CN110487831B - Preparation method of speckles and method and equipment for preparing gold nanoparticle coating speckles - Google Patents
Preparation method of speckles and method and equipment for preparing gold nanoparticle coating speckles Download PDFInfo
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Abstract
The invention discloses a preparation method of speckles and a method and equipment for preparing gold nanoparticle coating speckles. The preparation method of the speckle comprises the following steps: (1) attaching an active metal film on the surface of a sample to obtain a speckle precursor; (2) heating the speckle precursor in a steam atmosphere to convert the active metal film into the nanoparticle coating, wherein the steam is inert relative to the active metal, and the sample does not change in the heating process; (3) and stopping heating to prepare speckles on the surface of the sample. In the invention, the whole speckle preparation process is a physical process, so that the sample is not damaged or the properties of the sample are not changed, and the practicability of EBSD and DIC results is improved. Meanwhile, the speckles are generated in situ by the active metal film, and the thickness and the position of the active metal film are easy to control, so that the speckles are high in precision and easy to obtain and control, and the accuracy of a representation result is improved.
Description
Technical Field
The invention relates to the technical field of optical measurement mechanics and deformation measurement, in particular to a method for preparing speckles and a method and equipment for preparing gold nanoparticle coating speckles.
Background
With the development of modern material science, the microscopic characterization of the mechanical behavior of the material becomes a very important problem in the fields of material science, solid mechanics and the like. Electron Back Scattering Diffraction (EBSD) technology has been developed as a rapid analysis means in recent years, and can analyze the grain size, grain orientation, and texture of material crystals. Because the EBSD technology is based on electron diffraction imaging, there is a certain limitation that it cannot provide intuitive and more accurate measurement for displacement and strain of a material in a mesoscopic scale during deformation. The measurement of the displacement and strain of the material during deformation by non-contact methods becomes particularly important.
Digital Image Correlation (DIC) has the characteristics of high measurement precision, multi-scale measurement, non-contact type and the like, and is gradually one of measurement methods for researching displacement and strain in the material deformation process. DIC is a method of preparing speckles on the surface of a sample, photographing speckle patterns of the sample before and after an external force load is applied, and performing related operation according to the speckle patterns to obtain a displacement field and a strain field of the surface of the sample.
By effectively combining the EBSD and the DIC, the evolution of the microstructure of the material in the deformation process can be obtained, and the changes of the displacement field and the strain field in the deformation process of the material can be visually obtained, which is undoubtedly a great technical breakthrough. However, the speckle pattern used in the digital image correlation method generally consists of speckles with uniform size, random distribution and certain gray scale. Since the speckle is used as a carrier of deformation information of the material surface in the digital image correlation method, the quality of the speckle is a key factor for determining the success or failure of the test. As is known, the EBSD technology has a high requirement for the polishing degree of the surface of a sample to be tested, and a conventional experimental apparatus, such as a paint spraying method, cannot meet the requirement of EBSD on the surface of a material, and when an EBSD test is performed, speckles need to be removed and the surface needs to be polished, which is not only tedious in operation, but also cannot meet the in-situ loading experiment. It can be seen that the EBSD test requires high polishing of the substrate to be tested, and the DIC test requires speckle to be disposed on the surface of the substrate to be tested, which is one of the biggest technical obstacles to the combination of EBSD and DIC.
The inventor of the present application thinks that if speckle which satisfies DIC test and does not interfere with EBSD signal can be prepared, the obstacle that EBSD and DIC are difficult to combine can be overcome. However, local deformation of materials is often complex, and the conventional speckle preparation method cannot meet the required precision requirement, which means that DIC speckle needs higher precision to obtain accurate information. For example, chinese patent CN101832759A discloses a method for manufacturing micro-nano speckle, in which a focused ion beam system is used to etch the surface of a sample to obtain the speckle, and this method will not only damage the surface of the sample and affect the EBSD analysis, but also has high manufacturing cost and is difficult to popularize. The Chinese invention patent CN120506733B discloses a method for manufacturing micro-nano-scale speckles, which prepares the speckles by coating and curing epoxy curing agent and powder on the surface of a sample, the speckles can be agglomerated in the baking process and can also cause certain pollution on the surface of the sample to influence the capture of EBSD data, and the speckle manufactured by the method has insufficient contrast under a scanning electron microscope and influences the accuracy of DIC data. In summary, some of the existing speckle preparation methods cannot meet the requirements of EBSD testing, some are complex to operate and high in manufacturing cost, and the purpose of the speckle preparation method is to improve the quality of speckles and improve the accuracy of DIC testing, but it is not pointed out that the speckles can also be applied to EBSD testing.
Disclosure of Invention
The invention mainly aims to provide a speckle preparation method, a method and equipment for preparing gold nanoparticle coating speckles, and aims to solve the technical problems that in the prior art, the speckle resolution is low and the surface of a sample is damaged.
In order to achieve the above object, according to one aspect of the present invention, a method of preparing speckles is provided. The preparation method of the speckle comprises the following steps:
(1) attaching an active metal film on the surface of a sample to obtain a speckle precursor;
(2) heating the speckle precursor in a steam atmosphere to convert the active metal film into the nanoparticle coating, wherein the steam is inert relative to the active metal, and the sample does not change in the heating process;
(3) and stopping heating to prepare speckles on the surface of the sample.
Because the thickness of the active metal film is obviously different from the thickness of the sample in magnitude order, the sample can maintain the original property at a lower temperature, and the active metal film can be converted into the nano-particles by biological change on the premise that the sample maintains the original property. The whole heating process is carried out in the steam atmosphere, namely the whole reaction can be carried out in the atmosphere with small temperature difference, and the condensation and agglomeration phenomenon of the nano particles due to continuous large temperature difference is prevented. In the whole process, the vapor generates the physical movement process of diffusing to the surface of the active metal film, being adsorbed by the surface of the active metal film, being desorbed from the surface of the active metal film and diffusing to the air, and does not generate chemical reaction with the active metal film, thereby not influencing the activity of the active metal. Therefore, in the invention, the whole speckle preparation process is a physical process, so that the sample is not damaged or the properties of the sample are not changed, and the practicability of EBSD and DIC results is improved. Meanwhile, the speckles are generated in situ by the active metal film, and the thickness and the position of the active metal film are easy to control, so that the speckles are high in precision and easy to obtain and control, and the accuracy of a representation result is improved.
In order to achieve the above object, according to another aspect of the present invention, there is also provided a method for preparing the gold nanoparticle coating speckle. The preparation method of the gold nanoparticle coating speckle comprises the following steps:
(1) obtaining a sample;
(2) attaching a gold film on the surface of the sample to obtain a speckle precursor;
(3) heating the speckle precursor in a steam atmosphere to convert the gold film into a nano gold particle coating, wherein the steam is inert relative to gold, and the sample does not change in the heating process;
(4) and stopping heating, namely preparing the nano gold particle coating speckles on the surface of the sample.
In active metals such as gold, silver powder, aluminum powder, tungsten powder and the like, the atomic number of gold is large, and gold particles are brighter under an electron microscope, so that good contrast can be provided. Gold particles are expensive, and the common methods such as a paint spraying method and a focused ion beam etching method are easy to cause the waste of the nano gold particles. The preparation method of the gold nanoparticle coating speckles has the advantages of simple process, high precision of the obtained gold nanoparticle coating speckles, easiness in acquisition and control, contribution to improving the accuracy of characterization results, low cost and strong practicability.
Further, the thickness of the gold film is 40-100 nm. When the thickness of the gold film is higher than the above numerical range, it is difficult to form nano-sized gold particles. When the thickness of the gold film is lower than the numerical range, the formed nano gold particles are few and not dense enough, and the speckle effect cannot be achieved.
Further, the heating is carried out for 60-90min at the temperature of 270-300 ℃. When the temperature is higher than the range, lines can be formed, and the accuracy of speckles is reduced. When the temperature is lower than the above range, the physical change of the gold film into particles hardly occurs. Within the time range, the gold film can be completely converted into gold particles.
Further, the sample is nickel, nickel alloy, titanium alloy, chromium alloy, cobalt alloy, or stainless steel. The samples have good comprehensive performance, and can keep the stability of crystal grains at the temperature of converting the gold film into the nano gold particles, thereby maintaining the stability of physicochemical properties.
Further, the step (1) further comprises performing surface treatment on the sample. The surface treatment is preferably polishing, which may improve the accuracy of the speckle.
Further, the steam is water vapor. The chemical property of the water vapor is stable, the water vapor is harmless to human bodies, the water vapor is easy to obtain, and the sample cannot be damaged.
Further, the vapor is obtained by vaporizing a liquid heated together with the speckle precursor. Therefore, the process is further simplified, and the generation efficiency is improved.
Further, a vacuum coating instrument is adopted to attach a gold film on the surface of the sample. Thus, a gold film having good quality can be obtained quickly.
In order to achieve the above object, according to another aspect of the present invention, there is also provided an apparatus for preparing gold nanoparticle coated speckles. The equipment for preparing the gold nanoparticle coating speckles comprises a heating table for heating a speckle precursor, a heat collection cover arranged on the heating table and forming a steam storage space, a liquid storage tank arranged in the heat collection cover and heated by the heating table, and exhaust holes arranged on the heat collection cover, wherein the speckle precursor is arranged on the heating table where the heat collection cover is arranged, the speckle precursor comprises a sample and a gold film attached to the surface of the sample, and the gold film is converted into the gold nanoparticle coating speckles after the heating table is used for heating.
Therefore, compared with the equipment adopted by the traditional methods such as a paint spraying method, a focused ion beam etching method and the like, the equipment for preparing the nano gold particle coating speckles has a very simple structure, can be quickly assembled and disassembled, is very beneficial to maintenance, and is very suitable for preparing the high-quality speckles.
The invention is further described with reference to the following figures and detailed description. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to assist in understanding the invention, and are included to explain the invention and their equivalents and not limit it unduly. In the drawings:
FIG. 1 is an SEM photograph of an original sample (without speckle) of example 1 of the present invention.
Fig. 2 is a graph of IPF of the original sample (without speckle) of example 1 of the present invention.
FIG. 3 is an SEM photograph of a sample of example 1 of the present invention after the first loading.
FIG. 4 is a superimposed graph of the grain boundary graph and the strain field graph obtained after the sample of example 1 of the present invention is loaded for the first time.
FIG. 5 is an SEM photograph of the sample of example 1 after a second loading.
FIG. 6 is a superimposed graph of the grain boundary graph and the strain field graph obtained after the sample of example 1 of the present invention is loaded for the second time.
FIG. 7 is an SEM photograph of the sample of example 1 after a third loading.
FIG. 8 is a superimposed graph of the grain boundary graph and the strain field graph obtained after the sample of example 1 of the present invention is loaded for the third time.
FIG. 9 is an SEM photograph of speckles on the surface of an unloaded sample of example 1 of the present invention.
Fig. 10 is a schematic structural diagram of the apparatus for preparing gold nanoparticle coating speckles according to the present invention.
Detailed Description
The invention will be described more fully hereinafter with reference to the accompanying drawings. Those skilled in the art will be able to implement the invention based on these teachings. Before the present invention is described in detail with reference to the accompanying drawings, it is to be noted that:
the technical solutions and features provided in the present invention in the respective sections including the following description may be combined with each other without conflict.
Moreover, the embodiments of the present invention described in the following description are generally only some embodiments of the present invention, and not all embodiments. Therefore, all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
With respect to terms and units in the present invention. The terms "comprising," "having," and any variations thereof in the description and claims of this invention and the related sections are intended to cover non-exclusive inclusions.
The preparation method of the speckle comprises the following steps:
(1) attaching an active metal film on the surface of a sample to obtain a speckle precursor;
(2) heating the speckle precursor in a steam atmosphere to convert the active metal film into the nanoparticle coating, wherein the steam is inert relative to the active metal, and the sample does not change in the heating process;
(3) and stopping heating to prepare speckles on the surface of the sample.
Wherein the active metal is silver, gold, aluminum or tungsten. The sample is nickel, nickel alloy, titanium alloy, chromium alloy, cobalt alloy or stainless steel.
The advantageous effects of the present invention are illustrated below by specific examples.
Example 1
The preparation method of the gold nanoparticle coating speckle comprises the following steps:
(1) obtaining a sample: adopting the duplex stainless steel with polished surface as a sample, wherein the thickness of the sample is 8 mm;
(2) attaching a gold film to the surface of the sample to obtain a speckle precursor, wherein the thickness of the gold film is 80 nm;
(3) heating the speckle precursor in a water vapor atmosphere at 280 ℃ for 90min, wherein a gold film is converted into a nano gold particle coating in the heating process;
(4) and stopping heating, namely preparing the nano gold particle coating speckles on the surface of the sample.
And (3) characterization results:
SEM and EBSD characterization was first performed on the original sample (without speckle) and the results are shown in fig. 1 and 2. And then loading the sample with the speckles for 3 times, wherein the deformation of each loading is 2%, performing SEM representation after each loading, performing digital image correlation method processing on the SEM picture to obtain a strain field, and then overlapping the grain boundary pictures to obtain an overlay. Fig. 3 and 4 are a SEM photograph and a grain boundary map and a strain field map of the sample after the first loading, respectively, fig. 5 and 6 are a SEM photograph and a grain boundary map and a strain field map of the sample after the second loading, respectively, and fig. 7 and 8 are a SEM photograph and a grain boundary map and a strain field map of the sample after the third loading, respectively. The slip information and the local strain magnitude of the crystal can be clearly seen from fig. 4, 6 and 8, which shows that the speckle quality is high. Fig. 9 is an SEM photograph of speckles, and it can be seen that the gold film has been converted into gold particles having a particle size of several tens of nanometers.
Example 2
The preparation method of the gold nanoparticle coating speckle comprises the following steps:
(1) obtaining a sample: taking a nickel plate with a polished surface as a sample, wherein the thickness of the nickel plate is 10 mm;
(2) attaching a gold film to the surface of the sample to obtain a speckle precursor, wherein the thickness of the gold film is 40 nm;
(3) heating the speckle precursor in a water vapor atmosphere at 260 ℃ for 60min, wherein in the heating process, the gold film is converted into a nano gold particle coating;
(4) and stopping heating, namely preparing the nano gold particle coating speckles on the surface of the sample.
Example 3
The preparation method of the gold nanoparticle coating speckle comprises the following steps:
(1) obtaining a sample: adopting a titanium plate with a polished surface as a sample, wherein the thickness of the titanium plate is 5 mm;
(2) attaching a gold film to the surface of the sample to obtain a speckle precursor, wherein the thickness of the gold film is 100 nm;
(3) heating the speckle precursor in a water vapor atmosphere at 300 ℃ for 70min, wherein the gold film is converted into a nano gold particle coating in the heating process;
(4) and stopping heating, namely preparing the nano gold particle coating speckles on the surface of the sample.
Example 4
The preparation method of the gold nanoparticle coating speckle comprises the following steps:
(1) obtaining a sample: adopting a titanium alloy with a polished surface as a sample, wherein the thickness of the titanium alloy is 5 mm;
(2) attaching a gold film to the surface of the sample to obtain a speckle precursor, wherein the thickness of the gold film is 60 nm;
(3) heating the speckle precursor in a water vapor atmosphere at the heating temperature of 270 ℃ for 80min, wherein in the heating process, the gold film is converted into a nano gold particle coating;
(4) and stopping heating, namely preparing the nano gold particle coating speckles on the surface of the sample.
Example 5
Compared with the embodiment 1, the preparation method of the gold nanoparticle coating speckle of the embodiment has the following differences: the speckle precursor is directly heated without adopting steam for heat preservation. The resulting speckles were found to have gold particles of a size significantly larger than that of the gold particles of example 1.
In each of examples 1 to 5, a gold film was attached to the surface of the sample by a vacuum coater.
Fig. 10 shows the apparatus for preparing gold nanoparticle coating speckles used in embodiments 1 to 5, which includes a heating table 1 for heating a speckle precursor 5, a heat collection cover 2 placed on the heating table 1 and forming a vapor storage space, a liquid storage tank 3 disposed in the heat collection cover 2 and heated by the heating table 1, and an exhaust hole 4 disposed on the heat collection cover 2. The exhaust holes 4 are formed in the lower portion of the heat collection cover 2, so that steam can fully fill the whole heat collection cover 2, and a good heat preservation effect can be achieved. When the metal film metal speckle drying device is used, enough liquid is placed in the liquid storage tank 3, then the speckle precursor 5 is placed, the metal film is placed upwards, the metal film is fully contacted with steam, and then the heating table 1 is operated, so that the liquid in the liquid storage tank 3 and the speckle precursor 5 are heated together.
The contents of the present invention have been explained above. Those skilled in the art will be able to implement the invention based on these teachings. All other embodiments, which can be derived by a person skilled in the art from the above description without inventive step, shall fall within the scope of protection of the present invention.
Claims (5)
1. The testing method of the nanometer gold particle coating speckle is characterized in that: the method comprises the following steps:
(1) obtaining a sample;
(2) attaching a gold film on the surface of the sample to obtain a speckle precursor;
(3) heating the speckle precursor in a steam atmosphere to convert the gold film into a nano gold particle coating, wherein the steam is inert relative to gold, and the sample does not change in the heating process;
(4) stopping heating, namely preparing the gold nanoparticle coating speckles on the surface of the sample;
the thickness of the gold film is 40-100 nm;
the heating is carried out for 60-90min at the temperature of 270-300 ℃;
the sample with the gold nanoparticle coating speckles can be subjected to DIC analysis and EBSD test at the same time, and specifically comprises the following steps: directly carrying out SEM test and EBSD test on the same part of the sample after each loading, obtaining a strain field diagram through the SEM test, obtaining a grain boundary diagram through the EBSD test, superposing the grain boundary diagram and the strain field diagram to obtain a superposed diagram, and comparing the superposed diagram after each stretching to see the slippage information and the local strain of the crystal;
the sample is nickel, nickel alloy, titanium, chromium alloy, cobalt or cobalt alloy.
2. The method for testing the speckle of the gold nanoparticle coating of claim 1, wherein: the step (1) further comprises carrying out surface treatment on the sample.
3. The method for testing the speckle of the gold nanoparticle coating of claim 1, wherein: the steam is water vapor.
4. The method for testing the speckle of the gold nanoparticle coating of claim 1, wherein: the vapor is obtained by vaporizing a liquid heated together with the speckle precursor.
5. The method for testing the speckle of the gold nanoparticle coating of claim 1, wherein: and adhering a gold film on the surface of the sample by using a vacuum coating instrument.
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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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