CN106872246A - A kind of device and method for fission track chemical etching - Google Patents
A kind of device and method for fission track chemical etching Download PDFInfo
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- CN106872246A CN106872246A CN201710045131.5A CN201710045131A CN106872246A CN 106872246 A CN106872246 A CN 106872246A CN 201710045131 A CN201710045131 A CN 201710045131A CN 106872246 A CN106872246 A CN 106872246A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The present invention relates to a kind of device and method for fission track chemical etching, equipment includes thermostat, sample filling device, discharge mechanism, device and operating system.The present invention utilizes temperature control unit, including temperature sensor, semiconductor thermostat and valve unit to realize the constant temperature etching of fission track；Realize that sample is mounted and dismounted automatically using sample filling and discharge mechanism；By drive device, including pressure sensor, timing completes Sample Etch and cleaning.Present invention configuration operating system, can need adjustment etching period, etch temperature and sample size according to experiment, realize the automation of fission track chemical etching.Compared with prior art, security of the present invention is more preferable, etching efficiency is higher, etching period control is more accurate.
Description
Technical field
The present invention relates to the research field of hot chronology fission track method, specifically, it is related to a kind of for footpath of fissioning
The device and method of mark chemical etching.
Background technology
Hot chronology be output using the fission or decay constant of radioactive element in mineral in mineral and accumulation come
Isotopic geological age is explained, the theory and research method of geologic process Temperature-time track is quantitatively given, can be taken off
Show the ripe hydrocarbon history of hydrocarbon source rock and the position of " hydrocarbon source stove " and its made in the transition process in earth history period, quantitative analysis
Mountain belts constructs uplift processes, research Hydrothermal Deposits process etc..Conventional method has U-Pb methods, (U-Th)/He methods, fission-track method
Deng.
The formation of fission track is built upon238On the basis of U nuclear fissions,238U fissions can form two close height of quality
Can positive charge fragment, and do reverse high-speed motion and inject in solid insulation (apatite/zircon), because same sex electric charge is mutually arranged
Reprimand, the atom of solid insulation positively charged can leave original position and reach new balance, can be produced so in mineral lattice
One strong disturbance region, this radiation injury area is referred to as Latent track.Under natural conditions, the Latent track in solid insulation is difficult
Accurately observed and counted.The width of Latent track isOnly with electron microscope just it is observed that, through change
Learning engraving method can be expanded to observable scope (1-2 μm) by track widths, the use of light microscope be that observable is measured, this
Plant and be referred to as fission track by the track after chemical etching.Fission track shows Track density reduction, length as temperature is raised
The feature for reducing is spent, is referred to as annealed.Set up relation (the annealing mould of fission-track annealing rate, annealing temperature and annealing time three
Type), can be used to recover the thermal history of stratum experience where apatite/zircon.
In the prior art, etching solution is strong acid, and the etching solution of such as Apatite fission track chemical etching is mainly
The dense HNO of 5.5mol/L3.Specific etching operation is (by taking apatite as an example)：Inject a certain amount of 5.5mol/L's in beaker
HNO3, beaker is placed in the water bath (large beaker) that temperature is 21 ± 0.5 DEG C, using tweezers gripping sample immersion etching solution
In, and manual time-keeping is used, and sample is taken out after etching 20s is placed in being cleaned in deionized water, get rid of sample surfaces
HNO3Drying for standby after solution.Dense HNO3It is strong oxidizer, most metals and material can be corroded, pollutes skin or eyes
After can cause third-degree burn, in existing etching technique, experimenter and dense HNO3Time of contact is long, and operational hazards are big, Er Qietong
The time control error for crossing stopwatch and the manual timing of tweezers and etching is larger, and it is excessive that timing can excessively cause fission track to etch
(overetch), crosses undercut (underetching) at least, has a strong impact on the observation statistical work of later stage fission track.Due to etching process
In, dense HNO3Being reacted with sample can produce heat, cause etching solution temperature to raise, it is necessary to by etching solution temperature modulation in fact
Testing temperature can just proceed etching, and this process needs to take considerable time.
The content of the invention
Regarding to the issue above, the present invention provides a kind of device and method for fission track chemical etching.Set using this
Standby and method can quickly realize being fully etched for fission track, and personnel not damaged.
The technical solution used in the present invention is as follows：A kind of equipment for fission track chemical etching, it is characterised in that：
Including thermostat, sample drive device and operating system；
The thermostat includes a water containing pool, and pond is built with deionized water, while being provided with valve unit in pond, partly leading
Body thermostat, temperature sensor and etching ware, equipped with etching solution and being placed with thermometer in etching ware, the deionized water and erosion
Liquid is carved not mix mutually；
The sample drive device includes a support, and a motor, the motor drive connection are installed on support
One armed lever, makes the armed lever be rotated in vertical plane；The armed lever end connects a mold, the mold built with
Etched sample, the mold rotates with the armed lever, in the turnover deionized water and in etching solution；
The sample drive device also includes two pressure sensors, and one is placed in and can sense that the mold is complete
The full position in etching solution, another be placed in can sense the mold be completely in water in position；
The operating system includes all in controller, display screen, function key, instrument, operating system and the equipment
Electrical part is electrically connected.
Further, the equipment also includes sample filling device, and the sample filling device includes that sample stage, first drive
Dynamic motor, the second motor, the 3rd motor, filling bar, filling fixture；The sample stage is driven by the first motor
Rotate in the horizontal plane, while driven by the second motor translating in the horizontal plane, the filling of the 3rd motor drive connection
Bar, makes the filling bar can be with horizontal extension；Filling fixture is placed on sample stage, filling fixture, institute are pointed in the front of the filling bar
Patch and etched sample is stated to be previously placed in groups in filling fixture, sample in preceding, patch rear, when the mold and filling
When fixture is relative, the filling bar is by patch and etched sample propulsion mold.
Yet further, there are multiple parallel standing grooves on the filling fixture, one group of plug is placed in each standing groove
Piece and etched sample；The sample stage translates a distance for placement well width every time in the horizontal plane, filling bar gradually will
Patch and etched sample in each standing groove are released；
The mold accordingly also has multiple draw-in grooves, and one group of patch and etched sample can be placed in each draw-in groove,
The patch blocks etched sample.
Yet further, the mold is a dish type, uniform multiple draw-in groove on disk；The mold is driven by one
Motor is rotated, and the mold rotates through a distance for draw-in groove every time.
Further, the equipment also includes sample discharge mechanism, and the sample discharge mechanism includes sample stage, 4 wheel driven
Dynamic motor, the 5th motor, discharge arm, sample box, patch box, Electrical heads；4th motor drives sample stage to exist
Rotation, is placed with sample box and patch box in horizontal plane on the sample stage；The 5th motor drive connection discharge arm, makes
Discharge arm stretches in the horizontal direction, and the unloading boom end connection Electrical heads, the Electrical heads are powered and can draw the etching
Patch on mould.
The present invention also provides a kind of engraving method of the application equipment, briefly, comprises the following steps：
1) parameter setting, Preparatory work of experiment
Before etching experiment starts, need to carry out the setting of experiment parameter in an operating system according to experiment, including etching temperature
Degree, etching period, scavenging period, filling sample number and testing time, etching solution is dense HNO3；
After setting parameter, thermostat brings into operation；Prepare sample simultaneously；
2) sample filling
After etching solution temperature reaches setting value and stabilization, sample filling is carried out to the mold；
3) Sample Etch
Start motor, rotate armed lever, mold is rotated into etching solution, armed lever and one of pressure sensing
Device contact and start recording etching period, after etching period is reached, are again started up motor and drive mold to leave at once
Etching solution, is immersed in deionized water, carries out sample clean, while armed lever and another pressure sensor contacts and start recording
Scavenging period；
4) sample unloading
After the completion of cleaning, motor drives mold to leave deionized water, reaches unloading position, is unloaded.
Further, when sample is loaded, the sample stage in rotary sample filling device makes filling fixture reach filling position
Put, first group of sample and patch are directed at the mold and filling bar simultaneously, promote filling bar by first group of sample and patch
Simultaneously in push-in mold；Then motor drives sample stage and filling fixture to translate a distance for standing groove, while
Rotate the mold and turn over a distance for draw-in groove, make next group of sample and patch etched in alignment mould and filling bar, then
It is secondary to promote filling bar by second group of sample and patch simultaneously push-in mold；The like, complete the filling of all samples；
Then, motor drives sample stage and filling fixture to produce loading position, Sample Etch process described in without prejudice to.
Yet further, when sample is unloaded, the sample stage in the sample discharge mechanism is rotated, reaches discharge arm and unload
Carry position relative with the mold, then drive discharge arm to stretch out, draw a patch in the mold, then
Rotating the mold carries out the unloading of next patch, now goes up the corresponding sample of patch because losing the stop of patch
Simultaneously again because of Action of Gravity Field, slide and enter in sample box；Repeat the above steps, until completing the unloading of sample.
Etch temperature as 21 ± 0.5 DEG C is set in methods described, etching period is 20s, and scavenging period is 1min.
Compared with prior art, the present invention has advantages below：
1. safer.The present invention can farthest reduce the time of experimenter and the close contact of etching solution, dress
Put using safer.
2. more efficiency.The present invention can simultaneously carry out the etching experiment of multiple samples, significantly improve etching efficiency.Meanwhile,
The thermostat that the present invention is provided can make etching solution temperature stabilization in experiment allowed band with Quick temperature adjustment, save significantly
The temperature adjustment time is saved.
3. more accurate.The present invention realizes etching experiment mechanized operation, and etching period is finely controlled, it is ensured that each
There is sample identical to etch degree.
Other features and advantages of the present invention will illustrate in the following description, and partial become from specification
It is clear that or being understood by implementing the present invention.
Brief description of the drawings
Fig. 1 is fission track Etaching device schematic diagram.
Fig. 2 is the right side view that fission track Etaching device presses Fig. 1.
Fig. 3 is filling fixture structure figure.
Fig. 4 is mold structure chart.
Specific embodiment
By taking Apatite fission track etching as an example, embodiments of the present invention are described in detail with reference to the accompanying drawings.
As shown in Figure 1 and Figure 2, the fission track chemical etching device that the present invention is provided includes：Thermostat 1, sample is loaded
Device 2, sample discharge mechanism 3, sample drive device 4 and operating system 5.
Thermostat 1 includes a water containing pool 11, deionized water is full of in pond, while water proof is provided with valve unit in pond
12nd, semiconductor thermostat 13, temperature sensor 14, etching ware 15 (built-in etching solution 16) and thermometer 17.
Water containing pool 11 is made up of heat-barrier material, can play insulation effect, and temperature sensor 14 is used to monitor deionized water
Temperature, it is ensured that water temperature is identical with the temperature of etching solution 16, and deionized water is heated or cooled by semiconductor thermostat 13
Come that keeping temperature is constant, the agitation deionized water of valve unit 12 accelerates the diffusion of temperature, makes water and etching solution temperature Fast-Balance.
Water level in device is higher than etching solution, but is below etching the upper edge of ware 15.
Sample filling device 2 is located at the side of thermostat 1, including sample stage 21, the first motor 22, second drive
Motor 23, the 3rd motor 24, filling bar 25, filling fixture 26, patch 6 and etched sample 7 are placed in advance in loading fixture 26
In.
The horizontal positioned of sample stage 21, is driven and can be rotated in the horizontal plane, by the second motor by the first motor 22
23 are driven and can translate in the horizontal plane, and filling fixture 26 is placed on sample stage 21, and the drive connection of the 3rd motor 24 filling
Bar 25, allows filling bar 25 flexible in sample stage upper horizontal, and filling fixture 26 is pointed in the front for loading bar 25.Filling fixture
Standing groove is provided with 26, patch 6 and etched sample 7 can be one in front and one in back placed in standing groove.First motor 22 drives
In 0 ° and 90 ° of two stations conversions, when sample is loaded, sample stage 21 can rotate to loading position (against sample to sample stage 21
The position of mold 45 in drive device 4, sees below and chats), the 3rd motor 24 promotes filling bar 25, further promotes filling
Patch 6 and etched sample 7 in fixture 26, the two is passed in the mold 45 of sample drive device 4.
Further, as shown in Figures 2 and 3, in order that one-time pad quantity is more, etching operating efficiency, filling card are improved
Multiple parallel standing grooves, during driving sample stage 21 to move by the second motor 23, filling can be set on tool 26
Fixture 26 is also moved, and is made all the time with patch 6 and opposite filling bar 23 and the sample drive device 4, Ke Yilian of etched sample 7
It is continuous that sample is released into filling fixture 26.
Sample discharge mechanism 3 is located at the opposite side of thermostat 1, including sample stage 31, the 4th motor 32, discharge arm
33rd, sample box 34, patch box 35, the motor 37 of Electrical heads 36 and the 5th.Same principle, the 4th motor 32 drives sample
Platform 31 is rotated in the horizontal plane, and sample box 34 and patch box 35 are placed with sample stage 31；The drive connection of 5th motor 37
Discharge arm 33, can promote discharge arm to stretch in the horizontal direction；Unloading boom end carries Electrical heads 36, and Electrical heads 36 can be directed at sample
Mold 45 (see below and chat) in product drive device 4, draws patch 6 and is unloaded by the Electrical heads 36 on discharge arm 33.
Sample drive device 4 includes support 41, the 6th motor 42, first pressure sensor 43, armed lever 44, etching mould
The 45, the 7th motor 46 of tool, second pressure sensor 47.Support 41 stands in pond vertically, and top is fixed with the 6th driving
Motor 42, the radially connected armed lever 44 of output shaft of the 6th motor 42, control armed lever 44 rotates in vertical plane, the end of armed lever 44
Portion connects mold 45, and patch 6 and etched sample 7 can be deposited in mold 45, and sample can be carried out by the rotation of armed lever
Filling, etching, cleaning and unloaded operation (respectively corresponding diagram in tetra- positions of a, b, c, d).Further, armed lever 44 and the 6th
The axle of motor 42 prevents etching solution 16 from dripping device external in certain axial direction angle (Fig. 2).
Mold 45 is used to load sample to be etched.Further, as shown in figure 4, in order to increase in a cycle
Etching quantity, mold 45 can make disc, and multiple draw-in grooves can be set on disk, and one can be placed in each draw-in groove
Group sample and patch.Therefore, also further, the 7th motor 46 is fixed in the end of armed lever 44, the 7th motor 46 drives
Dynamic connection mold 45, make mold 45 can while vertical plane revolves round the sun with armed lever 44, also can autorotation, for filling
Fill out sample.When a certain room draw-in groove of mold 45 rotate to it is relative with a certain sample standing groove in foregoing filling fixture 26
When, so that it may filling bar 25 is promoted, etched sample and patch are together pushed into draw-in groove.
First pressure sensor 43 is placed in when mold 45 is totally immersed in etching solution, and armed lever 44 now can
The position arrived by the sensor sensing.Second pressure sensor 47 is placed in mold 45 is totally immersed in deionized water
When, the position that armed lever 44 now can be arrived by the sensor sensing.
In the embodiment shown in Fig. 3 and Fig. 4, mold 45 and 6 groups of sample cells should be provided with to filling fixture 26, it is real
The various factors such as visual sample size, disk size, fixture size, the sample size once tested, voluntarily adjusts in border, does not limit
System.
Further, the purpose for setting patch 6 is to prevent etched sample 7 in the process rotated with mold 45
In, come off because of gravity, so by patch 6 by sample card in groove.
Operating system 5, mainly include display screen 51, function key 52, instrument 53 and built-in controller, operating system 5 with
All motors and sensor, semiconductor thermostat etc. have control to connect, and can set sample by operating system 5 loads individual
The temperature of number, etching period and scavenging period, at-once monitor deionized water and etching solution.
The step of carrying out Apatite fission track chemical etching using equipment of the invention is as follows：
First, before etching experiment starts, needed to carry out the setting of experiment parameter in operating system 5 according to experiment, bag
Include etch temperature, etching period, scavenging period, filling sample number and testing time.When carrying out Apatite fission track etching,
Etching solution is dense HNO3, setting etch temperature as 21 ± 0.5 DEG C, etching period is 20s, scavenging period 1min, is etched in every time
6 samples are loaded in mold.After setting these parameters, click function key 52, thermostat 1 brings into operation, and determines and works as
The temperature of preceding deionized water and etching solution, semiconductor thermostat proceeds by temperature adjustment, until water temperature and etching solution temperature one
Cause.
Then, after etching solution temperature reaches 21 ± 0.5 DEG C and stabilization a period of time (2min), the band of the first motor 22
Dynamic sample stage 21 and the filling fixture 26 for being prefilled with etched sample 7 and patch 6,90 ° of rotate counterclockwise start to loading position
Sample is loaded, and the 3rd motor 24 promotes filling bar 25, by etched sample 7 and patch 6 simultaneously push-in mold 45；The
After one sample filling, the second motor 23 drives sample stage 21 and filling fixture 26 to translate a distance for placement groove width,
Make next group of sample and patch etched in alignment mould 45 and filling bar 25, meanwhile, the 7th motor control mold 45 is revolved
Turn 60 °, make next draw-in groove alignment filling fixture 26 on mould, carry out the filling of next sample.Six samples have been loaded successively
Product, then, the first motor drives sample stage 21 and filling fixture 26 to turn clockwise 90 ° to initial position.Then, test
Person starts to carry out filling fixture 26 filling of next group sample 7 and patch 6.
Next step ground, after sample stage 21 and filling bar 23 return to initial position, rotates the actuating arm of the 6th motor 42
Bar 44 and mold 45 are rotated into etching solution, and 6 samples are etched.Armed lever 44 connects with first pressure sensor 43
Touch the time of i.e. start recording etching, after etching 20s, motor with the rotate counterclockwise of semaphore 44, soaks mold 45 at once
Enter in deionized water, carry out the cleaning of sample, the dense HNO carried in removal mold3, while armed lever 44 is passed with second pressure
The contact of sensor 47 and the time of start recording cleaning.After cleaning sample 1min, the 6th motor 42 of rotation is suitable with semaphore 44
Hour hands are turned to up to unloading position.
Then, the 4th dynamic sample stage 31 of driving motor belt motor and discharge arm 33 turn clockwise 90 °, reach unloading position, so
The 5th motor 37 drives discharge arm 33 to stretch out afterwards, carries out sample unloading.In sample uninstall process, Electrical heads 36 are powered will plug
Piece 6 is suctioned out, and power supply disconnects magnetic and loses rear patch 6 into patch box 34, and subsequent mold 45 rotates 60 °, carries out next
The unloading of patch, while the corresponding sample of a upper patch is because of Action of Gravity Field, while the stop of patch 6 is lost again, so sliding
Into sample box 34.Repeat the above steps, complete 6 unloadings of sample.After six sample completions of discharge, experimenter changes patch
Box 35 and sample box 34, and patch 6 and sample 7 further cleaning and the drying to replacing, dried patch can continue
It is put into filling fixture and is used.
After sample unloading, the 6th motor 42 is rotated clockwise and returns to original " loaded " position again with semaphore 44, after
Continuous next round filling, repeats next round experiment, until completing the etching of all samples.
Finally, all drying samples for having etched are arranged, to carry out follow-up fission track testing research.Etching process
In, thermostat persistently adjusts temperature, the balance of etching solution temperature is kept, due to dense HNO3Can be chemically reacted with sample room
Etching solution temperature is caused to raise, as dense HNO3When temperature exceeds 21.5 DEG C, operating system can suspend the filling of sample, etching, clearly
Wash and unloading operation, after temperature adjustment to current operation is restarted again after 21 ± 0.5 DEG C, carry out follow-up experimental procedure.
In the present invention, realize the whole process by the way of " manipulator " and fetch and deliver Sample Etch, experimenter does not contact etching
Liquid, without corrosion and injury.Secondly the mold of the unique filling fixture of present invention design and uniqueness, etchable more with batch
Block sample, improves operating efficiency.The present invention has been merely given as a kind of above-mentioned embodiment, in practice, the side of any equivalent substitute
Case, in the present invention scheme all should be feasible and cover, such as, and the mold and dress of any shape and shipped quantity
Fixture is filled out, for another example, any method that can make sample etched in alignment mould, and any side that sample can be pushed mould
Method, for another example, any method that can remove patch and sample.In a word, the present invention is intended to provide a kind of automatic access sample, and
Sample can be made to be fixed on a certain device and to keep the automatic without infringement Etaching device and etching process of certain hour, it is real to realize losing
Carve the mechanized operation of experiment.
Claims (9)
1. a kind of equipment for fission track chemical etching, it is characterised in that：Including thermostat, sample drive device and behaviour
Make system；
The thermostat includes a water containing pool, and pond is built with deionized water, while being provided with valve unit, semiconductor constant in pond
Warm device, temperature sensor and etching ware, equipped with etching solution and being placed with thermometer in etching ware, the deionized water and etching solution
Do not mix mutually；
The sample drive device includes a support, and a motor, the arm of motor drive connection one are installed on support
Bar, makes the armed lever be rotated in vertical plane；The armed lever end connects a mold, and the mold is built with etching
Sample, the mold rotates with the armed lever, in the turnover deionized water and in etching solution；
The sample drive device also includes two pressure sensors, and one is placed in and can sense that the mold is located completely
Position in etching solution, another be placed in can sense the mold be completely in water in position；
The operating system includes all electrical equipment in controller, display screen, function key, instrument, operating system and the equipment
Part is electrically connected.
2. the equipment for fission track chemical etching according to claim 1, it is characterised in that：The equipment also includes
Sample filling device,
The sample filling device include sample stage, the first motor, the second motor, the 3rd motor, filling bar,
Filling fixture；The sample stage is driven by the first motor and rotated in the horizontal plane, while being driven by the second motor
Translation in horizontal plane, the 3rd motor drive connection filling bar makes the filling bar can be with horizontal extension；Filling is placed on sample stage
Filling fixture is pointed in fixture, the front of the filling bar, and the patch and etched sample are previously placed in filling fixture in groups, sample
In preceding, patch rear, when the mold is relative with filling fixture, the filling bar advances patch and etched sample to product
In mold.
3. the equipment for fission track chemical etching according to claim 2, it is characterised in that：On the filling fixture
With multiple parallel standing grooves, one group of patch and etched sample are placed in each standing groove；The sample stage is in the horizontal plane
One distance of placement well width of translation, makes filling bar gradually release the patch in each standing groove and etched sample every time；
The mold accordingly also has multiple draw-in grooves, and one group of patch and etched sample can be placed in each draw-in groove, described
Patch blocks etched sample.
4. the equipment for fission track chemical etching according to claim 3, it is characterised in that：The mold is
One dish type, uniform multiple draw-in groove on disk；The mold is rotated by a motor, and the mold rotates every time
Cross a distance for draw-in groove.
5. the equipment for fission track chemical etching according to claim 1 or 2 or 3 or 4, it is characterised in that：It is described
Equipment also includes sample discharge mechanism,
The sample discharge mechanism includes sample stage, the 4th motor, the 5th motor, discharge arm, sample box, patch
Box, Electrical heads；4th motor drives sample stage to rotate in the horizontal plane, and sample box and plug are placed with the sample stage
Film magazine；The 5th motor drive connection discharge arm, makes discharge arm stretch in the horizontal direction, the unloading boom end connection
Electrical heads, the Electrical heads can draw the patch in the mold.
6. the engraving method of equipment described in a kind of application claim 1 or 2 or 3, it is characterised in that comprise the following steps：
1) parameter setting, Preparatory work of experiment
Before etching experiment starts, need to carry out the setting of experiment parameter in an operating system according to experiment, including etch temperature, erosion
Time at quarter, scavenging period, filling sample number and testing time, etching solution is dense HNO3；
After setting parameter, thermostat brings into operation；Prepare sample simultaneously；
2) sample filling
After etching solution temperature reaches setting value and stabilization, sample filling is carried out to the mold；
3) Sample Etch
Start motor, rotate armed lever, mold is rotated into etching solution, armed lever connects with one of pressure sensor
Touch and start recording etching period, after etching period is reached, be again started up motor and drive mold to leave etching at once
Liquid, is immersed in deionized water, carries out sample clean, while armed lever and another pressure sensor contacts and start recording cleaning
Time；
4) sample unloading
After the completion of cleaning, motor drives mold to leave deionized water, reaches unloading position, is unloaded.
7. the engraving method of equipment described in a kind of application claim 4, it is characterised in that comprise the following steps：
1) parameter setting, Preparatory work of experiment
Before etching experiment starts, need to carry out the setting of experiment parameter in an operating system according to experiment, including etch temperature, erosion
Time at quarter, scavenging period, filling sample number and testing time, etching solution is dense HNO3；
After setting parameter, thermostat brings into operation；Prepare sample simultaneously, sample and patch are fitted into filling fixture；
2) sample filling
After etching solution temperature reaches setting value and stabilization, sample filling is carried out to the mold：
Sample stage in rotary sample filling device, makes filling fixture reach loading position, and first group of sample and patch are simultaneously right
The accurate mold and filling bar, promotion filling bar push first group of sample and patch in mold simultaneously；Then drive
Dynamic motor drives sample stage and filling fixture to translate a distance for standing groove, while rotating the mold turns over a card
The distance of groove, makes next group of sample and patch etched in alignment mould and filling bar, promote filling bar by second group of sample again and
Patch is pushed in mold simultaneously；The like, complete the filling of all samples；
Then, motor drives sample stage and filling fixture to produce loading position, the work of mold described in without prejudice to；
3) Sample Etch
Start motor, rotate armed lever, mold is rotated into etching solution, armed lever connects with one of pressure sensor
Touch and start recording etching period, after etching period is reached, be again started up motor and drive mold to leave etching solution, soak
Enter in deionized water, carry out sample clean, while armed lever and another pressure sensor contacts and start recording scavenging period；
4) sample unloading
After the completion of cleaning, motor drives mold to leave deionized water, reaches unloading position, is unloaded.
8. the engraving method of equipment described in a kind of application claim 5, it is characterised in that comprise the following steps：
1) parameter setting, Preparatory work of experiment
Before etching experiment starts, need to carry out the setting of experiment parameter in an operating system according to experiment, including etch temperature, erosion
Time at quarter, scavenging period, filling sample number and testing time, etching solution is dense HNO3；
After setting parameter, thermostat brings into operation；Prepare sample simultaneously；
2) sample filling
After etching solution temperature reaches setting value and stabilization, sample filling is carried out to the mold；
3) Sample Etch
Start motor, rotate armed lever, mold is rotated into etching solution, armed lever connects with one of pressure sensor
Touch and start recording etching period, after etching period is reached, be again started up motor and drive mold to leave etching at once
Liquid, is immersed in deionized water, carries out sample clean, while armed lever and another pressure sensor contacts and start recording cleaning
Time；
4) sample unloading
After the completion of cleaning, motor drives mold to leave deionized water, reaches unloading position, is unloaded：
The sample stage in the sample discharge mechanism is rotated, makes discharge arm arrival unloading position relative with the mold, so
Drive discharge arm to stretch out afterwards, draw a patch in the mold, then rotate the mold carry out it is next
The unloading of patch, now goes up the corresponding sample of patch because losing the stop of patch simultaneously again because of Action of Gravity Field, slides and enters
In sample box；Repeat the above steps, until completing the unloading of sample.
9. according to the method that one of claim 6-8 is described, it is characterised in that：Etch temperature as 21 ± 0.5 DEG C is set, during etching
Between be 20s, scavenging period is 1min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710045131.5A CN106872246B (en) | 2017-01-19 | 2017-01-19 | A kind of device and method for fission track chemical etching |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710045131.5A CN106872246B (en) | 2017-01-19 | 2017-01-19 | A kind of device and method for fission track chemical etching |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106872246A true CN106872246A (en) | 2017-06-20 |
| CN106872246B CN106872246B (en) | 2019-06-21 |
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| CN106872246B (en) | 2019-06-21 |
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