processing mode is various, can process target material covers
Capping is wide, process green non-pollution, and the nano material size for being obtained is controllable, surface is pure, and LASER Light Source is full light
Fibre laser, insensitive to environmental disturbances, high stability LASER Light Source, long-term processing work stabilization easily meets industrial
Practical, convenient, stabilization the requirement of system of processing.
Claims (9)
1. a kind of nanoparticle size control method based on multiple pulsed light fibre laser, it is characterised in that with multiple identicals
Subpulse constitutes a pulse envelope, and pulse envelope sends in serial fashion, and the time interval of adjacent pulse envelope is much larger than
The laser at the interval of adjacent subpulse is referred to as multi-pulse laser, using multi-pulse laser focussing force in the target of processing nano particle
On material, contained subpulse number is come the nano-particle diameter after controlling target material to process in controlling to adjust a pulse envelope.
2. the nanoparticle size control method of multiple pulsed light fibre laser is based on according to claim 1, it is characterised in that
The controllable nanon size granular materials of the processing, including metal, semiconductor, metal oxide, organic polymer, biological tissue
In any one.
3. the nanoparticle size control method of multiple pulsed light fibre laser is based on according to claim 1, it is characterised in that
The target material for processing nano particle, including in body material, powder, colloid, solution any one.
4. the nanoparticle size control method of multiple pulsed light fibre laser is based on according to claim 1, it is characterised in that
It is described for processing the target material processing environment of nano particle, including the deionized water of target material stable existence can be made, dissolved with molten
In the aqueous solution, organic solution, the gaseous environment of matter molecule any one.
5. realize that any one described in Claims 1-4 is based on the nanoparticle size control method of multiple pulsed light fibre laser
Device, it is characterised in that the multi-pulse laser that picosecond pulse laser that multiple-pulse is adjustable sends is through after optical fiber and collimation lens
A bundle of pulsed laser being exported in spatial light form, beam-expanding system is entered through may be reversed mirror, laser beam is by after beam-expanding system, entering
Enter the galvanometer pair of step motor control, change beam direction again via lens focus, vertical irradiation enters to be placed with processes nanometer
The shuttle of the target material of grain, shuttle is supported and controlled by adjustable three-dimensional sample platform.
6. the device of the nanoparticle size control method based on multiple pulsed light fibre laser is realized according to claim 5,
Characterized in that, the adjustable picosecond pulse laser multi-parameter of multiple-pulse is adjustable, adjustable parameter includes that power output is adjustable, weight
Complex frequency is adjustable, and subpulse number is adjustable.
7. the device of the nanoparticle size control method based on multiple pulsed light fibre laser is realized according to claim 5,
Characterized in that, the beam-expanding system is made up of coaxial placement before and after two panels condenser lens, light beam diameter after beam-expanding system increases
Greatly.
8. the device of the nanoparticle size control method based on multiple pulsed light fibre laser is realized according to claim 5,
Characterized in that, the galvanometer the silver completely reflecting mirror of two panels to being made up of, by step motor control, make the light beam can be along X-axis
Direction and Y direction both direction carry out uniform rectilinear's scanning, the face on the basis of processing platform, and the direction with input parallel light is
X-direction, the direction vertical with input light is Y direction.
9. the device of the nanoparticle size control method based on multiple pulsed light fibre laser is realized according to claim 8,
Characterized in that, the adjustable three-dimensional sample platform carries out the regulation control of 0.01 millimeter of X/Y/Z axles, 1.5 centimetres of precision range, Z
Axle is defined as the direction vertical with processing platform plane.
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|---|---|---|---|---|
| CN108893781A (en) * | 2018-07-27 | 2018-11-27 | 国家纳米科学中心 | A method of nanometer monocrystalline particle is prepared using laser beam |
| CN110253027A (en) * | 2019-06-24 | 2019-09-20 | 北京莱泽光电技术有限公司 | Nanometer powder alloy preparation method and device |
| CN113649586A (en) * | 2021-07-12 | 2021-11-16 | 杭州苏铂科技有限公司 | Laser-assisted seedless gold nanostar synthesis method |
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