CN216900304U - An EBSD sample preparation device for easily oxidized metals - Google Patents

Abstract

The utility model provides an EBSD sample preparation device for oxidizable metals, which can effectively solve the problem that the EBSD calibration rate is affected by the surface oxidation caused by the contact with air after the oxidizable metal samples are electropolished. The scheme includes a first container, a second container, a mobile sample holding mechanism and a sample transition device. The mobile sample holding mechanism is arranged above the first container, and its holding part faces downward and can move in the horizontal direction, so The first container is provided with a sample discharge hole, the sample transition device is arranged outside the sample discharge hole, the second container is docked with the sample transition device, and the sample can be discharged from the sample after the sample is released by the clamping part The hole exits and falls into the second container after passing through the sample transition device.

Description

An EBSD sample preparation device for easily oxidized metals

technical field

The utility model relates to the technical field of sample preparation devices for metal samples, in particular to an EBSD sample preparation device for easily oxidized metals.

Background technique

In recent years, EBSD technology has become an effective analysis method in material research, and has been widely used in the characterization of material microstructure and microtexture. EBSD technology, the full name of Electron Backscattered Diffraction, is the analysis technology of electron backscattered pattern crystal micro-domain orientation and crystal structure assembled on SEM. EBSD has changed the previous method of texture analysis and formed a new scientific field, called "microtexture" - combining microstructural and crystallographic analysis.

The EBSD test has extremely high requirements on the sample, especially the surface of the sample is required to be flat and free of residual stress. Electropolishing is an extremely important sample preparation method for EBSD characterization. In recent years, scholars have carried out a lot of research on electrolytic polishing devices and methods for metal samples. For example, Patent No. CN111551573A discloses a rotary motion type EBSD test sample automatic electrolytic polishing device and method. The disclosed electrolytic polishing tank on the inner bottom surface of the hemisphere has good conductivity and corrosion resistance. Metal cups with vertical walls. There are shortcomings such as the inability to observe the polishing of the surface of the sample to be polished during electrolytic polishing, and the lack of an insulating layer in the metal cup, which is easy to cause electric shock. Patent No. CN209941141U discloses a device suitable for electrolytic polishing of metal samples. The disclosed device can completely immerse the sample in the electrolytic polishing solution to obtain a better polished surface. Patent No. CN207738886U discloses a simple electrolytic polishing device for metallographic samples, and the disclosed device also makes the electrolytic polishing liquid submerge the sample. Patent No. CN112501681A discloses a preparation method for electrochemical polishing samples of high and low carbon martensitic stainless steel. The disclosed method includes sealing the edges of the polished samples with colorless nail polish, exposing the parts to be polished; nails After the oil is semi-dry, the sample is fixed on the outer side wall of the electrolytic cell, and then polished, using the method of partial immersion. There are many similar patents and will not be described here.

From the above results, it can be found that in the existing electropolishing device or method, whether the sample to be polished is completely immersed or partially immersed in the polishing solution, it is inevitable to take the polished sample out of the polishing solution after polishing, which will lead to sticking The surface of the polished sample of the polishing solution is in direct contact with the air, and the surface of the polished sample is highly active, which can easily cause the oxidation of easily oxidizable metals (such as magnesium alloys) and affect the subsequent EBSD calibration rate. Based on the above problems, it is urgent to develop a new EBSD sample preparation device for easily oxidized metals.

Utility model content

The utility model provides an EBSD sample preparation device for oxidizable metals, which can effectively solve the problem that the EBSD calibration rate is affected by the surface oxidation caused by contact with air after the oxidizable metal samples are electropolished.

The technical solution of the present invention is that it comprises a first container, a second container, a movable sample clamping mechanism and a sample transition device, wherein the movable sample clamping mechanism is arranged above the first container, and its clamping portion faces downward and Can move in the horizontal direction, the first container is provided with a sample discharge hole, the sample transition device is provided outside the sample discharge hole, the second container is butted with the sample transition device, and the sample is released by the clamping part. Afterwards, the sample can be discharged from the sample discharge hole and fall into the second container after passing through the sample transition device.

As a preference of the above solution, the first container includes a main container and an auxiliary container arranged on the upper side of the main container, the tops of the main container and the auxiliary container are both open, and there is a space between the main container and the auxiliary container to enable the The gap through which the clamping part passes, and the bottom of the auxiliary container is higher than the bottom of the main container.

As a preferred option of the above solution, the first container further comprises a base disposed at the bottom, the bottom of the main container is open, a circular groove is formed on the upper surface of the base, and an annular groove is formed on the inner side wall of the circular groove groove, an annular sealing ring is arranged in the annular groove, the lower part of the main body container is placed in the circular groove, the outer side wall of the main body container and the annular sealing ring are squeezed to form a seal, and the side wall of the circular groove is provided with a through hole The through hole is located under the annular sealing ring. The lowest point of the through hole is flush with the bottom surface of the circular groove or lower than the bottom surface of the circular groove. The through hole is provided with a metal drain pipe, which is an interference fit with the inner wall of the through hole. To form a seal, the end of the metal drain pipe located outside the main body container is provided with a sealing plug, which is used to block the drain pipe. The inner area of the vessel communicates with a metal drain.

As a preferred option of the above solution, the mobile sample clamping mechanism includes a guide rail, a slide block and a sample holder, the two ends of the guide rail are respectively overlapped with the side wall of the main container and the side wall of the auxiliary container, and the slide block is arranged on the lower surface of the guide rail, The slide block can slide along the guide rail from the top of the main container to the top of the auxiliary container. The sample holder is made of metal material, is connected to the slide block, and can move with the slide block. The negative and positive terminals of the power supply are connected.

As a preference of the above solution, the side wall of the main container and the side wall of the auxiliary container are each provided with a box body, the top of the box body is open, and the two box bodies are facing each other, the two ends of the guide rail are bent downward, and the two boxes are bent downward. The folded parts are respectively inserted into the corresponding boxes.

As a preferred option of the above solution, the sample discharge hole is provided at the bottom of the accessory container, just below the guide rail, the sample transition device is provided below the sample discharge hole, and the sample transition device is provided with a longitudinal through hole and two valve plate cavities , the longitudinal through hole and the sample discharge hole are arranged coaxially, each valve plate cavity is respectively provided with a valve plate, and the two valve plate cavities are opened from the outer side wall of the sample transition device to the interior of the sample transition device along the horizontal direction, and two The valve plate is inserted into the corresponding valve plate cavity from the outer side wall of the sample transition device, which can divide the longitudinal through hole into three independent areas of upper, middle and lower sections, and when the valve plate is pulled out, the longitudinal through hole can be opened. The top and bottom surfaces of the two valve plate cavities are provided with annular sealing rings, which can press the upper and lower surfaces of the corresponding valve plates to form a seal, and the sealing rings are arranged coaxially with the longitudinal through holes.

The lower surface of the sample transition device is provided with an annular boss, the annular boss is coaxial with the longitudinal through hole on the sample transition device, and the opening at the upper end of the second container is detachably sleeved on the annular boss In addition, it is possible to receive samples dropped from the longitudinal through holes.

As a preference of the above solution, both the first container and the second container are made of transparent materials.

The beneficial effects of the present utility model are:

1. The existing electropolishing methods cannot avoid the need to take out the polishing liquid from the polished sample, which will cause the surface of the polished sample with the polishing liquid to be in direct contact with the air, and the surface of the polished sample has high activity. It is easy to cause oxidation and affect the subsequent EBSD calibration rate. The device and method can effectively prevent the polished surface adhering the polishing liquid from contacting with the air, play the role of preventing the surface oxidation of the sample, and effectively improve the EBSD calibration rate of the sample.

2. In this device, the slider can drive the polishing sample to move back and forth in the polishing liquid, which can effectively remove the corrosion products generated during the polishing process of the surface of the sample in time, so as to avoid contaminating the surface of the sample and affecting the calibration effect.

3. The device can prevent the ethanol in the second container from entering the interior of the first container, so as to avoid contaminating the polishing liquid in the first container.

4. The first container and the second container of the device are made of transparent materials, and the electropolishing process can be observed through the container wall.

Description of drawings

FIG. 1 is a schematic diagram of the overall structure of the present invention.

2 and 5 are schematic diagrams of the internal structure of the utility model.

FIG. 3 is a schematic structural diagram of a sample transition device in the present invention.

FIG. 4 is a schematic structural diagram of the metal drain pipe in the utility model.

Detailed ways

Embodiments of the present utility model are described in detail below with reference to the accompanying drawings

As shown in FIG. 1 , the structure of this embodiment includes a first container 1 , a second container 2 , a mobile sample holder 303 holding mechanism 3 and a sample transition device 4 . The first and second containers are made of transparent materials. The sample holder 303 is provided above the first container 1 with the holding mechanism 3 , and its clamping portion faces downward and can move in the horizontal direction. The first container 1 is provided with a sample discharge hole 103 , and the sample transition device 4 is provided outside the sample discharge hole 103 , the second container 2 is docked with the sample transition device 4 , after the sample is released from the clamping part, the sample can be discharged from the sample discharge hole 103 , and then falls into the second container 2 after passing through the sample transition device 4 .

The first container 1 includes a main container 101 and an auxiliary container 102 provided on the upper side of the main container 101. The tops of the main container 101 and the auxiliary container 102 are both open. , the bottom of the accessory container 102 is higher than the bottom of the main container 101 .

The first container 1 also includes a base 5 arranged at the bottom, the bottom of the main container 101 is open, the upper surface of the base 5 is provided with a circular groove, the inner side wall of the circular groove is provided with an annular groove, and the annular groove is provided with an annular seal. Ring 8, the lower part of the main container 101 is placed in the circular groove, the outer side wall of the main container 101 and the annular sealing ring 8 are squeezed to form a seal, the side wall of the circular groove is provided with a through hole, and the through hole is located under the annular sealing ring 8 , the lowest point of the through hole is flush with the bottom surface of the circular groove or lower than the bottom surface of the circular groove, a metal drain pipe 6 is arranged in the through hole, and the interference fit with the inner wall of the through hole forms a seal. The outer end of the main container 101 is provided with a sealing plug 7 for blocking the drain pipe, and a gap 104 is formed at the lower end of the main container 101 opposite to the metal drain pipe 6 for draining the inner area of the main container 101 from the metal drain. The pipe 6 communicates.

The mobile sample holder 303 holding mechanism 3 includes a guide rail 301, a slider 302 and a sample holder 303. Both ends of the guide rail 301 are overlapped on the side wall of the main container 101 and the side wall of the auxiliary container 102 respectively. The slider 302 is arranged on the lower surface of the guide rail 301. The slider 302 can slide along the guide rail 301 from the top of the main container 101 to the top of the auxiliary container 102. The sample holder 303 is made of metal material, is connected to the slider 302, and can move with the slider 302. The metal drain pipe 6 and the sample holder 303 Connect to the negative and positive poles of the DC power supply through wires, respectively.

The side wall of the main container 101 and the side wall of the auxiliary container 102 are each provided with a box body 105, the top of the box body 105 is open, and the two box bodies 105 are facing each other. inside the box 105.

The sample discharge hole 103 is provided at the bottom of the accessory container 102, just below the guide rail 301. The sample transition device 4 is provided below the sample discharge hole 103. The sample transition device 4 is provided with a longitudinal through hole 403 and two valve plate cavities 404. The through hole 403 and the sample discharge hole 103 are arranged coaxially, each valve plate cavity 404 is respectively provided with a valve plate 401 , and the two valve plate cavities 404 are opened from the outer wall of the sample transition device 4 to the interior of the sample transition device 4 along the horizontal direction. , the two valve plates 401 are inserted into the corresponding valve plate cavity 404 from the outer side wall of the sample transition device 4, and the longitudinal through hole 403 can be divided into three independent areas of the upper, middle and lower sections, and when the valve plate 401 is pulled out , the longitudinal through hole 403 can be opened, and the top and bottom surfaces of the two valve plate cavities 404 are provided with annular sealing rings 405, which can squeeze the upper and lower surfaces of the corresponding valve plates 401 to form a seal. The holes 403 are arranged coaxially.

The lower surface of the sample transition device 4 is provided with an annular boss 406, the annular boss 406 is coaxial with the longitudinal through hole 403 on the sample transition device 4, and the upper opening of the second container 2 is detachably sleeved outside the annular boss, The sample dropped from the longitudinal through hole 403 can be received.

The working principle of the above device is described in detail below:

Taking the easily oxidizable metal magnesium alloy AZ31 as an example, the alloy is subjected to wire cutting. For better electropolishing effect, the length and width of the sample are not more than 8mm, and the thickness is not more than 6mm. Pay attention to the EBSD calibration direction of the sample.

Use clean water to clean all the containers of the device, use sandpaper to polish the bottom surface of the groove of the base 5 to remove the oxide layer on the surface, then clean with absolute ethanol, and then dry the first and second containers and the base 5 with a blower cold air.

Fill the second container 2 with absolute ethanol, connect the upper opening of the second container 2 to the annular boss on the lower surface of the sample transition device 4, and push the two valve plates 401 to fully extend into the longitudinal through holes of the sample transition device 4. 403, so as to divide the longitudinal through hole 403 into three independent areas of upper, middle and lower sections.

Further, use 400-mesh, 600-mesh, 800-mesh, 1000-mesh, 1500-mesh, and 2000-mesh SiC sandpaper to manually grind the samples in turn, rinse the ground samples with alcohol, and then dry them with the cold air of a hair dryer. The sample holder 303 is operated to hold the sample, the surface to be polished faces downward, and the slider 302 is slid so that the sample is located in the center of the main body container 101 .

Pour the polishing liquid into the main container 101, pay attention to make the polishing liquid submerge the bottom of the auxiliary container 102 and immerse the lower part of the sample into the polishing liquid. The sealing plug 7 is used to adjust the liquid level of the polishing liquid. For magnesium alloys, the well-established commercial polishing fluid AC2 can be used.

Manually set the voltage of the DC stabilized power supply at 20V. Use a wire to connect the metal drain tube 6 (as the cathode) of the base 5 with the negative electrode of the DC stabilized power supply, pour a certain amount of liquid nitrogen into the first container 1, adjust the temperature, insert a thermometer, and the temperature of the polishing liquid is - In the range of 30℃～-40℃, use a wire to connect the sample holder 303 (as the anode) to the positive electrode of the DC stabilized power supply, start polishing, observe the polishing condition of the sample through the inner wall of the first container 1, and slide it back and forth left and right. Block 302 can effectively remove the polished corrosive substances in time to avoid contaminating the surface of the sample. Take care to keep the sample above the base 5. When polishing for about 90 seconds, immediately disconnect the power supply and cut off the current.

Slide the slider 302 to the side of the accessory container 102, so that the sample is located directly above the sample discharge hole 103 of the accessory container 102, release the sample clamp, so that the sample falls on the inner hole at the bottom of the accessory container 102, pull out to the top The valve plate 401 of the sample transition device 4 is opened, and the upper and middle regions of the longitudinal through hole 403 of the sample transition device 4 are opened, so that the sample falls from the sample discharge hole 103 into the longitudinal through hole 403 of the sample transition device 4 and stays on the valve plate located below. 401 on. The upper valve plate 401 is closed, the lower valve plate 401 is opened, and the sample can be dropped into the second container 2 .

Finally, remove the second container 2, take out the sample at an appropriate time, and put it into the electron microscope device for EBSD calibration.

In the above embodiment, since the sample transition device 4 is provided, the two valve plates 401 open and close the longitudinal through holes 403 of the sample transition device 4 successively, so that the sample is dropped from the auxiliary container 102 into the second container 2, At the same time, it is ensured that the polishing liquid in the first container 1 is not polluted by the ethanol in the second container 2 .

In the above embodiment, the second container 2 and the annular boss of the sample transition device 4 are detachably connected, that is, directly connected by inner and outer circles. After the sample falls into the second container 2, the second container 2 can be directly removed. container 2.

The above are only preferred embodiments of the present invention, and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims (8)

1. an EBSD sample preparation device of easily oxidizable metal, is characterized in that: comprise a first container, a second container, a mobile sample clamping mechanism and a sample transition device, and the mobile sample clamping mechanism is located in the first container Above, the clamping part faces downward and can move in the horizontal direction, the first container is provided with a sample discharge hole, the sample transition device is arranged outside the sample discharge hole, and the second container is butted with the sample transition device, After the sample is released from the clamping part, the sample can be discharged from the sample discharge hole, and then fall into the second container after passing through the sample transition device. 2 . The EBSD sample preparation device according to claim 1 , wherein the first container comprises a main container and an auxiliary container arranged on the upper side of the main container, the main container and the auxiliary container are both open at the top, and the main container is open. 3 . A gap is provided between the container and the auxiliary container for allowing the clamping part to pass through, and the bottom of the auxiliary container is higher than the bottom of the main container. 3 . The EBSD sample preparation device according to claim 2 , wherein the first container further comprises a base disposed at the bottom, the bottom of the main container is open, and the upper surface of the base is provided with a circular groove, 4 . The inner side wall of the circular groove is provided with an annular groove, and an annular sealing ring is arranged in the annular groove. , the side wall of the circular groove is provided with a through hole, the through hole is located under the annular sealing ring, the lowest point of the through hole is flush with the bottom surface of the circular groove or lower than the bottom surface of the circular groove, and the through hole is provided with The metal drain pipe is formed by interference fit with the inner wall of the through hole to form a seal. The end of the metal drain pipe located outside the main container is provided with a sealing plug to block the drain pipe. The lower end of the main container is connected to the metal drain pipe. The opposite part of the pipe is provided with a gap, which is used to communicate the inner area of the main container with the metal drain pipe. 4 . The EBSD sample preparation device according to claim 3 , wherein the mobile sample clamping mechanism comprises a guide rail, a slider and a sample holder, and the two ends of the guide rail are respectively overlapped on the side wall of the main container and the accessory. 5 . The side wall of the container, the slide block is arranged on the lower surface of the guide rail, the slide block can slide along the guide rail from the top of the main container to the top of the auxiliary container, the sample holder is made of metal material, connected with the slide block, and can move with the slide block. The metal drain pipe and the sample holder are connected to the negative and positive electrodes of the DC power supply through wires, respectively. 5 . The EBSD sample preparation device according to claim 4 , wherein the side wall of the main container and the side wall of the auxiliary container are each provided with a box body, the top of the box body is open, and the two box bodies are opposite to each other, Both ends of the guide rail are bent downward, and the two bent portions are respectively inserted into the corresponding boxes. 6 . The EBSD sample preparation device according to claim 4 , wherein the sample discharge hole is located at the bottom of the accessory container, just below the guide rail, the sample transition device is located below the sample discharge hole, and the sample transition device is located on the bottom of the sample transition device. 7 . There is a longitudinal through hole and two valve plate cavities, the longitudinal through hole and the sample discharge hole are coaxially arranged, each valve plate cavity is respectively provided with a valve plate, and the two valve plate cavities are formed by the outer wall of the sample transition device. It opens into the interior of the sample transition device in the horizontal direction, and two valve plates are inserted into the corresponding valve plate cavity from the outer side wall of the sample transition device, which can divide the longitudinal through hole into three independent areas of upper, middle and lower sections, and outwards When the valve plate is drawn out, the longitudinal through hole can be opened, and the top and bottom surfaces of the two valve plate cavities are provided with annular sealing rings, which can squeeze the upper and lower surfaces of the corresponding valve plates to form a seal. The through holes are arranged coaxially. 7. The EBSD sample preparation device according to claim 6, characterized in that: the lower surface of the sample transition device is provided with an annular boss, and the annular boss is coaxial with the longitudinal through hole on the sample transition device, so The opening at the upper end of the second container is detachably sleeved outside the annular boss, and can receive the sample dropped from the longitudinal through hole. 8 . The EBSD sample preparation device according to claim 1 , wherein the first container and the second container are made of transparent materials. 9 .

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