CN110487831A - The preparation method of speckle and the method and apparatus for preparing nanogold particle coating speckle - Google Patents
The preparation method of speckle and the method and apparatus for preparing nanogold particle coating speckle Download PDFInfo
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- CN110487831A CN110487831A CN201910692609.2A CN201910692609A CN110487831A CN 110487831 A CN110487831 A CN 110487831A CN 201910692609 A CN201910692609 A CN 201910692609A CN 110487831 A CN110487831 A CN 110487831A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- 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]
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Abstract
The invention discloses the preparation method of speckle and the methods and apparatus for preparing nanogold particle coating speckle.The preparation method of the speckle is the following steps are included: (1) obtains speckle presoma in sample surfaces attachment activity metal film；(2) speckle presoma is heated under vapor atmosphere, active metal film is made to be converted into nanoparticle coating, the vapor phase is inert for the active metal, and the sample does not change during heating；(3) stop heating and speckle is prepared in sample surfaces.In the present invention, the preparation process of entire speckle is physical process, and damage will not be generated to sample or properties of samples is made to change, promotes the practicability of EBSD and DIC result.Meanwhile speckle is by active metal film in-situ preparation, and the thickness of active metal film and position are easily controllable, therefore the precision of speckle is high and easily obtain and control, facilitates the accuracy for promoting characterization result.
Description
Technical field
The present invention relates to optical measurement mechanicses, the technical field of deformation measurement, in particular to the preparation method and system of speckle
The method and apparatus of standby nanogold particle coating speckle.
Background technique
With modern material the reach of science, material science, solid power are had become to the microscopic sdIBM-2+2q.p.approach of material behavior
The problem of being paid much attention in etc. fields.Electron backscatter diffraction (EBSD) technology is as the analysis hand developed rapidly in recent years
Section can be orientated the crystallite dimension of material crystals, crystal grain, and texture is analyzed.Since EBSD technology is based on electronic diffraction
Imaging, has some limitations, can not provide intuitively to displacement of the material in deformation process under meso-scale and strain
With accurate measurement.Therefore the measurement of the displacement and strain by contactless method to material in deformation process becomes
It obtains particularly important.
Loading by means of digital image correlation method (DIC) have measurement accuracy it is higher, it is multiple dimensioned measurement and it is contactless the features such as, gradually at
For one of displacement and the measurement method strained in research material deformation process.DIC is that speckle is prepared on specimen surface, is passed through
Shooting applies the speckle pattern of sample before and after external force load, carries out relevant operation according to speckle pattern and obtains the displacement field of specimen surface
With the method for strain field.
By effective differentiation for combining not only available material microstructure in deformation process of EBSD and DIC, may be used also
Intuitively to obtain the variation of displacement field and strain field in material deformation process, this is undoubtedly a great technological break-through.But
It is that speckle pattern used in loading by means of digital image correlation method is usually by uniform in size, and distribution is random and scattered with certain gray scale
Spot composition.Since speckle is carrier as material surface deformation information, the quality of speckle in loading by means of digital image correlation method
It is the key factor for determining test success or failure.It is well known that EBSD technology is more demanding to the polishing on sample surface, pass
System experimental provision used, such as spraying, have been unable to reach requirement of the EBSD to material surface, if EBSD to be carried out test
It needs to remove speckle and surface is processed by shot blasting, it is not only cumbersome in this way, and it is unable to satisfy loading experiment in situ.It can
To see, EBSD test needs to be highly polished substrate to be measured, and DIC test needs that speckle is arranged in substrate surface to be measured,
This contradiction point is one of the maximum technology barrier for combining EBSD and DIC.
Present inventor expects, if it is possible to prepare and meet DIC test, and not generate interference to EBSD signal
Speckle, the obstacle that EBSD and DIC can be overcome to be difficult to combine.But the deformation of material part is often complexity, conventional dissipates
Required required precision has been not achieved in spot preparation method, this means that DIC speckle needs higher precision that can just obtain standard
True information.For example, Chinese invention patent CN101832759A discloses a kind of production method of micro-nano-scale speckle, the party
Method is etched specimen surface using focused ion beam system to obtain speckle, and this method can not only can make specimen surface
The parsing of EBSD is influenced at destruction, and cost of manufacture is high, it is difficult to promote.Chinese invention patent CN120506733B is disclosed
A kind of production method of micro-nano-scale speckle, this method are applied by using epoxy hardener and powder in sample surfaces solid
The mode of change prepares speckle, and this method speckle during baking can reunite, and can similarly cause to sample surfaces centainly
Pollution to influence the captures of EBSD data, and contrast is insufficient under a scanning electron microscope for speckle made from the method, shadow
Ring the accuracy of DIC data.In conclusion some are unable to satisfy the demand of EBSD test in the existing method for preparing speckle,
Some are complicated for operation, and cost of manufacture is high, and the purpose of the preparation method of above-mentioned speckle is only that and promotes speckle quality, is promoted
The accuracy of DIC test, and do not point out these speckles also and can be applied to the test of EBSD.
Summary of the invention
The main purpose of the present invention is to provide the preparation method of speckle and the methods for preparing nanogold particle coating speckle
And equipment, to solve the technical issues of speckled resolution is low in the prior art and has damage to sample surfaces.
To achieve the goals above, according to an aspect of the invention, there is provided the preparation method of speckle.The system of the speckle
Preparation Method the following steps are included:
(1) in sample surfaces attachment activity metal film, speckle presoma is obtained；
(2) speckle presoma is heated under vapor atmosphere, active metal film is made to be converted into nanoparticle coating, institute
It is inert for the active metal to state vapor phase, the sample does not change during heating；
(3) stop heating and speckle is prepared in sample surfaces.
Since there are the notable differences on the order of magnitude for the thickness and the thickness of sample of active metal film, in lower temperature
Under degree, sample can also maintain original property, and active metal film can occur under the premise of sample maintains original property
Physical change and be converted into nano particle.Entire heating process is reacted under vapor atmosphere, i.e., entire reaction can the temperature difference compared with
It is carried out under small atmosphere, prevents nano particle from occurring to condense agglomeration because of the lasting larger temperature difference.In the whole process, it steams
Gas occurs to spread to active metal film surface, desorb by the absorption of active metal film surface, from active metal film surface and to air
The physical motion process of middle diffusion can't be chemically reacted with active metal film, to will not influence the work of active metal
Property.As it can be seen that the preparation process of entire speckle is physical process in the present invention, damage will not be generated to sample or make properties of samples
It changes, promotes the practicability of EBSD and DIC result.Meanwhile speckle is by active metal film in-situ preparation, and active metal film
Thickness and position it is easily controllable, therefore the precision of speckle is high and easily obtain and control, helps to promote the accurate of characterization result
Property.
To achieve the goals above, according to another aspect of the present invention, nanogold particle coating speckle is additionally provided
Preparation method.The preparation method of the nanogold particle coating speckle the following steps are included:
(1) sample is obtained；
(2) adhere to golden film in sample surfaces, obtain speckle presoma；
(3) speckle presoma is heated under vapor atmosphere, golden film is made to be converted into nanogold particle coating, the steaming
Gas phase is inert for gold, and the sample does not change during heating；
(4) stop heating and nanogold particle coating speckle is prepared in sample surfaces.
In gold, silver powder, aluminium powder, tungsten powder isoreactivity metal, golden atomic number is big, and gold particle is more under an electron microscope
It is bright, good contrast can be provided.And gold particle is expensive, using common method such as spraying, focused ion beam etching method
Etc. the waste for be easy to causeing nanogold particle.Using the preparation method of nanogold particle coating speckle of the invention, simple process,
The precision of gained nanogold particle coating speckle is high and easily obtains and controls, and not only facilitates the accuracy for promoting characterization result,
And it is at low cost, practical.
Further, the golden film with a thickness of 40-100nm.When the thickness of golden film is higher than above-mentioned numberical range, it is difficult to
Form the gold particle of nano-scale.When the thickness of golden film is lower than above-mentioned numberical range, the nanogold particle of formation is seldom and not
Enough densifications, are not achieved the effect of speckle.
Further, it is described be heated to be keep the temperature 60-90min at 270-300 DEG C.When temperature is higher than above range, meeting
Lines is formed, the precision of speckle is reduced.When temperature is lower than above range, golden film is difficult to happen the physics change for being converted into particle
Change.In above-mentioned time range, it is ensured that golden film is fully converted to gold particle.
Further, the sample is nickel, nickel alloy, titanium, titanium alloy, chromium, evanohm, cobalt, cobalt alloy or stainless steel.This
The good combination property of a little samples, is able to maintain the stability of crystal grain, to tie up at a temperature of golden film is converted into nanogold particle
Hold the stability of physico-chemical property.
Further, step (1) further includes being surface-treated to sample.Surface treatment preferably polishes, in this way can be with
Promote the precision of speckle.
Further, the steam is vapor.The chemical property of vapor is stablized, harmless, easily obtains, will not
Damage sample.
Further, the steam vaporizes to obtain by the liquid being heated jointly with the speckle presoma.As a result, into one
It walks and simplifies technique, promote formation efficiency.
Further, golden film is adhered in sample surfaces using vacuum coater.Thus, it is possible to be quickly obtained the good gold of quality
Film.
To achieve the goals above, according to another aspect of the present invention, additionally provide prepare nanogold particle coating dissipate
The equipment of spot.This prepares the equipment of nanogold particle coating speckle, including speckle presoma is heated warm table, place
In on the warm table and form the collector mat in vapor storage space, in the collector mat and by the warm table heat
Liquid storage tank and the gas vent on the collector mat, the speckle presoma be placed in it is where the collector mat plus
In thermal station, the speckle presoma includes sample and the golden film for being attached to sample surfaces, after warm table heating, the gold
Film is converted into nanogold particle coating speckle.
As it can be seen that compared to the equipment that the methods of traditional spraying, focused ion beam etching method use, preparation of the invention
The structure of the equipment of nanogold particle coating speckle is very simple, can quick assembly and disassembly, and be especially advantageous for safeguarding, very
It is suitable for preparing the speckle of high-quality.
The present invention is described further with reference to the accompanying drawings and detailed description.The additional aspect of the present invention and excellent
Point will be set forth in part in the description, and partially will become apparent from the description below, or practice through the invention
It solves.
Detailed description of the invention
The attached drawing for constituting a part of the invention is used to assist the understanding of the present invention, content provided in attached drawing and its
Related explanation can be used for explaining the present invention in the present invention, but not constitute an undue limitation on the present invention.In the accompanying drawings:
Fig. 1 is the SEM photograph of the primary sample (being free of speckle) of the embodiment of the present invention 1.
Fig. 2 is the IPF figure of the primary sample (being free of speckle) of the embodiment of the present invention 1.
Fig. 3 is the SEM photograph after the sample of the embodiment of the present invention 1 is loaded for the first time.
Fig. 4 is the stacking chart of gained crystal boundary figure and strain field figure after the sample of the embodiment of the present invention 1 is loaded for the first time.
Fig. 5 is the SEM photograph after the sample of the embodiment of the present invention 1 is loaded for the second time.
Fig. 6 is the stacking chart of gained crystal boundary figure and strain field figure after the sample of the embodiment of the present invention 1 is loaded for the second time.
Fig. 7 is the SEM photograph after the sample of the embodiment of the present invention 1 is loaded for the third time.
Fig. 8 is the stacking chart of gained crystal boundary figure and strain field figure after the sample of the embodiment of the present invention 1 is loaded for the third time.
Fig. 9 is the SEM photograph of the non-load sample surface speckle of the embodiment of the present invention 1.
Figure 10 is the structural schematic diagram for the equipment that the present invention prepares nanogold particle coating speckle.
Specific embodiment
Clear, complete explanation is carried out to the present invention with reference to the accompanying drawing.Those of ordinary skill in the art are being based on these
The present invention will be realized in the case where explanation.Before in conjunction with attached drawing, the present invention will be described, of particular note is that:
The technical solution provided in each section including following the description and technical characteristic in the present invention are not rushing
In the case where prominent, these technical solutions and technical characteristic be can be combined with each other.
In addition, the embodiment of the present invention being related in following the description is generally only the embodiment of present invention a part, and
The embodiment being not all of.Therefore, based on the embodiments of the present invention, those of ordinary skill in the art are not making creativeness
Every other embodiment obtained, should fall within the scope of the present invention under the premise of labour.
About term in the present invention and unit.Term in description and claims of this specification and related part
" comprising ", " having " and their any deformation, it is intended that cover and non-exclusive include.
The preparation method of speckle of the invention the following steps are included:
(1) in sample surfaces attachment activity metal film, speckle presoma is obtained；
(2) speckle presoma is heated under vapor atmosphere, active metal film is made to be converted into nanoparticle coating, institute
It is inert for the active metal to state vapor phase, the sample does not change during heating；
(3) stop heating and speckle is prepared in sample surfaces.
Wherein, the active metal is silver, gold, aluminium or tungsten.The sample is nickel, nickel alloy, titanium, titanium alloy, chromium, chromium conjunction
Gold, cobalt, cobalt alloy or stainless steel.
Illustrate beneficial effects of the present invention below by way of specific embodiment.
Embodiment 1
The preparation method of nanogold particle coating speckle, comprising the following steps:
(1) sample is obtained: using the two phase stainless steel after surface polishing as sample, with a thickness of 8mm；
(2) adhere to golden film in sample surfaces, obtain speckle presoma, golden film with a thickness of 80nm；
(3) speckle presoma is heated under steam atmosphere, heating temperature is 280 DEG C, and soaking time is
90min, in heating process, golden film is converted into nanogold particle coating；
(4) stop heating and nanogold particle coating speckle is prepared in sample surfaces.
Characterization result:
It carries out SEM and EBSD to primary sample (being free of speckle) first to characterize, as a result as depicted in figs. 1 and 2.Then to system
Sample after obtaining speckle is loaded, and is loaded 3 times altogether, and the deflection loaded every time is 2%, and load carries out SEM after the completion every time
Characterization, and loading by means of digital image correlation method is carried out to SEM photograph and handles to obtain strain field, then it is superimposed crystal boundary figure to obtain stacking chart.
Fig. 3 and Fig. 4 is respectively the SEM photograph of sample and the stacking chart of crystal boundary figure and strain field figure after loading for the first time, and Fig. 5 and Fig. 6 divide
The SEM photograph of sample and the stacking chart of crystal boundary figure and strain field figure after Wei not loading for second, Fig. 7 and Fig. 8 are respectively third time
The stacking chart of the SEM photograph of sample and crystal boundary figure and strain field figure after load.It will be clear that crystal from Fig. 4,6,8
Slip information and local train size illustrate that the quality of speckle is high.Fig. 9 is the SEM photograph of speckle, it can be seen that golden film has converted
The gold particle for being tens nanometers for granularity.
Embodiment 2
The preparation method of nanogold particle coating speckle, comprising the following steps:
(1) sample is obtained: using the nickel plate after surface polishing as sample, with a thickness of 10mm；
(2) adhere to golden film in sample surfaces, obtain speckle presoma, golden film with a thickness of 40nm；
(3) speckle presoma is heated under steam atmosphere, heating temperature is 260 DEG C, and soaking time is
60min, in heating process, golden film is converted into nanogold particle coating；
(4) stop heating and nanogold particle coating speckle is prepared in sample surfaces.
Embodiment 3
The preparation method of nanogold particle coating speckle, comprising the following steps:
(1) sample is obtained: using the titanium plate after surface polishing as sample, with a thickness of 5mm；
(2) adhere to golden film in sample surfaces, obtain speckle presoma, golden film with a thickness of 100nm；
(3) speckle presoma is heated under steam atmosphere, heating temperature is 300 DEG C, and soaking time is
70min, in heating process, golden film is converted into nanogold particle coating；
(4) stop heating and nanogold particle coating speckle is prepared in sample surfaces.
Embodiment 4
The preparation method of nanogold particle coating speckle, comprising the following steps:
(1) sample is obtained: using the titanium alloy after surface polishing as sample, with a thickness of 5mm；
(2) adhere to golden film in sample surfaces, obtain speckle presoma, golden film with a thickness of 60nm；
(3) speckle presoma is heated under steam atmosphere, heating temperature is 270 DEG C, and soaking time is
80min, in heating process, golden film is converted into nanogold particle coating；
(4) stop heating and nanogold particle coating speckle is prepared in sample surfaces.
Embodiment 5
Compared with Example 1, the difference that the preparation method of the nanogold particle coating speckle of the present embodiment has is: not adopting
It is kept the temperature with steam, but directly speckle presoma is heated.As a result, it has been found that the gold particle size of gained speckle is obvious
Greater than the size of the gold particle of embodiment 1.
Embodiment 1-5 is all made of vacuum coater and adheres to golden film in sample surfaces.
The equipment for preparing nanogold particle coating speckle that above-described embodiment 1-5 is used is as shown in Figure 10, including to speckle
Warm table 1 that presoma 5 is heated, is set to the collector mat 2 for being placed on the warm table 1 and forming vapor storage space
The liquid storage tank 3 and the gas vent 4 on the collector mat 2 heated in the collector mat 2 and by the warm table 1.
The gas vent 4 is set to the lower part of collector mat 2, is sufficient filling with entire collector mat 2 in this way convenient for steam, to play preferable protect
Temperature effect.In use, enough liquid is placed in liquid storage tank 3 first, then place speckle presoma 5 and make golden film to
Then upper placement runs warm table 1, before making the liquid and speckle in liquid storage tank 3 so that golden film be made to come into full contact with steam
It is jointly heated to drive body 5.
Related content of the invention is illustrated above.Those of ordinary skill in the art are in the feelings illustrated based on these
The present invention will be realized under condition.Based on above content of the invention, those of ordinary skill in the art are not making creativeness
Every other embodiment obtained, should fall within the scope of the present invention under the premise of labour.
Claims (10)
1. the preparation method of speckle, it is characterised in that: the following steps are included:
(1) in sample surfaces attachment activity metal film, speckle presoma is obtained；
(2) speckle presoma is heated under vapor atmosphere, active metal film is made to be converted into nanoparticle coating, the steaming
Gas phase is inert for the active metal, and the sample does not change during heating；
(3) stop heating and speckle is prepared in sample surfaces.
2. the preparation method of nanogold particle coating speckle, it is characterised in that: the following steps are included:
(1) sample is obtained；
(2) adhere to golden film in sample surfaces, obtain speckle presoma；
(3) speckle presoma is heated under vapor atmosphere, golden film is made to be converted into nanogold particle coating, the vapor phase
Inert for gold, the sample does not change during heating；
(4) stop heating and nanogold particle coating speckle is prepared in sample surfaces.
3. the preparation method of nanogold particle coating speckle as claimed in claim 2, it is characterised in that: the thickness of the golden film
For 40-100nm.
4. the preparation method of nanogold particle coating speckle as claimed in claim 2, it is characterised in that: described to be heated to be
60-90min is kept the temperature at 270-300 DEG C.
5. the preparation method of nanogold particle coating speckle as claimed in claim 2, it is characterised in that: the sample be nickel,
Nickel alloy, titanium, titanium alloy, chromium, evanohm, cobalt, cobalt alloy or stainless steel.
6. the preparation method of nanogold particle coating speckle as claimed in claim 2, it is characterised in that: step (1) further includes
Sample is surface-treated.
7. the preparation method of nanogold particle coating speckle as claimed in claim 2, it is characterised in that: the steam is water steaming
Gas.
8. the preparation method of nanogold particle coating speckle as claimed in claim 2, it is characterised in that: the steam by with
The liquid that the speckle presoma is heated jointly vaporizes to obtain.
9. the preparation method of nanogold particle coating speckle as claimed in claim 2, it is characterised in that: use vacuum coater
Adhere to golden film in sample surfaces.
10. the equipment for preparing nanogold particle coating speckle, it is characterised in that: including the heating heated to speckle presoma
Platform, is set in the collector mat and by the heating collector mat for being placed on the warm table and forming vapor storage space
The liquid storage tank and the gas vent on the collector mat, the speckle presoma of platform heating are placed in the collector mat
On the warm table at place, the speckle presoma includes sample and the golden film for being attached to sample surfaces, is heated through the warm table
Afterwards, the golden film is converted into nanogold particle coating speckle.
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Cited By (2)
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| CN111380750A (en) * | 2020-04-13 | 2020-07-07 | 北京科技大学 | Amnion tissue non-contact full-field deformation measurement method using methylene blue to make spots |
| CN112485280A (en) * | 2020-11-23 | 2021-03-12 | 江苏理工学院 | Speckle preparation method for high-resolution local strain analysis of metal material |
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