CN106645805B - A method of laser liquid phase ablation test is carried out using laser liquid phase ablation system - Google Patents
A method of laser liquid phase ablation test is carried out using laser liquid phase ablation system Download PDFInfo
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- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
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Abstract
The present invention discloses a kind of method for carrying out laser liquid phase ablation test using laser liquid phase ablation system, and the entire test process of disposable progress can be controlled by computer.Device is made of laser, ablation optical path, ablation chamber, vacuum drying chamber, tem observation chamber, target control system, TEM sample transportation system；Including preparation ablation liquid, preparation ablation target, controlling the movement routine that target is set in computer, overturning sequence, flip-flop transition parameter, set the running parameter of laser, choose Investigation of Ablation Mode, starting laser transports after carrying out ablation experiments, drying to tem observation chamber progress tem observation, the interested position of tem observation is recorded simultaneously, control TEM sample transportation system transport TEM copper mesh flashes back and loses chamber, repeated observation.It can be carried out with Experiments of Automatic Control, high-efficient, control precisely, is contaminated and is aoxidized from sample, and can be tested in situ.
Description
Technical field
The present invention relates to laser liquid phase ablations to prepare field of nanometer material technology, and is burnt more particularly to a kind of using laser liquid phase
The method of erosion system progress laser liquid phase ablation test.
Background technique
Material, the energy and information are acknowledged as three big pillars of modern civilization, support the development of modern civilization.Green wood
The discovery and preparation of material constantly push the reach of science, the progress and the improvement of people's living standards of technology.Nano material
The it is proposed of concept and the development of nanotechnology are so that material plays more in the development and daily life of human civilization
Carry out more extensive and far-reaching influence.The phenomenon of the various novelties continued to bring out in nano materials research enriches the treasured of human knowledge
Library.Nano material is widely used so that various science and technology and life device constantly tend to micromation facilitation multifunction.Make
For a kind of method of the preparation nano material of novel simplicity, liquid-phase pulse laser ablation has been widely used for preparing various functions
Nano material.
In recent years, it emerges one after another about the research using laser liquid phase ablation preparation nano material.Someone uses
Laser liquid phase ablation is prepared for a variety of nano materials.Such as: PbS nano particle, ZnO/Zn core shell nanoparticles, Ag/Au core
Core-shell nanoparticles, Ag/Cu alloy nanoparticle etc..Preparing nano particle using laser liquid phase ablation can be swashed using continuous
Light can also carry out ablation to target using pulse laser.Electronics is generally carried out using the method for being prepared into TEM sample after ablation
Microscopical characterization.But the equipment for up to the present having the following deficiencies: 1) laser liquid phase ablation preparation nanostructure exists
The whole world is different, this causes the parameter fluctuation of laser very big, and the preparation parameter characterization between different experiments room does not have
Uniformity；2) prior art can only generally be tested using a kind of zlasing mode, cannot be carried out under different zlasing modes
Selection；3) liquid has absorption to laser energy in preparation process, causes the received energy of target unstable, the prior art cannot
Regulating liquid surface and target face distance；4) existing Preparation equipment can only generally test a kind of target, cannot be continuously to multiple
Target carries out ablation；5) the sample needs after preparing manually are prepared into TEM sample, not only time-consuming in this way but also will lead to sample
Pollution or oxidation are received in air；6) preparation TEM sample is difficult to carry out experiment in situ after tem observation, and is difficult again
It is secondary to be tested.
Summary of the invention
The present invention overcomes the above deficiency, devise it is a kind of utilize laser liquid phase ablation system carry out laser liquid phase ablation test
Method, can pass through that computer control is disposable to carry out entire test process.
This method includes the experimental provision that assembling is tested in situ for nanoparticles prepared by laser ablation structure first, and device is by swashing
Light device, ablation optical path, ablation chamber, vacuum drying chamber, tem observation chamber, target control system, TEM sample transportation system are constituted,
It is characterized in that, laser is frequency tripling solid laser device, can emit the continuous laser of 1064nm, 532nm, 355nm；Ablation light
Road has light path selector, spectroscope, galvanometer, beam merging apparatus, adjustable lens；Ablation chamber has the first air inlet pipeline, first goes out
Air pipe, the first vacuum pump；Vacuum drying chamber has the second outlet pipe, the second vacuum pump, molecular pump, drying device；TEM is seen
Ablation sample can be observed with transmission electron microscope by examining chamber；There is sample generating means ablation pond and target to control
System, the built-in ablation liquid in ablation pond, target control system have target elevating mechanism, target rotating translation mechanism and target overturning
Mechanism；TEM sample transportation system has sample driven rod, sample lifting platform, sample holder；The control system of all devices is equal
It is connect with control computer.
Ablation optical path has optical path selection function, can choose the first optical path, the second optical path and third optical path, and described first
Optical path is continuous laser ablation optical path, and the second optical path is single-pulse laser ablation optical path, and third optical path is multi-shot laser ablation
Optical path；The first optical path is constituted by the first beam splitter back reflection part by the laser of laser emitting, transmissive portion is through second point
Beam mirror back reflection part constitutes the second optical path, and transmissive portion is at third optical path；First optical path, the second optical path, third optical path difference
With electromagnetism control photoswitch, the on-off of optical path can control；Second optical path and third optical path all have galvanometer, have below galvanometer
Mask allows the second optical path and third optical path to export single laser pulse and more laser pulses by galvanometer and mask set.
It is described that there is pre-mixing apparatus into the first air pipe, ablation chamber is passed through after gas being mixed in a certain ratio；
Gas cylinder there are three connecting before pre-mixing apparatus, three gas cylinders are respectively oxygen cylinder, nitrogen cylinder, argon bottle；Described first
Air inlet pipeline is three sub- air inlet pipelines side by side, and three sub- air inlet pipelines side by side are equidistant in the rear wall of ablation chamber
Distribution, sub- air inlet pipeline is close to the streamlined expansion in the part of ablation chamber；It is in cuboid outside ablation chamber, inside is along air inlet pipe
The cylindrical body that road parallel direction extends, bottom surface have the bracket of installation sample generating means；Ablation chamber and the first air inlet pipeline connect
The opposite side of interface has the first outlet pipe, and ablation chamber is pyramidal structure, taper close to first outlet pipe one end
Structure can be opened with cylindrical structure junction, and realization picks and places sample generating means, and ablation chamber radial contraction extremely goes out with first
Air pipe connection；First outlet pipe connects the first vacuum pump.
Being dried in vacuo is in cube structure outside chamber, and inside is in ellipsoid structure；The drying device for being dried in vacuo chamber, which has, to be added
Thermal and humidity sensor, the heating device are mounted in a focus of vacuum drying chamber ellipsoid structure, humidity sensor
Device is located in another focus of vacuum drying chamber ellipsoid structure；One tip of ellipsoid structure connects the second outlet pipe；The
Two outlet pipes link the second vacuum pump and the second molecular pump.
Ablation liquid in ablation pond is one in deionized water, the solution containing surfactant or colloid to be ablated
Kind；Target set-up of control system in ablation pond there is target elevating mechanism can control distance of the target apart from liquid level, target
Rotating translation mechanism can control the ablated position of target, and can rotate to target, and target turnover mechanism has more
Different targets can be mounted in polygon prism different sides, overturn polygon prism when needed, make the position for needing ablation by prism
Upward.
TEM sample transportation system has sample holder, a TEM copper mesh specimen can be immersed ablation liquid；Sample passes
Send bar that can transmit TEM sample back and forth between ablation chamber, vacuum drying chamber and tem observation chamber；Sample lifting platform can be adjusted
TEM copper mesh is saved in ablation chamber and is dried in vacuo intracavitary height.
There is tem observation chamber transmission electron microscope can observe ablation sample, and can recorde the position of observation
It sets；TEM is sent back again using sample driven rod can be used after tem observation sending back sample after ablation chamber is further processed
Original position progress tem observation is directed to after observing chamber.
A method of laser liquid phase ablation test is carried out using the above experimental provision.It is characterized by comprising following steps
It is rapid:
Ablation liquid is prepared, ablation liquid is one in deionized water, the solution containing surfactant or colloid to be ablated
Kind, ablation pond is added in ablation liquid；
Ablation target is prepared, after the target for needing ablation is carried out surface polishing, successively in acetone, ethyl alcohol, deionized water
Target is mounted on the multi-prismatic surface of target turnover device by middle ultrasonic cleaning, opens ablation chamber, ablation pond is mounted on ablation
On the bottom surface of chamber, and fix；
The movement routine of target, overturning sequence are set in control computer, flip-flop transition parameter sets laser
Running parameter, choose Investigation of Ablation Mode, Investigation of Ablation Mode is continuous ablation, single pulse ablation, one kind of multi-shot ablation kind；
Start laser and carry out ablation experiments, the TEM sample transportation system clamping TEM that computerizeds control is made after ablation
Copper mesh takes out after immersing ablation liquid, transports to vacuum drying chamber drying, transports after dry to tem observation chamber and carry out tem observation, together
The interested position of Shi Jilu tem observation；
Control TEM sample transportation system transport TEM copper mesh, which flashes back, loses chamber, repeats above step and observes again.
Using technical solution of the present invention, have the advantages that
1) equipment of laser liquid phase ablation preparation nanostructure is unified, the parameter and standard of laser；2) a variety of laser are used
Mode is tested, and can be selected under different zlasing modes；3) liquid in preparation process is overcome to have suction to laser energy
It receives, the defect for causing the received energy of target unstable is adjustable liquid level and target face distance；4) equipment can to a variety of targets into
Row test continuously can carry out ablation to multiple targets；5) sample after preparing is without being manually prepared into TEM sample, so not
It is only time saving and sample can be protected from receiving pollution or oxidation in air；6) preparation TEM sample is by can be with after tem observation
Experiment in situ is carried out, and can be tested again.
Detailed description of the invention
Fig. 1 is the single unit system figure for the experimental provision that nanoparticles prepared by laser ablation structure is tested in situ；
Fig. 2 is the laser and ablation optical path for the experimental provision that nanoparticles prepared by laser ablation structure is tested in situ；
Fig. 3 is the sample generating means for the experimental provision that nanoparticles prepared by laser ablation structure is tested in situ；
Fig. 4 is the ablation chamber cross section and longitudinal section for the experimental provision that nanoparticles prepared by laser ablation structure is tested in situ；
Fig. 5 is that the cross section of the vacuum drying chamber for the experimental provision that nanoparticles prepared by laser ablation structure is tested in situ is cut with vertical
Face；
Fig. 6 is the TEM sample transmitting device for the experimental provision that nanoparticles prepared by laser ablation structure is tested in situ.
Specific embodiment
The technical solution of invention is completely illustrated with reference to the accompanying drawing.Obviously, the embodiment is only one
Part is had a try mode, rather than whole embodiments.According to embodiment, those skilled in the art can be in no creative work
Under the premise of obtain other all embodiments, belong to protection scope of the present invention.
Embodiment 1:
As shown in Figure 1, the experimental provision that assembling is tested in situ for nanoparticles prepared by laser ablation structure, by laser, burns
Optical path, ablation chamber, vacuum drying chamber, tem observation chamber, target control system, TEM sample transportation system composition are lost, feature exists
In laser is frequency tripling solid laser device, can emit the continuous laser of 1064nm, 532nm, 355nm；Ablation optical path has
Light path selector, spectroscope, galvanometer, beam merging apparatus, adjustable lens；Ablation chamber have the first air inlet pipeline, the first outlet pipe,
First vacuum pump；Vacuum drying chamber has the second outlet pipe, the second vacuum pump, molecular pump, drying device；Tem observation chamber tool
There is transmission electron microscope that can observe ablation sample；Sample generating means have ablation pond and target control system,
The built-in ablation liquid in ablation pond, target control system have target elevating mechanism, target rotating translation mechanism and target turnover mechanism；
TEM sample transportation system has sample driven rod, sample lifting platform, sample holder；The control system of all devices with control
Computer connection processed.
As shown in Fig. 2, ablation optical path has optical path selection function, the first optical path, the second optical path and third light can choose
Road, first optical path are continuous laser ablation optical path, and the second optical path is single-pulse laser ablation optical path, and third optical path is more arteries and veins
Rush laser ablation optical path；The first optical path, transmissive portions are constituted by the first beam splitter back reflection part by the laser of laser emitting
Lease making the second beam splitter back reflection part constitutes the second optical path, and transmissive portion is at third optical path；First optical path, the second optical path,
Three optical paths are respectively provided with electromagnetism control photoswitch, can control the on-off of optical path；Second optical path and third optical path all have galvanometer, vibration
There is mask below mirror, so that the second optical path and third optical path is exported single laser pulse and is swashed more by galvanometer and mask set
Light pulse.
As shown in figure 4, described have pre-mixing apparatus into the first air pipe, lead to after gas being mixed in a certain ratio
Enter ablation chamber；Gas cylinder there are three connecting before pre-mixing apparatus, three gas cylinders are respectively oxygen cylinder, nitrogen cylinder, argon bottle；
First air inlet pipeline is three sub- air inlet pipelines side by side, rear side of the three sub- air inlet pipelines side by side in ablation chamber
Wall equidistantly distributed, sub- air inlet pipeline is close to the streamlined expansion in the part of ablation chamber；It is in cuboid outside ablation chamber, inside is
The cylindrical body extended along air inlet pipeline parallel direction, bottom surface have the bracket of installation sample generating means；Ablation chamber and first into
The opposite side of air pipe connector has the first outlet pipe, and ablation chamber is taper knot close to first outlet pipe one end
Structure, pyramidal structure can be opened with cylindrical structure junction, realization sample generating means are picked and placed, ablation chamber radial contraction to
The connection of first outlet pipe；First outlet pipe connects the first vacuum pump.
As shown in figure 5, being in cube structure outside vacuum drying chamber, inside is in ellipsoid structure；It is dried in vacuo the drying of chamber
Device has heating device and humidity sensor, and the heating device is mounted on a focus of vacuum drying chamber ellipsoid structure
On, humidity sensor is located in another focus of vacuum drying chamber ellipsoid structure；The tip connection second of ellipsoid structure
Outlet pipe；Second outlet pipe links the second vacuum pump and the second molecular pump.
As shown in figure 3, the ablation liquid in ablation pond is deionized water, the solution containing surfactant or glue to be ablated
One of body；Target set-up of control system in ablation pond there is target elevating mechanism can control target apart from liquid level
Distance, target rotating translation mechanism can control the ablated position of target, and can rotate to target, target tipper
Structure has polygon prism, different targets can be mounted in polygon prism different sides, overturn polygon prism when needed, make to need to burn
The position of erosion is upward.
As shown in fig. 6, TEM sample transportation system has sample holder, a TEM copper mesh specimen can be immersed into ablation
Liquid；Sample driven rod can transmit TEM sample back and forth between ablation chamber, vacuum drying chamber and tem observation chamber；Sample lifting
The adjustable TEM copper mesh of platform is in ablation chamber and is dried in vacuo intracavitary height.
There is tem observation chamber transmission electron microscope can observe ablation sample, and can recorde the position of observation
It sets；TEM is sent back again using sample driven rod can be used after tem observation sending back sample after ablation chamber is further processed
Original position progress tem observation is directed to after observing chamber.
Embodiment 2:
The method for carrying out laser liquid phase ablation test using the above experimental provision.The following steps are included:
Step 1: preparation ablation liquid, ablation liquid are deionized water, the solution containing surfactant or colloid to be ablated
One of, ablation pond is added in ablation liquid；
Step 2: preparation ablation target, by need ablation target carry out surface polishing after, successively in acetone, ethyl alcohol, go
It is cleaned by ultrasonic in ionized water, target is mounted on the multi-prismatic surface of target turnover device, opens ablation chamber, ablation pond is installed
On the bottom surface of ablation chamber, and fix；
Step 3: the movement routine of target is set in control computer as rotation, overturning sequence is to rotate clockwise,
The every 10min of flip-flop transition parameter overturns 1 face, and set the running parameter of laser: 1064nm, 10W choose Investigation of Ablation Mode:
Continuous ablation；
Step 4: starting laser carries out ablation experiments, and TEM sample transportation system of computerizeing control is made after ablation
It is taken out after clamping TEM copper mesh immersion ablation liquid, transport is dry to vacuum drying chamber, and transport to tem observation chamber carries out TEM after drying
Observation, while recording the interested position of tem observation；
Step 5: control TEM sample transportation system transport TEM copper mesh, which flashes back, loses chamber, repeats step 1-4 observation.
Embodiment described above is only that embodiments of the present invention are described, not to design of the invention and
Range is defined.Without departing from the design concept of the invention, ordinary people in the field is to technical solution of the present invention
The all variations and modifications made, should all drop into protection scope of the present invention, the scope of the present invention by appended claims and
It is not that above description limits, it is intended that all changes that come within the meaning and range of equivalency of the claims are included
In the present invention, any reference signs in the claims should not be construed as limiting the involved claims.
Claims (6)
1. a kind of method for carrying out laser liquid phase ablation test using laser liquid phase ablation system, it is characterised in that including following step
It is rapid:
Step 1: preparation ablation liquid, ablation liquid are deionized water, the solution containing surfactant or colloid to be ablated, will be burnt
It loses liquid and ablation pond is added；
Step 2: preparation ablation target, after the target for needing ablation is carried out surface polishing, successively in acetone, ethyl alcohol, deionization
It is cleaned by ultrasonic in water, target is mounted on the multi-prismatic surface of target turnover device, opens ablation chamber, ablation pond is mounted on burning
On the bottom surface for losing chamber, and fix；
Step 3: the movement routine of target, overturning sequence are set in control computer, flip-flop transition parameter sets laser
The running parameter of device, chooses Investigation of Ablation Mode, and Investigation of Ablation Mode is continuous ablation, single pulse ablation, one of multi-shot ablation；
Step 4: starting laser carries out ablation experiments, and TEM sample transportation system clamping of computerizeing control is made after ablation
TEM copper mesh takes out after immersing ablation liquid, transports to vacuum drying chamber drying, transports after dry to tem observation chamber and carry out TEM sight
It examines, while recording the interested position of tem observation；
Step 5: control TEM sample transportation system transport TEM copper mesh, which flashes back, loses chamber, repeats step 1-4 observation；
Further include assembling experimental provision step: described device is by laser (1), ablation optical path (2), ablation chamber (3), vacuum drying
Chamber (4), tem observation chamber (5), sample generating means (6), TEM sample transportation system (7) are constituted, ablation chamber (3), vacuum drying
Between chamber (4), tem observation chamber (5) using vacuum valve connect, laser is frequency tripling solid laser device, can emit 1064nm,
The continuous laser of 532nm, 355nm；Ablation optical path (2) has spectroscope (201), galvanometer (202), mask (203), adjustable lens
(204)；Ablation chamber has the first air inlet pipeline (301), the first outlet pipe (302), the first vacuum pump (303)；Vacuum drying
Chamber has the second outlet pipe (401), the second vacuum pump (402), molecular pump (403), drying device (404)；Tem observation chamber tool
There is transmission electron microscope (501) that can observe ablation sample；Sample generating means have ablation pond (601) and target
Control system (602), the built-in ablation liquid in ablation pond, target control system have target elevating mechanism, target rotating translation mechanism
With target turnover mechanism；TEM sample transportation system has sample driven rod (701), sample elevating lever (702), sample holder
(703)；The target control system (602) connect with control computer；
Ablation optical path has optical path selection function, can choose the first optical path, the second optical path and third optical path, first optical path
For continuous laser ablation optical path, the second optical path is single-pulse laser ablation optical path, and third optical path is multi-shot laser ablation optical path；
The first optical path is constituted by the first beam splitter back reflection part by the laser of laser emitting, transmissive portion is after the second beam splitter
Reflective portion constitutes the second optical path, and transmissive portion is at third optical path；First optical path, the second optical path, third optical path are respectively provided with electricity
Magnetic control photoswitch can control the on-off of optical path；Second optical path and third optical path all have galvanometer, have mask below galvanometer,
The second optical path and third optical path is set to export single-pulse laser and multi-pulse laser by galvanometer and mask set.
2. a kind of method as described in claim 1 for carrying out laser liquid phase ablation test using laser liquid phase ablation system,
It is characterized in that, the first air inlet pipeline has pre-mixing apparatus, and ablation chamber is passed through after gas being mixed in a certain ratio；Premix
Attaching together connection before setting, there are three gas cylinders, and three gas cylinders are respectively oxygen cylinder, nitrogen cylinder, argon bottle；First air inlet
Pipeline is three sub- air inlet pipelines side by side, and three sub- air inlet pipelines side by side equidistantly divide in the rear wall of ablation chamber
Cloth, sub- air inlet pipeline is close to the streamlined expansion in the part of ablation chamber；It is in cuboid outside ablation chamber, inside is along air inlet pipeline
The cylindrical body that parallel direction extends, bottom surface have the bracket of installation sample generating means；Ablation chamber is connect with the first air inlet pipeline
The opposite side of mouth has the first outlet pipe, and ablation chamber is pyramidal structure, taper knot close to first outlet pipe one end
Structure can be opened with cylindrical structure junction, realization sample generating means are picked and placed, ablation chamber radial contraction to the first outlet
Piping connection；First outlet pipe connects the first vacuum pump.
3. a kind of method as claimed in claim 2 for carrying out laser liquid phase ablation test using laser liquid phase ablation system,
It is characterized in that, is in cube structure outside vacuum drying chamber, inside is in ellipsoid structure；The drying device for being dried in vacuo chamber, which has, to be added
Thermal and humidity sensor, the heating device are mounted in a focus of vacuum drying chamber ellipsoid structure, humidity sensor
Device is located in another focus of vacuum drying chamber ellipsoid structure；One tip of ellipsoid structure connects the second outlet pipe；The
Two outlet pipes connect the second vacuum pump and molecular pump.
4. a kind of method as claimed in claim 3 for carrying out laser liquid phase ablation test using laser liquid phase ablation system,
It is characterized in that, the ablation liquid in ablation pond is deionized water, the solution containing surfactant or colloid to be ablated；Target control
System processed is set in ablation pond, and there is target elevating mechanism can control distance of the target apart from liquid level, target rotation translation
Mechanism can control the ablated position of target, and can rotate to target, and target turnover mechanism has polygon prism, can be with
Different targets is mounted in polygon prism different sides, overturns polygon prism when needed, makes to need the position of ablation upward.
5. a kind of method as claimed in claim 4 for carrying out laser liquid phase ablation test using laser liquid phase ablation system,
It is characterized in that, TEM sample transportation system has sample holder, a TEM copper mesh specimen can be immersed ablation liquid；Sample passes
Send bar that can transmit TEM sample back and forth between ablation chamber, vacuum drying chamber and tem observation chamber；Sample elevating lever can be adjusted
TEM copper mesh is saved in ablation chamber and is dried in vacuo intracavitary height.
6. a kind of method as claimed in claim 5 for carrying out laser liquid phase ablation test using laser liquid phase ablation system,
It is characterized in that, there is tem observation chamber transmission electron microscope can observe ablation sample, and can recorde the position of observation
It sets；TEM is sent back again using sample driven rod can be used after tem observation sending back sample after ablation chamber is further processed
Original position progress tem observation is directed to after observing chamber.
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| CN104549292A (en) * | 2015-03-02 | 2015-04-29 | 天津大学 | Technological method for preparing nickel/silicon dioxide supported catalyst by laser liquid phase |
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| CN102701270A (en) * | 2012-06-12 | 2012-10-03 | 天津大学 | Preparation method for colloidal stannic sulfide hollow nanoparticles |
| CN104014800A (en) * | 2014-06-09 | 2014-09-03 | 天津大学 | Preparing method for controllably synthesizing monodisperse active metal nanoparticles through lasers |
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| CN104549292A (en) * | 2015-03-02 | 2015-04-29 | 天津大学 | Technological method for preparing nickel/silicon dioxide supported catalyst by laser liquid phase |
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