阅读说明：本技术 一种样品制备工艺方法 (Sample preparation process method ) 是由 张敬蕊 胡庆利 赵乃胜 周志超 谢新艳 张海燕 武甲 沈洁 于 2019-09-12 设计创作，主要内容包括：本发明提供一种样品制备工艺方法,包括：将具有表面缺陷的钢材进行切割,形成待测样品；根据待测样品的尺寸对辅助钢材进行切割,形成辅助样品,辅助样品的厚度为1～2mm,辅助样品及待测样品的平直度保持一致；利用双面铜导电胶将待测样品及辅助样品粘结,形成组合样品,双面铜导电胶与待测样品的待磨制边的距离为2～3mm；对组合样品进行缠绕固定,缠绕固定后,待测样品与辅助样品之间的缝隙为0.05～0.15mm；利用磨抛机对所述缠绕固定后的组合样品的待检测面进行打磨,磨制完成后,拆掉辅助样品；对磨制后的待测样品进行超声波清洗、烘干；对待测样品的待检测面进行清洁后,标记待检测面的缺陷。(The invention provides a sample preparation process method, which comprises the following steps: cutting the steel with the surface defects to form a sample to be detected; cutting the auxiliary steel according to the size of the sample to be detected to form an auxiliary sample, wherein the thickness of the auxiliary sample is 1-2 mm, and the straightness of the auxiliary sample and the straightness of the sample to be detected are kept consistent; bonding the sample to be tested and the auxiliary sample by using double-sided copper conductive adhesive to form a combined sample, wherein the distance between the double-sided copper conductive adhesive and the edge to be ground of the sample to be tested is 2-3 mm; winding and fixing the combined sample, wherein after the combined sample is wound and fixed, a gap between the sample to be detected and the auxiliary sample is 0.05-0.15 mm; polishing the surface to be detected of the combined sample after being wound and fixed by using a polishing machine, and removing the auxiliary sample after the polishing is finished; carrying out ultrasonic cleaning and drying on the ground sample to be detected; and after cleaning the surface to be detected of the sample to be detected, marking the defect of the surface to be detected.)

1. A sample preparation process, comprising:

cutting the steel with the surface defects to form a sample to be detected;

cutting the auxiliary steel according to the size of the sample to be detected to form an auxiliary sample, wherein the thickness of the auxiliary sample is 1-2 mm, and the straightness of the auxiliary sample and the straightness of the sample to be detected are kept consistent;

bonding the sample to be detected and the auxiliary sample by using double-sided copper conductive adhesive to form a combined sample, wherein the distance between the double-sided copper conductive adhesive and the edge to be ground of the sample to be detected is 2-3 mm;

winding and fixing the combined sample, wherein after the combined sample is wound and fixed, a gap between the sample to be detected and the auxiliary sample is 0.05-0.15 mm;

polishing the surface to be detected of the combined sample after being wound and fixed by using a polishing machine, and removing the auxiliary sample after the polishing is finished;

carrying out ultrasonic cleaning and drying on the ground sample to be detected;

and after cleaning the surface to be detected of the sample to be detected, marking the defects of the surface to be detected.

2. The method of claim 1, wherein the cutting the auxiliary sample according to the size of the sample to be tested to form the auxiliary sample comprises:

and grinding the auxiliary sample and the processing burrs of the sample to be detected by using 200-mesh sand paper.

3. The method of claim 1, wherein said wrapping said combined sample to secure comprises:

and winding and fixing the combined sample by using a transparent adhesive tape.

4. The method according to claim 1, wherein the grinding and polishing machine is used for grinding the surface to be detected of the combined sample after the winding and fixing, and comprises the following steps:

carrying out primary coarse grinding on the surface to be detected of the combined sample by using the grinding and polishing machine, wherein grinding parameters in the primary coarse grinding process comprise: the grinding rotating speed is 700-900 r/min, the grinding force is 5-35N, the grinding time is 15-30 s, and the mesh number of the abrasive paper is 200 meshes;

carrying out secondary coarse grinding on the surface to be detected after the primary coarse grinding, wherein the grinding parameters in the secondary coarse grinding process comprise: the grinding rotating speed is 700-900 r/min, the grinding force is 5-35N, the grinding time is 15-30 s, and the mesh number of the abrasive paper is 600 meshes;

and carrying out primary accurate grinding on the surface to be detected after the secondary coarse grinding, wherein the grinding parameters in the primary accurate grinding process comprise: the grinding rotating speed is 700-900 r/min, the grinding force is 5-35N, the grinding time is 15-30 s, and the mesh number of the abrasive paper is 1000 meshes;

and carrying out secondary fine grinding on the surface to be detected after the primary fine grinding, wherein the grinding parameters in the secondary fine grinding process comprise: the grinding rotating speed is 700-900 r/min, the grinding force is 5-35N, the grinding time is 15-30 s, and the mesh number of the abrasive paper is 1200 meshes;

and carrying out primary fine polishing on the surface to be detected after the secondary fine grinding by using a diamond suspension liquid with the diameter of 0.7 mu m, wherein the polishing parameters of the primary fine polishing process comprise: the grinding rotating speed is 900-1400 r/min, the grinding force is 5-35N, and the grinding time is 20-30 s;

and carrying out secondary fine polishing on the surface to be detected after the primary fine polishing by using a diamond suspension liquid with the diameter of 0.35 mu m, wherein the polishing parameters in the secondary fine polishing process comprise: the grinding rotating speed is 900-1400 r/min, the grinding force is 5-35N, and the grinding time is 20-30 s;

and performing water polishing on the surface to be detected after the secondary fine polishing by using deionized water.

5. The method of claim 1, wherein the step of ultrasonically cleaning and drying the ground sample to be tested comprises:

and carrying out ultrasonic cleaning on the ground sample to be detected by using industrial alcohol with the concentration of more than 95%. The cleaning time is 10-15 min;

and blowing the cleaned sample to be detected by using flowing warm air at the temperature of 30-40 ℃, wherein the blowing time is 5-10 min.

6. The method of claim 1, wherein the cleaning the surface of the sample to be tested comprises:

sticking off the particles on the surface to be detected by using a special cleaning adhesive tape;

and blowing and wiping the sample to be measured placed on the sample table by using compressed air.

7. The method of claim 6, wherein the blowing the sample to be tested placed on the sample stage with compressed air comprises:

controlling the compressed air nozzle to be at least 10cm away from the sample to be tested for blowing and wiping, wherein the blowing and wiping parameters comprise: spraying for 2-3 s each time, wherein the spraying frequency is 3-5 times.

8. The method of claim 1, wherein the method further comprises:

grinding the surface of the sample to be detected by using 200-mesh sand paper, wherein the surface roughness after grinding is 0.8 mu m; the surface of the sample to be detected is the surface of the sample to be detected, which is contacted with the sample stage.

9. The method of claim 2 or 8, wherein the sandpaper material is alumina.

10. The method according to claim 4, wherein after the secondary fine polishing of the surface to be detected after the primary fine polishing with a diamond suspension of 0.35 μm, the surface roughness of the sample to be detected is 0.02 μm.

Technical Field

The invention belongs to the technical field of sample preparation, and particularly relates to a sample preparation process method.

Background

Coil with surface defects often exist in the steel production process, and problem cause analysis is needed in the scientific research process.

Currently, the sample is generally observed and analyzed by a Scanning Electron Microscope (SEM). Generally, the cross-section analysis result of a sample is most representative, and a surface defect type cross-section sample needs to better ensure the perfect preparation of the sample at the edge defect of the cross section, not only can polish the defect, but also maximally present the most original appearance and components of the defect. Therefore, the accuracy and the precision of the analysis result of the section of the sample can be ensured.

However, conventional sample preparation methods in the prior art (such as inlaying, glue bonding, and the like) all have preparation defects of different degrees, such as deformation damage and pollution of edge defects of a sample or difficulty in positioning defect positions, which results in low analysis accuracy, and cannot provide objective and accurate data for process improvement and product quality improvement in actual production, and finally, the product quality cannot be ensured.

Disclosure of Invention

Aiming at the problems in the prior art, the embodiment of the invention provides a sample preparation process method, which is used for solving the technical problems that the conventional sample preparation method in the prior art can cause deformation, damage or pollution on the edge of a sample, so that the analysis result of the sample is inaccurate, objective and accurate data cannot be provided for process improvement and product quality improvement in actual production, and finally the product quality cannot be ensured.

The invention provides a sample preparation process method, which is characterized by comprising the following steps:

cutting the steel with the surface defects to form a sample to be detected;

cutting the auxiliary steel according to the size of the sample to be detected to form an auxiliary sample, wherein the thickness of the auxiliary sample is 1-2 mm, and the straightness of the auxiliary sample and the straightness of the sample to be detected are kept consistent;

bonding the sample to be detected and the auxiliary sample by using double-sided copper conductive adhesive to form a combined sample, wherein the distance between the double-sided copper conductive adhesive and the edge to be ground of the sample to be detected is 2-3 mm;

winding and fixing the combined sample, wherein after the combined sample is wound and fixed, a gap between the sample to be detected and the auxiliary sample is 0.05-0.15 mm;

polishing the surface to be detected of the combined sample after being wound and fixed by using a polishing machine, and removing the auxiliary sample after the polishing is finished;

carrying out ultrasonic cleaning and drying on the ground sample to be detected;

and after cleaning the surface to be detected of the sample to be detected, marking the defects of the surface to be detected.

In the above-mentioned scheme, cut the auxiliary sample according to the size of the sample that awaits measuring, after forming the auxiliary sample, include:

and grinding the auxiliary sample and the processing burrs of the sample to be detected by using 200-mesh sand paper.

In the above scheme, the winding and fixing the combined sample includes:

and winding and fixing the combined sample by using a transparent adhesive tape.

In the above scheme, the grinding and polishing machine is used for grinding the surface to be detected of the combined sample after being wound and fixed, and the grinding and polishing machine comprises:

carrying out primary coarse grinding on the surface to be detected of the combined sample by using the grinding and polishing machine, wherein grinding parameters in the primary coarse grinding process comprise: the grinding rotating speed is 700-900 r/min, the grinding force is 5-35N, the grinding time is 15-30 s, and the mesh number of the abrasive paper is 200 meshes;

carrying out secondary coarse grinding on the surface to be detected after the primary coarse grinding, wherein the grinding parameters in the secondary coarse grinding process comprise: the grinding rotating speed is 700-900 r/min, the grinding force is 5-35N, the grinding time is 15-30 s, and the mesh number of the abrasive paper is 600 meshes;

and carrying out primary accurate grinding on the surface to be detected after the secondary coarse grinding, wherein the grinding parameters in the primary accurate grinding process comprise: the grinding rotating speed is 700-900 r/min, the grinding force is 5-35N, the grinding time is 15-30 s, and the mesh number of the abrasive paper is 1000 meshes;

and carrying out secondary fine grinding on the surface to be detected after the primary fine grinding, wherein the grinding parameters in the secondary fine grinding process comprise: the grinding rotating speed is 700-900 r/min, the grinding force is 5-35N, the grinding time is 15-30 s, and the mesh number of the abrasive paper is 1200 meshes;

and carrying out primary fine polishing on the surface to be detected after the secondary fine grinding by using a diamond suspension liquid with the diameter of 0.7 mu m, wherein the polishing parameters of the primary fine polishing process comprise: the grinding rotating speed is 900-1400 r/min, the grinding force is 5-35N, and the grinding time is 20-30 s;

and carrying out secondary fine polishing on the surface to be detected after the primary fine polishing by using a diamond suspension liquid with the diameter of 0.35 mu m, wherein the polishing parameters in the secondary fine polishing process comprise: the grinding rotating speed is 900-1400 r/min, the grinding force is 5-35N, and the grinding time is 20-30 s;

and performing water polishing on the surface to be detected after the secondary fine polishing by using deionized water.

In the above scheme, to after the mill the sample that awaits measuring carry out ultrasonic cleaning, stoving, include:

and carrying out ultrasonic cleaning on the ground sample to be detected by using industrial alcohol with the concentration of more than 95%. The cleaning time is 10-15 min;

and blowing the cleaned sample to be detected by using flowing warm air at the temperature of 30-40 ℃, wherein the blowing time is 5-10 min.

In the above scheme, the cleaning the surface to be detected of the sample to be detected includes:

sticking off the particles on the surface to be detected by using a special cleaning adhesive tape;

and blowing and wiping the sample to be measured placed on the sample table by using compressed air.

In the above scheme, the blowing and wiping of the to-be-measured sample placed on the sample stage by using compressed air includes:

controlling the compressed air nozzle to be at least 10cm away from the sample to be tested for blowing and wiping, wherein the blowing and wiping parameters comprise: spraying for 2-3 s each time, wherein the spraying frequency is 3-5 times.

In the above scheme, the method further comprises:

grinding the surface of the sample to be detected by using 200-mesh sand paper, wherein the surface roughness after grinding is 0.8 mu m; the surface of the sample to be detected is the surface of the sample to be detected, which is contacted with the sample stage.

In the above scheme, the sand paper is made of alumina.

In the scheme, after the diamond suspension liquid with the thickness of 0.35 mu m is used for carrying out secondary fine polishing on the surface to be detected after the primary fine polishing, the surface roughness of the sample to be detected is 0.02 mu m.

The embodiment of the invention provides a sample preparation process method, which comprises the following steps: cutting the steel with the surface defects to form a sample to be detected; cutting the auxiliary steel according to the size of the sample to be detected to form an auxiliary sample, wherein the thickness of the auxiliary sample is 1-2 mm, and the straightness of the auxiliary sample and the straightness of the sample to be detected are kept consistent; bonding the sample to be detected and the auxiliary sample by using double-sided copper conductive adhesive to form a combined sample, wherein the distance between the double-sided copper conductive adhesive and the edge to be ground of the sample to be detected is 2-3 mm; winding and fixing the combined sample, wherein after the combined sample is wound and fixed, a gap between the sample to be detected and the auxiliary sample is 0.05-0.15 mm; polishing the surface to be detected of the combined sample after being wound and fixed by using a polishing machine, and removing the auxiliary sample after the polishing is finished; carrying out ultrasonic cleaning and drying on the ground sample to be detected; after cleaning the surface to be detected of the sample to be detected, marking the defect of the surface to be detected; the auxiliary sample and the sample to be detected are bonded together for polishing, namely the auxiliary sample is used for positioning and polishing the sample to be detected, the problems of edge rounding, damage, pollution and the like of the sample to be detected when the sample to be detected is independently polished are solved by sacrificing the auxiliary sample, the original appearance of the surface to be detected is reserved, and the edge retention of the sample to be detected is improved; the sample to be detected and the auxiliary sample are bonded by the bilateral copper conductive adhesive, so that the auxiliary sample can be easily detached, and secondary pollution and secondary damage to the sample to be detected are avoided; therefore, the analysis result of the sample can be ensured, objective and accurate data can be provided for process improvement and product quality improvement in actual production, and the product quality is finally ensured.

Drawings

FIG. 1 is a schematic view of a sample to be tested when a gap exists between the sample to be tested and an inlaid base material according to the prior art;

FIG. 2 is a schematic flow chart of a sample preparation process provided in an embodiment of the present invention;

fig. 3 is a schematic view of the appearance of a sample to be measured after grinding a combined sample according to an embodiment of the present invention.

Detailed Description

In order to solve the technical problems that in the prior art, a conventional sample preparation method causes deformation, damage or pollution of the edge of a sample, so that an analysis result of the sample is inaccurate, objective and accurate data cannot be provided for process improvement and product quality improvement in actual production, and finally the product quality cannot be ensured, the embodiment of the invention provides a sample preparation process method, which comprises the following steps: cutting the steel with the surface defects to form a sample to be detected; cutting the auxiliary steel according to the size of the sample to be detected to form an auxiliary sample, wherein the thickness of the auxiliary sample is 1-2 mm, and the straightness of the auxiliary sample and the straightness of the sample to be detected are kept consistent; bonding the sample to be detected and the auxiliary sample by using double-sided copper conductive adhesive to form a combined sample, wherein the distance between the double-sided copper conductive adhesive and the edge to be ground of the sample to be detected is 2-3 mm; winding and fixing the combined sample, wherein after the combined sample is wound and fixed, a gap between the sample to be detected and the auxiliary sample is 0.05-0.15 mm; polishing the surface to be detected of the combined sample after being wound and fixed by using a polishing machine, and removing the auxiliary sample after the polishing is finished; carrying out ultrasonic cleaning and drying on the ground sample to be detected; and after cleaning the surface to be detected of the sample to be detected, marking the defects of the surface to be detected.

In order to better understand the technical scheme of the invention, the conventional sample preparation method is introduced, generally, the sample to be detected is independently manually ground, inlaid or glued, and the like, but the conventional sample preparation method has preparation defects of different degrees and is not beneficial to analysis and observation under an electron microscope. For example, direct manual grinding can cause incomplete grinding of the edge part or arc-shaped conditions of the edge part, and cause deformation damage and pollution of the edge part defects of the sample. The inlaid sample is not beneficial to positioning the defects of the position of the surface to be detected of the sample, heat and pressure are needed in the inlaid forming process, the metal of the sample to be detected is pulled out due to the difference of heat shrinkage rates, shrinkage cavities are generated, edge maintenance is not facilitated, and an unavoidable gap exists between the sample to be detected and the inlaid base material, and the gap can be referred to as figure 1. Furthermore, after the sample is corroded, the edge of the sample is easy to cause corrosion interface pollution due to the existence of gaps. For the hot-mosaic sample, the scale is easy to fall off and stain for samples with certain properties, such as iron oxide scale samples, during the cooling process. The sample bonded by the glue also has the problems of difficult defect position positioning and corrosion and pollution of the edge part of the sample, and the glue can be dissolved and deformed to a certain degree under a high-energy electron beam, so that the surface layers such as iron scales, coatings and the like can fall off in the deformation process, and the edge part is damaged due to pollution and the like. The present embodiment thus provides a sample preparation process to overcome the above problems.

The technical solution of the present invention is further described in detail by the accompanying drawings and the specific embodiments.

This embodiment provides a sample preparation process method, as shown in fig. 1, the method includes:

s210, cutting the steel with the surface defects to form a sample to be detected;

when a plurality of samples to be detected exist, each steel product needs to be marked by a typewriting pen, and the mark is generally marked on the opposite side of the surface to be detected (the side section of the sample to be detected) of the sample to be detected, so that the placing order of the sample in the sample cabin can be observed at any time in a TV mode.

Then, cutting the steel with the surface defects by using a linear cutting machining mode to form a sample to be detected; the width of the sample to be measured is 20mm, and the length is 30 mm.

S211, cutting the auxiliary steel according to the size of the sample to be detected to form an auxiliary sample;

and then selecting auxiliary steel with the thickness of 1-2 mm, wherein the auxiliary steel is generally scrap steel, and cutting the auxiliary steel according to the size of the sample to be detected to form an auxiliary sample. Wherein, the straightness of the auxiliary sample and the sample to be measured is kept consistent.

And after cutting, polishing the auxiliary sample and the processing burrs of the sample to be detected by using 200-mesh abrasive paper.

In order to increase the adhesive force between the sample to be detected and the sample stage, the conductivity of the sample to be detected is convenient to improve, and the observation effect of the sample is ensured; the method further comprises the following steps:

grinding the surface of a sample to be detected by using 200-mesh sand paper, wherein the surface roughness after grinding is 0.8 mu m; the surface of the sample to be detected is the surface of the sample to be detected, which is contacted with the sample table.

S212, bonding the sample to be tested and the auxiliary sample by using double-sided copper conductive adhesive to form a combined sample, wherein the distance between the double-sided copper conductive adhesive and the to-be-ground edge of the sample to be tested is 2-3 mm;

in order to avoid the problems of edge rounding, damage, pollution and the like of a sample to be detected in the grinding process, the sample to be detected and the auxiliary sample are bonded by using double-sided copper conductive adhesive to form a combined sample, the auxiliary sample and the sample to be detected are ground together in the grinding process, the auxiliary sample is equivalently used for positioning the sample to be detected, and the auxiliary sample is sacrificed in the grinding process to protect the complete appearance of the sample to be detected.

In order to avoid damage and pollution to the surface of the sample caused by grinding of the double-sided copper conductive adhesive in the grinding process and to improve the bonding effect, the distance between the double-sided copper conductive adhesive and the to-be-ground edge (to-be-detected surface) of the to-be-detected sample is 2-3 mm.

S213, winding and fixing the combined sample, wherein after the combined sample is wound and fixed, the gap between the sample to be detected and the auxiliary sample is 0.05-0.15 mm;

in order to avoid the sliding of the auxiliary sample and the sample to be tested during grinding, uneven stress on the whole grinding surface and failure in grinding of the sample, the transparent adhesive tape is further used for winding and fixing the combined sample, and the winding and binding positions are as same as the bonding positions of the double-sided copper conductive adhesive between the samples as possible. This achieves the effect of maximum adhesion. After the winding is fixed, the gap between the sample to be measured and the auxiliary sample is 0.05-0.15 mm, so that the stability between the sample to be measured and the auxiliary sample is increased.

In practical applications, a plurality of samples to be tested are ground at the same time, and then a plurality of combined samples need to be bonded together by using a transparent adhesive tape. The grinding device has the advantages that the surfaces to be ground of the samples are ensured to be on the same horizontal plane, the later grinding is facilitated, the dispersing force of friction between the samples in the grinding process is reduced, and the adhesive force between the samples is ensured.

S214, polishing the surface to be detected of the combined sample after being wound and fixed by using a polishing machine, and removing the auxiliary sample after the polishing is finished;

after bonding, the metallographic specimen grinding and polishing machine is utilized to polish the surface to be detected of the combined sample after winding and fixing, and the method specifically comprises the following steps:

carrying out primary coarse grinding on the surface to be detected of the combined sample by using the grinding and polishing machine, wherein grinding parameters in the primary coarse grinding process comprise: the grinding rotating speed is 700-900 r/min, the grinding force is 5-35N, the grinding time is 15-30 s, and the mesh number of the abrasive paper is 200 meshes;

and carrying out secondary coarse grinding on the surface to be detected after the primary coarse grinding until the surface to be detected is wholly ground flat, and removing the deformation layer. Grinding parameters of the secondary coarse grinding process comprise: the grinding rotating speed is 700-900 r/min, the grinding force is 5-35N, the grinding time is 15-30 s, and the mesh number of the abrasive paper is 600 meshes; wherein the sandpaper material is alumina particles.

And carrying out primary accurate grinding on the surface to be detected after the secondary coarse grinding, wherein the grinding parameters in the primary accurate grinding process comprise: the grinding rotating speed is 700-900 r/min, the grinding force is 5-35N, the grinding time is 15-30 s, and the mesh number of the abrasive paper is 1000 meshes;

the wait to detect after the primary finish grinding carries out the secondary finish grinding to the face, until the mar that produces in the primary finish grinding process is got rid of completely, and the grinding parameter of secondary finish grinding process includes: the grinding rotating speed is 700-900 r/min, the grinding force is 5-35N, the grinding time is 15-30 s, and the mesh number of the abrasive paper is 1200 meshes;

and carrying out primary fine polishing on the surface to be detected after the secondary fine grinding by using a diamond suspension liquid with the diameter of 0.7 mu m, wherein the polishing parameters of the primary fine polishing process comprise: the grinding rotating speed is 900-1400 r/min, the grinding force is 5-35N, and the grinding time is 20-30 s;

and performing secondary fine polishing on the surface to be detected after the primary fine polishing by using a diamond suspension of 0.35 mu m until the surface to be detected is as bright as a mirror, and has no scratches and no dirt. The polishing parameters of the secondary fine polishing process comprise: the grinding rotating speed is 900-1400 r/min, the grinding force is 5-35N, and the grinding time is 20-30 s; and after the secondary fine polishing, the surface roughness of the sample to be measured is 0.02 mu m.

And (3) performing water polishing on the surface to be detected after the secondary fine polishing in a polishing disc by using a metallographic sample polishing machine by using deionized water, so that the surface to be detected is cleaner, wherein the polishing disc is ensured to be free of pollutants such as polishing solution.

After the milling was completed, the scotch tape was torn off with a sharp forceps and the auxiliary sample was carefully removed. This allows the original topography of the surface to be inspected to be preserved to the greatest extent, as shown in FIG. 3.

S215, carrying out ultrasonic cleaning and drying on the ground sample to be detected; and after cleaning the surface to be detected of the sample to be detected, marking the defects of the surface to be detected.

And carrying out ultrasonic cleaning on the ground sample to be detected by using industrial alcohol with the concentration of more than 95%. The cleaning time is 10-15 min, so that pollutants such as sticky velvet, muddy water, polishing paste particles and the like in the preparation process can be cleaned. After the ultrasonic cleaning is finished, the sample to be detected is taken out firstly, and then the ultrasonic equipment is closed, so that the dirt is prevented from being attached to the sample to be detected again due to the stopping of the equipment.

Blowing the cleaned sample to be tested by utilizing flowing warm air at the temperature of 30-40 ℃, wherein the blowing time is 5-10 min, so that the sample to be tested is ensured to be dry, and if the sample has defects such as cracks, the warm air blowing time needs to be prolonged, so that no moisture is left in the cracks.

Then sticking off the particles on the surface to be detected by using a special cleaning adhesive tape; and the compressed air is used for blowing and wiping the sample to be tested placed on the sample table, so that the overall cleanliness is ensured.

The blowing and wiping of the sample to be measured placed on the sample stage by using compressed air includes:

controlling a compressed air nozzle to blow and wipe when the distance between the compressed air nozzle and the sample to be tested is at least 10cm, wherein the blowing and wiping parameters comprise: spraying for 2-3 s each time, wherein the spraying frequency is 3-5 times. If the number of samples to be detected is more, the times can be increased, and the spraying interval is more than 3S.

Here, the effect of the presence of some defects on the surface to be detected is not significant. Therefore, a sample to be detected is placed in an electron microscope, a tungsten carbide nicking pen is utilized to follow the shape of the surface defect of the sample, and position marking is carried out on the surface to be detected, so that the defect can be accurately positioned in the analysis process under the electron microscope.

The sample preparation process method provided by the embodiment of the invention has the following beneficial effects that:

the embodiment of the invention provides a sample preparation process method, which comprises the following steps: cutting the steel with the surface defects to form a sample to be detected; cutting the auxiliary steel according to the size of the sample to be detected to form an auxiliary sample, wherein the thickness of the auxiliary sample is 1-2 mm, and the straightness of the auxiliary sample and the straightness of the sample to be detected are kept consistent; bonding the sample to be detected and the auxiliary sample by using double-sided copper conductive adhesive to form a combined sample, wherein the distance between the double-sided copper conductive adhesive and the edge to be ground of the sample to be detected is 2-3 mm; winding and fixing the combined sample, wherein after the combined sample is wound and fixed, a gap between the sample to be detected and the auxiliary sample is 0.05-0.15 mm; polishing the surface to be detected of the combined sample after being wound and fixed by using a polishing machine, and removing the auxiliary sample after the polishing is finished; carrying out ultrasonic cleaning and drying on the ground sample to be detected; after cleaning the surface to be detected of the sample to be detected, marking the defect of the surface to be detected; the auxiliary sample and the sample to be detected are bonded together for polishing, namely the auxiliary sample is used for positioning and polishing the sample to be detected, the problems of edge rounding, damage, pollution and the like of the sample to be detected when the sample to be detected is independently polished are solved by sacrificing the auxiliary sample, the original appearance of the surface to be detected is reserved, and the edge retention of the sample to be detected is improved; the sample to be detected and the auxiliary sample are bonded by the bilateral copper conductive adhesive, so that the auxiliary sample can be easily detached, secondary pollution and secondary damage to the sample to be detected are avoided, and secondary utilization of the sample to be detected is not influenced; therefore, the analysis result of the sample can be ensured, objective and accurate data can be provided for process improvement and product quality improvement in actual production, and the product quality is finally ensured.

And, still have following beneficial effect: firstly, the double-sided conductive adhesive does not influence the conductivity of a sample to be detected and does not influence the next electron microscope analysis; the conductive adhesive is pure copper, and does not cause element interference in EDS component analysis of a sample to be detected.

Secondly, compare and inlay and glue system sample, when the scanning electron microscope utilized high energy electron beam to the sample that awaits measuring to bombard, can not cause the thermal damage at sample and the bonding department of inlaying or bonding base material.

And thirdly, the thickness of the iron sheet on the surface of the hot rolled plate is more accurately counted aiming at different steel types by optimizing the preparation method of the electron microscope sample. At present, the requirement of customers on the thickness precision of products is increasingly strict, the thickness of the iron sheet of the hot rolled plate is accurately mastered, so that the strong support is provided for the order receiving capacity of high-end customer orders, and quality objections caused by the over-tolerance of the thickness precision are effectively reduced.

And fourthly, through optimizing the preparation method of the electron microscope sample, the iron sheet structure on the surface of the pickling plate of different steel grades is accurately known and mastered in scientific research experiments. Under the guidance of the conclusion obtained by a series of experiments, the acid liquor concentration in the pickling production process is continuously adjusted and optimized aiming at different steel grades on the premise of ensuring the good and stable surface quality of the hot rolled plate after pickling, thereby not only reducing the pressure of acid liquor circulation regeneration, but also effectively reducing the pickling cost,

the above description is only exemplary of the present invention and should not be taken as limiting the scope of the present invention, and any modifications, equivalents, improvements, etc. that are within the spirit and principle of the present invention should be included in the present invention.