CN216900304U

CN216900304U - EBSD sample preparation device for easily oxidized metal

Info

Publication number: CN216900304U
Application number: CN202220211264.1U
Authority: CN
Inventors: 余辉辉; 胡强; 曾延琦
Original assignee: Institute of Applied Physics of Jiangxi Academy of Sciences
Current assignee: Institute of Applied Physics of Jiangxi Academy of Sciences
Priority date: 2022-01-25
Filing date: 2022-01-25
Publication date: 2022-07-05
Anticipated expiration: 2032-01-25

Abstract

The utility model provides an EBSD sample preparation device for easily oxidized metal, which can effectively solve the problem that the EBSD calibration rate is influenced due to the fact that the surface of an easily oxidized metal sample is oxidized due to the fact that the easily oxidized metal sample is in contact with air after being electropolished.

Description

EBSD sample preparation device of easy oxidation metal

Technical Field

The utility model relates to the technical field of sample preparation devices for metal samples, in particular to an EBSD (electron back scattering diffraction) sample preparation device for easily oxidized metal.

Background

In recent years, the EBSD technology has become an effective analysis means in material research, and has been widely applied to material microstructure and microtexture characterization. EBSD technology, totally called Electron backscattering Diffraction (Electron Backscattered Diffraction, is an analysis technology of the orientation of the crystal micro-area and the crystal structure of the Electron backscattering pattern crystal assembled on SEM), changes the traditional texture analysis method and forms a brand new scientific field called microtexture, namely combines the microstructure with the crystallographic analysis.

The EBSD test has extremely high requirements on the sample, and particularly requires that the sample has a smooth surface and no residual stress. Electropolishing is an extremely important sample preparation method for performing EBSD characterization. In recent years, researchers have conducted extensive research into an apparatus and a method for electropolishing metal samples. For example, patent No. CN111551573A discloses a rotary motion type automatic electropolishing apparatus and method for EBSD test specimens, which discloses a hemispherical inner bottom electropolishing cell that is a metal cup with good conductivity and corrosion resistance, a hemispherical inner bottom surface, and vertical walls at the periphery. The defects that the polishing condition of the surface of a sample to be polished cannot be observed during electrolytic polishing, a metal cup does not have an insulating layer, and people are easy to get an electric shock exist. Patent No. CN209941141U discloses an apparatus suitable for electropolishing a metal sample, which can completely immerse the sample in an electropolishing solution to obtain a better polished surface. Patent No. CN207738886U discloses a simple metallographic sample electrolytic polishing device, which also enables the electrolytic polishing liquid to flood the sample. The patent number CN112501681A discloses a preparation method of a high-low carbon martensitic stainless steel electrochemical polishing sample, which comprises the steps of sealing the edge of the sample by using colorless nail polish to expose the part to be polished; and fixing the sample on the outer side wall of the electrolytic cell after the nail polish is semi-dried, and polishing by adopting a local soaking method. Similar patents are numerous and not much described here.

From the above results, it can be found that, in the conventional electrolytic polishing device or method, no matter the sample to be polished is completely immersed or partially immersed in the polishing solution, the polished sample cannot be taken out of the polishing solution after polishing, which may cause direct contact between the surface of the polished sample adhered with the polishing solution and air, and the surface of the polished sample has high activity, which is very likely to cause oxidation of easily-oxidizable metal (such as magnesium alloy), thereby affecting the subsequent EBSD calibration rate. In view of the above problems, there is a need to develop a new EBSD sample preparation apparatus for easily oxidized metals.

SUMMERY OF THE UTILITY MODEL

The utility model provides an EBSD sample preparation device for easily oxidized metal, which can effectively solve the problem that the EBSD calibration rate is influenced by surface oxidation caused by contact with air after an easily oxidized metal sample is subjected to electrolytic polishing.

The technical scheme of the utility model is as follows: including first container, second container, portable sample fixture and sample transition device, portable sample fixture locates first container top, and its clamping part down just can follow the horizontal direction and remove, be equipped with the sample discharge hole on the first container, sample transition device locates outside the sample discharge hole, the second container docks with sample transition device, after the sample was released the sample by the clamping part, the sample can be followed the sample and discharged the hole and discharged, falls into in the second container behind sample transition device.

Preferably, the first container includes a main container and an auxiliary container disposed on one side of an upper portion of the main container, wherein both top portions of the main container and the auxiliary container are open, a notch allowing the holding portion to pass therethrough is provided between the main container and the auxiliary container, and a bottom of the auxiliary container is higher than a bottom of the main container.

Preferably, the first container further comprises a base arranged at the bottom, the bottom of the main container is open, a circular groove is formed in the upper surface of the base, an annular groove is formed in the inner side wall of the circular groove, an annular sealing ring is arranged in the annular groove, the lower portion of the main container is arranged in the circular groove, the outer side wall of the main container is in press fit with the annular sealing ring to form sealing, a through hole is formed in the side wall of the circular groove, the through hole is located below the annular sealing ring, the lowest point of the through hole is flush with or lower than the bottom surface of the circular groove, a metal liquid discharge pipe is arranged in the through hole and is in interference fit with the inner wall of the through hole to form sealing, a sealing plug is arranged at one end of the metal liquid discharge pipe, which is located outside the main container, and used for blocking the liquid discharge pipe, a notch is formed in the position, opposite to the metal liquid discharge pipe, of the lower end of the main container, for communicating the interior region of the main container with a metal drain pipe.

Preferably, the movable sample clamping mechanism comprises a guide rail, a sliding block and a sample clamp, two ends of the guide rail are respectively lapped on the side wall of the main container and the side wall of the auxiliary container, the sliding block is arranged on the lower surface of the guide rail and can slide from the upper part of the main container to the upper part of the auxiliary container along the guide rail, the sample clamp is made of a metal material and is connected with the sliding block and can move along with the sliding block, and the metal liquid discharge pipe and the sample clamp are respectively connected with the negative electrode and the positive electrode of the direct-current power supply through leads.

Preferably, the side wall of the main container and the side wall of the auxiliary container are respectively provided with a box body, the top of the box body is open, the two box bodies are right opposite, the two ends of the guide rail are bent downwards, and the two bent parts are respectively inserted into the corresponding box bodies.

Preferably, the sample discharge hole is provided in the bottom of the auxiliary container, directly below the guide rail, the sample transition device is arranged below the sample discharge hole, a longitudinal through hole and two valve plate cavities are arranged on the sample transition device, the longitudinal through hole and the sample discharge hole are coaxially arranged, a valve plate is respectively arranged in each valve plate cavity, the two valve plate cavities are arranged in the sample transition device along the horizontal direction from the outer side wall of the sample transition device, the two valve plates are inserted into the corresponding valve plate cavities from the outer side wall of the sample transition device, the longitudinal through hole can be divided into an upper section, a middle section and a lower section which are independent, when the valve plates are drawn outwards, the longitudinal through holes can be opened, the top surfaces and the bottom surfaces of the two valve plate cavities are provided with annular sealing rings, the upper surfaces and the lower surfaces of the corresponding valve plates can be squeezed to form sealing, and the sealing rings and the longitudinal through holes are coaxially arranged.

The lower surface of the sample transition device is provided with an annular boss which is coaxial with a longitudinal through hole in the sample transition device, and the opening part at the upper end of the second container is detachably sleeved outside the annular boss and can accept samples falling from the longitudinal through hole.

Preferably, the first container and the second container are both made of transparent materials.

The utility model has the beneficial effects that:

1. the existing electrolytic polishing method avoids the problem that the polished sample does not need to be taken out of polishing solution, which can cause the surface of the polished sample stuck with the polishing solution to be in direct contact with air, and the surface of the polished sample has high activity, is easy to oxidize and influences the subsequent EBSD calibration rate. The device and the method can effectively prevent the polished surface adhered with the polishing solution from contacting with air, play a role in preventing the surface of the sample from being oxidized, and effectively improve the EBSD calibration rate of the sample.

2. Can drive the polishing sample round trip movement in the polishing solution through the slider among this device, can effectively make the corrosive substance that sample surface polishing in-process produced in timely break away from, avoid polluting the sample surface, influence the demarcation effect.

3. The device can prevent the ethanol in the second container from entering the first container, and plays a role in preventing the polishing solution in the first container from being polluted.

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

Drawings

Fig. 1 is a schematic view of the overall structure of the present invention.

Fig. 2 and 5 are schematic views of the internal structure of the present invention.

Fig. 3 is a schematic structural diagram of a sample transition device according to the present invention.

FIG. 4 is a schematic view of the structure of the metal drain pipe according to the present invention.

Detailed Description

Embodiments of the present invention 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 movable sample clamp 303 holding mechanism 3 and a sample transition device 4, both the first container and the second container are made of transparent materials, the movable sample clamp 303 holding mechanism 3 is disposed above the first container 1, a clamping portion thereof faces downward and can move along a horizontal direction, the first container 1 is provided with a sample discharge hole 103, the sample transition device 4 is disposed outside the sample discharge hole 103, the second container 2 is butted with the sample transition device 4, after the sample is released from the clamping portion, the sample can be discharged from the sample discharge hole 103, and fall 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 one side of an upper portion of the main container 101, wherein both the main container 101 and the auxiliary container 102 have open tops, a notch allowing a clamping portion to pass therethrough is provided between the main container 101 and the auxiliary container 102, and a bottom of the auxiliary container 102 is higher than a bottom of the main container 101.

The first container 1 also comprises a base 5 arranged at the bottom, the bottom of the main container 101 is provided with an opening, 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, an annular sealing ring 8 is arranged in the annular groove, the lower part of the main container 101 is arranged in the circular groove, the outer side wall of the main container 101 is in extrusion fit with the annular sealing ring 8 to form sealing, the side wall of the circular groove is provided with a through hole, the through hole is positioned below 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 liquid discharge pipe 6 is arranged in the through hole, sealing is formed by interference fit with the inner wall of the through hole, a sealing plug 7 is arranged at one end of the metal liquid discharge pipe 6 positioned outside the main body container 101, for blocking the drain pipe, a notch 104 is formed at a position of the lower end of the main body container 101 facing the metal drain pipe 6, for communicating the inner region of the main body container 101 with the metal drain pipe 6.

The movable sample clamp 303 holding mechanism 3 comprises a guide rail 301, a sliding block 302 and a sample clamp 303, two ends of the guide rail 301 are respectively lapped on the side wall of the main body container 101 and the side wall of the auxiliary container 102, the sliding block 302 is arranged on the lower surface of the guide rail 301, the sliding block 302 can slide from the upper part of the main body container 101 to the upper part of the auxiliary container 102 along the guide rail 301, the sample clamp 303 is made of a metal material and is connected with the sliding block 302 and can move along with the sliding block 302, and the metal liquid discharge pipe 6 and the sample clamp 303 are respectively connected with the negative electrode and the positive electrode of a direct-current power supply through conducting wires.

The side wall of the main container 101 and the side wall of the auxiliary container 102 are respectively provided with a box body 105, the top of the box body 105 is opened, the two box bodies 105 are right opposite, two ends of the guide rail 301 are bent downwards, and the two bent parts are respectively inserted into the corresponding box bodies 105.

The sample discharge hole 103 is arranged at the bottom of the auxiliary container 102 and is positioned right below the guide rail 301, the sample transition device 4 is arranged 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 longitudinal through hole 403 and the sample discharge hole 103 are coaxially arranged, a valve plate 401 is respectively arranged in each valve plate cavity 404, the two valve plate cavities 404 are opened towards the interior of the sample transition device 4 along the horizontal direction from the outer side wall of the sample transition device 4, the two valve plates 401 are inserted into the corresponding valve plate cavities 404 from the outer side wall of the sample transition device 4, and can divide the longitudinal through hole 403 into an upper section, a middle section and a lower section of independent areas, when the valve plate 401 is drawn out, the longitudinal through hole 403 can be opened, the top surface and the bottom surface of the two valve plate cavities 404 are both provided with annular sealing rings 405, the upper surface and the lower surface of the corresponding valve plate 401 can be squeezed to form sealing, and the sealing rings 405 and the longitudinal through hole 403 are coaxially arranged.

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 opening part at the upper end of the second container 2 is detachably sleeved outside the annular boss and can receive a sample falling from the longitudinal through hole 403.

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

taking the easily oxidized magnesium alloy AZ31 as an example, the alloy is subjected to wire cutting, and for better electropolishing effect, the length and width of the sample are not more than 8mm, the thickness is not more than 6mm, and attention is paid to the EBSD calibration direction of the sample.

All containers of the device are cleaned by clean water, the bottom surface of the groove of the base 5 is polished by abrasive paper, an oxide layer on the surface is removed, then the containers are cleaned by absolute ethyl alcohol, and the first container, the second container and the base 5 are dried by cold air of a blower.

Filling the second container 2 with absolute ethyl alcohol, butting the opening part at the upper end of the second container 2 with the annular boss on the lower surface of the sample transition device 4, and pushing the two valve plates 401 to completely extend into the longitudinal through hole 403 of the sample transition device 4 so as to divide the longitudinal through hole 403 into an upper section, a middle section and a lower section of independent areas.

Further, the test piece was manually ground using 400 mesh, 600 mesh, 800 mesh, 1000 mesh, 1500 mesh and 2000 mesh SiC paper in this order, the ground test piece was rinsed with alcohol, and then dried with cold air blown by an electric blower, the test piece was held by the sample holder 303 with the surface to be polished facing downward, and the slide block 302 was slid so that the test piece was positioned at the center of the main body container 101.

The polishing liquid is poured into the main body container 101, taking care that the polishing liquid is made to flood the bottom of the sub-container 102 and that the lower portion of the sample is immersed in the polishing liquid, and the sealing stopper 7 is used to adjust the liquid level of the polishing liquid. For magnesium alloys, mature commercial polishing liquid AC2 was used.

The voltage of the direct current stabilized power supply is manually set to be 20V. A metal liquid discharge pipe 6 (as a cathode) of a base 5 is connected with a negative electrode of a direct current stabilized power supply by using a lead, a certain amount of liquid nitrogen is poured into the first container 1, the temperature is adjusted, a thermometer is inserted, when the temperature of polishing liquid is in a range of-30 ℃ to-40 ℃, a sample clamp 303 (as an anode) is connected with a positive electrode of the direct current stabilized power supply by using the lead, polishing is started, the polishing condition of a sample is observed through the inner wall of the first container 1, a sliding block 302 slides back and forth left and right, polished corrosive substances can be effectively separated in time, and the surface of the sample is prevented from being polluted. Care is taken to hold the sample above the base 5. When the polishing time is about 90 seconds, the power supply is immediately cut off, and the current is cut off.

Sliding the slider 302 to the side of the sub-tank 102 so that the test sample is positioned right above the sample discharge hole 103 of the sub-tank 102, releasing the sample holder so that the test sample falls at the bottom inner hole of the sub-tank 102, pulling the valve plate 401 positioned above outward, opening the upper and middle regions of the longitudinal through hole 403 of the sample transition device 4 so that the test sample falls from the sample discharge hole 103 into the longitudinal through hole 403 of the sample transition device 4, and rests on the valve plate 401 positioned below. The upper valve plate 401 is closed, and the lower valve plate 401 is opened, so that the sample is dropped into the second container 2.

Finally, the second container 2 is taken down, and the sample is taken out at an appropriate time and placed in an electron microscope device for EBSD calibration.

In the above embodiment, since the sample transition device 4 is provided, the two valve plates 401 sequentially open and close the longitudinal through hole 403 of the sample transition device 4, thereby dropping the sample from the subsidiary container 102 into the second container 2 while ensuring that the polishing solution in the first container 1 is not contaminated by the ethanol in the second container 2.

In the above embodiment, the second container 2 is detachably connected to the annular boss of the sample transition device 4, that is, the annular boss is directly connected to the inner circle and the outer circle in a matching manner, and after the sample falls into the second container 2, the second container 2 can be directly taken down.

The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. An EBSD sample preparation device of easy oxidation metal which characterized in that: including first container, second container, portable sample fixture and sample transition device, portable sample fixture locates first container top, and its clamping part down just can follow the horizontal direction and remove, be equipped with the sample discharge hole on the first container, sample transition device locates outside the sample discharge hole, the second container docks with sample transition device, after the sample was released the sample by the clamping part, the sample can be followed the sample and discharged the hole and discharged, falls into in the second container behind sample transition device.

2. The EBSD sample preparation apparatus of claim 1, wherein: the first container comprises a main container and an auxiliary container arranged on one side of the upper portion of the main container, the tops of the main container and the auxiliary container are both open, a notch enabling the clamping portion to pass through is formed between the main container and the auxiliary container, and the bottom of the auxiliary container is higher than that of the main container.

3. The EBSD sample preparation apparatus of claim 2, wherein: the first container also comprises a base arranged at the bottom, the bottom of the main container is opened, a circular groove is arranged on the upper surface of the base, the inner side wall of the circular groove is provided with an annular groove, an annular sealing ring is arranged in the annular groove, the lower part of the main container is arranged in the circular groove, the outer side wall of the main container is in extrusion fit with the annular sealing ring to form sealing, the side wall of the circular groove is provided with a through hole, the through hole is positioned below the annular sealing ring, the lowest point of the through hole is flush with the bottom surface of the circular groove or is lower than the bottom surface of the circular groove, a metal liquid discharge pipe is arranged in the through hole, sealing is formed by interference fit with the inner wall of the through hole, a sealing plug is arranged at one end of the metal liquid discharge pipe positioned outside the main body container, the liquid discharge pipe is used for being blocked, and a notch is formed in the position, opposite to the metal liquid discharge pipe, of the lower end of the main container and used for communicating the inner area of the main container with the metal liquid discharge pipe.

4. The EBSD sample preparation apparatus of claim 3, wherein: the movable sample clamping mechanism comprises a guide rail, a sliding block and a sample clamp, wherein two ends of the guide rail are respectively lapped on the side wall of the main container and the side wall of the auxiliary container, the sliding block is arranged on the lower surface of the guide rail, the sliding block can slide from the upper part of the main container to the upper part of the auxiliary container along the guide rail, the sample clamp is made of a metal material and is connected with the sliding block and can move along with the sliding block, and the metal liquid discharge pipe and the sample clamp are respectively connected with the cathode and the anode of the direct-current power supply through leads.

5. The EBSD sample preparation device according to claim 4, wherein: the main part container lateral wall and subsidiary container lateral wall respectively are equipped with a box body, box body open-top, and two box bodies are just relative, the guide rail both ends are buckled downwards, and two bent portions insert respectively to the box body that corresponds.

6. The EBSD sample preparation device according to claim 4, wherein: the sample discharge hole is arranged at the bottom of the auxiliary container and is positioned under the guide rail, the sample transition device is arranged below the sample discharge hole, a longitudinal through hole and two valve plate cavities are arranged on the sample transition device, the longitudinal through hole and the sample discharge hole are coaxially arranged, a valve plate is respectively arranged in each valve plate cavity, the two valve plate cavities are formed in the sample transition device from the outer side wall of the sample transition device along the horizontal direction, the two valve plates are inserted into the corresponding valve plate cavities from the outer side wall of the sample transition device and can separate the longitudinal through hole into an upper section, a middle section and a lower section which are independent, when the valve plates are drawn outwards, the longitudinal through hole can be opened, the top surfaces and the bottom surfaces of the two valve plate cavities are respectively provided with an annular sealing ring, the upper surface and the lower surface of the corresponding valve plate can be squeezed to form sealing, and the sealing rings are coaxially arranged with the longitudinal through hole.

7. The EBSD sample preparation apparatus of claim 6, wherein: the lower surface of the sample transition device is provided with an annular boss which is coaxial with a longitudinal through hole in the sample transition device, and the opening part at the upper end of the second container is detachably sleeved outside the annular boss and can accept samples falling from the longitudinal through hole.

8. The EBSD sample preparation apparatus of claim 1, wherein: the first container and the second container are both made of transparent materials.