CN110346390A - The device and method of high flux film preparation and Characterization for Microstructure in situ - Google Patents
The device and method of high flux film preparation and Characterization for Microstructure in situ Download PDFInfo
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- CN110346390A CN110346390A CN201910564205.5A CN201910564205A CN110346390A CN 110346390 A CN110346390 A CN 110346390A CN 201910564205 A CN201910564205 A CN 201910564205A CN 110346390 A CN110346390 A CN 110346390A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20058—Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method
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Abstract
The present invention provides the device and method of a kind of high flux film preparation and Characterization for Microstructure in situ, belongs to the preparation of thin-film material high throughput, micro-nano technology and Characterization for Microstructure technical field.The device includes matrix, laser, laser heater, filming equipment, clamping specimen holder, infrared radiation thermometer, stripping apparatus, Characterization for Microstructure chamber, micro-structure test sample bar, plate, wherein, matrix is placed on the clamping specimen holder of filming equipment, laser, laser heater and infrared radiation thermometer are separately mounted on filming equipment, and filming equipment, stripping apparatus, micro-structure measuring part are successively sequentially connected by plate.The present invention completes the realization of delivered in situ and chamber in vivo functionality by clamping specimen holder and micro-structure test sample bar, influence of the external environmental condition to film performance can utmostly be avoided, the advantage of high flux film technology is played, the structure of high-throughput component and thickness thin film and the changing rule of physical property are precisely obtained.
Description
Technical field
The present invention relates to the preparation of thin-film material high throughput, micro Process and Characterization for Microstructure fields, particularly relate to a kind of high pass
Measure the device and method of film preparation and Characterization for Microstructure in situ.
Background technique
Traditional material scientific research relies primarily on " trial and error " experimental method, in the way of " proposing hypothesis-experimental verification "
Sequential iteration, to constantly approach target material.This method will cause material development and isolate with what is applied, and have low efficiency
Under, control variable the obviously defect such as can not accomplish really to guarantee.Then for shortening R&D cycle and research and development cost, material
Material genome plan is proposed out.2012, China started " material genome " engineering project, it is intended to be prepared by high throughput
The development of technology and iron-enriched yeast technology drives the change of material development mode, greatly improve new material research and development speed, makes
State catches up with and surpasses rapidly the industrial powers such as America and Europe in Material Field.The high Throughput Preparation of mainstream mainly has mask method and coprecipitated at present
Area method, both methods can obtain ingredient or the continuously distributed material of thickness.
Here the principle of Characterization for Microstructure is: the electron beam emitted by electron gun, along mirror body in vacuum passage
Optical axis passes through condenser, it is converged to a branch of uniform electronic beam spot by condenser, is radiated on the indoor sample of sample；Thoroughly
Electron beam after crossing sample carries the structural information of sample interior, and the amount of electrons penetrated at densification in sample is few, and sparse place is saturating
The amount of electrons crossed is more；After the convergence focusing of object lens and electromagnetic lens amplification, it can be seen that can not see under an optical microscope
The clear fine structure less than 0.2um, belongs to angstrom " atom " magnitude, but before testing sample need it is very thin, to allow electronics can be with
It is perforated through film, so needing film to be thinned to by using the mode of ion beam bombardment can be saturating before testing micro-structure
The thickness crossed.
The present apparatus prepares high flux film, thinned and Characterization for Microstructure couples the original that can complete high flux film together
Position Characterization for Microstructure device.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation of high flux film and the devices of Characterization for Microstructure in situ
And method.The present invention obtains the bivariate film of ingredient and thickness change and then clamps specimen holder by particular design
It is then real in incoming Characterization for Microstructure component in situ with micro-structure test sample bar to which in-situ thinning is Characterization for Microstructure sample preparation
Now Characterization for Microstructure in situ.
The device includes matrix, laser, laser heater, filming equipment, clamping specimen holder, infrared radiation thermometer, is thinned
Equipment, Characterization for Microstructure chamber, micro-structure test sample bar, plate, wherein matrix is placed on the clamping specimen holder of filming equipment,
Laser, laser heater and infrared radiation thermometer are separately mounted on filming equipment, and filming equipment, stripping apparatus, micro-structure are surveyed
It tries chamber successively sequentially to connect by plate, micro-structure test sample bar is installed in Characterization for Microstructure chamber.
Wherein:
The filming equipment is located at the surface for being sputtered target position of filming equipment using double target position, matrix.Laser heating
Device acts on the back side of matrix, and heat radiation mode is to be evenly heated.
Detector, liquid gallium source metal, electric field acceleration accessory built in stripping apparatus.Characterization for Microstructure is intracavitary containing Flied emission electricity
Sub- rifle, condenser microscope group, condenser diaphragm, lens isis, constituency diaphragm, accelerating tube, imaging and amplification system.
Clamping specimen holder can be dismantled, and this specimen holder central area sample cell can be dismantled again and be placed in Characterization for Microstructure
On specimen holder, the design of this sample rod-shape is also to complete the key of in-situ thinning and micro-structure test, the article shape of fixed clamp
Shape is tablet, having a size of 10*10mm；Matrix is having a size of 10*10mm, with a thickness of several hundred um.
Plate includes plate one and plate two, and centerboard one connects filming equipment and stripping apparatus, and the connection of plate two subtracts
Thin equipment and Characterization for Microstructure chamber；Stripping apparatus and Characterization for Microstructure chamber maintain vacuum shape all the time by mechanical pump and molecular pump
State.
The application method of the device, comprises the following steps that
S1: substrate matrix cleans up, and matrix is first put into the clamping specimen holder disassembled, then will clamp sample
Bar is put into filming equipment cavity, there is mask plate one and mask plate two in filming equipment cavity, automatically controls mask plate using PLC
One and mask plate two it is mobile, making film sample, horizontally component gradient is distributed, and thickness gradient is distributed in the longitudinal direction；
S2: the film of S1 preparation being distributed with component gradient and thickness gradient passes in situ together with clamping specimen holder
Enter and carry out reduction processing in stripping apparatus, all bombardment is fallen and then is passed in Characterization for Microstructure chamber by substrate, will clamp sample
Thinned film on bar is placed in micro-structure test sample bar using mechanized manner, then the electron beam in Characterization for Microstructure chamber
Emission source launching electronics carry out the characterization of micro-structure to high flux film.
Wherein:
Specific step is as follows by S1:
S11: matrix is successively respectively washed 5 minutes removal surface oils with acetone, dehydrated alcohol in ultrasonic washing instrument
Dirty and impurity dries up matrix surface with nitrogen air gun, then simultaneously clamping in the sample cell of merging clamping specimen holder；
S12: clamping specimen holder in S11 is put into the pulsed laser deposition film coating sputtering cavity of filming equipment together with matrix
In, it is heated using the laser heater irradiation matrix back side, and thermometric is carried out to matrix by infrared radiation thermometer；It is high-throughput thin
Film preparation target position selects A target and B target respectively, and stepper motor one controls target position revolution, and stepper motor two controls mask plate one laterally
It at the uniform velocity moves, stepper motor three controls the movement of the vertical discontinuous of mask plate two, stepper motor one, stepper motor two and stepper motor
Three control progress by PLC program；Laser is sputtered simultaneously.
S13:PLC program setting:
1. initial position A target is in immediately ahead of matrix, matrix is 15mm away from mask plate one, and can be complete along central axis translation
The window one of full fitting mask plate one, two lower edge of mask plate are bonded matrix lower edge completely；
2. opening laser, sputtering parameter is set；Start to bombard A target, while the rapidly moving upward 0.5mm of mask plate two,
Mask plate one at the uniform velocity moves to right simultaneously, and mask plate two is motionless, and mask plate one at the uniform velocity moves 10mm, until matrix right side and mask plate one
When being overlapped on the left of window one, pause movement；The bombardment of B target is turned to, until the continuation of mask plate one at the uniform velocity moves to left 10mm when B target position,
When being overlapped to matrix with the window two of mask plate one, a cycle is completed；
3. laser continues to bombard B target, the rapidly moving upward 0.5mm of mask plate two, while mask plate one at the uniform velocity moves to left 10mm,
When on the left of to matrix with being overlapped on the right side of the window two of mask plate one, pause movement；It is moved to A target, until when A target position, mask plate
One continues at the uniform velocity to move to right 10mm, until completing second period when matrix is overlapped with the window one of mask plate one；
4. recycle 2., 3. in one, two cycles are until the 20th end cycle.
Specific step is as follows by S2:
S21: will clamp specimen holder and be transferred in stripping apparatus with the high flux film prepared by transmission device, sample
Bar in the vertical direction towards constant, be integrally placed on the sample stage of stripping apparatus, downward, substrate is upward for film at this time；
S22: disconnecting the plate one between stripping apparatus and filming equipment, and vacuum is evacuated to lower than after working vacuum, passing through prison
Device is surveyed, substrate is found on sample stage, then fine tuning clamping specimen holder, makes sample be in ion beam current center, and according to subtracting
Thin rate and substrate thickness carry out sample and are thinned；
It is as follows that detailed process is thinned:
S221: then active ions beam window selects click pause after suitable acceleration voltage and line to obtain tpo substrate
Picture；
S222: being dragged to center Screen for characteristic point in ion beam window, chooses entire film regional location, and setting is carved
Dimensional parameters are lost, processing is then performed etching, complete to be thinned；
S23: the film of thinned completion is passed in Characterization for Microstructure chamber together with clamping specimen holder, then passes through machinery
Mode will clamp the detachable sample cell in specimen holder central area and be ejected by the push rod of lower section and be pushed into micro-structure test always
On specimen holder, micro-structure test sample bar has specific shape, and the side of specifically specimen holder is can be with movable similar
The detachably conversion of sample cell can be completed entirely in I-shaped card slot mouth, and by external manipulation, withdraws push rod later,
Clamping specimen holder is drawn back, plate two is closed, after being evacuated to working vacuum, carries out the Characterization for Microstructure measurement of film；
Measurement procedure is as follows:
S231: being moved to region to be measured for micro-structure test sample bar, and target voltage is then arranged, and waits beam
After current stablizes, by adjusting bias adjustment filament emission measure, then open filament finds sample, and sample is moved to
The heart switches MAG mode, and suitable amplification factor is selected under the mode, and adjustment height first adjusts the rate of change of Z value, if sample
Product examine not on positive coke it can be seen that having Bai Ying beside sample, until the profile of shadow and sample itself contour convergence
Then be positive coke；
S232: it after adjustment height, focuses after being inserted into diaphragm.Verting for sample is finally carried out, by observing Kikuchi
Specimen holder is quickly tilted to some orientation by line, contrast of spreading out, electronic diffraction, phase morphology, matrix orientation etc..It is inserted into constituency light bar
Diaphragm, entangles the object phase that need to be analyzed, and adjustment intermediate mirror electric current makes constituency diaphragm edge clear.Object lens electric current is adjusted, is made in constituency
Image is clear, extracts object lens light bar diaphragm out, weakens intermediate mirror electric current, and intermediate mirror object plane is made to move on to object lens back focal plane, fluorescent screen
On can be observed amplification electron diffraction pattern.
The advantageous effects of the above technical solutions of the present invention are as follows:
Filming equipment, stripping apparatus and Characterization for Microstructure equipment are realized three's integration in situ by the device, can be saved
A large amount of time and scientific research cost.The disposable preparation for completing high flux film and Characterization for Microstructure, and completely avoid outer
The influence of bound pair film can play the advantage of high flux film preparation, the relatively microcosmic knot of high flux film in situ to the greatest extent
Structure, to accurately obtain the changing rule of high flux film component and thickness.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of high flux film preparation of the invention and the device of Characterization for Microstructure in situ；
Fig. 2 is high flux film preparation of the invention and the space of the clamping specimen holder of the device of Characterization for Microstructure shows in situ
It is intended to；
Fig. 3 is the micro-structure test sample bar of high flux film preparation of the invention and the device of Characterization for Microstructure in situ
Space schematic diagram；
Fig. 4 is the high flux film thickness of sample of high flux film preparation of the invention and the device of Characterization for Microstructure in situ
With component distributing figure；
Fig. 5 is the Characterization for Microstructure sample cavity knot of high flux film preparation of the invention and the device of Characterization for Microstructure in situ
Structure detail view；
Fig. 6 is high flux film preparation of the invention and the thinned sample of the device of Characterization for Microstructure is transferred to micro- knot in situ
Structure guarantees specimen holder detail view.
Wherein: 1- matrix；2- laser；3- laser heater；4- filming equipment；5- clamps specimen holder；6- infrared measurement of temperature
Instrument；7- stripping apparatus；8- Characterization for Microstructure chamber；9- micro-structure test sample bar；10- plate one；11- plate two.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with attached drawing and tool
Body embodiment is described in detail.
The present invention provides the device and method of a kind of high flux film preparation and Characterization for Microstructure in situ.
As shown in Figure 1, the device include matrix 1, laser 2, laser heater 3, filming equipment 4, clamping specimen holder 5,
Infrared radiation thermometer 6, stripping apparatus 7, Characterization for Microstructure chamber 8, saturating micro-structure test sample bar 9 and plate, wherein matrix 1 is placed in
On the clamping specimen holder 5 of filming equipment 4, laser 2, laser heater 3 and infrared radiation thermometer 6 are separately mounted to filming equipment 4
On, successively sequence is connected by plate for filming equipment 4, stripping apparatus 7, Characterization for Microstructure chamber 8, is installed in Characterization for Microstructure chamber 8
There is micro-structure test sample bar 9.
Wherein, filming equipment 4 is located at the surface for being sputtered target position of filming equipment 4 using double target position, matrix 1.Laser
Heater 3 acts on the back side of matrix 1, and heat radiation mode is to be evenly heated, and be monitored temperature by infrared radiation thermometer 6.
7 built-in scan monitor of stripping apparatus, liquid gallium source metal, electric field acceleration accessory.In the Characterization for Microstructure chamber 8
Containing field emission gun, condenser microscope group, condenser diaphragm, lens isis, constituency diaphragm, accelerating tube, imaging and amplification system.
As shown in Fig. 2, the clamping specimen holder 5 can be dismantled, and this specimen holder central area can dismantle again and be placed in
On Characterization for Microstructure specimen holder, the design of this sample rod-shape is also to complete the key of in-situ thinning and micro-structure test, fixing clamp
The contoured article held is tablet, having a size of 10*10mm；Matrix 1 is having a size of 10*10mm, with a thickness of 100-900um.
Plate includes plate 1 and plate 2 11, and centerboard 1 connects filming equipment 4 and stripping apparatus 7, plate
2 11 connection stripping apparatus 7 and Characterization for Microstructure chamber 8；Stripping apparatus 7 and Characterization for Microstructure chamber 8 are protected by mechanical pump and molecular pump
Hold vacuum state.
Using the method for the device, comprise the following steps that
S1: substrate matrix cleans up, and matrix 1 is first put into the clamping specimen holder 5 disassembled, then will clamp sample
Product bar 5 is put into 4 cavity of filming equipment, is had mask plate one and mask plate two in 4 cavity of filming equipment, is automatically controlled using PLC
Mask plate one and mask plate two are mobile, and making film sample, horizontally component gradient is distributed, and thickness gradient is distributed in the longitudinal direction；
S2: the film of S1 preparation being distributed with component gradient and thickness gradient is passed with clamping specimen holder 5 together original position
Enter and carry out reduction processing in stripping apparatus 6, all bombardment is fallen and then is passed in Characterization for Microstructure chamber 8 by substrate, will clamp sample
Thinned film on product bar 5 is placed in micro-structure test sample bar 9 using mechanized manner, then in Characterization for Microstructure chamber 8
Electron beam emitting source launching electronics carry out the characterization of micro-structure to high flux film.
In practical applications, pulse laser deposition plating equipment bombards target using laser, and substrate is located at laser pulse
Before the target target of deposition and the extended line of mask plate central axis at 15mm.
Film thickness prepared by the method for the present invention and the distribution of ingredient situation, the ingredient consecutive variations illustrated such as Fig. 4 are as follows: at
A content is from 100% → 0 point on the direction film z (towards outside paper), and B content is from 0 → 100%.Thickness steps formula variation: thick
Degree on the direction film y thickness be at the beginning xnm thickness, every 500um improve xnm, finally have 20 thickness steps, from x →
20xnm。
By the high flux film prepared with can clamp together with specimen holder be passed to stripping apparatus in, then looked for by monitor
Quasi- film backing substrate position carries out matrix and is thinned, and when film is thinned to 100nm or less, completes to be thinned.
It by thinned sample and specimen holder can be clamped is passed in Characterization for Microstructure chamber together, wherein characterization cavity configuration details is such as
Then film and entire central area sample cell are transferred on micro-structure test sample bar, micro- knot by Fig. 5 by way of Fig. 6
Design such as Fig. 3 of structure test sample bar completes to turn then by the external stretching clamping sample cell for controlling microstructure sample bar
It changes, then electron beam injects the Characterization for Microstructure for being thinned to and carrying out different zones in 100nm sample below, and whole region is complete
Portion characterizes.
It is explained combined with specific embodiments below.
Step 1: substrate matrix is cleaned up first, matrix is placed in first to be clamped in the sample cell of specimen holder, and one
It rises and is put into pulsed laser deposition filming equipment cavity, there is mask plate one and mask plate two in filming equipment cavity, certainly using PLC
Dynamic control mask plate one and mask plate two are mobile, so that horizontally component gradient is distributed film sample, thickness is terraced in the longitudinal direction
Degree distribution；
Step 1.1: matrix is successively respectively washed 5 minutes removal tables with acetone, dehydrated alcohol in ultrasonic washing instrument
Face greasy dirt and impurity dry up matrix surface with nitrogen air gun, can clamp specimen holder sample trench bottom and side is pasted into conducting resinl,
Matrix is placed in the sample cell of clamping specimen holder and is clinged；
Step 1.2 plated film: by matrix and can clamp specimen holder and be put into pulsed laser deposition film coating sputtering cavity, using swashing
The heating of light device, sets the temperature heating of needs, and detects substrate temperature by infrared radiation thermometer.Target selects A target and B target, point
Not Wei a ingredient and b ingredient, target revolution is controlled using stepper motor one, stepper motor two controls mask plate one and laterally at the uniform velocity moves
Dynamic, stepper motor three controls the movement of the vertical discontinuous of mask plate two, and three's movement is carried out by a PLC program control.Simultaneously
Laser impact target is sputtered.Coating chamber controls vacuum by a mechanical pump and molecular pump.
Step 1.3:PLC program setting:
1. initial position A target is in immediately ahead of matrix, matrix is 15mm away from mask plate one, and can be complete along central axis translation
The window one of full fitting mask plate one, two lower edge of mask plate are bonded matrix lower edge completely；
2. opening laser, sputtering parameter is set；Start to bombard A target, while the rapidly moving upward 0.5mm of mask plate two,
Mask plate one at the uniform velocity moves to right simultaneously, and mask plate two is motionless, and mask plate one at the uniform velocity moves 10mm, until matrix right side and mask plate one
When being overlapped on the left of window one, pause movement；The bombardment of B target is turned to, until the continuation of mask plate one at the uniform velocity moves to left 10mm when B target position,
When being overlapped to matrix with the window two of mask plate one, a cycle is completed；
3. laser continues to bombard B target, the rapidly moving upward 0.5mm of mask plate two, while mask plate one at the uniform velocity moves to left 10mm,
When on the left of to matrix with being overlapped on the right side of the window two of mask plate one, pause movement；It is moved to A target, until when A target position, mask plate
One continues at the uniform velocity to move to right 10mm, until completing second period when matrix is overlapped with the window one of mask plate one；
4. recycle 2., 3. in one, two cycles are until the 20th end cycle.
Step 2: the film being distributed with component gradient and thickness gradient prepared by step 1, together with clamping specimen holder
Reduction processing is carried out in incoming stripping apparatus in situ, all bombardment is fallen and then is passed in Characterization for Microstructure chamber by substrate, will press from both sides
The thinned film held on specimen holder is placed in micro-structure test sample bar using mechanized manner, then in Characterization for Microstructure chamber
Electron beam emitting source launching electronics carry out the characterization of micro-structure to high flux film.
Step 2.1: it will can clamp specimen holder and be transferred in stripping apparatus with the high flux film prepared by transmission, it is whole
Body is placed on the sample stage of stripping apparatus, and downward, substrate is upward for film；
Step 2.2: disconnecting the plate one between stripping apparatus and filming equipment, vacuum is evacuated to lower than after working vacuum, is led to
Monitor is crossed, substrate is found on sample stage, then fine tuning clamping specimen holder, makes sample be in ion beam current center, and root
Sample is carried out according to thinned rate and substrate thickness to be thinned, and it is as follows that detailed process is thinned:
1. then active ions beam window selects click pause after suitable acceleration voltage and line to obtain substrate image；
2. characteristic point is dragged to center Screen in ion beam window, entire film rear surface regions position, setting are chosen
Dimensional parameters are thinned, are then processed, complete to be thinned；
Step 2.3: the film of thinned completion being passed in Characterization for Microstructure chamber together with clamping specimen holder, then passes through machine
The mode of tool will clamp the detachable sample cell in specimen holder central area and be ejected by the push rod of lower section and be pushed into micro-structure always
It characterizes on specimen holder, micro-structure test sample bar has specific shape, as shown in figure 3, the side of specifically specimen holder is
It movable can be similar to I-shaped card slot mouth, and turning for entire detachable sample cell can be completed by external manipulation
It changes, withdraws push rod later, draw back clamping specimen holder, close plate two and carry out the micro-structure table of film after being evacuated to working vacuum
Sign measurement.
Measurement procedure is as follows:
1. micro-structure test sample bar is moved to region to be measured, then target voltage is set, waits beam current
After stabilization, by adjusting bias adjustment filament emission measure, then open filament finds sample, and sample is moved to center, switches
MAG mode, suitable amplification factor is selected under the mode, and adjustment height first adjusts the rate of change of Z value, if sample does not exist
On positive coke, examine it can be seen that having Bai Ying beside sample, until the profile of shadow and sample itself contour convergence are then positive
It is burnt；
2. after adjusting height, focusing after being inserted into diaphragm.Sample is finally carried out to vert, by observation Kikuchi lines,
Specimen holder is quickly tilted to some orientation by contrast, electronic diffraction, phase morphology, the matrix orientation etc. of spreading out.It is inserted into constituency light bar light
Door screen, entangles the object phase to be analyzed, and adjustment intermediate mirror electric current makes constituency diaphragm edge clear.Object lens electric current is adjusted, object in constituency is made
It as clear, extract object lens light bar diaphragm out, weakens intermediate mirror electric current, intermediate mirror object plane is made to move on to object lens back focal plane, on fluorescent screen
The electron diffraction pattern of amplification can be observed.
This covering device and method, can be disposably in situ complete using can specifically clamp specimen holder and micro-structure test sample bar
It is observed at the preparation of high flux film and the transmittance structure of micro-structure, the excellent of high flux film preparation can be played to the greatest extent
Gesture, it is in situ to measure high flux film microstructure features, it finally can accurately obtain the variation of high flux film component and thickness
Rule.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, several improvements and modifications can also be made, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (9)
1. the device of a kind of high flux film preparation and Characterization for Microstructure in situ, it is characterised in that: including matrix (1), laser
(2), laser heater (3), filming equipment (4), clamping specimen holder (5), infrared radiation thermometer (6), stripping apparatus (7), micro-structure
Characterize chamber (8), micro-structure test sample bar (9) and plate, wherein matrix (1) is placed in the clamping specimen holder of filming equipment (4)
(5) on, laser (2), laser heater (3) and infrared radiation thermometer (6) are separately mounted on filming equipment (4), filming equipment
(4), successively sequence is connected by plate for stripping apparatus (7), Characterization for Microstructure chamber (8), is equipped in Characterization for Microstructure chamber (8) micro-
Structured testing specimen holder (9).
2. the device of high flux film preparation according to claim 1 and Characterization for Microstructure in situ, it is characterised in that: described
Filming equipment (4) is located at the surface for being sputtered target position of filming equipment (4) using double target position, matrix (1)；Laser heater
(3) back side of matrix (1) is acted on, heat radiation mode is to be evenly heated, and be monitored temperature by infrared radiation thermometer (6).
3. the device of high flux film preparation according to claim 1 and Characterization for Microstructure in situ, it is characterised in that: described
Detector, liquid gallium source metal, electric field acceleration accessory built in stripping apparatus (7)；Setting Flied emission electricity in Characterization for Microstructure chamber (8)
Sub- rifle, condenser microscope group, condenser diaphragm, lens isis, constituency diaphragm, accelerating tube, imaging and amplification system.
4. the device of high flux film preparation according to claim 1 and Characterization for Microstructure in situ, it is characterised in that: described
Clamping specimen holder (5) can dismantle, and clamping specimen holder (5) central area can dismantle again and be placed in micro-structure test sample bar
(9) on, the contoured article of clamping specimen holder (5) fixed clamp is sheet, having a size of 10*10mm；Matrix (1) is having a size of 10*
10mm, with a thickness of 100-900um.
5. the device of high flux film preparation according to claim 1 and Characterization for Microstructure in situ, it is characterised in that: described
Plate includes plate one (10) and plate two (11), wherein plate one (10) connects filming equipment (4) and stripping apparatus (7), inserts
Plate two (11) connects stripping apparatus (7) and Characterization for Microstructure chamber (8)；Stripping apparatus (7) and Characterization for Microstructure chamber (8) pass through machinery
Pump and molecular pump keep vacuum state.
6. the method for the device of the preparation of application high flux film described in claim 1 and Characterization for Microstructure in situ, feature exist
In: it comprises the following steps that
S1: substrate matrix cleans up, and matrix (1) is first put into the clamping specimen holder (5) disassembled, sample then will be clamped
Product bar (5) is put into filming equipment (4) cavity, has mask plate one and mask plate two in filming equipment (4) cavity, certainly using PLC
Dynamic control mask plate one and mask plate two are mobile, and making film sample, horizontally component gradient is distributed, in the longitudinal direction thickness gradient
Distribution；
S2: in situ incoming together with clamping specimen holder (5) by the film of S1 preparation being distributed with component gradient and thickness gradient
Reduction processing is carried out in stripping apparatus (7), all bombardment is fallen and then is passed in Characterization for Microstructure chamber (8) by substrate, will clamp
Thinned film on specimen holder (5) is placed in micro-structure test sample bar (9) using mechanized manner, then Characterization for Microstructure chamber
(8) the electron beam emitting source launching electronics in carry out the characterization of micro-structure to high flux film.
7. the method for high flux film preparation according to claim 6 and the device of Characterization for Microstructure in situ, feature exists
In:
Specific step is as follows by the S1:
S11: matrix (1) is successively respectively washed 5 minutes removal surface and oil contaminants with acetone, dehydrated alcohol in ultrasonic washing instrument
And impurity, matrix surface is dried up with nitrogen air gun, conducting resinl is pasted into clamping specimen holder (5) sample trench bottom and side, by base
It is clinged in the sample cell of body (1) merging clamping specimen holder (5)；
S12: it is splashed the pulsed laser deposition plated film that specimen holder (5) are put into filming equipment (4) with matrix (1) together is clamped in S11
Penetrate in cavity, using laser heater (3) irradiation the matrix back side heated, and by infrared radiation thermometer (6) to matrix (1) into
Row thermometric；High flux film prepares target position and selects A target and B target in the double target position of filming equipment respectively, and stepper motor one controls target
Position revolution, stepper motor two control mask plate one and laterally at the uniform velocity move, and stepper motor three controls the vertical discontinuous of mask plate two and moves
Dynamic, stepper motor one, stepper motor two and stepper motor three are controlled by PLC program and are carried out；Laser (2) is splashed simultaneously
It penetrates；
S13:PLC program setting:
1. initial position A target is in immediately ahead of matrix (1), matrix (1) is 15mm away from mask plate one, and can along central axis translation
The window one of fitting mask plate one, two lower edge of mask plate are bonded matrix (1) lower edge completely completely；
2. opening laser (2), sputtering parameter is set；Start to bombard A target, while the rapidly moving upward 0.5mm of mask plate two, together
When mask plate one at the uniform velocity move to right, mask plate two is motionless, and mask plate one at the uniform velocity moves 10mm, until matrix (1) on the right side of with mask plate one
Window one on the left of when being overlapped, pause movement；The bombardment of B target is turned to, until the continuation of mask plate one at the uniform velocity moves to left when B target position
10mm, until completing a cycle when matrix (1) is overlapped with the window two of mask plate one；
3. laser continues to bombard B target, the rapidly moving upward 0.5mm of mask plate two, while mask plate one at the uniform velocity moves to left 10mm, until base
When on the left of body (1) with being overlapped on the right side of the window two of mask plate one, pause movement；It is moved to A target, until when A target position, mask plate one
Continuation at the uniform velocity moves to right 10mm, until completing second period when matrix (1) is overlapped with the window one of mask plate one；
4. recycle 2., 3. in one, two cycles are until the 20th end cycle.
8. the method for high flux film preparation according to claim 6 and the device of Characterization for Microstructure in situ, feature exists
In:
Specific step is as follows by the S2:
S21: specimen holder (5) will be clamped and be transferred in stripping apparatus (7) with the high flux film prepared by transmission device, pressed from both sides
Hold specimen holder (5) in the vertical direction towards constant, be integrally placed on the sample stage of stripping apparatus (7), at this time film downward,
Substrate is upward；
S22: disconnecting the plate one (10) between stripping apparatus (7) and filming equipment (4), and vacuum is evacuated to lower than after working vacuum,
By monitor, substrate is found on sample stage, then fine tuning clamping specimen holder (5), makes sample be in ion beam current center,
And sample is carried out according to thinned rate and substrate thickness and is thinned；
S23: the film of thinned completion and clamping specimen holder (5) are passed in Characterization for Microstructure chamber (8) together, then pass through machinery
Mode will clamp the detachable sample cell in specimen holder (5) central area by the ejection of the push rod of lower section and be pushed into micro-structure always
On test sample bar (9), micro-structure test sample bar (9) side be can movable I-shaped card slot mouth, pass through external manipulation
The conversion for completing entire detachable sample cell, withdraws push rod later, draws back clamping specimen holder (5), close plate two (11), wait take out
To working vacuum, the Characterization for Microstructure measurement of film is carried out.
9. the method for high flux film preparation according to claim 8 and Characterization for Microstructure in situ, it is characterised in that:
Thinned detailed process in the S22 is as follows:
S221: then active ions beam window selects click pause after acceleration voltage and line to obtain substrate image；
S222: being dragged to center Screen for characteristic point in ion beam window, chooses entire film rear surface regions position, sets beam
Dimensional parameters are flowed, then carry out that processing is thinned, complete to be thinned；
Measurement procedure is as follows in the S23:
S231: being moved to region to be measured for micro-structure test sample bar (9), and target voltage is then arranged, and waits beam
After current stablizes, by adjusting bias adjustment filament emission measure, then open filament finds sample, and sample is moved to
The heart switches MAG mode, and suitable amplification factor is selected under the mode, and adjustment height first adjusts the rate of change of Z value, if sample
Product examine not on positive coke it can be seen that having Bai Ying beside sample, until the profile of shadow and sample itself contour convergence
Then be positive coke；
S232: after adjustment height, insertion diaphragm is focused, and finally carries out verting for sample, and by observation Kikuchi lines, spread out lining
Contrast, electronic diffraction, phase morphology, matrix orientation, are quickly tilted to some orientation for specimen holder, and orientation depends on the crystal of material
Structure；It is inserted into constituency diaphragm, entangles the object phase that need to be analyzed, adjustment intermediate mirror electric current makes constituency diaphragm edge clear；Adjust object lens
Electric current keeps image in constituency clear, extracts lens isis out, weakens intermediate mirror electric current, so that intermediate mirror object plane is moved on to object lens back burnt
Face is able to observe that the electron diffraction pattern of amplification on fluorescent screen.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111474196A (en) * | 2020-04-16 | 2020-07-31 | 宸鸿科技(厦门)有限公司 | Method for controlling deformation generated by preparation of transmission electron microscope sample |
| CN111910149A (en) * | 2020-07-09 | 2020-11-10 | 杭州电子科技大学 | Preparation method of periodic multi-directional thickness gradient film |
| CN112962068A (en) * | 2021-02-01 | 2021-06-15 | 北京中科泰龙电子技术有限公司 | Preparation device and method of high-flux film |
| CN114481027A (en) * | 2022-01-29 | 2022-05-13 | 中国航空制造技术研究院 | Diamond-like thick film and preparation method thereof |
| CN114918087A (en) * | 2022-04-14 | 2022-08-19 | 重庆理工大学 | Circular tube outer wall coating device |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040056249A1 (en) * | 2001-01-12 | 2004-03-25 | Russell Phillip E. | Chemically enhanced focused ion beam micro-machining of copper |
| CN102002668A (en) * | 2010-09-28 | 2011-04-06 | 大连理工大学 | Polysilicon film low-temperature physical vapor deposition device and method thereof |
| CN105441893A (en) * | 2014-12-04 | 2016-03-30 | 宁波英飞迈材料科技有限公司 | Preparation device and method for high-throughput combined material |
| CN105823908A (en) * | 2016-06-08 | 2016-08-03 | 中国科学院宁波材料技术与工程研究所 | Whole-temperature-range thermoelectric-field transmission electron microscope in-situ sample rod |
| CN205449835U (en) * | 2016-03-18 | 2016-08-10 | 镇江乐华电子科技有限公司 | Detachable vert sample pole and mount |
| CN207300918U (en) * | 2017-07-31 | 2018-05-01 | 中国科学院宁波材料技术与工程研究所 | A kind of chip fixing structure in situ of example of transmission electron microscope bar |
| CN108034928A (en) * | 2017-12-04 | 2018-05-15 | 北京科技大学 | Devices and methods therefor prepared by a kind of film high throughput of controllable tissue |
| CN108183059A (en) * | 2017-12-13 | 2018-06-19 | 中国科学院宁波材料技术与工程研究所 | Transmission electron microscope original position sample club head and the specimen holder with the head |
| CN108385110A (en) * | 2018-04-04 | 2018-08-10 | 西安工业大学 | A kind of burnishing device and polishing method using in-situ sputtering coupled ion beam etching |
| CN109852936A (en) * | 2019-03-19 | 2019-06-07 | 北京科技大学 | High flux film is prepared in situ and in situ to the device and method of micro-nano technology |
-
2019
- 2019-06-26 CN CN201910564205.5A patent/CN110346390A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040056249A1 (en) * | 2001-01-12 | 2004-03-25 | Russell Phillip E. | Chemically enhanced focused ion beam micro-machining of copper |
| CN102002668A (en) * | 2010-09-28 | 2011-04-06 | 大连理工大学 | Polysilicon film low-temperature physical vapor deposition device and method thereof |
| CN105441893A (en) * | 2014-12-04 | 2016-03-30 | 宁波英飞迈材料科技有限公司 | Preparation device and method for high-throughput combined material |
| CN205449835U (en) * | 2016-03-18 | 2016-08-10 | 镇江乐华电子科技有限公司 | Detachable vert sample pole and mount |
| CN105823908A (en) * | 2016-06-08 | 2016-08-03 | 中国科学院宁波材料技术与工程研究所 | Whole-temperature-range thermoelectric-field transmission electron microscope in-situ sample rod |
| CN207300918U (en) * | 2017-07-31 | 2018-05-01 | 中国科学院宁波材料技术与工程研究所 | A kind of chip fixing structure in situ of example of transmission electron microscope bar |
| CN108034928A (en) * | 2017-12-04 | 2018-05-15 | 北京科技大学 | Devices and methods therefor prepared by a kind of film high throughput of controllable tissue |
| CN108183059A (en) * | 2017-12-13 | 2018-06-19 | 中国科学院宁波材料技术与工程研究所 | Transmission electron microscope original position sample club head and the specimen holder with the head |
| CN108385110A (en) * | 2018-04-04 | 2018-08-10 | 西安工业大学 | A kind of burnishing device and polishing method using in-situ sputtering coupled ion beam etching |
| CN109852936A (en) * | 2019-03-19 | 2019-06-07 | 北京科技大学 | High flux film is prepared in situ and in situ to the device and method of micro-nano technology |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111474196A (en) * | 2020-04-16 | 2020-07-31 | 宸鸿科技(厦门)有限公司 | Method for controlling deformation generated by preparation of transmission electron microscope sample |
| CN111474196B (en) * | 2020-04-16 | 2024-01-30 | 宸鸿科技(厦门)有限公司 | Method for controlling deformation generated by sample preparation of transmission electron microscope |
| CN111910149A (en) * | 2020-07-09 | 2020-11-10 | 杭州电子科技大学 | Preparation method of periodic multi-directional thickness gradient film |
| CN112962068A (en) * | 2021-02-01 | 2021-06-15 | 北京中科泰龙电子技术有限公司 | Preparation device and method of high-flux film |
| CN114481027A (en) * | 2022-01-29 | 2022-05-13 | 中国航空制造技术研究院 | Diamond-like thick film and preparation method thereof |
| CN114481027B (en) * | 2022-01-29 | 2023-10-20 | 中国航空制造技术研究院 | Diamond-like thick film and preparation method thereof |
| CN114918087A (en) * | 2022-04-14 | 2022-08-19 | 重庆理工大学 | Circular tube outer wall coating device |
| CN114918087B (en) * | 2022-04-14 | 2023-01-20 | 重庆理工大学 | Coating device for outer wall of circular tube |
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