CN109632415A - A method of improving the electric conductivity of irregular sample - Google Patents
A method of improving the electric conductivity of irregular sample Download PDFInfo
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- CN109632415A CN109632415A CN201811542568.0A CN201811542568A CN109632415A CN 109632415 A CN109632415 A CN 109632415A CN 201811542568 A CN201811542568 A CN 201811542568A CN 109632415 A CN109632415 A CN 109632415A
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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 methods of electric conductivity for improving irregular sample, belong to analysis test sample preparation technical field.The technical problem to be solved by the present invention is to provide a kind of methods of electric conductivity for improving irregular sample.This method determines the region to be observed of sample first, with region to be observed upwards for initial position;Then sample is overturn 110~130 degree, vacuumized gold-plated;Sample is overturn to 110~130 degree in same direction again, is vacuumized gold-plated;Sample is overturn in same direction to initial position again, vacuumizes gold-plated, obtains conducting sample.By gold-plated three times along specific direction setting to irregular sample respectively, as allow the surface of sample conductive in all directions as possible, in addition sample all-directional conductive may be implemented in the winding of conducting resinl cloth silk, for irregular block, sphere or even complicated and diversified biological sample have relatively good effect.This method is not only suitable for sem test, can be applicable to those various application regions for needing conductor.
Description
Technical field
The present invention relates to a kind of methods of electric conductivity for improving irregular sample, belong to analysis test sample technology of preparing
Field.
Background technique
Many irregular samples (such as common biological sample) simultaneously do not have good electric conductivity.Many morphology observations and analysis
Testing field (for example scanning electron microscope SEM, scanning tunneling microscope STM, Auger electron spectroscopy AES and electron paramagnetic are total
Shake ESR etc.) in order to improve resolution ratio, generally require test sample that there is good electric conductivity.By taking scanning electron microscope as an example,
When observing its surface topography to study the scientific researches purposes such as various biomimetic material designs, 10- is usually first plated with sample
The golden film of 20nm left and right thickness just can be used high voltage and wavelength be smaller so that surface can produce more secondary electrons
Electron beam, improve the resolution ratio of secondary electron, improve maximum amplification, it is allowed to better meet analysis test request.
Conventional gold-plated method for making sample is that sample is fixed on sample stage, and region to be observed is upward, then gold-plated, observation
, using this kind of method it is gold-plated after, the contact conduction of sample is bad, can not meet conductive requirement, when observation, is easy to appear figure
As distortion, the defects of deforming, shake.And because biological sample shape is changeable, such as ant and butterfly insect, in conventional gold-plated system
Be difficult to find in sample a proper region be in close contact with two-sided conducting resinl by it and sample stage it is (mobile and survey in sample
There may be movements when examination rotation, influence the electric conductivity of sample).It can not make sample sufficiently fixed, also be more difficult that it is allowed sufficiently to lead
Electricity, then finding a kind of can sufficiently fix various special-shaped samples and its perfect conductive method is allowed to become particularly significant.It is raw simultaneously
(scanning electron microscope needs 10 for object sample and porous material pumping high vacuum-3The high vacuum of Pa or more) it is more difficult, and part functional regions
Under Electronic Speculum and bad identification, it is therefore desirable to which a kind of gold-plated and conducting adhesive cloth prepares the conducting sample technique of irregular body to solve
Above-mentioned problem.
Summary of the invention
For disadvantages described above, the technical problem to be solved by the present invention is to provide a kind of electric conductivities for improving irregular sample
Method.
The method that the present invention improves the electric conductivity of irregular sample, includes the following steps:
A, the region to be observed of sample is determined, with region to be observed upwards for initial position;
B, the torsion shaft of the sample of a step in the horizontal direction is overturn 110~130 degree, then carries out vacuumizing for the first time
It is gold-plated;
C, by vacuumize for the first time it is gold-plated after sample along b step reverses direction overturn 110~130 degree, then carry out
It vacuumizes for the second time gold-plated;
D, by vacuumize for the second time it is gold-plated after sample overturn along the reverses direction of step c it is upward to region to be observed, so
Progress third time vacuumizes gold-plated afterwards, obtains conductive sample.
Preferably, b step and step c overturn 120 degree.
Preferably, it is provided with sample carrier and sample is bonded in by sample carrier using conducting adhesive cloth after b step and step c are overturn
On carry out vacuumizing again it is gold-plated, Step d overturning after, sample is fixed on sample carrier by conductive seat, then carries out third
It is secondary vacuumize it is gold-plated.
Preferably, the conductive seat is the conducting adhesive cloth being bonded on sample carrier, and conductive seat has locating slot, step
In d, sample is placed in locating slot and Nian Jie with conductive seat, and the region to be observed of sample is upward.
Preferably, the top of sample is longitudinally bypassed after Step d using the first conducting adhesive cloth, the first conducting adhesive cloth is avoided wait see
Region is surveyed, the both ends of the first conducting adhesive cloth are fixed to sample carrier, sample is compressed downwards.
Preferably, first conducting adhesive cloth is 2~3, and is in cross-distribution.
Preferably, sample is pressed downward next, recycling second by the top that sample is longitudinally bypassed using the first conducting adhesive cloth
Conducting adhesive cloth banding is located at the first conducting adhesive cloth of sample bottom.
Preferably, vacuumize gold-plated using magnetron sputtering method, vacuum degree is≤6Pa, coating with a thickness of 10~20nm.
Compared with prior art, beneficial effects of the present invention mainly have following 5 aspects:
(1) irregular sample is carried out with conducting adhesive cloth three times sufficiently to fix, avoid possibility position of the sample in moving process
It moves, sample can be securely fastened on sample carrier.
(2) simultaneously by gold-plated three times along every 120 degree of specific direction to irregular sample respectively, sample is allowed as far as possible
Surface is conductive in all directions, in addition sample all-directional conductive may be implemented in the winding of conducting resinl cloth silk.
(3) it is vacuumized three times gold-plated with during changing face, it is fine for porous material and biomaterial exhaust effect, have
It is vacuumized conducive to the scanning electron microscope later period and test operation.
(4) simultaneously as the fabulous identification of conducting resinl under low power number in Electronic Speculum, being laid out by reasonable wrapping wire can quickly really
Specific region (such as related functional group etc.) is determined, convenient for testing quick constituency.
(5) if dissatisfied to the region (face C) currently surveyed, adhesive plaster can also be taken down, rewinds cloth with adhesive plaster
Office (as long as avoiding by conducting resinl Polluted area, general adhesive plaster and it is gold-plated after sample it is viscous not close), and avoid weight
New gold-plated and sample preparation again.For irregular block, sphere or even complicated and diversified biological sample have relatively good this technology
Effect.Not only it is suitable for sem test, can be applicable to those various application regions for needing conductor.
Detailed description of the invention
Fig. 1 is that sample is bonded in the cross-sectional view on sample carrier by conductive seat in Step d.
Fig. 2 is that sample winds the cross-sectional view after the first conducting adhesive cloth.
Fig. 3 is the top view of the first conducting adhesive cloth right-angled intersection winding.
Fig. 4 is the top view of the star-like cross winding of the first conducting adhesive cloth.
Fig. 5 is the cross-sectional view after the second conducting adhesive cloth banding.
In figure, 1- sample;2- conductive seat;3- sample carrier;The first conducting adhesive cloth of 4-;The second conducting adhesive cloth of 5-;6- sample
Region to be observed.
Specific embodiment
The method that the present invention improves the electric conductivity of irregular sample, includes the following steps:
A, the region to be observed 6 of sample 1 is determined, with region 6 to be observed upwards for initial position, by 6 institute of region to be observed
Face be defined as the face C;
B, the torsion shaft of the sample 1 of a step in the horizontal direction is overturn 110~130 degree, by the upward region after the overturning
It is set to the face A, then carries out vacuumizing for the first time gold-plated;Torsion shaft can be arbitrary horizontal direction;
C, by vacuumize for the first time it is gold-plated after sample 1 along b step reverses direction overturn 110~130 degree, by the overturning
Upward region afterwards is set to the face B, is then vacuumized for the second time gold-plated;
D, by vacuumize for the second time it is gold-plated after sample 1 along the reverses direction of step c overturn to region to be observed upwards (i.e.
Overturn to initial position), the upward region after the overturning is the face C, and then progress third time vacuumizes gold-plated, is obtained irregular
The conducting sample of body.
The method of the present invention, it is gold-plated using rotating three times, it allows the surface of sample 1 conductive in all directions as far as possible, is convenient for
The Electronic Speculum in later period is observed.The study found that if be divided into twice or once it is gold-plated if, it will cause gold-plated effect bad, from
And observation is influenced, and if number of revolutions is excessive, on the one hand cause cost higher, it is often more important that thickness of coating mistake will be will cause
Thickness covers the details of sample surfaces itself, sample is caused to be distorted.Therefore, the present invention uses rotates gold-plated, plated film Bao Erjun three times
It is even, and itself is without structure, can be good at the intrinsic form on reproducing samples surface, additionally it is possible to improve the electric conductivity of sample, improves
The yield of secondary electron can improve the quality of image, and can also enhance the mechanical strength of sample.
Preferably, b step and step c overturn 120 degree.In such manner, it is possible to guarantee that overturning every time is 120 degree, so that plating
Layer is more uniform.
Preferably, it is provided with sample carrier 3, sample carrier 3 is usually the aluminium disks of 1~3cm of diameter.B step
After rapid and step c is overturn, be directly bonded using conducting adhesive cloth, sample 1 be fixed on sample carrier 3, then vacuumize it is gold-plated,
After Step d overturning, sample 1 is fixed on sample carrier 3 by conductive seat 2, then carries out vacuumizing for the third time gold-plated.Three times
It is sufficiently fixed to carry out irregular sample with conducting adhesive cloth, avoids possible displacement of the sample 1 in moving process, can preferably by
Sample 1 is securely fastened on sample carrier 3, guarantees to be displaced with sample 1 in gold plating process vacuumizing.
Preferably, as shown in Figure 1, the conductive seat 2 is the conducting adhesive cloth being bonded on sample carrier 3, conductive seat 2 has
There is a locating slot, the sample 1 of step d is placed in locating slot and Nian Jie with conductive seat 2, and the region to be observed 6 of sample is upward.
In this way, facilitating fixed sample, and conductive seat 2 and 3 contact surface of sample carrier are larger, and conductive effect can be enhanced.
The main component of conducting adhesive cloth is carbon, and conducting adhesive cloth commonly used in the art is suitable for the present invention.For example, can adopt
With the conducting adhesive cloth bought on the market.
Further, as shown in Fig. 2, in order to preferably realize biological sample conduction, can Step d it is gold-plated after, adopt
With the longitudinal top for bypassing sample 1 of the first conducting adhesive cloth 4, the first conducting adhesive cloth 4 avoids region 6 to be observed, the first conducting adhesive cloth 4
Both ends be fixed to sample carrier 3, by sample 1 downwards compress.(sample can be avoided mobile more preferably fixing irregular sample in this way
It is middle generate conducting adhesive cloth pedestal loosening) while, moreover it is possible to allow it preferably with 3 bottom conductive of sample carrier.First conducting adhesive cloth 4
More can be used, is separately fixed in conductive support, also extends to 3 bottom of sample carrier, or even down around sample carrier 3.
Preferably, 2~3 first conducting adhesive cloths 4, and cross-distribution can be used, for example, as shown in figure 3, can use
2 first conducting adhesive cloths 4 are wound in cross type.It is as also shown in fig. 4, it is in star-like friendship using three first conducting adhesive cloths 4
Forked type winding.
Further, using the longitudinal top for bypassing sample 1 of the first conducting adhesive cloth 4, sample 1 is pressed downward next then sharp
It is located at the first conducting adhesive cloth 4 of 1 bottom of sample with 5 banding of the second conducting adhesive cloth, as shown in Figure 5.The banding is using second
At least one circle of circumferential direction winding at sample carrier 3 in the first conducting adhesive cloth 4 of conducting adhesive cloth 5.Before so on the one hand can be by handle
First conducting adhesive cloth 4 of face winding becomes broken line from straight line, preferably fixes irregular biological sample.It simultaneously can also be better
It carries out conductive.Finally allow irregular sample (face C especially to be measured) each region that can be connected to well with sample carrier 3
Conduction reaches and secondary electron, backscattered electron and X-ray signal etc. can easily be escaped from sample C Surface, to carry out
The purpose of the high-resolution observation pattern of high quality.
The present invention vacuumizes gold-plated three times, can use common gold plating method.Preferably, using magnetron sputtering method,
Vacuum degree is≤6Pa, and the thickness of coating of single is 10~20nm.
For block in irregular shape, sphere or even complicated and diversified biological sample have relatively good the method for the present invention
Effect.For example, the primary sample is non-irrigated lotus seed, chalk, fly, honeybee, screw or nut.The method of the present invention is not only fitted
For scanning electron microscope example preparation and validity test, it can be applicable to those various application regions for only needing conductor.For example,
Scanning tunneling microscope STM, Auger electron spectroscopy AES and electron paramagnetic resonance ESR etc..
A specific embodiment of the invention is further described below with reference to embodiment, is not therefore limited the present invention
System is among the embodiment described range.
Embodiment 1 uses scanning electron microscope observation drought lotus seed
Using non-irrigated lotus seed as sample 1, interested region to be observed 6 is chosen, the face where the region is defined as the face C,
Determine its direction for needing gold-plated overturning simultaneously, i.e. the loop wire that naturally occurs of non-irrigated lotus surface.
Then sample 1 is overturn 120 ° by horizontal direction, the point of test is analyzed most unlikely with sample 1 and sample carrier 3 is used
A little two-sided conducting adhesive cloth is simply fixed, and position movement is generated when avoiding vacuumizing, gold-plated effect is influenced, at this point, will be with sample
The opposite side that support 3 contacts is defined as the face A, vacuumize for the first time gold-plated, and vacuum degree is 6Pa or so, thickness of coating about 20nm.
After the completion of the face A is gold-plated, then sample 1 overturn 120 degree according to previous reverses direction, is coated with 20nm thick gold membrane at this time
The face biological sample A should tilt downward, choose a point most unlikely tested and sample carrier 3 with double in the face A adjacent edges
Face conducting adhesive cloth vacuumizes after carrying out simple bonding again, then plates the golden film of 10~20nm thickness again on plated film instrument, plates
The golden film face obtained is defined as B surface.Because low vacuum magnetron sputtering (physical sputtering PVD) it is gold-plated be space sputtering, at this time the face B and
The face A juncture area can also be plated a thin layer of golden film again, be able to satisfy sufficiently conducting requirement.
After the completion of second gold-plated, sample 1 is overturn 120 degree according to previous reverses direction again, determines that third time is plated
The face C of gold designs one with conducting adhesive cloth (and its filament) according to the true form of the opposite side (i.e. the face AB intersection) in the face C at this time
The unique and matched conductive seat 2 of opposite side shape, for example, with two-sided conducting adhesive cloth or its conducting resinl cloth silk in sample carrier 3
Surface is suitably wound, and the conductive seat 2 for being suitable for the support of the face AB junctional area institute unique design is finally made into.In AB
Juncture area selects a sample test point most unlikely analyzed firmly to be fixed on non-irrigated lotus seed as bottom and sweep
It retouches on electron microscopic sample support conductive seat 2, as shown in Figure 1.At this point, C is face-up, carries out third time and vacuumize gold-plated, then plate one layer
The thin golden film of 10~20nm thickness, the face C will thicken again with the face A, the face C and the golden film in region similar in the face B, and the face C center
Domain can plate thicker, so as to sufficiently meet conductive requirement because with gold target apart from close.It is plated three times by tri- face ABC
Gold.1 surface of sample can have been made to have obtained everywhere abundant gold-plated.
After the face C is gold-plated, in order to make it preferably fixed and conductive, after avoiding region 6 to be observed, one is determined
A suitable similar cross adhesive plaster silk winding scenario, as shown in Figure 3.Using the first conducting adhesive cloth 4 securely with 3 bottom of sample carrier
Seat (extending to 3 bottom of sample carrier) is fixed, as shown in Fig. 2, (sample is avoided to move for more preferably fixing irregular sample
The loosening of conducting adhesive cloth pedestal is generated in dynamic) while, can allow it preferably with 3 bottom conductive of scanning electron microscope example support.
As shown in figure 5, in order to further improve its electric conductivity, while increasing the reliability of adhesive plaster silk winding, then with second
Conducting adhesive cloth 5, close to circumferential at least one circle of winding in the place of sample carrier 3, is convenient for fixed and more preferable again in the first conducting adhesive cloth 4
Conduction.Because cross binding may not be tight, if it is necessary, can directly be connect with sample carrier 3 with the second conducting adhesive cloth 5
Touching, to reduce the distance between 1 top of sample and 3 contact point of sample carrier (original binding straight line is become broken line), on the one hand
It can become broken line from straight line by the first conducting adhesive cloth 4 of the right-angled intersection that front is wound, it is preferably fixed irregular raw
Object sample.It can also more preferably be carried out simultaneously in right-angled intersection section conductive.Finally allow each region of non-irrigated lotus seed (especially to
The face C where observation area 6) conduction can be connected to well with sample carrier 3.
On the one hand final sample obtained passes through 3 adhesive plasters can fix very secured, while be divided into tri- face all standing of ABC
Gold-plated 3 times, sample can be made sufficiently to meet conductive and contact stable requirement, be advantageous to subsequent scanning electron microscope operation.
It is repeatedly vacuumized simultaneously as introducing, is also beneficial to biological sample and porous material sample preparation, and conscious introducing adhesive plaster
Winding technology is also very helpful for being quickly found out test zone interested.
The method of the present invention has relatively good effect for irregular block, sphere or even complicated and diversified biological sample
Fruit.Not only it is suitable for scanning electron microscope example preparation and validity test, can be applicable to those various applications for only needing conductor
Region.
Claims (8)
1. a kind of method for the electric conductivity for improving irregular sample, which comprises the steps of:
A, the region to be observed of sample is determined, with region to be observed upwards for initial position;
B, the torsion shaft of the sample of a step in the horizontal direction is overturn 110~130 degree, then carries out vacuumizing for the first time gold-plated;
C, by vacuumize for the first time it is gold-plated after sample along b step reverses direction overturn 110~130 degree, then carry out second
It is secondary vacuumize it is gold-plated;
D, by vacuumize for the second time it is gold-plated after sample overturn along the reverses direction of step c it is upward to region to be observed, then into
Row third time vacuumizes gold-plated, obtains conductive sample.
2. the method for the electric conductivity according to claim 1 for improving irregular sample, it is characterised in that: b step and c step
Suddenly 120 degree are overturn.
3. the method for the electric conductivity according to claim 1 for improving irregular sample, it is characterised in that: be provided with sample
After support, b step and step c overturning, sample is bonded on sample carrier using conducting adhesive cloth and carries out vacuumizing gold-plated, Step d again
After overturning, sample is fixed on sample carrier by conductive seat, then carries out vacuumizing for the third time gold-plated.
4. the method for the electric conductivity according to claim 3 for improving irregular sample, it is characterised in that: the conduction bottom
Seat is the conducting adhesive cloth that is bonded on sample carrier, and conductive seat has a locating slot, and in step d, sample is placed in locating slot simultaneously
It is Nian Jie with conductive seat, and the region to be observed of sample is upward.
5. the method for the electric conductivity according to claim 4 for improving irregular sample, it is characterised in that: adopted after Step d
Longitudinally bypassing the top of sample with the first conducting adhesive cloth, the first conducting adhesive cloth avoids region to be observed, and the two of the first conducting adhesive cloth
End is fixed to sample carrier, and sample is compressed downwards.
6. the method for the electric conductivity according to claim 5 for improving irregular sample, it is characterised in that: described first leads
Electric adhesive plaster is 2~3, and is in cross-distribution.
7. the method for the electric conductivity according to claim 6 for improving irregular sample, it is characterised in that: led using first
Electric adhesive plaster longitudinally bypasses the top of sample, sample is pressed downward it is next, recycle the second conducting adhesive cloth banding be located at sample bottom
The first conducting adhesive cloth.
8. the method for described in any item electric conductivities for improving irregular sample according to claim 1~7, it is characterised in that:
Vacuumize gold-plated using magnetron sputtering method, vacuum degree is≤6Pa, coating with a thickness of 10~20nm.
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CN113081298A (en) * | 2021-03-18 | 2021-07-09 | 甘肃省动物疫病预防控制中心 | Intelligent controllable temperature's animal doctor's sampling box |
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