CN107703169A - A kind of experimental provision of the laser ablation nanostructured monitored in real time - Google Patents
A kind of experimental provision of the laser ablation nanostructured monitored in real time Download PDFInfo
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- CN107703169A CN107703169A CN201611237414.1A CN201611237414A CN107703169A CN 107703169 A CN107703169 A CN 107703169A CN 201611237414 A CN201611237414 A CN 201611237414A CN 107703169 A CN107703169 A CN 107703169A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/36—Removing material
- B23K26/361—Removing material for deburring or mechanical trimming
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Abstract
The present invention discloses a kind of experimental provision of the laser ablation nanostructured monitored in real time, the whole experiment process of disposable progress can be controlled by computer, and video recording can be monitored in experimentation.It is made up of laser, ablation light path, ablation chamber, vacuum drying chamber, tem observation chamber, target control system, TEM sample transportation system, it can be carried out with Experiments of Automatic Control, efficiency high, control is accurate, it is contaminated and aoxidize from sample, and can original position tested.
Description
Technical field
The present invention relates to laser liquid phase ablation to prepare field of nanometer material technology, and is specifically related to a kind of laser monitored in real time
The experimental provision of ablation nanostructured.
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 it is proposed of concept and the development of nanometer technology cause material to be played 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 is widely used so that various science and technology and life device constantly tend to that facilitation multifunction is miniaturized.Make
For a kind of method of new easy preparation nano material, liquid-phase pulse laser ablation has been widely used for preparing various functions
Nano material.
In recent years, the research on being prepared nano material using laser liquid phase ablation is emerged in an endless stream.Someone uses
Laser liquid phase ablation is prepared for a variety of nano materials.Such as：PbS nano particles, ZnO/Zn core shell nanoparticles, Ag/Au cores
Core-shell nanoparticles, Ag/Cu alloy nanoparticles etc..Prepare nano particle using laser liquid phase ablation and can use and continuously swash
Light, pulse laser can also be used to carry out ablation to target.Electronics is carried out using the method for being prepared into TEM sample as ablation is latter
Microscopical sign.But following defect up to the present be present：1) laser liquid phase ablation prepares nanostructured and tested
It is difficult observation in journey；2) prior art can only typically be tested using a kind of zlasing mode, it is impossible in different zlasing modes
Under selected；3) liquid has absorption to laser energy in preparation process, and the energy for causing target to receive is unstable, prior art
It is unable to regulating liquid surface and target face distance；4) existing Preparation equipment can only be typically tested a kind of target, it is impossible to continuous
Ablation is carried out to multiple targets；5) sample after preparing needs manually to be prepared into TEM sample, so not only time-consuming but also can lead
Sample is caused to receive pollution or oxidation in atmosphere；6) it is difficult to carry out experiment in situ after tem observation to prepare TEM sample, and
It is difficult to tested again.
The content of the invention
The present invention overcomes the above insufficient, devises a kind of experiment dress for the experiment in situ of nanoparticles prepared by laser ablation structure
Put, the whole experiment process of disposable progress can be controlled by computer.
A kind of experimental provision of the laser ablation nanostructured monitored in real time, by laser (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 formed, ablation
Connected between chamber (3), vacuum drying chamber (4), tem observation chamber (5) using vacuum valve, it is characterised in that ablation chamber has first
Camera, vacuum drying chamber have second camera, can monitor experimental phenomena in real time；Laser is frequency tripling Solid State Laser
Device, 1064nm, 532nm, 355nm continuous laser can be launched；Ablation light path (2) have spectroscope (201), galvanometer (202),
Mask (203), adjustable lens (204)；Ablation chamber possesses the first air inlet pipeline (301), the first outlet pipe (302), first true
Empty pump (303)；Vacuum drying chamber possesses the second outlet pipe (401), the second vavuum pump (402), molecular pump (403), dry dress
Put (404)；There is tem observation chamber transmission electron microscope (501) ablation sample can be observed；Sample generating means have
There are ablation pond (601) and target control system (602), the built-in ablation liquid in ablation pond, target control system has target lift
Structure, target rotating translation mechanism and target switching mechanism；TEM sample transportation system has sample driven rod (701), sample lifting
Bar (702), sample holder (703)；First camera (304), second camera (405), the control system of all devices are equal
It is connected with control computer to realize control in real time and monitoring.
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 is formed 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 forms 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, have below galvanometer
Mask, the second light path and the 3rd light path is set to export single laser pulse and more laser pulses by galvanometer and mask set.
It is described enter the first air pipe there is 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 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 cylinder of road parallel direction extension, bottom surface has the bracket of installation sample generating means；Ablation chamber and the first air inlet pipeline connect
The relative side of interface has the first outlet pipe, and ablation chamber is pyramidal structure close to described first outlet pipe one end, taper
Structure can be opened with cylindrical structure junction, realize and pick and place sample generating means, and ablation chamber radial contraction extremely goes out with first
Air pipe connects；First outlet pipe connects the first vavuum pump；First camera is arranged in the side wall of ablation chamber.
It is in cube structure to be dried in vacuo outside chamber, and inside is in ellipsoid structure；The drying device of vacuum drying chamber, which has, to be added
Thermal and humidity sensor, the heater are arranged in a focus of vacuum drying chamber ellipsoid structure, humidity sensor
Device is 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；Second camera is arranged in the side wall of vacuum drying chamber.
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 target apart from the distance of liquid level, target
Rotating translation mechanism can control the ablated position of target, and target can be rotated, and target switching mechanism has more
Prism, different targets can be arranged in polygon prism different faces, overturn polygon prism when needed, 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 passes
Bar is sent to 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 the height of vacuum drying intracavitary.
There is tem observation chamber transmission electron microscope ablation sample can be observed, and can record the position of observation
Put；TEM is sent back again using sample driven rod can be used to send back sample after ablation chamber is further handled after tem observation
Original position progress tem observation is directed to after observing chamber.
A kind of method that laser liquid phase ablation test is carried out using above experimental provision.It is characterized in that including following step
Suddenly：
Ablation liquid is prepared, ablation liquid is one 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 after the target of ablation carries out surface polishing, successively in acetone, ethanol, deionized water
Middle ultrasonic cleaning, target is arranged on the multi-prismatic surface of target turning device, opens ablation chamber, ablation pond is arranged on ablation
On the bottom surface of chamber, and fix；
The mobile route of target is set in control computer, upset order, 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, control
Camera video recording processed, and by image real-time display on screen；
Start laser and carry out ablation experiments, ablation makes the TEM sample transportation system clamping TEM that computerizeds control after terminating
Copper mesh is taken out after immersing ablation liquid, and transport to vacuum drying chamber is dried, and transport to tem observation chamber carries out tem observation after drying, together
The interested position of Shi Jilu tem observations；
Control TEM sample transportation system transport TEM copper mesh, which flashes back, loses chamber, and repetition is tested and observed, and preserves video recording.
Using technical scheme, have the advantages that：
1) there is the equipment that laser liquid phase ablation prepares nanostructured camera can be recorded a video with Real Time Observation；2) use more
Kind zlasing mode is tested, and can be selected under different zlasing modes；3) liquid is overcome in preparation process to laser energy
The defects of amount has absorption, and the energy for causing target to receive is unstable, can regulating liquid surface and target face distance；4) equipment can be to a variety of
Target is tested, and continuously can carry out ablation to multiple targets；5) sample after preparing need not manually be prepared into TEM sample,
It is so not only time saving and can protect sample from receive in atmosphere pollution or oxidation；6) TEM sample is prepared by tem observation
After can carry out experiment in situ, and can be tested again.
Brief description of the drawings
Fig. 1 is the single unit system schematic diagram of the experimental provision of nanoparticles prepared by laser ablation structure experiment in situ；
Fig. 2 is the laser 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 of 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.
Embodiment
The technical scheme of invention is completely illustrated below in conjunction with the accompanying drawings.Obviously, described embodiment is only one
Have a try mode, rather than whole embodiments part.According to embodiment, those skilled in the art can be in no creative work
On the premise of obtain other all embodiments, belong to protection scope of the present invention.
Embodiment 1：
As shown in figure 1, a kind of experimental provision of the laser ablation nanostructured monitored in real time, by laser (1), ablation light
Road (2), ablation chamber (3), vacuum drying chamber (4), tem observation chamber (5), sample generating means (6), TEM sample transportation system (7)
Form, connected between ablation chamber (3), vacuum drying chamber (4), tem observation chamber (5) using vacuum valve, it is characterised in that ablation chamber
With the first camera, vacuum drying chamber has second camera, can monitor experimental phenomena in real time；Laser is consolidated for frequency tripling
Body laser, 1064nm, 532nm, 355nm continuous laser can be launched；Ablation light path (2) has 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 tem observation chamber transmission electron microscope (501) ablation sample can be observed；Sample generates
Device has ablation pond (601) and target control system (602), the built-in ablation liquid in ablation pond, and 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)；First camera, second camera, all devices control system with control
Computer connection processed is controlled and monitored to realize in real time.
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 is formed 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 forms 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, have below galvanometer
Mask, the second light path and the 3rd light path is set to export single laser pulse and more laser pulses by galvanometer and mask set.
It is described enter the first air pipe there is 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 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 cylinder of road parallel direction extension, bottom surface has the bracket of installation sample generating means；Ablation chamber and the first air inlet pipeline connect
The relative side of interface has the first outlet pipe, and ablation chamber is pyramidal structure close to described first outlet pipe one end, taper
Structure can be opened with cylindrical structure junction, realize and pick and place sample generating means, and ablation chamber radial contraction extremely goes out with first
Air pipe connects；First outlet pipe connects the first vavuum pump；First camera is arranged in the side wall of ablation chamber.
It is in cube structure to be dried in vacuo outside chamber, and inside is in ellipsoid structure；The drying device of vacuum drying chamber, which has, to be added
Thermal and humidity sensor, the heater are arranged in a focus of vacuum drying chamber ellipsoid structure, humidity sensor
Device is 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；Second camera is arranged in the side wall of vacuum drying chamber.
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 target apart from the distance of liquid level, target
Rotating translation mechanism can control the ablated position of target, and target can be rotated, and target switching mechanism has more
Prism, different targets can be arranged in polygon prism different faces, overturn polygon prism when needed, 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 passes
Bar is sent to 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 the height of vacuum drying intracavitary.
There is tem observation chamber transmission electron microscope ablation sample can be observed, and can record the position of observation
Put；TEM is sent back again using sample driven rod can be used to send back sample after ablation chamber is further handled after tem observation
Original position progress tem observation is directed to after observing chamber.
Embodiment 2：
A kind of method that laser liquid phase ablation test is carried out using above experimental provision.Comprise the following steps：
Ablation liquid is prepared, ablation liquid is one 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 after the target of ablation carries out surface polishing, successively in acetone, ethanol, deionized water
Middle ultrasonic cleaning, target is arranged on the multi-prismatic surface of target turning device, opens ablation chamber, ablation pond is arranged on ablation
On the bottom surface of chamber, and fix；
The mobile route of target is set in control computer as rotation, upset order is turns clockwise, during upset
Between parameter 1 face is overturn per 10min, set the running parameter of laser：1064nm, 10W, choose Investigation of Ablation Mode：It is continuous to burn
Erosion, control camera video recording, and by image real-time display on screen；
Start laser and carry out ablation experiments, ablation makes the TEM sample transportation system clamping TEM that computerizeds control after terminating
Copper mesh is taken out after immersing ablation liquid, and transport to vacuum drying chamber is dried, and transport to tem observation chamber carries out tem observation after drying, together
The interested position of Shi Jilu tem observations；
Control TEM sample transportation system transport TEM copper mesh, which flashes back, loses chamber, repeat step 1-4 observations, preserves video recording.
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 design concept of the present invention is not departed from, ordinary people in the field is to technical scheme
The all variations and modifications made, all should drop into protection scope of the present invention, the scope of the present invention by appended claims and
It is not that described above limits, it is intended that all changes fallen in the implication and scope of the equivalency of claim are included
In the present invention, any reference in claim should not be considered as to the involved claim of limitation.
Claims (8)
- A kind of 1. experimental provision of the laser ablation nanostructured monitored in real time, it is characterised in that including laser, ablation light path, Ablation device, drying device, TEM equipment are formed, and ablation device and drying device can carry out video record.
- 2. a kind of experimental provision of the laser ablation nanostructured monitored in real time as claimed in claim 1, by laser (1), Ablation light path (2), ablation chamber (3), vacuum drying chamber (4), tem observation chamber (5), sample generating means (6), TEM sample transport System (7) is formed, and is connected between ablation chamber (3), vacuum drying chamber (4), tem observation chamber (5) using vacuum valve, its feature exists In ablation chamber has the first camera, and vacuum drying chamber has second camera, can monitor experimental phenomena in real time；Laser For frequency tripling solid laser device, 1064nm, 532nm, 355nm continuous laser can be launched；Ablation light path (2) has spectroscope (201), galvanometer (202), mask (203), adjustable lens (204)；Ablation chamber possesses the first air inlet pipeline (301), the first outlet Pipeline (302), the first vavuum pump (303)；Vacuum drying chamber possesses the second outlet pipe (401), the second vavuum pump (402), divided Sub- pump (403), drying device (404)；There is tem observation chamber transmission electron microscope (501) ablation sample can be seen Examine；Sample generating means have ablation pond (601) and target control system (602), the built-in ablation liquid in ablation pond, target control system System has target elevating mechanism, target rotating translation mechanism and target switching mechanism；TEM sample transportation system has sample transmission Bar (701), sample elevating lever (702), sample holder (703)；The control of first camera, second camera, all devices System is connected with control computer to realize control in real time and monitoring.
- 3. a kind of experimental provision of the laser ablation nanostructured as claimed in claim 2 monitored in real time, it is characterised in that burn Erosion light path has light path selection function, can select the first light path, the second light path and the 3rd light path, first light path is continuous Laser ablation light path, the second light path are single-pulse laser ablation light path, and the 3rd light path is multi-shot laser ablation light path；By laser The laser of device outgoing forms the first light path by the first beam splitter back reflection part, and transmissive portion is through the second beam splitter back reflection portion Point the second light path is formed, transmissive portion is into the 3rd light path；First light path, the second light path, the 3rd light path have electromagnetism control light respectively Switch, the break-make of light path can be controlled；Second light path and the 3rd light path are respectively provided with galvanometer, have mask below galvanometer, by shaking Mirror allows the second light path and the 3rd light path to export single laser pulse and more laser pulses with mask set.
- 4. a kind of experimental provision as claimed in claim 3 for the experiment in situ of nanoparticles prepared by laser ablation structure, its feature Be, it is described enter the first air pipe there is pre-mixing apparatus, ablation chamber is passed through after can gas be mixed by a certain percentage；Premix Attach together and be connected with three gas cylinders before putting, 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 cylinder of parallel direction extension, bottom surface have the bracket of installation sample generating means；Ablation chamber is connected with the first air inlet pipeline Mouthful relative side has the first outlet pipe, and ablation chamber is pyramidal structure close to described first outlet pipe one end, taper knot Structure can be opened with cylindrical structure junction, realize and pick and place sample generating means, ablation chamber radial contraction to the first outlet Pipeline connects；First outlet pipe connects the first vavuum pump；First camera is arranged in ablation chamber side wall.
- 5. a kind of experimental provision of the laser ablation nanostructured as claimed in claim 4 monitored in real time, it is characterised in that true It is in cube structure outside empty drying chamber, inside is in ellipsoid structure；The drying device of vacuum drying chamber has heater and wet Sensor is spent, the heater is arranged in a focus of vacuum drying chamber ellipsoid structure, and humidity sensor is located at vacuum In another focus of drying chamber ellipsoid structure；One the second outlet pipe of tip connection of ellipsoid structure；Second outlet pipe Link the second vavuum pump and the second molecular pump；Second camera is arranged in vacuum drying chamber side wall.
- 6. a kind of experimental provision as claimed in claim 5 for the experiment in situ of nanoparticles prepared by laser ablation structure, its feature It is, the ablation liquid in ablation pond is one kind in deionized water, the solution containing surfactant or colloid to be ablated；Target Material set-up of control system can control target apart from the distance of liquid level, target rotation in ablation pond with target elevating mechanism Translation mechanism can control the ablated position of target, and target can be rotated, and target switching mechanism has polygon prism, Different targets can be arranged in polygon prism different faces, overturn polygon prism when needed, make to need the position of ablation upward.
- A kind of 7. experimental provision of the laser ablation nanostructured as claimed in claim 6 monitored in real time, it is characterised in that TEM sample transportation system has sample holder, a TEM copper mesh specimen can be immersed into ablation liquid；Sample driven rod can be with TEM sample is transmitted back and forth between ablation chamber, vacuum drying chamber and tem observation chamber；Sample lifting platform can adjust TEM copper mesh In ablation chamber and the height of vacuum drying intracavitary.
- A kind of 8. experimental provision of the laser ablation nanostructured as claimed in claim 7 monitored in real time, it is characterised in that There is tem observation chamber transmission electron microscope ablation sample can be observed, and can record the position of observation；Use Sample driven rod can be used to send back sample after ablation chamber is further handled after tem observation and send back tem observation chamber again Afterwards tem observation is carried out for original position.
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