CN217651345U - A electrolytic polishing device for preparing EBSD sample - Google Patents

Abstract

The utility model discloses an electrolytic polishing device for preparing EBSD sample, the device integrates power supply ware, electrical source controller and magnetic stirrers, set up magnetic stirrers in the top of power supply ware and electrical source controller, electrolysis trough and washing tank setting are on magnetic stirrers, be provided with two magnetic stirrers on the magnetic stirrers for can stir electrolysis trough and washing tank simultaneously, the device has that the structure is retrencied, parameter control is simple and convenient, the electrolytic polishing time is controllable, electrolytic voltage is adjustable, convenient washing, make characteristics such as appearance efficient.

Description

A electrolytic polishing device for preparing EBSD sample

Technical Field

The utility model belongs to the technical field of metal material electrolytic polishing, concretely relates to electrolytic polishing device for preparing EBSD sample.

Background

The metal material is characterized by adopting an Electron Backscatter Diffraction (EBSD) technology, and the method plays an important role in analyzing the aspects of poor grain orientation, grain size, grain boundary characteristics, micro texture and the like of the material by scientific researchers. The sample for EBSD test has high requirement on surface quality, the test surface is smooth and flat, no stress is introduced by sample preparation, and the conductivity is good. At present, the method for preparing the sample by adopting electrolytic polishing is the simplest and most convenient and effective, the electrolytic polishing is to ensure that the test surface of the sample is flat, smooth and stress-free by the electrochemical action, and the method has the advantages of simple operation, high speed, low cost and the like.

The principle of the metal material electrolytic polishing method is as follows: in the electrolytic polishing solution, a sample to be polished is used as an anode, insoluble metal is used as a cathode, a voltage is applied between the anode and the cathode, and current passes between the anode and the cathode, so that the anode, namely a microscopic convex part on the surface of the sample to be polished is selectively dissolved to form a smooth surface. In electrolysis, the electrolyte is often stirred or cooled to prevent overheating of the electrolyte. According to the information such as the material of the sample to be electropolished, a proper electrolyte is selected and used, the prepared electrolyte is injected into an electrolytic cell, the electrolyte is fully stirred and cooled, the temperature of the electrolyte reaches the required use temperature, and the preparation and use temperature of the electrolyte are generally ensured to be lower than 30 ℃.

Through research on related reports, most of the electrolytic polishing devices divide a power supply and a stirrer into two independent parts, so that the device integration effect is poor; when the sample is subjected to electrolytic polishing, the electrolytic polishing time cannot be accurately controlled, and the determination of experimental parameters in the sample preparation process is influenced, so that the sample preparation effect is unstable; there is not corresponding belt cleaning device after system appearance electrolytic polishing finishes, if do not rinse immediately, remaining electrolyte can continue to react with the sample, to the material that easily oxidizes, can take place to oxidize in the air and also can seriously influence system appearance effect.

SUMMERY OF THE UTILITY MODEL

The utility model aims to overcome the defects of the prior art and provide an electrolytic polishing device for preparing an EBSD sample and a using method thereof. The problems that experiment parameters such as electrolytic polishing time are difficult to accurately control, a polished sample is rapidly cleaned and the like in the prior art are solved.

In order to achieve the above purpose, the utility model adopts the following technical scheme to realize:

an electrolytic polishing device for preparing an EBSD sample comprises a power supply and a power supply controller which are adjacently arranged in parallel, wherein the power supply controller is electrically connected with the power supply; a magnetic stirrer is arranged above the power supply device and the power supply controller together, and an electrolytic bath and a cleaning tank are arranged at the upper part of the magnetic stirrer; the power supply device is electrically connected with the magnetic stirrer;

the magnetic stirrer is internally provided with a first magnetic rotary table and a second magnetic rotary table, the electrolytic bath is arranged on the first magnetic rotary table, and the cleaning tank is arranged on the second magnetic rotary table;

the electrolytic bath is internally provided with a cathode clamp, the electrolytic bath or the cleaning tank is internally provided with an anode clamp, the upper end of the cathode clamp is connected with a power supply device through a cathode wire, and the upper end of the anode clamp is connected with the power supply device through an anode wire.

The utility model discloses a further improvement lies in:

preferably, the power supply has a case surface provided with a device switch, a cathode socket into which one end of a cathode lead is inserted, and an anode socket into which one end of an anode lead is inserted.

Preferably, the power controller is connected with the cathode socket, and the power controller is connected with the anode socket.

Preferably, a first magnetic rotary table in the magnetic stirrer is electrically connected with a first rotating speed control button, and a second magnetic rotary table is electrically connected with a second rotating speed control knob.

Preferably, the top of the electrolytic cell is provided with an electrolytic cell cover plate, and the top of the cleaning tank is provided with a cleaning tank cover plate;

the cathode clamp is arranged on the cover plate of the electrolytic cell, and the anode clamp is arranged on the cover plate of the electrolytic cell or the cover plate of the cleaning tank.

Preferably, the cathode clamp is mounted on the electrolytic cell cover plate through a positioning slide block, and the anode clamp is mounted on the electrolytic cell cover plate or the cleaning tank cover plate through a positioning slide block.

Preferably, the positioning slide block is provided with a through hole, and the anode clamp or the cathode clamp penetrates through the through hole; the anode clamp or the cathode clamp is fixed in the through hole by the bolt.

Preferably, the bottom of the cathode clamp and the bottom of the anode clamp are both provided with two clamping arms, and the two clamping arms are connected and screwed through bolts.

Compared with the prior art, the utility model discloses following beneficial effect has:

the utility model discloses an electrolytic buffing device for preparing EBSD sample, the device integrates the power supply ware, electrical source controller and magnetic stirrers, set up magnetic stirrers in the top of power supply ware and electrical source controller, electrolysis trough and washing tank setting are on magnetic stirrers, be provided with two magnetic stirrers on the magnetic stirrers, make and to stir electrolysis trough and washing tank simultaneously, the device has that the structure is retrencied, parameter control is simple and convenient, the electrolytic buffing time is controllable, electrolytic voltage is adjustable, convenient washing, make characteristics such as appearance efficient.

Furthermore, a cathode wire socket and an anode wire socket are arranged on the power supply device, so that the cathode clamp and the anode clamp are conveniently electrically connected.

Furthermore, two magnetic rotary tables are arranged in the magnetic stirrer, and each magnetic rotary table is provided with an independent control button, so that the magnetic rotary tables are convenient to control independently.

Furthermore, the tops of the electrolytic cell and the cleaning tank are respectively provided with a cover plate, so that the cathode clamp and the anode clamp can be conveniently mounted.

Furthermore, the cathode clamp and the anode clamp are both fixed in the positioning slide block through bolts, so that the clamping objects at the bottom can be conveniently detached and replaced.

Drawings

FIG. 1 is a schematic front view of an electropolishing apparatus in accordance with the present invention;

FIG. 2 is a schematic top view of an electropolishing apparatus in accordance with the present invention;

FIG. 3 is a schematic diagram of an electropolishing process in an embodiment of the present invention;

FIG. 4 is a schematic diagram of a cleaning process according to an embodiment of the present invention;

fig. 5 shows the original BC chart of the EBSD test of the magnesium alloy in example 1 of the present invention;

fig. 6 shows the original BC map of the titanium alloy EBSD test in example 2 of the present invention;

the device comprises a cathode clamp 1, an electrolytic cell cover plate 2, an electrolytic cell 3, an electrolyte 4, a first magnetic rotor 5, a magnetic stirrer 6, a first magnetic rotary table 7, a first speed control knob 8, a power supply 9, an equipment switch 10, a cathode lead 11, a cathode jack 12, an anode jack 13, an anode lead 14, a display screen 15, a power supply controller 16, a time control knob 17, a current control knob 18, a voltage control knob 19, a second speed control knob 20, a second magnetic rotary table 21, a second magnetic rotor 22, a cleaning solution 23, a cleaning tank 24, a cleaning tank cover plate 25, an anode clamp 26, a device shell 27, a positioning slide block 28, a cathode metal block 29 and a test sample 30.

Detailed Description

The present invention will be described in further detail with reference to the accompanying drawings:

in the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention; the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance; furthermore, unless expressly stated or limited otherwise, the terms "mounted," "connected," and "coupled" are to be construed broadly and encompass, for example, both fixed and removable coupling arrangements; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood in specific cases to those skilled in the art.

The utility model provides an electrolytic polishing device for preparing EBSD sample, including device shell 27, power supply 9, power supply controller 16, magnetic stirrers 6.

With particular reference to fig. 1, the power supply 9 and the power controller 16 are arranged together in the lower part of the housing 27. The surface of the shell of the power supply 9 is provided with an equipment switch 10, a cathode socket 12 and an anode socket 13, the power supply 9 is used for converting alternating current into direct current which can be used in the device, the direct current is respectively provided for a cathode lead 11 and an anode lead 14 through the cathode socket 12 and the anode socket 13 in the electrolysis and polishing process, and the power supply 9 is simultaneously connected with the magnetic stirrer 6 and provides power for the magnetic stirring process in the magnetic stirrer 6; the power controller 16 is electrically connected with the power supply 9 and is used for controlling the output parameter of the power supply 9. Specifically, the surface of the housing of the power controller 16 is provided with a display screen 15, a time controller, a time control knob 17, a current control knob 18 and a voltage control knob 19. The time control knob 17 is connected with a time controller, the time controller can adjust the direct current power supply time of the power supply device, the current control knob 18 and the voltage control knob 19 are respectively connected with a current controller and a voltage controller in the power supply device, the current controller and the voltage controller are respectively connected with the cathode jack 12 and the anode jack 13 and are used for controlling the current and the voltage of the direct current output from the cathode jack 12 and the anode jack 13, and specific parameter values are displayed through a display screen; the current and voltage values of the output direct current are adjusted through a current control knob and a voltage control knob; the power supply time is adjusted by a time control knob.

The magnetic stirrer 6 is assembled on the upper part of the device shell 27, and the magnetic stirrer 6 is arranged on the upper parts of the power supply 9 and the power supply controller 16. The upper portion of magnetic stirrers 6 is provided with two and is provided with two first magnetic force revolving stage 7 and the second magnetic force revolving stage 21 that set up side by side, and the first speed control knob 8 of first magnetic force is connected with first magnetic force revolving stage 7 for the magnetic force of control first magnetic force revolving stage 7 output, and second magnetic force revolving stage 21 is connected with second speed control knob 20, and second speed control knob 20 is used for controlling the magnetic force of second magnetic force revolving stage 21 output.

Referring to fig. 1, an electrolytic cell 3 is placed above a first magnetic turntable 7, electrolytic polishing liquid 4 is placed in the electrolytic cell 3, a magnetic rotor 5 is arranged at the bottom of the electrolytic cell 3, preferably, the first magnetic rotor 5 is arranged right above the first magnetic turntable 5, the top of the electrolytic cell 3 is connected with an electrolytic cell cover plate 2 through a clamping groove, and the electrolytic cell cover plate 2 is in a strip plate shape and is erected at the top of the electrolytic cell 3; the cleaning tank 24 is placed above the second magnetic rotary table 21, the cleaning solution 23 is placed in the cleaning tank 24, the second magnetic rotor 22 is arranged at the bottom of the cleaning tank 24, preferably, the second magnetic rotor 22 is arranged right above the second magnetic rotary table 21, the top of the cleaning tank 24 is connected with a cleaning tank cover plate 25 through a clamping groove, and the cleaning tank cover plate 25 is in a strip-shaped plate shape and is erected at the top of the cleaning tank 24.

Referring to fig. 2 and 3, the cathode clamp 1 is mounted on the electrolytic cell cover plate 2, the cathode metal block 29 is clamped at the bottom of the cathode clamp 1, the cathode clamp 1 is mounted on the electrolytic cell cover plate 2 through a positioning slide block 28, the cathode lead 11 is welded at the top of the cathode clamp 1, and the cathode clamp is connected with the power supply cathode jack 12 through the cathode lead 11. The anode clamp 26 is placed on the electrolytic tank cover plate 2 or the cleaning tank cover plate 25 through a positioning slide block 28, the test sample 30 is clamped at the bottom of the anode clamp 26, the anode lead 14 is welded at the top of the anode clamp 26, and the anode clamp is connected with the power supply anode socket 13 through the anode lead 14. The positioning slide block 28 is internally provided with holes penetrating through the upper and lower surfaces, when the cathode clamp 1 or the anode clamp 26 is clamped, the cathode clamp 1 or the anode clamp 2 is inserted into the positioning slide block 28, bolts are inserted from the side surface of the positioning slide block 28, and the bolts abut against the side edge of the cathode clamp 1 or the anode clamp 2, so that the cathode clamp 1 or the anode clamp 2 can be fixed by the positioning slide block 28.

The bottom that negative pole pressed from both sides 1 or positive pole pressed from both sides 2 all is provided with clamping structure, and clamping structure includes two centre gripping arms, is used for centre gripping negative pole metal block 29 or test sample 30 between two centre gripping arms, and it has the bolt to pass through between two centre gripping arms through the bolt of screwing for the centre gripping arm can centre gripping negative pole metal block 29 or test sample 30, be provided with the spring on the bolt, place two centre gripping arms and press from both sides the equipment and damage negative pole metal block 29 or test sample 30.

The utility model also discloses an electrolyte for preparing EBSD sample, this electrolyte have that the prescription is simple, with low costs, polluting characteristics such as little to can carry out metal material's electrolytic polishing at room temperature, especially material electrolytic polishing effect such as preparation magnesium alloy, titanium alloy, stainless steel is showing, the resolution of sample can reach more than 85% when carrying out the EBSD test.

The utility model discloses device working method:

with reference to fig. 1-4, one embodiment of the electropolishing apparatus and electrolyte solution for preparing EBSD samples is as follows:

(1) The metal sample 30 to be measured is firstly polished on the abrasive paper of different models, and the sample is polished to No. 2000 abrasive paper, and the surface to be measured is cleaned and dried by blowing when the smooth scratch direction is consistent.

(2) The above-mentioned electrolytic solution 4 is poured into the electrolytic bath 3, and the volume of the electrolytic solution 4 occupies approximately two thirds of the capacity of the electrolytic bath 3. The cleaning liquid 23 is poured into the cleaning tank 24, and the volume of the cleaning liquid 23 occupies about two thirds of the capacity of the cleaning tank 24, as shown in fig. 1.

(3) The cathode 29 is clamped at the bottom of the cathode clamp 1 by taking a nickel-based alloy as the cathode 29, then the cathode clamp 1 is placed at the cathode on the cover plate 2 of the electrolytic bath, and the cathode is partially immersed in the electrolyte by adjusting a positioning slide block on the cathode clamp, as shown in figures 2 and 3.

(4) The device switch 10 is turned on, the voltage control knob 19 is adjusted to preset the electropolishing voltage, and the time control knob 17 is adjusted to preset the electropolishing time, so that the specific voltage, current and time information can be viewed on the display 15, as shown in fig. 1.

(5) The magnetic rotor 5 in the electrolytic bath 3 is rotated at a proper rotation speed by adjusting the first rotation speed control knob 8, and the magnetic rotor 22 in the cleaning bath 24 is rotated at a proper rotation speed by adjusting the second rotation speed control knob 20, see fig. 1.

(6) The sample to be measured 29 is clamped at the bottom of the anode clamp 26, then the anode clamp 26 is placed at the anode on the cover plate 2 of the electrolytic cell, the anode surface to be measured is immersed in the electrolyte 4 by adjusting the positioning slide block 28, at this time, the electrolytic polishing is started, the time controller is started to work, and the power supply is automatically cut off when the preset time is cut off, see fig. 2 and fig. 3.

(7) Immediately after the electrolytic polishing is completed, the anode holder 26 is placed on the cleaning tank cover plate 25, and the sample is completely immersed in the cleaning solution 23 by adjusting the positioning slider 28, see fig. 4. And (5) taking out the sample after cleaning for a period of time, drying the sample by using a blower with cold air, and storing the sample, wherein the sample preparation is finished at the moment.

The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Example 1:

in this example, the additive manufacturing AZ31 magnesium alloy was electropolished with 5% vol of perchloric acid and 95% vol of absolute ethanol at room temperature. Before electrolytic polishing, an AZ31 magnesium alloy sample needs to be ground and roughly polished, wherein the electrolytic polishing parameters are as follows: voltage 30V, time 30S and current 0.2-0.3A. The specific operation steps are shown in the implementation process (1-7), and the magnesium alloy cleaning agent is absolute ethyl alcohol. The EBSD test result of the prepared sample is shown in figure 5, the green part in the figure is an unresolved area, the resolution of the local area of the sample reaches 97.3 percent, and the sample preparation efficiency is high and the effect is good.

Example 2:

in this example, the additive manufacturing titanium alloy was electropolished with 5% vol of perchloric acid and 95% vol of absolute ethanol, and electropolished at room temperature. The titanium alloy sample needs to be ground before electrolytic polishing, and the electrolytic polishing parameters are as follows: voltage 30V, time 30S and current 0.2-0.5A. The specific operation steps are shown in the implementation process (1-7), and the cleaning agent is purified water. The EBSD test result of the prepared sample is shown in figure 6, wherein the green part in the figure is an unresolved area, the resolution of the local area of the sample reaches 97.7 percent, and the sample preparation efficiency is high and the effect is good.

The above description is only for the preferred embodiment of the present invention, and should not be taken as limiting the invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (8)

1. An electrolytic polishing device for preparing an EBSD sample is characterized by comprising a power supply (9) and a power supply controller (16) which are adjacently arranged in parallel, wherein the power supply controller (16) is electrically connected with the power supply (9); a magnetic stirrer (6) is arranged above the power supply (9) and the power controller (16), and an electrolytic tank (3) and a cleaning tank (24) are arranged at the upper part of the magnetic stirrer (6); the power supply device (9) is electrically connected with the magnetic stirrer (6);

a first magnetic rotary table (7) and a second magnetic rotary table (21) are arranged in the magnetic stirrer (6), the electrolytic cell (3) is arranged on the first magnetic rotary table (7), and the cleaning tank (24) is arranged on the second magnetic rotary table (21);

install negative pole in electrolysis trough (3) and press from both sides (1), install positive pole in electrolysis trough (3) or washing tank (24) and press from both sides (26), the upper end that the negative pole pressed from both sides (1) is connected with power supply ware (9) through negative pole wire (14), the upper end that the positive pole pressed from both sides (26) is connected with power supply ware (9) through positive pole wire (11).

2. The electropolishing apparatus for preparing an EBSD sample, according to claim 1, wherein the power supply (9) has a housing surface provided with a device switch (10), a cathode socket (12), and an anode socket (13), wherein one end of a cathode lead (14) is inserted into the cathode socket (12), and one end of an anode lead (11) is inserted into the anode socket (13).

3. An electropolishing apparatus for preparing an EBSD sample according to claim 2, wherein power controller (16) is connected to cathode jack (12), and power controller (16) is connected to anode jack (13).

4. The electropolishing apparatus for preparing an EBSD sample according to claim 1, wherein a first magnetic turret (7) of the magnetic stirrer (6) is electrically connected to a first rotational speed control button (8), and a second magnetic turret (21) is electrically connected to a second rotational speed control knob (20).

5. The electropolishing apparatus for preparing an EBSD sample, according to claim 1, wherein an electrolyzer lid plate (2) is mounted on the top of the electrolyzer (3), and a cleaning tank lid plate (25) is mounted on the top of the cleaning tank (24);

the cathode clamp (1) is arranged on the electrolytic tank cover plate (2), and the anode clamp (26) is arranged on the electrolytic tank cover plate (2) or the cleaning tank cover plate (25).

6. The electropolishing apparatus for preparing an EBSD sample, according to claim 5, characterized in that the cathode clamp (1) is mounted on the cell cover plate (2) by means of a positioning slide (28), and the anode clamp (26) is mounted on the cell cover plate (2) or the cleaning tank cover plate (25) by means of a positioning slide (28).

7. The electropolishing apparatus for preparing an EBSD sample according to claim 6, wherein the positioning slide (28) has a through-hole, and the anode clamp (26) or the cathode clamp (1) passes through the through-hole; the anode clamp (26) or the cathode clamp (1) is fixed in the through hole by being pressed against by a bolt.

8. The electropolishing apparatus for preparing an EBSD sample, according to claim 1, wherein the bottom of the cathode clamp (1) and the anode clamp (26) are each provided with two clamping arms, which are screwed together by a screw.

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