CN118130191A - Preparation method and application of high-temperature laser scanning confocal microscope small-size in-situ observation sample - Google Patents
Preparation method and application of high-temperature laser scanning confocal microscope small-size in-situ observation sample Download PDFInfo
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Abstract
The invention relates to the technical field of in-situ observation sample preparation, in particular to a preparation method and application of a high-temperature laser scanning confocal microscope small-size in-situ observation sample. The preparation method comprises the following steps: obtaining an observation sample to be treated; obtaining a hand-held embedded sample through a metallographic sample embedding machine and forming a blind hole; placing an observation sample to be treated in each blind hole, bonding a first plane of the observation sample to be treated to the blind holes through an adhesive, and then carrying out first grinding on a second plane; separating the observation sample to be treated from the blind hole, and adhering a second plane of the observation sample to be treated to the bottom of the blind hole through an adhesive, wherein the second plane is parallel to the first plane, then carrying out second grinding and polishing on the first plane, and separating the observation sample to be treated from the blind hole after polishing is finished. The method can realize the preparation of the high-temperature laser scanning confocal microscope small-size in-situ observation sample through the conventional metallographic sample embedding machine, and is simple in operation, efficient and quick.
Description
Technical Field
The invention relates to the technical field of in-situ observation sample preparation, in particular to a preparation method and application of a high-temperature laser scanning confocal microscope small-size in-situ observation sample.
Background
The high-temperature laser scanning confocal microscope is used as a powerful tool for researching the phase change and microstructure change of the metal material at high temperature, can realize real-time, in-situ and high-definition observation and analysis of the microstructure change (melting, solidification, crystallization, solid phase change and the like) of the metal material such as steel and the like, and is mainly applied to the scientific research fields such as mineral processing, metal smelting, heat treatment of the metal material, research on the phase change mechanism in the steel and the like. The high-temperature laser scanning confocal microscope consists of a high-temperature image heating observation system and a digital purple laser scanning confocal microscope, can present images with large depth of field and high quality in the temperature change range of room temperature to 1800 ℃ and continuously and automatically store the images according to a program temperature control curve.
The problem is that the in-situ observation of the sample size is usually required to be a small cylinder with a diameter of less than 8mm and a height of less than 4mm due to the uniqueness of the heating furnace body structure of the high-temperature laser scanning confocal microscope. Before an in-situ observation experiment is carried out by using a high-temperature laser scanning confocal microscope, the preparation of a small-size sample meeting the requirements is a necessary link, however, the small-size sample is not easy to hold and run, the difficulty of grinding and polishing is greatly increased, uneven stress is caused when the small-size sample is ground and polished, inclination, multiple surface scratches and poor flatness are caused, the high-temperature laser scanning confocal microscope is not easy to focus in a plane and image suddenly and suddenly appears dark due to a final inclined-plane sample, meanwhile, the solid-state phase transformation and dynamic process analysis are hindered by scratch ravines with different depths, the in-situ observation effect and the image data processing result are seriously influenced, the capturing details are lost, and the uniqueness of the in-situ observation function cannot be exerted.
In order to solve the problems, application number CN201911054641.4 discloses an observation auxiliary tool for a high-temperature laser confocal microscope sample and a use method, the auxiliary tool comprises a seat body, a screw and a wafer sample, the seat body is cylindrical, a plurality of threaded holes penetrating through are uniformly formed in the circumference of the seat body, the screw is meshed in the threaded holes, the screw is formed by removing the top of a traditional screw and grinding, a placing groove is formed in the top surface of the screw, the wafer sample is fixedly connected in the placing groove, and the use method comprises sample installation, sample grinding and sample observation. But this kind of utensil of assisting has restricted the shape and the size of sample, only is suitable for the disk sample to the diameter size of requiring the disk sample is less than the diameter of standing groove, and it is fixed to blow the rosin with the hot-blast rifle in addition, when lofting, sampling, with manual adjustment disk sample roughness of glass piece, the installation dismantlement is loaded down with trivial details, and is difficult for guaranteeing that the sample is pure flat, need handheld the utensil of assisting of pressing downwards during the grinding, can't guarantee that the observation face after the preparation is even, the circumstances that the observation face is inclined easily appears after the grinding.
Application number CN202110202128.6 discloses a preparation method of a steel sample for high-temperature confocal microscope observation, which comprises the following steps: selecting a target sample, embedding the target sample, polishing the target sample, and taking out the target sample; placing a target sample grinding surface a on a first mosaic cylinder base downwards, and adding mosaic materials to prepare a first mosaic block; placing the surface b of the first mosaic block opposite to the surface a downwards on a second mosaic cylinder base, and adding mosaic materials to prepare a second mosaic block; polishing the b surface of the second mosaic block until the cross section of the target sample is completely exposed, and automatically polishing; and taking out the target sample in the treated second mosaic block, cleaning the target sample by an ultrasonic cleaner, and then placing the target sample under a high-temperature confocal microscope for experiments. However, the method needs to inlay the sample for 3 times, and after the inlaid sample is ground and polished, the inlaid sample is destroyed twice by hammering and cutting to take out the in-situ observation sample.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide a preparation method of a high-temperature laser scanning confocal microscope small-size in-situ observation sample, which is simple and convenient, and can realize the preparation of the high-temperature laser scanning confocal microscope small-size in-situ observation sample by a conventional metallographic sample embedding machine, thereby solving the problems that a fixture is specially designed, the fixture cannot be worn, the sample is embedded for a plurality of times, the time and the material are wasted, the sample is not easy to take out, the upper bottom surface and the lower bottom surface of the sample cannot be absolutely parallel, the scratches are more and the like in the prior art.
The second object of the invention is to provide an application of the high-temperature laser scanning confocal microscope small-size in-situ observation sample prepared by the preparation method of the high-temperature laser scanning confocal microscope small-size in-situ observation sample in observing and analyzing the phase change and microstructure change of the metal material.
In order to achieve the above object of the present invention, the following technical solutions are specifically adopted:
the invention firstly provides a preparation method of a small-size in-situ observation sample of a high-temperature laser scanning confocal microscope, which comprises the following steps:
(a) Obtaining one or more observation samples to be treated;
(b) Obtaining a hand-held embedded sample through a metallographic sample embedding machine, and forming one or more blind holes matched with the observation sample to be processed on the hand-held embedded sample;
(c) Placing each observation sample to be treated in each blind hole, bonding a first plane of the observation sample to be treated to the bottom of each blind hole through an adhesive, and then carrying out first grinding on the second plane;
(d) And separating the observation sample to be treated from the blind hole, and adhering a second plane of the observation sample to be treated to the bottom of the blind hole through an adhesive, wherein the second plane is parallel to the first plane, then carrying out second grinding and polishing on the first plane, and separating the observation sample to be treated from the blind hole after polishing is finished to obtain the small-size in-situ observation sample of the treated high-temperature laser scanning confocal microscope.
The invention further provides application of the high-temperature laser scanning confocal microscope small-size in-situ observation sample prepared by the preparation method of the high-temperature laser scanning confocal microscope small-size in-situ observation sample in observing and analyzing phase change and microstructure change of the metal material.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the preparation method of the small-size in-situ observation sample of the high-temperature laser scanning confocal microscope, provided by the invention, the used auxiliary device is simple in structure, convenient and easy to obtain, the solid embedded sample is obtained on the basis of fully utilizing a tool (namely a metallographic sample embedding machine) used for preparing a conventional metallographic sample in the field of metal materials, the surfaces of the solid embedded sample are flexibly processed according to actual requirements, blind holes with various sizes and shapes are obtained for combined installation with the small-size in-situ observation sample, and the method does not need to design and customize a small-size sample clamp specially, and the processed blind holes have low requirements on precision, so that the requirements on the blind holes are really changed according to requirements.
(2) According to the preparation method of the small-size in-situ observation sample of the high-temperature laser scanning confocal microscope, which is provided by the invention, the in-situ observation sample is simple to mount and dismount, the high-efficiency and convenient sample preparation can be realized, the hand-held embedded sample with the blind hole and the small-size sample to be treated can be quickly adhered together through the adhesive, the structure is firm and stable, and the problems of running, tilting and the like of the sample are avoided; meanwhile, the adhered glue is dissolved through the organic reagent after polishing, so that the quick disassembly can be realized, and the dissolution and separation process is finished under the condition of liquid seal, so that the problem that the surface of part of materials is easy to oxidize after polishing is solved.
(3) The preparation method of the small-size in-situ observation sample of the high-temperature laser scanning confocal microscope is easy to operate, the used handheld embedded sample is easy to hold, so that the grinding and polishing operation difficulty of the small-size sample is greatly reduced, the method is not only suitable for metallographic grinding and polishing personnel with long experience, but also is suitable for personnel for preparing the small-size sample by first contacting, the large shell is assembled through the small sample, the purposes of large size, low difficulty and finishing grinding and polishing are realized, and a smooth, parallel and nearly traceless in-situ observation surface can be obtained.
(4) The preparation method of the high-temperature laser scanning confocal microscope small-size in-situ observation sample can improve the surface quality and reduce the raw material cost. Compared to custom permanent sample holders, it is often not possible to wear due to the precision requirements that they have. The in-situ observation handheld mosaic sample used in the invention has low cost, one-time processing combination can be used for multiple times, the grinding and polishing flatness of the surface of the small-size sample can be worn along with the grinding and polishing process of the surface of the small-size sample, the difficult problem that the grinding and polishing flatness of the surface of the small-size sample is seriously dependent on the original machining surface is solved, the correction function is realized, even if the upper bottom surface and the lower bottom surface of the original sample which are not ground and polished are seriously unparallel, the sample with the upper bottom surface and the lower bottom surface being parallel can be prepared through absolute parallelism of the upper bottom surface of the mosaic sample and firm combination of the small-size sample and the blind hole mosaic sample.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of a method for obtaining a hand-held mosaic sample by a metallographic sample mosaic machine according to the present invention;
FIG. 2 is a schematic diagram of a hand-held inlay sample with blind holes according to the present invention;
FIG. 3 is a schematic view of the installation of a hand-held inlay sample and an observation sample to be treated in example 1 provided by the present invention;
FIG. 4 is a graph of a room temperature golden phase of a small-sized in situ observation sample obtained in example 1 according to the present invention;
FIG. 5 is a real-time image of the transformation process of the weld heat affected zone of a sample observed in situ with a high temperature laser scanning confocal microscope of example 1 according to the present invention;
FIG. 6 is a schematic view of the installation of a hand-held inlay sample and an observation sample to be treated in example 2 provided by the present invention;
FIG. 7 is a graph of a room temperature golden phase of a small size in situ observation sample obtained in example 2 of the present invention;
FIG. 8 is a real-time image of the solidification process of the hand-held inlay sample and the observation sample to be treated in example 2 provided by the present invention;
FIG. 9 is a real-time image of the transformation process of the weld heat affected zone of a defective test piece made in accordance with comparative example 1 provided by the present invention;
Fig. 10 is a real-time image of the transformation process of the welding heat affected zone of a small-sized in-situ observation sample using the high-temperature laser scanning confocal microscope prepared in comparative example 2 provided by the present invention.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings and detailed description, but it will be understood by those skilled in the art that the examples described below are some, but not all, examples of the present invention, and are intended to be illustrative of the present invention only and should not be construed as limiting the scope of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
In the present invention, unless specifically stated otherwise, the terms "first", "second", "third", "fourth", etc. are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or quantity or as implicitly indicating the importance or quantity of the indicated technical feature. Moreover, the terms "first," "second," "third," "fourth," and the like are used for non-exhaustive list description purposes only, and are not to be construed as limiting the number of closed forms.
The terms "comprising" and "including" as used herein mean open ended or closed ended, unless otherwise noted. For example, the terms "comprising" and "comprises" may mean that other components not listed may be included or included, or that only listed components may be included or included.
In the present invention, "one or more" or "at least one" means any one, any two or more of the listed items unless specifically stated otherwise. Wherein "several" means any two or more.
In a first aspect, the present invention provides a method for preparing a small-sized in-situ observation sample by a high-temperature laser scanning confocal microscope, comprising the steps of:
(a) One or more (i.e., at least one) observation samples to be treated are obtained. For example, one, two, three, four, five, six, seven, eight, nine or ten observation samples to be treated are obtained.
In some embodiments, one or more observation samples to be treated are obtained by machining at a predetermined size.
(B) Obtaining a hand-held mosaic sample by a metallographic sample mosaic machine, and forming one or more (i.e. at least one, for example one, two, three, four, five, six, seven, eight, nine or ten, as required) blind holes on one surface of the hand-held mosaic sample, which blind holes are matched with the observation sample to be treated, as shown in fig. 2. Wherein, the blind hole refers to an unperforated hole, and can also be understood as a groove. Matching means that the size of the treated observation sample is matched with the size of the blind hole.
(C) And placing each observation sample to be processed in each blind hole of the metallographic sample embedding machine respectively, bonding a first plane of the observation sample to be processed at the bottom of the blind hole (namely bonding the first plane and the bottom in a groove of the metallographic sample embedding machine) through an adhesive to form a bonded hand-held grinding and polishing sample, and then carrying out first grinding on the exposed second plane.
The purpose of the first grinding is to make the second plane flat, without concave or convex, so that the phenomenon that the first plane is inclined and shaded when being observed due to the fact that the second plane is uneven is avoided, and in-situ observation results are affected.
(D) Separating the observation sample to be treated from the blind hole, transferring the observation sample to be treated, and adhering a second plane of the observation sample to be treated to the bottom of the blind hole through an adhesive, wherein the second plane and the first plane are opposite planes which are parallel to each other, such as a top surface and a bottom surface, sequentially carrying out second grinding and polishing on the exposed first plane to serve as observation surfaces, separating the observation sample to be treated from the blind hole after the polishing is completed, and obtaining the high-temperature laser scanning confocal microscope small-size in-situ observation sample which can be used for in-situ observation after the treatment (grinding and polishing).
The preparation method of the high-temperature laser scanning confocal microscope small-size in-situ observation sample, provided by the invention, directly uses the thermal mosaic sample commonly used by a sample preparation worker to carry out handheld grinding and polishing, is simple to operate, does not need to customize a clamp, is not limited by the clamp, can process and assemble the small-size in-situ observation sample with various specifications at any time to obtain the handheld mosaic sample, is beneficial to improving the surface quality of the sample, can obtain a flat, parallel and nearly traceless in-situ observation surface, can simultaneously prepare a plurality of samples at one time, greatly saves sample preparation time, saves sample preparation cost, improves the efficiency and success rate of preparing the small-size sample, and meets the in-situ observation effect.
The invention provides a novel method for preparing a sample by utilizing a handheld thermal mosaic sample to assemble and mount a small-size in-situ observation sample, namely, the upper surface of the thermal mosaic sample is drilled and the small-size sample is adhered and fixed in the hole, so that the convenience and high efficiency of grinding and polishing are realized.
Specifically, in order to fully ensure the absolute parallelism of the upper surface and the lower surface of a small-size in-situ observation sample, the polishing process is carried out in two stages, firstly, the second plane of the in-situ observation sample is subjected to first polishing in the first stage to obtain a flat plane aiming at the combined handheld mosaic sample, then the first plane of the in-situ observation sample is subjected to second polishing and polishing in the second stage based on the flat second plane to obtain a flat, parallel and nearly traceless in-situ observation surface.
In addition, the size of the sample to be treated and the size of the handheld embedded sample are not limited, the sample to be treated and the size of the handheld embedded sample can be flexibly modified according to the model of experimental equipment and the personal habit characteristics of polishing personnel, so that the preparation of small-size samples is personalized, the high cost of a custom fixture is avoided, a plurality of samples can be prepared at one time, the cost is saved, and the efficiency and the success rate are improved.
In some specific embodiments, in step (a), the shape of the observation sample to be treated includes at least one of a cylinder and a cube, and may be specifically set as required.
In some embodiments, in step (a), the observation sample to be treated is obtained by machining.
In some embodiments, the method of machining includes at least one of wire-cut electric discharge machining, diamond cutting, laser cutting, and water cutting.
In some embodiments, the machining is followed by rough grinding and/or washing of the observation sample to be treated.
Preferably, one or more observation samples to be treated are obtained by machining, and each observation sample to be treated is then subjected to rough grinding and washing in sequence.
Preferably, rough grinding is carried out on the surface and the circumference of the observation sample to be treated through sand paper, the lines, greasy dirt and rust left by mechanical processing are removed until the metallic luster is completely exposed, then the observation sample to be treated after rough grinding is washed clean by water, and the water is sucked by filter paper for standby.
As an example, but not limited to, 800# silicon carbide metallographic sandpaper may be used for rough grinding.
The size of the observation sample to be treated can be set according to the requirement, and on the premise of meeting the requirement that the high-temperature laser scanning confocal microscope cavity contains the sample, different specifications and sizes and different shapes can be processed according to the purpose of in-situ observation and the size of the experimental crucible.
As an example, the observation sample to be treated is a cylindrical shape having a diameter of 5mm and a thickness of 4 mm.
In some specific embodiments, in step (b), the method for obtaining a hand-held mosaic sample by a metallographic sample mosaic machine comprises: and placing the mosaic material between an upper module and a lower module of the metallographic specimen mosaic machine, heating and extruding, and cooling to obtain the handheld mosaic specimen.
The size of the hand-held embedded sample can be set according to requirements, including but not limited to a cylinder with phi of 30 multiplied by 12mm, and embedded samples with different diameters and different thicknesses can be adopted.
In some embodiments, the inlay material includes at least one of bakelite powder and a resin containing a filler.
In some embodiments, the filler-containing resin comprises at least one of a mineral filler-containing epoxy resin, a carbon filler-containing phenolic resin, and a wood flour filler-containing phenolic resin. Wherein the mineral filler comprises at least one of quartz powder, glass fiber, metal powder and carbon fiber; the carbon filler comprises at least one of light calcium carbonate, heavy calcium carbonate, fly ash and boron carbide.
In some embodiments, the temperature of the heating is 130 to 180 ℃; including, but not limited to, any one of the spot values or a range of values between any two of 130 ℃, 135 ℃, 140 ℃, 145 ℃, 150 ℃, 155 ℃, 160 ℃, 165 ℃, 170 ℃, 175 ℃, 180 ℃.
In some embodiments, the pressure of the extrusion is 25-35 Mpa, including but not limited to a point value of any one of 25Mpa, 28Mpa, 30Mpa, 32Mpa, 35Mpa, or a range of values between any two.
In some embodiments, the heating and/or the pressing is for a period of time ranging from 5 to 15 minutes, including but not limited to a point value of any one of 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes, 10 minutes, 11 minutes, 12 minutes, 13 minutes, 14 minutes, 15 minutes, or a range value between any two.
As an example, in the step (b), the hand-held mosaic sample is a solid hand-held mosaic sample, and the method for obtaining the hand-held mosaic sample by using a metallographic sample mosaic machine is shown in fig. 1, and specifically includes the following steps: the hand wheel of the metallographic specimen embedding machine is rotated, a lower module for embedding materials is adjusted to move in a die sleeve, the lower module and a platform are parallel to each other, then the hand wheel is rotated anticlockwise for 10-15 circles to enable the lower module to sink, the distance from the platform is 30-35 mm, embedding materials such as bakelite powder are filled in the die sleeve (above the lower module) and are parallel to each other, then the upper module is pressed on the embedding materials, the upper module is pressed, meanwhile, the hand wheel is rotated anticlockwise to enable the upper module to sink to the upper surface of the upper module to be slightly lower than the platform, a cover plate of the embedding machine is closed and screwed, the temperature of the embedding machine is set, and then the hand wheel is rotated clockwise until the pressure lamp is turned on, then the hand wheel is rotated clockwise for 1-2 circles, such as 1.5 circles, the filled embedding materials are enabled to be compacted, after the set temperature and proper pressure are reached, the embedding materials begin to be inverted for 5 minutes, the pressure lamp is kept long and is turned on, if the pressure lamp is turned off in the process, the hand wheel is rotated clockwise for 5 circles again, the pressure lamp is enabled to be turned on again, and finally the embedding materials are formed. And then demoulding and sampling are started, firstly, the hand wheel is rotated anticlockwise to unload pressure so as to extinguish the pressure lamp, then, the hand wheel is rotated anticlockwise again so as to separate the lower module from the mosaic sample to vacate a demoulding space, then, the octagonal knob on the cover plate of the mosaic machine is rotated clockwise to downwards push the upper module so as to demould the compacted handheld mosaic sample, the step can ensure that the upper module does not collapse and bounce during sampling, then the octagonal knob is rotated anticlockwise to open the cover plate, the hand wheel is rotated clockwise to push the upper module out until the lower surface of the upper module is parallel to the platform, the upper module is taken down and placed beside the mosaic machine (at the moment, the upper module is hotter and cannot be directly contacted by hands), and the hand-held mosaic sample prepared is completely exposed by lifting the lower module by continuously rotating the hand wheel clockwise, so that the handheld mosaic sample is obtained.
In some specific embodiments, in step (c), the adhesive comprises at least one of 502 glue, 402 glue, 401 glue, rosin, epoxy glue, and acrylic glue (i.e., acrylate adhesive).
Preferably, in the step (c), the method for adhering the first plane of the observation sample to be treated to the bottom of the blind hole by using an adhesive specifically includes: 2-4 drops (about 0.1-0.2 ml) of adhesive are respectively dripped into each blind hole, then the observation sample to be treated is rapidly put into the blind holes, one end of the observation sample to be treated is attached to the bottoms of the blind holes, and the adhered hand-held grinding and polishing sample is obtained after drying. More preferably, before dropping the adhesive, the surface and blind holes of the metallographic specimen embedding machine are cleaned first, avoiding dust and embedding material residues.
Preferably, in step (c), the method of first grinding comprises: the second plane is ground by using 400# silicon carbide metallographic sand paper, 800# silicon carbide metallographic sand paper and 1000# silicon carbide metallographic sand paper in sequence, wherein each mesh of sand paper is ground for 3-5 min, and then washed clean by water and dried.
Preferably, in the step (d), the method for adhering the second plane of the observation sample to be treated to the bottom of the blind hole by using an adhesive specifically includes: 2-4 drops (about 0.1-0.2 ml) of adhesive are respectively dripped into each blind hole, then the observation sample to be treated is rapidly put into the blind holes, the second plane of the observation sample to be treated is attached to the bottoms of the blind holes, and the adhered hand-held grinding and polishing sample is obtained after drying. More preferably, before dropping the adhesive, the surface and blind holes of the metallographic specimen embedding machine are cleaned first, avoiding dust and embedding material residues.
In some embodiments, in step (d), the second grind and polish is to have no macroscopic scratches.
In some specific embodiments, in step (d), the method of second grinding comprises: rough grinding is firstly carried out, then fine grinding is carried out until scratches formed by the upper-pass grinding disappear.
In some embodiments, in step (d), the method of polishing comprises: polishing to mirror surface with polishing paste with particle size of 0.25-0.05 μm.
In some embodiments, in step (d), the second grinding and polishing method specifically comprises: sequentially using 400# and 800# silicon carbide metallographic sand paper to coarsely grind a first plane, using 1000# water sand paper, 1500# water sand paper and 2000# water sand paper to finely grind, forming 90 degrees in the grinding direction between two adjacent sand paper, grinding until scratches formed in the upper pass completely disappear, polishing on a velvet polishing cloth to a mirror surface by using water-soluble diamond polishing paste with the particle sizes of 0.25 mu m and 0.05 mu m respectively, wiping and washing the surface of a sample with absorbent cotton soaked in water under water flow, spraying alcohol, and drying.
In some embodiments, in step (c) and step (d), the method of separating comprises: and immersing the hand-held polished sample after the observation sample to be treated is adhered to the blind hole in an organic solvent to dissolve the adhesive.
The adhesion and separation of the hand-held embedded sample and the small-size observation sample to be treated are realized through the adhesive and the soaking of the organic solvent, the operation is convenient, and the hand-held embedded sample and the small-size observation sample are finished under the condition of liquid sealing, so that the problem that the surface of the polished metal material such as aluminum, magnesium and the like is easy to oxidize is solved.
In some embodiments, the organic solvent comprises at least one of acetone, tena water, methylene chloride, and alcohol.
Wherein, the tenna water is also called banana oil and pear oil, and the chemical formula of the tenna water is CH 3CH(CH3)CH2CH2OOCCH3.
In some embodiments, the soaking time is 1-5 hours, including but not limited to a point value of any one of 1,2,3, 4, 5 hours or a range value between any two.
In a second aspect, the invention provides an application of the high-temperature laser scanning confocal microscope small-size in-situ observation sample prepared by the preparation method of the high-temperature laser scanning confocal microscope small-size in-situ observation sample in observing and analyzing phase change and microstructure change of a metal material.
In some embodiments, the metallic material includes, but is not limited to, iron alloys, copper alloys, titanium alloys, aluminum alloys, and the like.
In some embodiments, the in-situ observation of the first plane in the small-sized in-situ observation sample is performed by a high temperature laser scanning confocal microscope.
In some specific embodiments, the method for in-situ observation of a first plane in a sample under in-situ observation of a small size of the high temperature laser scanning confocal microscope by the high temperature laser scanning confocal microscope comprises: placing the prepared small-size in-situ observation sample of the high-temperature laser scanning confocal microscope into an alumina ceramic crucible, placing the alumina ceramic crucible on a Pt sample bracket, sealing a heating furnace body, cleaning the Pt sample bracket with high-purity argon (99.99%) for 3-5 times, discharging air in a heating bin, simultaneously filling argon for protection in the whole experiment to prevent the oxidation of the small-size in-situ observation sample of the high-temperature laser scanning confocal microscope, fixing magnification, selecting an observation view field of the small-size in-situ observation sample of the high-temperature laser scanning confocal microscope, which has a flat surface and no scratch, setting a specific welding thermal cycle curve, specially used for reproducing a welding thermal cycle process of a coarse-grain heat affected zone under the condition of manual arc welding with the heat input of 15-20 kJ/cm, and capturing real-time images at the speed of 10-20 frames/s through a Charge Coupler (CCD) piece camera of the high-temperature laser scanning confocal microscope.
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
The embodiment provides a preparation method of a small-size sample for in-situ observation of solid-state phase transformation of a heat-resistant steel welding heat affected zone of 1.25Cr-0.5Mo by a high-temperature laser scanning confocal microscope, which comprises the following steps:
(1) In-situ observing the sample by machining according to preset dimensions: firstly, taking 5 cylinder samples with the diameter of 5mm and the thickness of 4mm (abbreviated as phi 5 multiplied by 4 mm) from a delivered state 1.25Cr-0.5Mo heat-resistant steel base material through wire electric discharge machining, then, roughly grinding the upper surface, the lower surface and the circumference of the cylinder sample by using 800# silicon carbide metallographic sand paper to remove lines, greasy dirt and rust left by machining until the metallic luster is completely exposed, finally, washing the cylinder sample with water, and drying the water by using filter paper to obtain 5 observation samples to be treated for standby.
(2) Preparing and processing a handheld mosaic sample: using XQ-2B metallographic specimen embedding machine to prepare hand-held embedded specimen, as shown in figure 2, first turning the hand wheel of the embedding machine, adjusting the lower module of the pressed specimen to move in the die sleeve, making the lower module parallel to the platform, then turning the hand wheel 13 turns counterclockwise to make the lower module sink 31mm away from the platform, filling filler bakelite powder (phenolic moulding compound, model PF2A2-141 black) in the die sleeve and making it parallel to the platform, then pressing the steel upper module with a size phi 30X 20mm (diameter 30mm, height 20 mm) onto the filler bakelite powder, pushing the upper module by the left finger and applying downward pressure, simultaneously, the right hand rotates the hand wheel anticlockwise again, so that the upper module sinks to the upper surface slightly lower than the platform, the cover plate of the mosaic machine is closed and screwed, then the temperature of the mosaic machine is set to 140 ℃, the hand wheel is rotated clockwise until the pressure lamp is on, then the hand wheel is rotated clockwise for 1.5 circles again, the filled bakelite powder is ensured to be compacted, the pressing lamp is kept to be turned upside down for 5 minutes (the pressure lamp is kept to be on for a long time after the temperature reaches 140 ℃ and the proper pressure, if the pressure lamp is extinguished in the process, the hand wheel is rotated clockwise again so that the pressure lamp is on again, and finally the bakelite powder is formed; and then demoulding and sampling are started, firstly, the hand wheel is rotated anticlockwise to unload pressure so as to extinguish the pressure lamp, then, the hand wheel is rotated anticlockwise to enable the lower module and the mosaic sample to be separated to vacate a demoulding space, then, the octagonal knob on the cover plate of the mosaic machine is rotated clockwise to downwards push the upper module to demould the sample, then, the octagonal knob is rotated anticlockwise to open the cover plate, the hand wheel is rotated clockwise to eject the upper module until the lower surface of the upper module is parallel to the platform, the upper module is taken down by wearing a heat insulation glove and placed beside the mosaic machine, the hand wheel is rotated clockwise continuously to lift the lower module so as to completely expose the mosaic sample, and then, the cylindrical handheld mosaic sample with the diameter of 30mm and the thickness of 12mm (abbreviated as phi 30 multiplied by 12 mm) is taken out.
Then, the upper surface of the phi 30 multiplied by 12mm cylindrical handheld embedded sample is concentric with a diameter of 14mm, five points are equidistantly taken on the circumference, and 5 cylindrical blind holes with a diameter of 5mm and a depth of 4mm are drilled by taking the five points as the centers respectively, as shown in figure 2.
(3) The combined installation of the observation sample to be treated and the handheld mosaic sample: firstly, cleaning the surface and cylindrical blind holes of the hand-held embedded sample obtained in the step (2) to avoid dust and embedded powder residues, then respectively dripping 2 drops of 502 glue into the 5 cylindrical blind holes of the hand-held embedded sample, respectively placing 5 phi 5 multiplied by 4mm observation samples to be processed obtained in the step (1) into the cylindrical blind holes with the A surface facing upwards by using tweezers, placing the observation samples in a ventilation place as shown in fig. 3, and tightly adhering the observation samples to be processed and the hand-held embedded sample by using 502 glue in the blind holes to obtain the hand-held polished sample.
(4) Grinding the A surface of the hand-held grinding and polishing sample (namely, first grinding): placing the target grinding surface A of the observation sample to be treated in the hand-held grinding and polishing sample obtained in the step (3) on a carrying disc of a UNIPOL-1200M automatic pressure grinding and polishing machine, fixing the sample by pneumatic pressurization to ensure that the carrying disc is uniformly stressed, setting the rotating speed of the carrying disc (upper disc) to be 30rpm, setting the rotating speed of the grinding and polishing disc (lower disc) to be 300rpm, then opening a water supply pipe to sequentially grind the surface A by using 400# silicon carbide metallographic abrasive paper, 800# silicon carbide metallographic abrasive paper and 1000# silicon carbide metallographic abrasive paper, grinding each mesh abrasive paper for 4min, taking out the abrasive paper from the carrying disc, washing the abrasive paper cleanly by water, spraying alcohol and drying the abrasive paper by a blower.
(5) Grinding and polishing (i.e., second grinding and polishing) the B-side of the in-situ observation sample: placing the observation sample to be treated which is ground in the step (4) into a beaker filled with acetone for soaking for 1h, completely dissolving 502 glue, taking out the observation sample to be treated, spraying alcohol to the observation sample to be treated and the embedded sample for cleaning and drying, respectively dripping 2 drops of 502 glue into 5 cylindrical blind holes of the embedded sample to be treated, placing the observation sample to be treated into an embedded sample hole by forceps, taking care that the ground surface A faces downwards, the unground surface B faces upwards, placing a ventilated place for airing, and tightly adhering the 502 glue in the hole to the observation sample to be treated to obtain the hand-held grinding and polishing sample again.
And then the target grinding surface B of the hand-held grinding and polishing sample faces downwards, 400# and 800# silicon carbide metallographic sand paper is sequentially used for carrying out rough grinding on the surface B, 1000# water sand paper, 1500# water sand paper and 2000# water sand paper are used for carrying out fine grinding, the grinding direction between two adjacent sand paper forms 90 degrees, the grinding is carried out until scratches formed in the upper pass completely disappear, then water-soluble diamond polishing paste with the particle size of 0.25 μm and 0.05 μm is respectively used for polishing to a mirror surface on a velvet polishing cloth, the surface of the sample is wiped and washed clean by absorbent cotton soaked by water under water flow, alcohol is sprayed, and a blower is used for carrying out quick blow-drying along the 45-degree inclined direction of the surface of the sample.
And then putting the polished handheld embedded sample into a beaker filled with acetone again for soaking for 1h to completely dissolve 502 glue, taking out the observation sample to be treated by using tweezers, spraying alcohol to clean the observation sample, drying the observation sample to obtain the small-size in-situ observation sample of the high-temperature laser scanning confocal microscope after treatment, and wrapping the observation sample in a transparent bag by using absorbent cotton for preservation.
(6) In situ observation was performed using a high temperature laser scanning confocal microscope: firstly, placing a small-size in-situ observation sample of a phi 5 multiplied by 4mm high-temperature laser scanning confocal microscope prepared in the step (5) into an alumina ceramic crucible with the size of 6.5mm and the thickness of 4mm, then placing the sample on a Pt sample bracket, cleaning 3 times by using high-purity argon (99.99%) after sealing a heating furnace body, discharging air in a heating bin, simultaneously filling argon for protection in the whole experiment to prevent sample oxidization, fixing magnification, selecting an observation view with a flat and scratch-free sample surface, as shown in fig. 4, setting a specific welding thermal cycle curve, specially used for reproducing a welding thermal cycle process of a coarse-grain heat affected zone under the condition of 18kJ/cm manual arc welding, capturing real-time images at the speed of 15 frames/s by a Charge Coupler (CCD) piece camera of the high-temperature laser scanning confocal microscope, and recording the whole-time in-situ observation result in the experiment in a video file, wherein part of the continuous form evolution of typical solid-state phase transition is shown in fig. 5.
Example 2
The embodiment provides a preparation method of a small-size sample for in-situ observation of copper-titanium alloy solidification behavior by a high-temperature laser scanning confocal microscope, which comprises the following steps:
(1) In-situ observing the sample by machining according to preset dimensions: firstly, taking 5 cylinder samples with the diameter of 6.5mm and the thickness of 3mm (abbreviated as phi 6.5 multiplied by 3 mm) from a smelted copper-titanium alloy cast ingot through wire-cut electric discharge machining, then, carrying out rough grinding on the upper surface, the lower surface and the circumference of the cylinder sample by using 800# silicon carbide metallographic sand paper to remove lines, greasy dirt and rust left by machining until metallic luster is completely exposed, finally, washing the cylinder sample with water, and sucking water with filter paper to obtain 5 observation samples to be treated for later use.
(2) Preparing and processing a handheld mosaic sample: using an XQ-2B metallographic specimen embedding machine to prepare a handheld embedded specimen, firstly rotating a hand wheel of the embedding machine, adjusting a lower module of the pressed specimen to move in a die sleeve, enabling the lower module to be parallel to a platform, then rotating the hand wheel 13 circles anticlockwise to enable the lower module to sink and be 31mm away from the platform, filling phenolic resin (PF 2A4-161J red) filled with wood powder filler in the die sleeve and enabling the phenolic resin to be parallel to the platform, pressing a steel upper module with the size phi 30X 20mm (with the diameter of 30mm and the height of 20 mm) on the phenolic resin filled with wood powder filler, enabling a left hand to press the upper module and exert downward pressure, simultaneously enabling a right hand to rotate the hand wheel anticlockwise again, enabling the upper module to sink to be slightly lower than the platform, closing a cover plate of the embedding machine and screwing, setting the temperature of the embedding machine to be 140 ℃, and enabling the hand wheel to rotate clockwise again for 1.5 circles after the pressure lamp is turned on, guaranteeing that the filled phenolic resin filled with wood powder filler is compressed tightly, enabling the phenolic resin filled with wood powder filler to reach the set temperature of 140 ℃ and the proper pressure after the pressure lamp is turned off, and keeping the pressure for a proper time after the time when the pressure lamp is turned on, and finally turning the pressure lamp is turned off again when the pressure lamp is kept to be turned on for a proper time; and then demoulding and sampling are started, firstly, the hand wheel is rotated anticlockwise to unload pressure so as to extinguish the pressure lamp, then, the hand wheel is rotated anticlockwise to enable the lower module and the mosaic sample to be separated to vacate a demoulding space, then, the octagonal knob on the cover plate of the mosaic machine is rotated clockwise to downwards push the upper module to demould the sample, then, the octagonal knob is rotated anticlockwise to open the cover plate, the hand wheel is rotated clockwise to eject the upper module until the lower surface of the upper module is parallel to the platform, the upper module is taken down by wearing a heat insulation glove and placed beside the mosaic machine, the hand wheel is rotated clockwise continuously to lift the lower module so as to completely expose the mosaic sample, and then, the cylindrical handheld mosaic sample with the diameter of 30mm and the thickness of 12mm (abbreviated as phi 30 multiplied by 12 mm) is taken out.
Then, the upper surface of the phi 30 multiplied by 12mm cylindrical handheld embedded sample is concentric with a diameter of 14mm, five points are equidistantly taken on the circumference, and 5 cylindrical blind holes with a diameter of 6.5mm and a depth of 3mm are drilled by taking the five points as the centers respectively, as shown in fig. 6.
(3) The combined installation of the observation sample to be treated and the handheld mosaic sample: firstly, cleaning the surface and cylindrical blind holes of the hand-held embedded sample obtained in the step (2) to avoid dust and embedded powder residues, then respectively dripping 2 drops of epoxy resin glue (Lei 53574AB glue) into the 5 cylindrical blind holes of the hand-held embedded sample, then rapidly putting 5 phi 6.5X3 mm observation samples to be treated obtained in the step (1) into the cylindrical blind holes respectively by using tweezers, enabling the A surface to face upwards as shown in fig. 6, then placing a ventilation place of the observation samples, and tightly adhering the observation samples to be treated with the hand-held embedded sample by using the epoxy resin glue in the blind holes to obtain the hand-held polished sample.
(4) Grinding the A surface of the hand-held grinding and polishing sample (namely, first grinding): placing the target grinding surface A of the observation sample to be treated in the hand-held grinding and polishing sample obtained in the step (3) on a carrying disc of a UNIPOL-1200M automatic pressure grinding and polishing machine, fixing the sample by pneumatic pressurization to ensure that the carrying disc is uniformly stressed, setting the rotating speed of the carrying disc (upper disc) to be 30rpm, setting the rotating speed of the grinding and polishing disc (lower disc) to be 300rpm, then opening a water supply pipe to sequentially grind the surface A by using 400# silicon carbide metallographic abrasive paper, 800# silicon carbide metallographic abrasive paper and 1000# silicon carbide metallographic abrasive paper, grinding each mesh abrasive paper for 5min, taking out the abrasive paper from the carrying disc, washing the abrasive paper cleanly by water, spraying alcohol and drying the abrasive paper by a blower.
(5) Grinding and polishing (i.e., second grinding and polishing) the B-side of the in-situ observation sample: soaking the to-be-treated observation sample ground in the step (4) in a beaker filled with alcohol for 1.5 hours to completely dissolve epoxy resin glue, taking out the to-be-treated observation sample, spraying alcohol to clean the to-be-treated observation sample and the embedded sample, drying, respectively dripping 2 drops of epoxy resin glue into 5 cylindrical blind holes of the handheld embedded sample, putting the to-be-treated observation sample into an embedded sample hole by forceps, taking care that the ground A face is downward, the unground B face is upward, then placing the unground B face in a ventilation place, airing, and sticking the epoxy resin glue and the to-be-treated observation sample in the hole to obtain the handheld polished sample again.
And then the target grinding surface B of the hand-held grinding and polishing sample faces downwards, 400# and 800# silicon carbide metallographic sand paper is sequentially used for carrying out rough grinding on the surface B, 1000# water sand paper, 1500# water sand paper and 2000# water sand paper are used for carrying out fine grinding, the grinding direction between two adjacent sand paper forms 90 degrees, the grinding is carried out until scratches formed in the upper pass completely disappear, then water-soluble diamond polishing paste with the particle size of 0.25 μm and 0.05 μm is respectively used for polishing to a mirror surface on a golden velvet polishing cloth, the surface of the sample is wiped and washed clean by absorbent cotton soaked by water under the water flow, alcohol is sprayed, and a blower is used for carrying out quick blow-drying along the 45-degree inclined direction of the surface of the sample.
And then putting the polished handheld embedded sample into a beaker filled with alcohol again for soaking for 1.5 hours to completely dissolve the epoxy resin glue, taking out the observation sample to be treated by using tweezers, spraying alcohol to clean and blow-drying the observation sample to obtain the small-size in-situ observation sample of the high-temperature laser scanning confocal microscope after treatment, and packaging the observation sample into a transparent bag by using absorbent cotton for preservation.
(6) In situ observation was performed using a high temperature laser scanning confocal microscope: firstly, placing a small-size in-situ observation sample of a phi 6.5X3 mm high-temperature laser scanning confocal microscope prepared in the step (5) into an alumina ceramic crucible with the size of 9mm and the thickness of 4mm, then placing the sample on a Pt sample bracket, cleaning 3 times by using high-purity argon (99.99%) after sealing a heating furnace body, discharging air in a heating bin, simultaneously filling argon for protection in the whole experiment to prevent sample oxidization, fixing magnification, selecting an observation view with a flat and scratch-free sample surface, as shown in fig. 7, setting specific heating and cooling rates, specially used for reproducing the solidification process during copper-titanium alloy smelting, capturing real-time images at the rate of 15 frames/s by a charge-coupled device (CCD) piece camera of the high-temperature laser scanning confocal microscope, and recording the whole-experiment in-situ observation result in a video file, wherein continuous morphological evolution of part of typical solidification behavior is shown in fig. 8.
Example 3
The preparation method of the small-size sample for in-situ observation of the solid-state phase transition of the heat affected zone of the heat resistant steel welding of 1.25Cr-0.5Mo by the high-temperature laser scanning confocal microscope provided by the embodiment is basically the same as that of the embodiment 1, except that bakelite powder is replaced by phenolic resin (Mei-Emi HM 3) containing carbon filler.
Example 4
The preparation method of the small-size sample for in-situ observation of the solid-state phase change of the heat affected zone of the heat resistant steel welding of 1.25Cr-0.5Mo by the high-temperature laser scanning confocal microscope provided by the embodiment is basically the same as that of the embodiment 1, except that 502 glue is replaced by rosin, and the rosin dosage is 0.1g.
Example 5
The preparation method of the small-size sample for in-situ observation of the solid phase transformation of the heat affected zone of the 1.25Cr-0.5Mo heat resistant steel by the high-temperature laser scanning confocal microscope provided by the embodiment is basically the same as that of the embodiment 1, and the difference is that in the step (1), 8 square samples with the edge length of 4mm are taken from the delivered 1.25Cr-0.5Mo heat resistant steel base material by wire-cut electric discharge machining; and in the step (2), 8 cube blind holes with the edge length of 4mm are drilled on the upper surface of the cylindrical handheld embedded sample.
Comparative example 1
The preparation method of the small-size sample for in-situ observation of the solid-state phase change of the heat affected zone of the heat resistant steel welding of 1.25Cr-0.5Mo by the high-temperature laser scanning confocal microscope provided by the comparative example is prepared by adopting the prior conventional technology, is completely different from the example 1, and specifically comprises the following steps:
(1) Taking 1 cylindrical sample with the diameter of 5mm and the thickness of 4mm (abbreviated as phi 5 multiplied by 4 mm) from a delivered state 1.25Cr-0.5Mo heat-resistant steel base material through wire electric discharge machining, roughly grinding the upper surface, the lower surface and the circumference of the cylindrical sample by using 800# silicon carbide metallographic sand paper, removing lines marks, greasy dirt and rust left by machining until metallic luster is completely exposed, and finally washing the cylindrical sample with water to obtain the cylindrical sample to be observed;
(2) Putting the cylindrical sample to be observed obtained in the step (1) into a metallographic sample embedding machine for directly performing thermal embedding, and then grinding and polishing the embedded sample according to a conventional metallographic sample preparation method; after finishing grinding and polishing, damaging the inlaid sample by using a hammer, taking out a cylinder sample to be observed, then carrying out subsequent cleaning treatment on the cylinder sample, and then carrying out a high-temperature laser scanning confocal in-situ observation experiment.
As shown in FIG. 9, the in-situ observation real-time image obtained in the comparative example can obviously show that the surface of the sample has a plurality of problems of large scratch quantity, poor flatness, large number of pollutant impurity black spots and the like, and the defects not only lead the high-temperature laser scanning confocal microscope to be difficult to focus in a plane and to image suddenly and suddenly, so that the continuous in-situ observation effect of a fixed area in the plane is poor, the selectivity is reduced, but also scratch ravines with different depths can obstruct the solid-state phase transition generation and the dynamic process analysis, seriously influence the solid-state phase transition in-situ observation effect and the image data processing result, lose capturing details and finally fail to exert the uniqueness of the in-situ observation function.
Comparative example 2
The preparation method of the small-size sample for in-situ observation of the solid-state transformation of the heat affected zone of the heat resistant steel welding of 1.25Cr-0.5Mo by the high-temperature laser scanning confocal microscope provided by the embodiment is basically the same as that of the embodiment 1, except that the A surface is not ground in the step (4). The bottom of the sample is uneven, so that the focusing of an observation plane is difficult, the depth of field is inconsistent, and finally the problems of inconsistent brightness, reduced definition and the like in the same plane of an in-situ observation real-time image are caused, as shown in fig. 10, so that the experimental detail capturing and quantitative result analysis are seriously affected.
While the invention has been illustrated and described with reference to specific embodiments, it is to be understood that the above embodiments are merely illustrative of the technical aspects of the invention and not restrictive thereof; those of ordinary skill in the art will appreciate that: modifications may be made to the technical solutions described in the foregoing embodiments, or equivalents may be substituted for some or all of the technical features thereof, without departing from the spirit and scope of the present invention; such modifications and substitutions do not depart from the spirit of the corresponding technical solutions; it is therefore intended to cover in the appended claims all such alternatives and modifications as fall within the scope of the invention.
Claims (10)
1. The preparation method of the high-temperature laser scanning confocal microscope small-size in-situ observation sample is characterized by comprising the following steps of:
(a) Obtaining one or more observation samples to be treated;
(b) Obtaining a hand-held embedded sample through a metallographic sample embedding machine, and forming one or more blind holes matched with the observation sample to be processed on the hand-held embedded sample;
(c) Placing each observation sample to be treated in each blind hole, bonding a first plane of the observation sample to be treated to the bottom of each blind hole through an adhesive, and then carrying out first grinding on the second plane;
(d) And separating the observation sample to be treated from the blind hole, and adhering a second plane of the observation sample to be treated to the bottom of the blind hole through an adhesive, wherein the second plane is parallel to the first plane, then carrying out second grinding and polishing on the first plane, and separating the observation sample to be treated from the blind hole after polishing is finished to obtain the small-size in-situ observation sample of the treated high-temperature laser scanning confocal microscope.
2. The method for preparing a small-sized in-situ observation sample for a high-temperature laser scanning confocal microscope according to claim 1, wherein in step (a), the shape of the observation sample to be treated comprises at least one of a cylinder and a cube.
3. The method for preparing a small-sized in-situ observation sample by a high-temperature laser scanning confocal microscope according to claim 1, wherein in the step (a), the observation sample to be treated is obtained by machining;
preferably, the method of machining includes at least one of wire-cut electric discharge machining, diamond cutting, laser cutting, and water cutting;
Preferably, the machining is followed by rough grinding and/or washing of the observation sample to be treated.
4. The method for preparing a small-sized in-situ observation sample by a high-temperature laser scanning confocal microscope according to claim 1, wherein in the step (b), the method for obtaining a hand-held mosaic sample by a metallographic sample mosaic machine comprises: placing an embedding material between an upper module and a lower module of the metallographic specimen embedding machine, heating and extruding, and cooling to obtain the handheld embedding specimen; preferably, the mosaic material comprises at least one of bakelite powder and a resin containing a filler; preferably, the heating temperature is 130-180 ℃;
preferably, the extrusion pressure is 25-35 MPa;
Preferably, the heating and/or the pressing is for a period of 5 to 15 minutes.
5. The method for preparing a small-sized in-situ observation sample using a high-temperature laser scanning confocal microscope according to claim 1, wherein in the step (c), the adhesive comprises at least one of 502 glue, 402 glue, 401 glue, rosin, epoxy glue and acrylic glue.
6. The method of claim 1, wherein in step (d), the second grinding and polishing is performed until no macroscopic scratches are present.
7. The method for preparing a small-sized in-situ observation sample using a high-temperature laser scanning confocal microscope according to claim 1, wherein in step (d), said second grinding method comprises: firstly, carrying out rough grinding, and then carrying out fine grinding until scratches formed in the upper pass disappear; and/or, in step (d), the polishing method comprises: polishing to mirror surface with polishing paste with particle size of 0.25-0.05 μm.
8. The method for preparing a small-sized in-situ observation sample using a high-temperature laser scanning confocal microscope according to claim 1, wherein in step (c) and step (d), said separation method comprises: immersing the hand-held polished sample after the observation sample to be treated is adhered to the blind hole in an organic solvent to dissolve the adhesive;
Preferably, the organic solvent includes at least one of acetone, tena water, methylene chloride and alcohol;
preferably, the soaking time is 1-5 hours.
9. The use of a high temperature laser scanning confocal microscope small-size in-situ observation sample prepared by the method for preparing a high temperature laser scanning confocal microscope small-size in-situ observation sample according to any one of claims 1 to 8 for observing and analyzing phase changes and microstructure changes of a metal material.
10. The use of claim 9, wherein the first plane in the sample is viewed in situ by a high temperature laser scanning confocal microscope of small size.
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