CN116024644A - Electrochemical mechanical polishing method for wet particle electrolyte of metal complex structural member - Google Patents

Electrochemical mechanical polishing method for wet particle electrolyte of metal complex structural member Download PDF

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CN116024644A
CN116024644A CN202310042627.2A CN202310042627A CN116024644A CN 116024644 A CN116024644 A CN 116024644A CN 202310042627 A CN202310042627 A CN 202310042627A CN 116024644 A CN116024644 A CN 116024644A
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electrolyte
wet
polishing
metal complex
mechanical polishing
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CN202310042627.2A
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康仁科
程吉瑞
高尚
董志刚
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Dalian University of Technology
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Dalian University of Technology
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Abstract

The invention provides a wet particle electrolyte electrochemical mechanical polishing method for a metal complex structural member. The method comprises the following steps: the metal sample is fixed on a rotating main shaft with a special clamp, axially rotates along with the rotating main shaft, and is immersed in a reaction tank filled with wet particle electrolyte. Under the drive of the rotary spindle, the metal sample piece and the wet particle electrolyte generate relative motion; the contact area of the single wet particle electrolyte and the metal sample is smaller than the area of the metal sample; in the polishing process, a metal sample is connected with the anode of a direct current power supply, the cathode of the power supply is connected with the cathode of the reaction tank wall, and the anode and the cathode are communicated through wet particle electrolyte. The invention has the advantages of adopting wet particles as electrolyte, no additional liquid electrolyte, capability of selectively removing rough peaks on the surface of a metal sample by using the wet particle electrolyte, high polishing rate, obviously improved roughness before and after polishing, simple operation and flexible and adjustable technological parameters.

Description

Electrochemical mechanical polishing method for wet particle electrolyte of metal complex structural member
Technical Field
The invention relates to the technical field of polishing processing, in particular to a wet particle electrolyte electrochemical mechanical polishing method for a metal complex structural member.
Background
The complex structural member has a series of excellent mechanical properties such as high strength and light weight, and is widely applied to the fields of aerospace, ship military, vehicle industry and the like, and the duty ratio of the complex structural member applied to high-end equipment is gradually increased. With the complexity of the part structure, the surface polishing technology of the complex structural member is also an urgent problem to be solved. The polishing process of the complex structural member can remove the processing damaged layer and the internal residual stress of the previous working procedure, and improve the overall mechanical property of the part. Because the surface shape of the complex structural member is complex, the characteristics of an inner cavity, a thin wall and the like exist, the traditional polishing technology cannot polish the complex structural member efficiently.
The traditional mechanical polishing method for complex structural parts is high in equipment research and development cost and low in polishing efficiency, and cannot meet the high-efficiency polishing requirement of parts. The abrasive particle flow polishing is suitable for polishing small complex structural parts with inner cavities, and cannot meet the polishing requirements of large-size parts. Electrochemical polishing is widely used for polishing complex structural members because of its advantages of high polishing efficiency, simple equipment, capability of polishing large-sized parts, etc. However, most of the electrolyte used in electrochemical polishing is prepared from harmful components, which causes a certain damage to the environment. In addition, the sharp structure of complex structural members can be damaged by the point discharge principle of electrochemical polishing, and the application of electrochemical polishing in engineering is limited. During the electrochemical polishing process, passivation films are enriched at rough peaks on the surface of the workpiece, and further progress of the reaction is hindered. The removal rate is limited by the dissolution rate of the oxide, and the removal rate of the material cannot be further improved. In the prior art, (Millet, p.s. (2020) Method for smoothing and polishing metals via ion transport free solid bodies and solid bodies for performing the method.us10683583b 2.) the polishing effect is primarily achieved by adsorbing the electrolyte with porous resin particles, but the method still uses conventional electrolyte and causes a certain harm to the environment and personnel.
Disclosure of Invention
According to the technical problem set forth above, a method for electrochemical mechanical polishing of a wet particulate electrolyte of a metal complex structure is provided. The invention adopts the following technical means:
a method of electrochemical mechanical polishing of a wet particulate electrolyte of a metal complex structure comprising the steps of:
step 1, fixing a metal sample on a rotating main shaft with a special clamp so that the metal sample can axially rotate along with the rotating main shaft;
step 2, filling the reaction tank with wet particle electrolyte, and completely immersing the metal sample piece in the wet particle electrolyte;
step 3, under the drive of the rotary spindle, the metal sample piece and the wet particle electrolyte generate relative motion; the contact area of the wet particle electrolyte and the metal sample is smaller than the area of the metal sample;
step 4, connecting the metal sample piece with the positive electrode of the direct current power supply in the polishing process to serve as an anode; the cathode arranged on the wall of the reaction tank is connected with the cathode of the direct current power supply; the wet particle electrolyte communicates the anode with the cathode;
the wet particle electrolyte is cation exchange resin with a porous structure, and acidic groups can be fixed on a crosslinked framework of electrolyte particles.
The electrochemical mechanical polishing based on the wet particle electrolyte is a processing mode for increasing the material removal rate through the mechanical action of the wet particle electrolyte by replacing the original electrolyte with the wet particle electrolyte.
Under the drive of the rotary spindle, the metal sample piece and the wet particle electrolyte generate relative motion, so that the wet particle electrolyte and the surface of the metal sample piece can generate the functions of scratching, collision and plowing.
Preferably, the special fixture is a disc-type fixture made of nylon, PEEK, acrylic and other materials, polishing of 4 metal samples can be simultaneously carried out, and the fixture does not have conductivity.
The fixable acidic group includes a sulfonic acid group-SO 3 H. Acid groups such as carboxylic acid group-COOH and the like, and no additional electrolysis is neededThe liquid needs to reasonably regulate the water content of the conductive particle medium;
the water content of the particulate electrolyte can affect the degree of ionization of the acidic groups and thus the conductivity of the wet particulate electrolyte.
The reaction tank is a cylindrical reaction tank made of non-conductive materials such as acrylic, the size of the reaction tank is proper, and the metal sample can be completely immersed.
The cathode is made of inert materials such as stainless steel or graphite rings, and the cathode materials are attached to the inner wall of the reaction tank and distributed in a ring shape.
Preferably, the polishing spindle can simultaneously carry out translational movement during rotational movement, so that the surface polishing uniformity of the metal sample is ensured.
Preferably, the pressure control during polishing can be controlled by the speed of the rotating spindle.
The contact area of the wet particle electrolyte and the metal sample is far smaller than the area of the metal sample; the electrolyte particles are made to selectively remove the rough peaks on the surface of the material without the addition of mechanical scratches.
Further, the wet particulate electrolyte particle size is 0.5-0.8mm.
As a preferred solution, the wet particulate electrolyte is controlled in water content using the following process:
a) Immersing the wet particulate electrolyte in deionized water for 30 minutes;
b) Heating the wet particle electrolyte for 10-30min through a hot oven; measuring the electrolyte water content of the wet particles every 5 min;
preferably, the instrument used for measuring the moisture content of the wet particle electrolyte is a soil parameter rapid measuring instrument.
Furthermore, the applied voltage on the surface of the metal complex structural member is not easy to be too large, and the voltage needs to be controlled between 0 and 3V.
Further, the motor rotation speed needs to be controlled at 50-300 rpm, and the polishing time needs to be reasonably controlled at 0.5-1.5 h.
Compared with the prior art, the electrochemical mechanical polishing method for the wet particle electrolyte of the metal complex structural member has the following advantages:
1. the polishing and removing efficiency is high. The invention directly removes the rough peak on the surface of the sample piece through the electrochemical mechanical coupling removal function of the wet particle electrolyte. An oxide film is generated on the rough peaks of the sample piece through electrochemical oxidation, and then the oxide film is removed through the mechanical action of wet particle electrolyte, so that a new surface is exposed, and the removal rate in the whole polishing process is improved.
2. The wet particle electrolyte internally contains acidic groups, and electrolyte is not required to be additionally added, so that the oxidation of a rough peak on the surface of a sample can be promoted under the electrochemical action, and the removal rate in the whole electrochemical mechanical polishing process is improved.
3. The polishing main shaft can simultaneously carry out translational motion during rotary motion, so that the polishing uniformity of the complex characteristic curved surface of the metal sample is ensured. In particular, pressure control during polishing can be controlled by the speed of the rotating spindle.
Compared with the prior art, the electrochemical mechanical polishing method for the wet particle electrolyte of the metal complex structural member has the following advantages:
1. the polishing and removing efficiency is high. The invention directly removes the rough peak on the surface of the sample piece through the electrochemical mechanical coupling removal function of the wet particle electrolyte. An oxide film is generated on the rough peaks of the sample piece through electrochemical oxidation, and then the oxide film is removed through the mechanical action of wet particle electrolyte, so that a new surface is exposed, and the removal rate in the whole polishing process is improved.
2. The wet particle electrolyte internally contains acidic groups, and electrolyte is not required to be additionally added, so that the oxidation of a rough peak on the surface of a sample can be promoted under the electrochemical action, and the removal rate in the whole electrochemical mechanical polishing process is improved.
3. The polishing main shaft can simultaneously carry out translational motion during rotary motion, so that the polishing uniformity of the complex characteristic curved surface of the metal sample is ensured. In particular, pressure control during polishing can be controlled by the speed of the rotating spindle.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to the drawings without inventive effort to a person skilled in the art.
FIG. 1 is a schematic view of an electrochemical mechanical polishing apparatus for wet particulate electrolytes of metal complex structures according to the present invention.
FIG. 2 shows the surface topography of pure copper prior to polishing in an embodiment of the present invention, wherein (a) is a field emission scanning electron microscope surface topography image and (b) is a ZYGO white light interferometer surface topography image.
FIG. 3 shows the surface topography of a polished pure copper in an embodiment of the invention, wherein (a) is a field emission scanning electron microscope surface topography image and (b) is a ZYGO white light interferometer surface topography image.
In the figure: 1. a reaction tank; 2. a stainless steel cathode; 3. a wet particulate electrolyte; 4. a direct current power supply; 5. a clamp; 6. a metal sample; 7. the spindle is rotated.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
As shown in fig. 1, the embodiment of the invention discloses an electrochemical mechanical polishing method for wet particle electrolyte of a metal complex structural member, and a polishing device adopted by the method comprises a reaction tank 1, a stainless steel cathode 2, a wet particle electrolyte 3, a direct current power supply 4, a clamp 5, a metal sample 6 and a rotary spindle 7. The clamp 5 is in threaded connection with the rotating main shaft 7 and is fixed at the bottom end of the rotating main shaft 7. The metal sample 6 is fixed on the fixture 5, and the annular stainless steel cathode 2 is embedded on the inner wall of the reaction tank 1. A wet particulate electrolyte 3 is added to the reaction cell 1, and the metal sample 6 is completely immersed in the wet particulate electrolyte 3. The positive electrode of the direct current power supply 4 is connected with the metal sample 6, and the negative electrode of the direct current power supply 4 is connected with the stainless steel cathode 2. The polishing method comprises the following steps: the direct current power supply is regulated to a proper voltage, so that electrochemical reaction occurs on the surface of the metal sample. The metal sample piece is driven by a rotating main shaft driven by a motor to axially rotate, the wet particle electrolyte is in contact with the metal sample piece to obtain acceleration, the wet particle electrolyte is continuously collided with the metal sample piece, and rough peaks on the surface of the metal sample piece are mechanically removed.
The technical effects of the present invention will be described below with a specific example. In this example, a cation exchange resin was used as the wet particle electrolyte, and the metal sample was pure copper, and the surface of the pure copper was polished by a 600# sandpaper before polishing, to deteriorate the surface. The surface of the pure copper sample piece before polishing is observed by a scanning electron microscope, obvious scratches are visible on the surface, the surface is rough, and the surface morphology measurement result is shown in fig. 2.
The electrochemical mechanical polishing process of the wet particle electrolyte of the metal complex structural member comprises the following specific steps:
(1) The surface of pure copper was polished by 600# sandpaper prior to polishing to deteriorate the surface. And sequentially ultrasonically cleaning the sample by adopting ethanol and deionized water. The original morphology before polishing was measured by using a field emission scanning electron microscope and a ZYGO white light interferometer as shown in fig. 2 (a) (b), and it was seen that the surface had obvious scratches, the surface was rough, and the surface roughness was 433.507nm.
(2) The wet particle electrolyte is selected from polystyrene cation exchange resin, the water content of the wet particle electrolyte is regulated, and the water content is controlled to be 35-55%.
(3) The pure copper sample was fixed to a jig and immersed in the wet granular electrolyte.
(4) A dc voltage of 0 to 3V is applied between the anode and the cathode. And starting the motor, and controlling the rotating speed of the rotating main shaft to be 50-300 rpm. The polishing time is 0.5-1.5 h.
Preferably, the polishing voltage should be controlled in a reasonable range, and 1V is used as the best, and the voltage and the rotating speed should be controlled in reasonable combination to realize controllable removal.
(5) And after finishing polishing, taking down the metal sample, sequentially ultrasonically cleaning the sample by adopting ethanol and deionized water, and measuring the surface roughness after polishing.
In the step (4), the polishing effect under different parameters is shown in Table 1
TABLE 1
Name of the name Water content Motor speed Polishing time Surface roughness
Example 1 50.2% 160 r/min 1h 98.178nm
Example 2 50.2% 300r/min 1 h 36.709nm
Example 3 40% 160r/min 1 h 64.283nm
Example 4 40% 300r/min 1 h 22.434nm
After the pure copper sample is polished, the surface quality is obviously better, scratches in fig. 2 disappear, the surface becomes flat, the roughness value is reduced to about 22.434nm, and the measurement results of the polished surface morphology are shown in fig. 3 (a) and (b). The invention has the advantages of high polishing removal rate, obviously improved roughness before and after polishing, simple operation and flexible and adjustable process parameters.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.

Claims (10)

1. A method of electrochemical mechanical polishing of a wet particulate electrolyte of a metal complex structure, comprising the steps of:
step 1, fixing a metal sample on a rotating main shaft with a special clamp so that the metal sample can axially rotate along with the rotating main shaft;
step 2, filling the reaction tank with wet particle electrolyte, and completely immersing the metal sample piece in the wet particle electrolyte;
step 3, under the drive of the rotary spindle, the metal sample piece and the wet particle electrolyte generate relative motion; the contact area of the wet particle electrolyte and the metal sample is smaller than the area of the metal sample;
step 4, connecting the metal sample piece with the positive electrode of the direct current power supply in the polishing process to serve as an anode; the cathode arranged on the wall of the reaction tank is connected with the cathode of the direct current power supply; the wet particle electrolyte communicates the anode with the cathode;
the wet particle electrolyte is cation exchange resin with a porous structure, and acidic groups can be fixed on a crosslinked framework of electrolyte particles.
2. The method of electrochemical mechanical polishing of wet particulate electrolytes for metal complex structures according to claim 1, wherein the dedicated fixture is not conductive and the reaction cell is a non-conductive material.
3. The method for electrochemical mechanical polishing of wet particulate electrolyte of a metal complex structure according to claim 1, wherein the cathode is made of inert material and is attached to the inner wall of the reaction tank in a ring-shaped distribution.
4. The method for electrochemical mechanical polishing of a wet particulate electrolyte of a metal complex structure according to claim 1, wherein the fixable acidic groups comprise sulfonic acid groups-SO 3 H. And the carboxylic acid group-COOH does not need to be additionally added with electrolyte, and the water content of the conductive particle medium is regulated and controlled according to preset requirements.
5. The method for electrochemical mechanical polishing of a wet particulate electrolyte of a metal complex structure according to claim 1 or 4, wherein the wet particulate electrolyte has a particle size of 0.5-0.8mm.
6. The method of electrochemical mechanical polishing of wet particulate electrolytes of metal complex structures according to claim 1, characterized in that the pressure control during polishing is controlled by the speed of the rotating spindle, which is accompanied by a translational movement during the rotational movement.
7. The method for electrochemical mechanical polishing of a wet particulate electrolyte of a metal complex structure according to claim 4, wherein the wet particulate electrolyte has a controlled moisture content using the following process:
a) Immersing the wet particulate electrolyte in deionized water for 30 minutes;
b) Heating the wet particle electrolyte for 10-30min through a hot oven; the moisture content of the wet particle electrolyte was measured every 5 min.
8. The method for electrochemical mechanical polishing of a wet particulate electrolyte of a metal complex structure according to claim 7, wherein the instrument used for measuring the moisture content of the wet particulate electrolyte comprises a soil parameter tachometer.
9. The method for electrochemical mechanical polishing of a wet particulate electrolyte of a metal complex structure according to claim 1, wherein the applied voltage to the surface of the metal complex structure is controlled to be 0-3V.
10. The electrochemical mechanical polishing method of wet particle electrolyte for metal complex structural members according to claim 1, wherein the rotation speed of the motor is controlled to be 50-300 rpm, and the polishing time is controlled to be 0.5-1.5 h.
CN202310042627.2A 2023-01-28 2023-01-28 Electrochemical mechanical polishing method for wet particle electrolyte of metal complex structural member Pending CN116024644A (en)

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