CN109459460A - A kind of scanning electron microscope observation device and method of intact loess humidification sample - Google Patents
A kind of scanning electron microscope observation device and method of intact loess humidification sample Download PDFInfo
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- CN109459460A CN109459460A CN201811594086.XA CN201811594086A CN109459460A CN 109459460 A CN109459460 A CN 109459460A CN 201811594086 A CN201811594086 A CN 201811594086A CN 109459460 A CN109459460 A CN 109459460A
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- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000004575 stone Substances 0.000 claims abstract description 50
- 239000002689 soil Substances 0.000 claims abstract description 40
- 230000008569 process Effects 0.000 claims abstract description 16
- 239000003292 glue Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000005520 cutting process Methods 0.000 claims description 16
- 229940099259 vaseline Drugs 0.000 claims description 14
- 239000002184 metal Substances 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000000428 dust Substances 0.000 claims description 7
- 238000007605 air drying Methods 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 230000003321 amplification Effects 0.000 claims description 3
- 238000003199 nucleic acid amplification method Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000004544 sputter deposition Methods 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 abstract description 16
- 238000010835 comparative analysis Methods 0.000 abstract description 5
- 230000008859 change Effects 0.000 abstract description 4
- 238000007654 immersion Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 description 6
- 230000009471 action Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000004927 clay Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
Classifications
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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
- G01N23/22—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
- G01N23/225—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 using electron or ion
- G01N23/2251—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 using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
-
- 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
- G01N23/22—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
- G01N23/2202—Preparing specimens therefor
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a kind of scanning electron microscope observation device and methods of intact loess humidification sample, including shell, permeable stone, push-pull rod and rubber stopper；Shell is transparent outer cover, and permeable stone is horizontally placed in outer casing inner wall, and rubber stopper one end is connect with permeable stone point, and the other end connects push-pull rod；Rubber stopper connects one end of push-pull rod and outer casing inner wall is tightly connected；Push-pull rod stretches out interior of shell far from one end of rubber stopper；Rubber stopper can move up and down inside the housing under the push-and-pull of push-pull rod；Drainage hole is opened up on shell between the link position and permeable stone of rubber stopper and shell and the link position of shell.Apparatus structure is simple, and sample preparation is convenient, and cost is relatively low, and soil sample disturbance is small, and injecting glue is not necessarily to during sample preparation, can quickly batch sample preparation, work efficiency is high, and sample is easy to carry about with one.The method of the present invention can obtain the multiple observation image of same soil sample same position, being capable of the microstructure change of the same soil sample of intuitive comparative analysis, same position in repeatedly immersion humidification process.
Description
Technical field
The invention belongs to intact loess Study on Microstructure field, the scanning electron microscope for being related to a kind of intact loess humidification sample is seen
Survey device and method.
Background technique
Collapsibility caused by loess water sensitivity is to perplex Loess Plateau engineering construction, resident living production mainly
Geological Problems.Observing loess microstructure by electron-microscope scanning and disclosing collapsible mechanics is studying collapsibility of loess at this stage
Main means.
But sample made by existing method has the following problems: 1, injecting glue method sample preparation, can only in addition to the sample preparation time is long
The observation for carrying out a loess sample can not be humidified after observation, can not continue to observe the loess microstructure after water effect；
2, injecting glue method in edge is unable to control reserved observation position, and observation position is smaller；3, edge injecting glue method can not in humidification process
It determines whether humidification water sufficiently acts on soil sample, and sample is easy to crack, one can not be provided continually and steadily for soil, water effect
Place.The existing method for making sample one side sample preparation time is long, on the other hand cannot achieve same soil sample be repeatedly humidified observation purpose.
Therefore, quickly preparing soil body humidification sample and being continuously Tu Shui effect to provide the scanning electron microscope device of stable condition is soil
The key of body Study on Microstructure.
Summary of the invention
It is an object of the invention to overcome the above-mentioned prior art, a kind of scanning electricity of intact loess humidification sample is provided
Mirror observation device and method.
In order to achieve the above objectives, the present invention is achieved by the following scheme:
A kind of scanning electron microscope observation device of intact loess humidification sample, including shell, permeable stone, push-pull rod and rubber stopper；
Shell is transparent outer cover, and permeable stone is connect with outer casing inner wall, and rubber stopper one end is connect with permeable stone point, other end connection push-and-pull
Bar；Rubber stopper connects one end of push-pull rod and outer casing inner wall is tightly connected；Push-pull rod stretches out in shell far from one end of rubber stopper
Portion；Rubber stopper can move up and down inside the housing under the push-and-pull of push-pull rod；The link position and permeable stone of rubber stopper and shell
Drainage hole is opened up on shell between the link position of shell.
Observation device of the present invention further improvement is that
Vaseline is uniformly smeared between permeable stone and outer casing inner wall, vaseline is for sealing between permeable stone and outer casing inner wall
Gap.
Cutting edge is arranged in the top of shell, and the thickness of cutting edge is not more than 0.2mm.
Permeable stone with a thickness of 4~8mm.
The diameter of drainage hole is 2~6mm.
Shell is cylindrical shell, and the rubber stopper is cone rubber plug.
Laminar protrusion is arranged in one end that the bottom end of shell and push-pull rod are located at shell exterior outward, and protrusion is along shell
With being arranged radially for push-pull rod.
Shell with a thickness of 1mm, outer diameter 16mm.
A kind of scanning electron microscope observation method of intact loess humidification sample, which comprises the following steps:
S1: the diameter cylindric intact loess soil sample that identical and outer wall uniformly smears vaseline with internal diameter of outer cover is put vertically
Enter interior of shell and is contacted with permeable stone；Soil sample is broken into dust that is disconnected, and removing incision position along the cutting edge that housing top end is arranged, is obtained
Sample is scanned to intact loess；
S2: repeating S1 and obtain several intact loess scanning sample, and intact loess scanning sample is used glue according to every 8 for one group
Water is bonded together, and is horizontally fixed on the circular metal pallet for being provided with datum mark 9, and one group of scanning observation sample is obtained；
S3: will be vacuumized and metal spraying 120 seconds after observation sample natural air drying with ion sputtering instrument, be put into scanning electron microscope into
Row observation sample scanning, obtains scanned photograph；
S4: judge whether the number of repetition of S3 is equal to preset value: being, terminate；It is no, carry out S5；
S5: it is humidified after the completion of scanning to observation sample, stops water filling when having moisture exudation below permeable stone；When permeable
There is no humidification process when moisture exudation to terminate below stone；The initial number of repetition of S3 is denoted as 1；S3 number of repetition adds 1, carries out S3.
Observation method of the present invention further improvement is that
The method that sample scanning uses magnified sweep step by step is observed, method particularly includes:
Same position is carried out according to 100 times, 200 times, 400 times, 800 times, 1600 times, 3200 times of amplification factor sequence
It scans and takes pictures；
The specific mode that observation sample is humidified is artificial humidification or instrument humidification；
Remove the concrete mode of the dust of incision position are as follows: the dust of incision position is blown off using ear washing bulb.
Compared with prior art, the invention has the following advantages:
By using transparent outer cover be soil, water effect a place is provided and make the soil body have a lateral restriction without
As for loose；Transparent outer cover can also preferably control reserved observation position, and observation position is big, be convenient for observing.Device can
To be directly placed in scanning electron microscope, implement convenient for operation；Also, pass through by dropper or by spraying from device top plus water, water
It is discharged after permeable stone exudation by drainage hole, same sample is humidified observation repeatedly, raising working efficiency.Compared to biography
The injecting glue method sample preparation of system, the device produce sample and do not need injecting glue link, greatly save the sample preparation time, reduce sample preparation cost.Together
When, the configuration of the present invention is simple, processing and fabricating facilitate, are readily produced, implementing convenient for operation.
Further, vaseline is uniformly smeared between permeable stone and outer casing inner wall, by vaseline by permeable stone and shell
Clearance seal between inner wall prevents gap outflow of the water directly between permeable stone and outer casing inner wall, is unable to complete to soil sample
Humidification.
Further, the top of shell is arranged cutting edge, and when preparation of soil sample is easier to be broken disconnected, is easier to obtain fresh section.
Further, the thickness of permeable stone is set as 4~8mm, on the one hand, has sufficient intensity support scanning sample；It is another
Aspect, the thickness also can control the action time of moisture and soil sample.When moisture exudation is arranged at permeable stone bottom, stop humidification plus water
Process indicates that humidification process terminates when the exudation of permeable stone bottom no moisture.
Further, laminar protrusion is arranged in one end that the bottom end of shell and push-pull rod are located at shell exterior outward,
It is convenient for the position adjustment of rubber stopper inside the housing, device is simple to operate.
The scanning electron microscope observation method of intact loess humidification sample of the present invention carries out repeated measures by repeatedly humidification, can obtain
To same soil sample, the multiple observation image of same position, intuitively the same soil sample of comparative analysis, same position can repeatedly soak
Microstructure change in water humidification process, compensating for previous same sample can only observe once, or can only comparative analysis not
With the deficiency of the micro-variations in the immersion humidification process between sample.Three labels are done on the edge of metal tray as base
On schedule, guarantee that the datum mark is respectively positioned on same position when putting into scanning electron microscope every time, the scanning after convenience can faster, more
Accurately find the same position of last time soil sample scanning.
Detailed description of the invention
Fig. 1 is the structural diagram of the present invention；
Fig. 2 is that the present invention produces the structural schematic diagram after sample；
Fig. 3 is the top view of present invention observation sample.
Wherein: 1- shell；2- drainage hole；3- permeable stone；4- cutting edge；5- push-pull rod；6- rubber stopper；The scanning of 7- undisturbed soil
Sample；8- metal tray；9- datum mark.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, below in conjunction in the embodiment of the present invention
Attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only
The embodiment of a part of the invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill people
The model that the present invention protects all should belong in member's every other embodiment obtained without making creative work
It encloses.
It should be noted that description and claims of this specification and term " first " in above-mentioned attached drawing, "
Two " etc. be to be used to distinguish similar objects, without being used to describe a particular order or precedence order.It should be understood that using in this way
Data be interchangeable under appropriate circumstances, so as to the embodiment of the present invention described herein can in addition to illustrating herein or
Sequence other than those of description is implemented.In addition, term " includes " and " having " and their any deformation, it is intended that cover
Cover it is non-exclusive include, for example, the process, method, system, product or equipment for containing a series of steps or units are not necessarily limited to
Step or unit those of is clearly listed, but may include be not clearly listed or for these process, methods, product
Or other step or units that equipment is intrinsic.
The invention will be described in further detail with reference to the accompanying drawing:
Referring to Fig. 1 and 2, a kind of scanning electron microscope observation device of intact loess humidification sample of the present invention, including it is shell 1, permeable
Stone 3, push-pull rod 5 and rubber stopper 6；Shell 1 is transparent outer cover, and permeable stone 3 connect with 1 inner wall of shell, 6 one end of rubber stopper with it is permeable
3 points of stone connections, the other end connect push-pull rod 5；Rubber stopper 6 connects one end of push-pull rod 5 and outer casing inner wall is tightly connected；Push-pull rod
5 one end far from rubber stopper 6 are stretched out inside shell 1；Rubber stopper 6 can under the push-and-pull of push-pull rod 5 inside the shell 1 on move down
It is dynamic；Drainage hole is opened up on shell 1 between the link position and permeable stone 3 and the link position of shell 1 of rubber stopper 6 and shell 1
2。
Preferably, vaseline is uniformly smeared between 1 inner wall of permeable stone 3 and shell, vaseline is for sealing permeable stone 3 and outer
Gap between 1 inner wall of shell.
Preferably, cutting edge 4 is arranged in the top of shell 1, and the thickness of cutting edge 4 is not more than 0.2mm.The design of cutting edge 4 is conducive to
It is easier to be broken disconnected when the preparation of soil sample, obtains fresh section, stress is avoided not enough to cause sample broke, raising prepares the qualification of sample
Rate.
Preferably, permeable stone 3 with a thickness of 4~8mm, preferably 5mm.On the one hand there is sufficient intensity support scanning sample；
On the other hand, which also can control the action time of moisture and soil sample, when moisture exudation is arranged at 3 bottom of permeable stone, stop increasing
Wet plus water process indicates that humidification process terminates when the exudation of 3 bottom no moisture of permeable stone.
Preferably, the diameter of drainage hole 2 is 2~6mm, preferably 2mm.Drainage hole 2 is used to be discharged to be oozed out by permeable stone 3
Moisture.
Preferably, shell 1 is cylindrical shell, and the wall thickness of shell 1 is 1mm, outer diameter 16mm, internal diameter 14mm.Rubber
Plug 6 is cone rubber plug.
Preferably, the bottom end of shell 1 and push-pull rod 5 be located at one end outside shell 1 outward setting flake protrusion, it is convex
Play being arranged radially along shell 1 and push-pull rod 5.The setting of protrusion is easy to use push-pull rod 5 that rubber stopper 6 is adjusted in shell 1
Internal position, whole device are simple, convenient.
Device prepare observation sample after, can for soil, water effect a place be provided and make the soil body have one laterally
Restraining force and be unlikely to occur loose.Meanwhile device is suitable for loess, redeposited loess, red clay, swelled ground, weak soil, remodeling
The microstructure of the various soil bodys such as soil, backfill is observed.
Application method of the invention:
Rubber stopper 6 is first pushed into 2 lower section of drainage hole, and the space that reserved part is up and down by push-pull rod 5.By side
The permeable stone 3 for uniformly smearing vaseline lies in a horizontal plane in 2 top of drainage hole inside shell 1, and connects with the rubber stopper of taper 6
Touching.The smooth cylindric loess surrounding in the bottom cut according to 1 inner diameter size of shell is uniformly smeared into one layer of vaseline, is slowly put
Enter in shell 1, cylindric Bottom of Loess is contacted with permeable stone 3.Sample is adjusted to suitable position and along device top by push-pull rod 5
The cutting edge 4 of portion 0.2mm thickness is broken disconnected, fresh section is obtained, as observing samples.It is few at the top of sample using dropper or spraying device
Amount repeatedly adds water, and big yield excessively is avoided once to destroy sample surface structure.The scanning electron microscope observation dress of intact loess humidification sample
Setting can be directly placed in scanning electron microscope, and same sample can be humidified observation repeatedly.
A kind of scanning electron microscope observation method of intact loess humidification sample, comprising the following steps:
Step 1: pushing push-pull rod 5, so that rubber stopper 6 is reached 2 following distance of drainage hole, and reserved certain activity is empty
Between, it is unlikely to block drainage hole 2, to influence the draining of drainage hole 2.
Step 2: the position for 2 top of 3 periphery of permeable stone and 1 internal drainage hole of shell that diameter is 13.8mm is uniform
One layer of vaseline is smeared, achievees the purpose that be in close contact between 1 inner wall of permeable stone 3 and shell.
Step 3: the permeable stone 3 that diameter is 13.8mm being lain in a horizontal plane in shell 1, and is contacted with the top of rubber stopper 6.
Step 4: intact loess cutting with a knife be cut into the square strip of 2cm*2cm first, bottom end is scabbled, and keeps former
Vertical direction of the shape soil at field.
Step 5: pruned with the corner angle of the careful square strip by 2cm*2cm of pocket knife, back rotation soil sample side cut
Soil, and frequently compared with the shell of device 1, until the soil sample of square strip is trimmed to the cylinder that diameter is about 15.8mm
Soil sample.
Step 6: the soil sample surrounding for being put into 1 part of shell uniformly being smeared into one layer of vaseline, is then put into shell 1 vertically
And it is contacted with permeable stone 3.
Step 7: in the soil sample at 1 top cutting edge 4 of shell, along the height pocket knife of cutting edge 4 it is simple portray one
Thin trace.
Step 8: soil sample is acted at 1 top cutting edge 4 of shell firmly break it is disconnected, and with ear washing bulb by incision position dust gently
It blows away, obtains an intact loess scanning sample.
Step 9: repeating step 1- step 8 and obtain multiple intact loess scanning samples.
Step 10: the scanning sample that preparation is completed being bonded together for one group with glue according to every 8, is not advised in one
It is then cylindric, and lie in a horizontal plane in a circular metal tray 8, observation sample is obtained, as shown in Figure 3.
Step 11: scanning for the first time: will be vacuumized and sprayed with ion sputtering instrument after the observation sample natural air drying prepared
Gold 120 seconds.
Step 12: the scanning after for convenience faster can more accurately find the same position of last time soil sample scanning,
It should when doing three labels on the edge of circular metal tray 8 as datum mark 9, and guaranteeing to put into scanning electron microscope every time
Datum mark 9 is respectively positioned on same position.
Step 13: observation sample scans the method using magnified sweep step by step, i.e., to same position according to 100 times, 200
Times, 400 times, 800 times, 1600 times, 3200 times of amplification factor sequence is scanned and takes pictures.
Step 14: be humidified after scanning to observation sample: humidification is carried out in the environment of a relative closure, is increased
Wet mode is divided into artificial humidification and instrument is humidified two kinds.Artificial humidification is completed by 1ml injector for medical purpose.Guaranteeing needle tubing
Oral fluid drop with sample contact while, syringe needle cannot be contacted with sample surfaces, herein under the premise of can be filled the water.When
After the completion of primary water filling, and sample surfaces do not have to carry out filling the water for the second time when the stop of obvious moisture.The injecting process should follow few
Measure multiple principle.Instrument humidification is completed by small-sized humidifier, in closed environment, is atomized moisture by humidifier
It acts on specimen surface and reaches humidification purpose.
Step 15: stopping water filling when having moisture exudation below permeable stone in device.
Step 16: when there is no show that humidification process terminates when moisture oozes out for permeable stone in device.
Step 17: the moisture in device will observe sample natural air drying again after drainage hole is discharged.
Step 18: repeating step 11 to 13, carry out second of microstructure observing, that is, the microcosmic of sample that be humidified for the first time
Structure observation.
Step 19: repeating step 14 to 18, implement microstructure observing, the third time humidification sample of second of humidification sample in succession
Microstructure observing ..., until off-test, number is default according to different observation requirements.
The scanning electron microscope observation apparatus structure of intact loess humidification sample of the present invention is simple, and sample preparation is convenient, and cost is relatively low, soil sample
Disturb it is small, during sample preparation be not necessarily to injecting glue, can quickly batch sample preparation, the sample preparation time is short, and work efficiency is high, and sample is easy to carry about with one；
Device can be directly placed in scanning electron microscope, and same sample can be humidified observation repeatedly.
The scanning electron microscope observation method of intact loess humidification sample of the present invention can obtain the multiple of same soil sample same position
Image is observed, it being capable of the microstructure change of the same soil sample of intuitive comparative analysis, same position in repeatedly immersion humidification process
Change, compensating for previous same sample can only observe once, or can only immersion humidification process between comparative analysis difference sample
In micro-variations deficiency.
The above content is merely illustrative of the invention's technical idea, and this does not limit the scope of protection of the present invention, all to press
According to technical idea proposed by the present invention, any changes made on the basis of the technical scheme each falls within claims of the present invention
Protection scope within.
Claims (10)
1. a kind of scanning electron microscope observation device of intact loess humidification sample, which is characterized in that including shell (1), permeable stone (3),
Push-pull rod (5) and rubber stopper (6)；Shell (1) is transparent outer cover, and permeable stone (3) is connect with shell (1) inner wall, rubber stopper (6) one
End is connected with permeable stone (3) point, and the other end connects push-pull rod (5)；Rubber stopper (6) connects in the one end and shell of push-pull rod (5)
Wall is tightly connected；Push-pull rod (5) stretches out shell (1) inside far from the one end of rubber stopper (6)；Rubber stopper (6) can be in push-pull rod (5)
Push-and-pull under move up and down inside the shell (1)；The link position and permeable stone (3) and shell of rubber stopper (6) and shell (1)
(1) drainage hole (2) are opened up on the shell (1) between link position.
2. the scanning electron microscope observation device of intact loess humidification sample according to claim 1, which is characterized in that described permeable
Vaseline is uniformly smeared between stone (3) and shell (1) inner wall, vaseline is for sealing between permeable stone (3) and shell (1) inner wall
Gap.
3. the scanning electron microscope observation device of intact loess humidification sample according to claim 1, which is characterized in that the shell
(1) cutting edge (4) are arranged in top, and the thickness of cutting edge (4) is not more than 0.2mm.
4. the scanning electron microscope observation device of intact loess humidification sample according to claim 1, which is characterized in that described permeable
Stone (3) with a thickness of 4~8mm.
5. according to the scanning electron microscope observation device of the humidification sample of intact loess described in claim (1), which is characterized in that the row
The diameter in water hole (2) is 2~6mm.
6. the scanning electron microscope observation device of intact loess humidification sample according to claim 1, which is characterized in that the shell
It (1) is cylindrical shell, the rubber stopper (6) is cone rubber plug.
7. the scanning electron microscope observation device of intact loess humidification sample according to claim 1, which is characterized in that the shell
(1) bottom end and push-pull rod (5) is located at the external one end of shell (1) and laminar protrusion is arranged outward, and protrusion is along shell (1)
With being arranged radially for push-pull rod (5).
8. the scanning electron microscope observation device of intact loess humidification sample according to claim 6, which is characterized in that the shell
(1) with a thickness of 1mm, outer diameter 16mm.
9. a kind of scanning electron microscope observation method of the intact loess humidification sample based on claim 3 described device, which is characterized in that
The following steps are included:
S1: the diameter cylindric intact loess soil sample that identical and outer wall uniformly smears vaseline with shell (1) internal diameter is put vertically
Enter shell (1) inside and is contacted with permeable stone (3)；Soil sample is broken along the cutting edge (4) that shell (1) top is arranged disconnected, and removed disconnected
Dust at mouthful obtains intact loess scanning sample；
S2: repeating S1 and obtain several intact loess scanning sample, and intact loess scanning sample is glued for one group with glue according to every 8
Knot together, and is horizontally fixed on the circular metal pallet for being provided with datum mark 9, obtains one group of scanning observation sample；
S3: it will be vacuumized simultaneously metal spraying 120 seconds after observation sample natural air drying with ion sputtering instrument, and be put into scanning electron microscope and seen
Test sample scanning, obtains scanned photograph；
S4: judge whether the number of repetition of S3 is equal to preset value: being, terminate；It is no, carry out S5；
S5: it is humidified after the completion of scanning to observation sample, stops water filling when having moisture exudation below permeable stone (3)；When permeable
There is no humidification process when moisture exudation to terminate below stone (3)；The initial number of repetition of S3 is denoted as 1；S3 number of repetition adds 1, carries out
S3。
10. the scanning electron microscope observation method of intact loess humidification sample according to claim 9, which is characterized in that the sight
The method that test sample scanning uses magnified sweep step by step, method particularly includes:
Same position is scanned according to 100 times, 200 times, 400 times, 800 times, 1600 times, 3200 times of amplification factor sequence
And it takes pictures；
The specific mode that the observation sample is humidified is artificial humidification or instrument humidification；
The concrete mode of the dust of the removal incision position are as follows: blown off the dust of incision position using ear washing bulb.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811594086.XA CN109459460B (en) | 2018-12-25 | 2018-12-25 | Scanning electron microscope observation device and method for undisturbed loess humidification sample |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811594086.XA CN109459460B (en) | 2018-12-25 | 2018-12-25 | Scanning electron microscope observation device and method for undisturbed loess humidification sample |
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| Publication Number | Publication Date |
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| CN109459460A true CN109459460A (en) | 2019-03-12 |
| CN109459460B CN109459460B (en) | 2023-10-27 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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