CN106645805A - Method of carrying out laser liquid phase ablation test by using laser liquid phase ablation system - Google Patents
Method of carrying out laser liquid phase ablation test by using laser liquid phase ablation system Download PDFInfo
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- CN106645805A CN106645805A CN201611237421.1A CN201611237421A CN106645805A CN 106645805 A CN106645805 A CN 106645805A CN 201611237421 A CN201611237421 A CN 201611237421A CN 106645805 A CN106645805 A CN 106645805A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/20—Sample handling devices or methods
Abstract
The invention discloses a method of carrying out a laser liquid phase ablation test by using a laser liquid phase ablation system. A whole test process is controlled once by a computer. An experimental device is constituted by a laser, an ablation optical path, an ablation cavity, a vacuum drying cavity, a TEM observation cavity, a target control system, and a TEM sample conveying system. Ablation liquid is prepared, and an ablation target is prepared, and the moving path, the turning sequence, and the turning time parameter of the target are set in the control computer, and thereafter the working parameters of the laser are set, and then an ablation mode is selected, and in addition, the laser is started for the ablation test, and after drying, the target is conveyed to the TEM observation cavity for TEM observation, and at the same time, the interested position of the TEM observation is recorded, a TEM copper wire mesh is conveyed back to the ablation cavity by controlling a TEM sample conveying system, and observation is repeated. Experiment is carried out automatically, efficiency is high, and control is accurate, and in addition, pollution and oxidation of samples are prevented, and tests can be carried out at an original position.
Description
Technical field
The present invention relates to laser liquid phase ablation prepares field of nanometer material technology, and it is specifically related to a kind of using laser liquid phase burning
The method that erosion system carries out laser liquid phase ablation test.
Background technology
Material, the energy and information are acknowledged as three big pillars of modern civilization, support the development of modern civilization.Green wood
The discovery of material constantly promotes the reach of science, the progress and the improvement of people's living standards of technology with preparing.Nano material
The proposition of concept and the development of nanometer technology cause material to play in the development of human civilization and daily life more
Carry out more extensive and far-reaching influence.The various novel phenomenons continued to bring out in nano materials research enrich the treasured of human knowledge
Storehouse.Nano material widely use so that it is various science and technology and life device constantly tend to miniaturization facilitation multifunction.Make
For a kind of method of new easy preparations nano material, liquid-phase pulse laser ablation has been widely used for preparation various functions
Nano material.
In recent years, the research with regard to being prepared nano material using laser liquid phase ablation is emerged in an endless stream.Someone adopts
Laser liquid phase ablation is prepared for various nano materials.For example：PbS nano particles, ZnO/Zn core shell nanoparticles, Ag/Au cores
Core-shell nanoparticles, Ag/Cu alloy nanoparticles etc..Preparing nano particle using laser liquid phase ablation can be swashed using continuous
Light, it would however also be possible to employ pulse laser carries out ablation to target.Electronics is carried out using the method for being prepared into TEM sample as ablation is latter
Microscopical sign.But up to the present there is following defect：1) equipment of laser liquid phase ablation preparation nanostructured exists
The whole world is different, and this causes the parameter fluctuation of laser very big, and the preparation parameter between different experiments room is characterized not to be had
Uniformity；2) prior art typically can only be tested using a kind of zlasing mode, it is impossible to be carried out under different zlasing modes
Select；3) liquid has absorption to laser energy in preparation process, and the energy for causing target to receive is unstable, and prior art can not
Regulating liquid surface and target face distance；4) existing Preparation equipment typically can only be tested a kind of target, it is impossible to continuous to multiple
Target carries out ablation；5) sample after preparing needs manually to be prepared into TEM sample, so not only time-consuming but also can cause sample
Pollution is received in atmosphere or is aoxidized；6) prepare TEM sample to be difficult after tem observation to carry out experiment in situ, and be difficult again
It is secondary to be tested.
The content of the invention
The present invention overcomes the above not enough, and devise one kind carries out laser liquid phase ablation test using laser liquid phase ablation system
Method, can by computer control disposably carry out whole process of the test.
The method includes first assembling for the experimental provision of nanoparticles prepared by laser ablation structure experiment in situ, and device is by swashing
Light device, ablation light path, ablation chamber, vacuum drying chamber, tem observation chamber, target control system, TEM sample transportation system are constituted, its
It is characterised by, laser instrument is frequency tripling solid laser device, the continuous laser of 1064nm, 532nm, 355nm can be launched；Ablation light
Road has light path selector, spectroscope, galvanometer, beam merging apparatus, adjustable lens；Ablation chamber possesses the first air inlet pipeline, first goes out
Air pipe, the first vavuum pump；Vacuum drying chamber possesses the second outlet pipe, the second vavuum pump, molecular pump, drying device；TEM sees
There is transmission electron microscope ablation sample can be observed to examine chamber；Sample generating means have ablation pond and target control
System, the built-in ablation liquid in ablation pond, target control system has target elevating mechanism, and target rotating translation mechanism and target overturn
Mechanism；TEM sample transportation system has sample driven rod, sample lifting platform, sample holder；The control system of all devices is equal
It is connected with control computer.
Ablation light path has light path selection function, can select the first light path, the second light path and the 3rd light path, and described first
Light path is continuous laser ablation light path, and the second light path is single-pulse laser ablation light path, and the 3rd light path is multi-shot laser ablation
Light path；The first light path, second point of transmissive portions lease making are constituted by the laser of laser emitting through the first beam splitter back reflection part
Beam mirror back reflection part constitutes the second light path, and transmissive portion is into the 3rd light path；First light path, the second light path, the 3rd light path difference
With electromagnetism control photoswitch, the break-make of light path can be controlled；Second light path and the 3rd light path are respectively provided with galvanometer, and galvanometer lower section has
Mask, allows the second light path and the 3rd light path to export single laser pulse and many laser pulses by galvanometer and mask set.
It is described enter the first air pipe there are pre-mixing apparatus, ablation chamber is passed through after can gas be mixed by a certain percentage；
Three gas cylinders are connected with 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 the rear wall of described three sub- air inlet pipelines side by side in ablation chamber is equidistant
Distribution, part streamlined expansion of the sub- air inlet pipeline near ablation chamber；Ablation chamber outside is in cuboid, and inside is along air inlet pipe
The cylinder that road parallel direction extends, bottom surface has the bracket for installing sample generating means；Ablation chamber connects with the first air inlet pipeline
The relative side of interface have the first outlet pipe, ablation chamber near described first outlet pipe one end be pyramidal structure, taper
Structure can be opened with column structure junction, and realization picks and places sample generating means, and ablation chamber radial contraction extremely goes out with first
Air pipe connects；First outlet pipe connects the first vavuum pump.
Vacuum drying chamber outside is in cube structure, and inside is in ellipsoid structure；Vacuum drying chamber drying device have plus
Thermal and humidity sensor, the heater is arranged in a focus of vacuum drying chamber ellipsoid structure, humidity sensor
Device is located in another focus of vacuum drying chamber ellipsoid structure；One the second outlet pipe of tip connection of ellipsoid structure；The
Two outlet pipes link the second vavuum pump and the second molecular pump.
Ablation liquid in ablation pond is in deionized water, the solution containing surfactant or colloid to be ablated
Kind；Target set-up of control system can control distance of the target apart from liquid level, target in ablation pond with target elevating mechanism
Rotating translation mechanism can control the ablated position of target, it is possible to which target is rotated, and target switching mechanism has many
Prism, can when needed overturn polygon prism by different targets on polygon prism not coplanar, make the position for needing ablation
Upward.
TEM sample transportation system has sample holder, a TEM copper mesh specimen can be immersed into ablation liquid；Sample is passed
Bar is sent back and forth to transmit TEM sample between ablation chamber, vacuum drying chamber and tem observation chamber；Sample lifting platform can be adjusted
Height of the section TEM copper mesh in ablation chamber with vacuum drying chamber.
There is transmission electron microscope ablation sample can be observed in tem observation chamber, and can record the position of observation
Put；TEM is sent back again using sample being sent back after ablation chamber is further processed using sample driven rod after tem observation
Observation carries out tem observation behind chamber for original position.
A kind of method that utilization above experimental provision carries out laser liquid phase ablation test.It is characterized in that including following step
Suddenly：
Ablation liquid is prepared, ablation liquid is in deionized water, the solution containing surfactant or colloid to be ablated
Kind, ablation liquid is added into ablation pond；
Prepare ablation target, it would be desirable to which the target of ablation is carried out after the polishing of surface, successively in acetone, ethanol, deionized water
Middle ultrasonic cleaning, target is arranged on the multi-prismatic surface of target turning device, opens ablation chamber, and ablation pond is arranged on into ablation
On the bottom surface in chamber, and fix；
The mobile route of target is set in control computer, upset order, flip-flop transition parameter sets laser instrument
Running parameter, choose Investigation of Ablation Mode, Investigation of Ablation Mode is continuous ablation, single pulse ablation, one kind of multi-shot ablation kind；
Starting laser instrument carries out ablation experiments, and ablation uses computer controls TEM sample transportation system to clamp TEM after terminating
Take out after copper mesh immersion ablation liquid, transport to vacuum drying chamber and be dried, transporting to tem observation chamber after being dried carries out tem observation, together
The interested position of Shi Jilu tem observations；
Control TEM sample transportation system transport TEM copper mesh flashes back and loses chamber, repeats above step and observes again.
Using technical scheme, have the advantages that：
1) laser liquid phase ablation prepares the equipment unification of nanostructured, the parameter and standard of laser；2) using various laser
Pattern is tested, and can be selected under different zlasing modes；3) liquid in preparation process is overcome to have suction to laser energy
Receive, the defect for causing the energy that target is received unstable, can regulating liquid surface and target face distance；4) equipment can enter to various targets
Multiple targets continuously can be carried out ablation by row test；5) sample after preparing need not manually be prepared into TEM sample, so not
Only save time and can protect sample to avoid receiving pollution in atmosphere or aoxidize；6) TEM sample is prepared by can be with after tem observation
Experiment in situ is carried out, and can be tested again.
Description of the drawings
Fig. 1 is the single unit system figure of the experimental provision of nanoparticles prepared by laser ablation structure experiment in situ；
Fig. 2 is the laser instrument and ablation light path of the experimental provision of nanoparticles prepared by laser ablation structure experiment in situ；
Fig. 3 is the sample generating means of the experimental provision of nanoparticles prepared by laser ablation structure experiment in situ；
Fig. 4 is the ablation chamber cross section and longitudinal section of the experimental provision of nanoparticles prepared by laser ablation structure experiment in situ；
Fig. 5 is that the cross section in the vacuum drying chamber of the experimental provision of nanoparticles prepared by laser ablation structure experiment in situ is cut with vertical
Face；
Fig. 6 is the TEM sample transmitting device of the experimental provision of nanoparticles prepared by laser ablation structure experiment in situ.
Specific embodiment
Below in conjunction with the accompanying drawings the technical scheme to inventing carries out complete explanation.Obviously, described embodiment is only one
Part is had a try mode, rather than whole embodiments.According to embodiment, those skilled in the art can be without creative work
On the premise of obtain other all of embodiments, belong to protection scope of the present invention.
Embodiment 1：
As shown in figure 1, assembling the experimental provision for the experiment in situ of nanoparticles prepared by laser ablation structure, by laser instrument, burn
Erosion light path, ablation chamber, vacuum drying chamber, tem observation chamber, target control system, TEM sample transportation system are constituted, and its feature exists
In laser instrument is frequency tripling solid laser device, can launch the continuous laser of 1064nm, 532nm, 355nm；Ablation light path has
Light path selector, spectroscope, galvanometer, beam merging apparatus, adjustable lens；Ablation chamber possess the first air inlet pipeline, the first outlet pipe,
First vavuum pump；Vacuum drying chamber possesses the second outlet pipe, the second vavuum pump, molecular pump, drying device；Tem observation chamber has
There is transmission electron microscope to observe ablation sample；Sample generating means have ablation pond and target control system,
The built-in ablation liquid in ablation pond, target control system has target elevating mechanism, target rotating translation mechanism and target switching 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 light path has light path selection function, the first light path, the second light path and the 3rd light can be selected
Road, first light path is continuous laser ablation light path, and the second light path is single-pulse laser ablation light path, and the 3rd light path is many arteries and veins
Rush laser ablation light path；The first light path, transmissive portions are constituted by the laser of laser emitting through the first beam splitter back reflection part
Lease making the second beam splitter back reflection part constitutes the second light path, and transmissive portion is into the 3rd light path；First light path, the second light path,
Three light paths have respectively electromagnetism control photoswitch, can control the break-make of light path；Second light path and the 3rd light path are respectively provided with galvanometer, shake
Mirror lower section has mask, the second light path and the 3rd light path is exported single laser pulse and is swashed more by galvanometer and mask set
Light pulse.
As shown in figure 4, it is described enter the first air pipe there are pre-mixing apparatus, after can gas be mixed by a certain percentage lead to
Enter ablation chamber；Three gas cylinders are connected with 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 described three sub- air inlet pipelines side by side in ablation chamber
Wall equidistantly distributed, part streamlined expansion of the sub- air inlet pipeline near ablation chamber；Ablation chamber outside is in cuboid, and inside is
Along the cylinder that air inlet pipeline parallel direction extends, bottom surface has the bracket for installing sample generating means；Ablation chamber is entered with first
The relative side of air pipe connector has the first outlet pipe, and ablation chamber is taper knot near described first outlet pipe one end
Structure, pyramidal structure can be opened with column structure junction, realization sample generating means are picked and placeed, ablation chamber radial contraction to
First outlet pipe connects；First outlet pipe connects the first vavuum pump.
As shown in figure 5, vacuum drying chamber outside is in cube structure, inside is in ellipsoid structure；The drying in vacuum drying chamber
Device has heater and humidity sensor, and the heater is arranged on a focus of vacuum drying chamber ellipsoid structure
On, humidity sensor is located in another focus of vacuum drying chamber ellipsoid structure；One tip connection second of ellipsoid structure
Outlet pipe；Second outlet pipe links the second vavuum 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 kind in body；Target set-up of control system can control target apart from liquid level in ablation pond with target elevating mechanism
Distance, target rotating translation mechanism can control the ablated position of target, it is possible to which target is rotated, target tipper
Structure has polygon prism, can when needed overturn polygon prism by different targets on polygon prism not coplanar, makes 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 ablation
Liquid；Sample driven rod can back and forth transmit TEM sample between ablation chamber, vacuum drying chamber and tem observation chamber；Sample is lifted
Platform can adjust height of the TEM copper mesh in ablation chamber with vacuum drying chamber.
There is transmission electron microscope ablation sample can be observed in tem observation chamber, and can record the position of observation
Put；TEM is sent back again using sample being sent back after ablation chamber is further processed using sample driven rod after tem observation
Observation carries out tem observation behind chamber for original position.
Embodiment 2：
The method for carrying out laser liquid phase ablation test using above experimental provision.Comprise the following steps：
Step 1：Ablation liquid is prepared, ablation liquid is deionized water, the solution containing surfactant or colloid to be ablated
In one kind, ablation liquid is added into ablation pond；
Step 2：Prepare ablation target, it would be desirable to the target of ablation is carried out after the polishing of surface, successively in acetone, ethanol, go
It is cleaned by ultrasonic in ionized water, target is arranged on the multi-prismatic surface of target turning device, open ablation chamber, ablation pond is installed
On the bottom surface in ablation chamber, and fix；
Step 3：The mobile route that target is set in control computer is rotation, and upset order is to turn clockwise,
Flip-flop transition parameter overturns 1 face per 10min, sets the running parameter of laser instrument：1064nm, 10W, choose Investigation of Ablation Mode：
Continuous ablation；
Step 4：Starting laser instrument carries out ablation experiments, and ablation uses computer controls TEM sample transportation system after terminating
Take out after clamping TEM copper mesh immersion ablation liquid, transport to vacuum drying chamber and be dried, transporting to tem observation chamber after being dried carries out TEM
Observation, while recording the interested position of tem observation；
Step 5：Control TEM sample transportation system transport TEM copper mesh flashes back and loses chamber, the observation of repeat step 1-4.
Embodiment described above be only embodiments of the present invention are described, not to the present invention design and
Scope is defined.On the premise of without departing from design concept of the present invention, this area ordinary person is to technical scheme
The various modifications made and improvement, all should drop into protection scope of the present invention, and the scope of the present invention is by claims
It is not that described above is limited, it is intended that all changes in the implication and scope of the equivalency of claim that will fall are included
In the present invention, any reference in claim should not be considered as and limit involved claim.
Claims (8)
1. a kind of method that utilization laser liquid phase ablation system carries out laser liquid phase ablation test.It is characterized in that including following step
Suddenly：
Step 1：Ablation liquid is prepared, ablation liquid is in deionized water, the solution containing surfactant or colloid to be ablated
One kind, by ablation liquid ablation pond is added；
Step 2：Prepare ablation target, it would be desirable to which the target of ablation is carried out after the polishing of surface, successively in acetone, ethanol, deionization
It is cleaned by ultrasonic in water, target is arranged on the multi-prismatic surface of target turning device, open ablation chamber, ablation pond is arranged on and is burnt
On the bottom surface in erosion chamber, and fix；
Step 3：The mobile route of target is set in control computer, upset order, 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 kind of multi-shot ablation kind；
Step 4：Starting laser instrument carries out ablation experiments, and ablation is clamped after terminating using computer controls TEM sample transportation system
Take out after TEM copper mesh immersion ablation liquid, transport to vacuum drying chamber and be dried, transporting to tem observation chamber after being dried carries out TEM sights
Examine, while recording the interested position of tem observation；
Step 5：Control TEM sample transportation system transport TEM copper mesh flashes back and loses chamber, the observation of repeat step 1-4.
2. a kind of method that utilization laser liquid phase ablation system as claimed in claim 1 carries out laser liquid phase ablation test, its
It is characterised by：Also include assembling experimental provision step：Described device contain laser instrument (1), ablation light 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),
Connected using vacuum valve between vacuum drying chamber (4), tem observation chamber (5), it is characterised in that laser instrument swashs for frequency tripling solid
Light device, can launch the continuous laser of 1064nm, 532nm, 355nm；Ablation light path (2) is with spectroscope (201), galvanometer
(202), mask (203), adjustable lens (204)；Ablation chamber possess the first air inlet pipeline (301), the first outlet pipe (302),
First vavuum pump (303)；Vacuum drying chamber possess the second outlet pipe (401), the second vavuum pump (402), molecular pump (403),
Drying device (404)；There is transmission electron microscope (501) ablation sample can be observed in tem observation chamber；Sample is generated
Device has ablation pond (601) and target control system (602), and the built-in ablation liquid in ablation pond, target control system has target
Elevating mechanism, target rotating translation mechanism and target switching mechanism；TEM sample transportation system has sample driven rod (701), sample
Product elevating lever (702), sample holder (703)；The control system of all devices is connected with control computer.
3. a kind of method that utilization laser liquid phase ablation system as claimed in claim 2 carries out laser liquid phase ablation test, its
It is characterised by that ablation light path has light path selection function, can selects the first light path, the second light path and the 3rd light path, described first
Light path is continuous laser ablation light path, and the second light path is single-pulse laser ablation light path, and the 3rd light path is multi-shot laser ablation
Light path；The first light path, second point of transmissive portions lease making are constituted by the laser of laser emitting through the first beam splitter back reflection part
Beam mirror back reflection part constitutes the second light path, and transmissive portion is into the 3rd light path；First light path, the second light path, the 3rd light path difference
With electromagnetism control photoswitch, the break-make of light path can be controlled；Second light path and the 3rd light path are respectively provided with galvanometer, and galvanometer lower section has
Mask, allows the second light path and the 3rd light path to export single laser pulse and many laser pulses by galvanometer and mask set.
4. a kind of method that utilization laser liquid phase ablation system as claimed in claim 3 carries out laser liquid phase ablation test, its
Be characterised by, it is described enter the first air pipe there are pre-mixing apparatus, ablation chamber is passed through after can gas be mixed by a certain percentage；
Three gas cylinders are connected with 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 the rear wall of described three sub- air inlet pipelines side by side in ablation chamber is equidistant
Distribution, part streamlined expansion of the sub- air inlet pipeline near ablation chamber；Ablation chamber outside is in cuboid, and inside is along air inlet pipe
The cylinder that road parallel direction extends, bottom surface has the bracket for installing sample generating means；Ablation chamber connects with the first air inlet pipeline
The relative side of interface have the first outlet pipe, ablation chamber near described first outlet pipe one end be pyramidal structure, taper
Structure can be opened with column structure junction, and realization picks and places sample generating means, and ablation chamber radial contraction extremely goes out with first
Air pipe connects；First outlet pipe connects the first vavuum pump.
5. a kind of method that utilization laser liquid phase ablation system as claimed in claim 4 carries out laser liquid phase ablation test, its
It is characterised by, vacuum drying chamber outside is in cube structure, inside is in ellipsoid structure；Vacuum drying chamber drying device have plus
Thermal and humidity sensor, the heater is arranged in a focus of vacuum drying chamber ellipsoid structure, humidity sensor
Device is located in another focus of vacuum drying chamber ellipsoid structure；One the second outlet pipe of tip connection of ellipsoid structure；The
Two outlet pipes link the second vavuum pump and the second molecular pump.
6. a kind of method that utilization laser liquid phase ablation system as claimed in claim 5 carries out laser liquid phase ablation test, its
It is characterised by, the ablation liquid in ablation pond is in deionized water, the solution containing surfactant or colloid to be ablated
Kind；Target set-up of control system can control distance of the target apart from liquid level, target in ablation pond with target elevating mechanism
Rotating translation mechanism can control the ablated position of target, it is possible to which target is rotated, and target switching mechanism has many
Prism, can when needed overturn polygon prism by different targets on polygon prism not coplanar, make the position for needing ablation
Upward.
7. a kind of method that utilization laser liquid phase ablation system as claimed in claim 6 carries out laser liquid phase ablation test, its
It is characterised by, TEM sample transportation system has sample holder, a TEM copper mesh specimen can be immersed ablation liquid；Sample is passed
Bar is sent back and forth to transmit TEM sample between ablation chamber, vacuum drying chamber and tem observation chamber；Sample lifting platform can be adjusted
Height of the section TEM copper mesh in ablation chamber with vacuum drying chamber.
8. a kind of method that utilization laser liquid phase ablation system as claimed in claim 7 carries out laser liquid phase ablation test, its
It is characterised by, there is transmission electron microscope ablation sample can be observed in tem observation chamber, and can record the position of observation
Put；TEM is sent back again using sample being sent back after ablation chamber is further processed using sample driven rod after tem observation
Observation carries out tem observation behind chamber for original position.
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| CN102701270A (en) * | 2012-06-12 | 2012-10-03 | 天津大学 | Preparation method for colloidal stannic sulfide hollow nanoparticles |
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| CN204182917U (en) * | 2014-10-10 | 2015-03-04 | 北京工业大学 | A kind of pulse laser liquid phase ablation that adopts prepares nano-structured device |
| 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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