CN113463178B - Electrolytic polishing solution and electrolytic polishing method for tungsten-based wire or sheet - Google Patents
Electrolytic polishing solution and electrolytic polishing method for tungsten-based wire or sheet Download PDFInfo
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- CN113463178B CN113463178B CN202110837607.5A CN202110837607A CN113463178B CN 113463178 B CN113463178 B CN 113463178B CN 202110837607 A CN202110837607 A CN 202110837607A CN 113463178 B CN113463178 B CN 113463178B
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25F3/00—Electrolytic etching or polishing
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- C25F3/22—Polishing of heavy metals
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Abstract
The invention discloses an electrolytic polishing solution for tungsten-based wire or sheetAn electrolytic polishing method relates to the technical field of metal surface treatment, and comprises quaternary ammonium hydroxide, absolute ethyl alcohol, 2-methyl-1-hexene, sodium sulfate and water, wherein the concentration of the quaternary ammonium hydroxide is 20-40 g/L, the concentration of the absolute ethyl alcohol is 10-50 g/L, the concentration of the 2-methyl-1-hexene is 1-5 g/L, and the concentration of the sodium sulfate is 50-100 g/L; placing the tungsten-based wire or sheet to be treated in an electrolytic polishing solution as an anode and nickel as a cathode, and adjusting the current density of a direct-current stabilized voltage supply to 1.0-4.0A/cm 2 The stirring speed is 5 to 40r/s. The invention has the advantages of bright and flat surface of the treated tungsten-based wire rod, low roughness, good polishing effect, no generation of dangerous gas in the polishing process, no need of heating and temperature rise, high ion flow speed, safety, environmental protection, controllability and high efficiency.
Description
Technical Field
The invention relates to the technical field of refractory metal surface treatment, in particular to safe, environment-friendly, controllable and efficient electrolytic polishing solution for tungsten-based wires or sheets and an electrolytic polishing method thereof.
Background
The tungsten-based wire or sheet has the characteristics of high melting point, high strength, high hardness and the like, and is widely applied to the high-tech fields of space motors, nuclear reactors and the like. In the development and preparation process of tungsten-based wire or sheet, multiple passes of extrusion, drawing, rolling and the like are often required, but because the material has poor plasticity and high hardness, the mechanical processing difficulty is higher, and the workpiece surface with a smoother surface and low roughness is difficult to obtain. Therefore, a simple and efficient method for treating the surface of a workpiece is needed.
The electrolytic polishing is a special anode electrochemical processing mode, in the process, a polished piece is used as an anode, insoluble metal is used as a cathode, and the electrochemical anode is used for dissolving, so that the effects of removing scratches, burrs and the like on the surface of a workpiece are achieved, and the surface of the workpiece is flat and bright. The currently accepted principle of electropolishing is the mucosa theory, i.e., the metal ions separated from the workpiece and the phosphoric acid in the polishing solution form a phosphate film to be adsorbed on the surface of the workpiece, and the mucosa has a thin convex part and a thick concave part, and is dissolved quickly due to the high current density at the convex part, flows along with the mucosa, and the concave and convex parts change continuously, and the rough surface is leveled gradually. With the increasing application of metal materials, particularly high-hardness materials, the electrolytic polishing is gradually a widely applied surface treatment process, and the process has the advantages of low cost, high efficiency, good effect and convenient operation, and can be well applied to the material surface treatment of tungsten-based wires or sheets.
For example, chinese patent CN200410103517 discloses an electrolytic polishing method for a high-precision tungsten sheet, and the polishing solution is prepared from NaOH and KClO 3 And K 2 CO 3 The preparation is carried out according to the proportion of 1 3 Belongs to an explosive reagent and has higher requirements on transportation and storage; chinese patent CN104060320A discloses a polishing solution for tungsten spiral line electrolytic polishing, wherein the polishing solution is prepared from sodium phosphate, sodium hydroxide, glycerol and water, and when the electrolytic polishing solution is adopted for electrolytic polishing, insoluble electrolytic products on the surface of a workpiece need to be cleaned at certain intervals, so that the polishing efficiency is low; chinese patent CN105887179 discloses an electrolytic polishing solution and an electrolytic polishing method for tungsten alloy or molybdenum alloy, wherein the polishing solution is prepared from sodium hydroxide, sodium carbonate and sodium molybdate according to the weight ratio of 35. Therefore, it is necessary to develop a safe, environment-friendly, controllable and efficient electropolishing method.
Disclosure of Invention
The invention aims to solve the technical problem of providing the electrolytic polishing solution for the tungsten-based wire or sheet, which is an aqueous solution of quaternary ammonium hydroxide, absolute ethyl alcohol, 2-methyl-1-hexene and sodium sulfate, and the electrolytic polishing solution is safe, environment-friendly, controllable and efficient in electrolytic polishing without heating in the electrolytic polishing process.
The technical solution of the invention is as follows:
an electrolytic polishing solution for tungsten-based wires or sheets comprises the following components: quaternary ammonium base, absolute ethyl alcohol, 2-methyl-1-hexene, sodium sulfate and water, wherein the concentration of the quaternary ammonium base in the electrolytic polishing solution is 20-40 g/L, the concentration of the absolute ethyl alcohol is 10-50 g/L, the concentration of the 2-methyl-1-hexene is 1-5 g/L, and the concentration of the sodium sulfate is 50-100 g/L.
In a specific embodiment of the invention, the concentration of quaternary ammonium hydroxide is 25-35 g/L, the concentration of absolute ethyl alcohol is 30-40 g/L, the concentration of 2-methyl-1-hexene is 2-4 g/L, and the concentration of sodium sulfate is 70-80 g/L.
In one embodiment of the present invention, the concentration of quaternary ammonium hydroxide is 35g/L, the concentration of absolute ethyl alcohol is 35g/L, the concentration of 2-methyl-1-hexene is 3g/L, and the concentration of sodium sulfate is 80g/L.
In one embodiment of the invention, the concentration of quaternary ammonium hydroxide is 35g/L, the concentration of absolute ethyl alcohol is 40g/L, the concentration of 2-methyl-1-hexene is 3g/L, and the concentration of sodium sulfate is 80g/L.
In one embodiment of the invention, the concentration of quaternary ammonium hydroxide is 25g/L, the concentration of absolute ethyl alcohol is 35g/L, the concentration of 2-methyl-1-hexene is 5g/L, and the concentration of sodium sulfate is 75g/L.
In one embodiment of the present invention, the concentration of quaternary ammonium hydroxide is 20g/L, the concentration of absolute ethyl alcohol is 30g/L, the concentration of 2-methyl-1-hexene is 2g/L, and the concentration of sodium sulfate is 100g/L.
In one embodiment of the present invention, the concentration of quaternary ammonium hydroxide is 35g/L, the concentration of absolute ethyl alcohol is 50g/L, the concentration of 2-methyl-1-hexene is 5g/L, and the concentration of sodium sulfate is 50g/L.
In one embodiment of the present invention, the quaternary ammonium hydroxide is one or more selected from the group consisting of tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide and trimethylethylammonium hydroxide.
The invention also provides a method for electropolishing tungsten-based wire or sheet by using the electropolishing solution, which comprises the following steps: tungsten to be treatedThe base wire or the sheet is placed in the electrolytic polishing solution to be used as an anode, nickel is used as a cathode, and the current density of the direct current stabilized voltage power supply is adjusted to be 1.0-4.0A/cm 2 Preferably, the current density is 2.0 to 3.0A/cm 2 More preferably, the current density is 2.5A/cm 2 And controlling the stirring speed of the electrolytic polishing solution to be 5-40 r/s, preferably 10-20 r/s, more preferably 15r/s, and performing electrolytic polishing on the surface of the tungsten-based wire or sheet, wherein the polishing time of the electrolytic polishing is not less than 30s, preferably 100-350 s.
The invention has at least one of the following beneficial effects:
the electrolytic polishing solution is an aqueous solution containing quaternary ammonium hydroxide, absolute ethyl alcohol, 2-methyl-1-hexene and sodium sulfate, the alkaline polishing solution mainly containing the quaternary ammonium hydroxide can dissolve an anode electrolytic polishing product, and is matched with a proper amount of absolute ethyl alcohol, 2-methyl-1-hexene and sodium sulfate, and the absolute ethyl alcohol, 2-methyl-1-hexene and sodium sulfate which are proper in the electrolytic polishing process can improve the polishing quality and efficiency of the surface of a workpiece and prevent the defects of lines, pinholes and the like. Because the raw materials and the content of the electrolytic polishing solution are selected and reasonably matched, and the synergistic effect of the absolute ethyl alcohol, the 2-methyl-1-hexene, the sodium sulfate and the quaternary ammonium hydroxide is utilized, the surface of the treated tungsten-based wire rod is bright and flat, the roughness is low, no scratch and groove are generated by processing, and the polishing effect is good; and 2-methyl-1-hexene has addition reaction to the gas produced, thus the electrolytic polishing solution of the invention does not produce insoluble gas in the electrolytic polishing process, does not need to be heated and heated, and has fast ion flow speed and fast polishing speed. Meanwhile, the effective components in the electrolytic polishing solution are stable and easy to store.
The electrolytic polishing method disclosed by the invention is simple to operate and high in polishing efficiency, and the electrolytic polishing speed of the electrolytic polishing solution is controlled by the stirring speed without heating, so that the controllability and the environmental friendliness are good. Therefore, the electrolytic polishing solution has reasonable composition and electrolytic polishing technological parameters, and the tungsten-based wire or sheet electrolytically polished by the electrolytic polishing solution and the method has high surface glossiness, good polishing effect and high efficiency.
Drawings
FIG. 1 is a scanning electron microscope (magnification 150) photograph of a tungsten-based wire of the present invention before electropolishing;
FIG. 2 is a SEM photograph (magnification of 200 times) of an electropolished tungsten-based wire of example 1;
FIG. 3 is a scanning electron micrograph (500 times magnification) of a tungsten-based wire rod after electropolishing in accordance with example 1 of the present invention;
FIG. 4 is an atomic force profile (Ra =0.06 μm) of the tungsten-based wire after electropolishing in accordance with example 1 of the present invention;
FIG. 5 is a scanning electron micrograph (500 times magnification) of a tungsten-based wire rod after electropolishing in accordance with example 2 of the present invention;
FIG. 6 is an atomic force topography (Ra =0.08 μm) of the tungsten-based wire after electropolishing in accordance with example 2 of the present invention;
FIG. 7 is a SEM photograph (500 times magnification) of an electropolished tungsten-based wire of example 3;
FIG. 8 is a SEM photograph (500 Xmagnification) of an electropolished tungsten-based wire of example 4 of the present invention;
FIG. 9 is a scanning electron micrograph (magnification 200) of a tungsten-based wire rod after electropolishing comparative example 1;
FIG. 10 is an atomic force topography (Ra =5.2 μm) of a tungsten-based wire of comparative example 1 after electropolishing;
FIG. 11 is a scanning electron micrograph (magnification 200) of a tungsten-based wire rod after electropolishing comparative example 2;
fig. 12 is an atomic force topography (Ra =2.5 μm) of the tungsten-based wire rod of comparative example 2 after electropolishing.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
The embodiment provides an electrolytic polishing solution for tungsten-based wires or sheets and an electrolytic polishing method thereof, wherein the electrolytic polishing solution for tungsten-based wires or sheets is prepared by mixing tetramethylammonium hydroxide quaternary ammonium hydroxide, absolute ethyl alcohol, 2-methyl-1-hexene, sodium sulfate and water, and the concentration of the quaternary ammonium hydroxide, the absolute ethyl alcohol, the 2-methyl-1-hexene and the sodium sulfate in the prepared electrolytic polishing solution is 35g/L, 40g/L, 3g/L and 80g/L.
The surface area of the electrolytic polishing solution used in the present example was about 30mm 2 The electrolytic polishing is carried out on the tungsten-based wire, and the specific process is as follows: placing a tungsten-based wire to be treated in an electrolytic polishing solution as an anode, taking a nickel rod as a cathode, separating a cathode and an anode by 30mm, controlling the stirring speed of the electrolytic polishing solution to be 15r/s, and adjusting the current density of a direct-current stabilized power supply to be 2.5A/cm 2 And performing electrolytic polishing on the surface of the tungsten-based wire, wherein the polishing time of the electrolytic polishing is 100s, cleaning the tungsten-based wire with deionized water after the electrolytic polishing is completed, and blow-drying with cold air to obtain the tungsten-based wire with a bright surface.
The results of observing the tungsten-based wire rods before and after the treatment of example 1 under a scanning electron microscope are shown in fig. 1 to 4, wherein fig. 1 is a scanning electron microscope photograph (magnification of 150 times) of the tungsten-based wire rods before electrolytic polishing, fig. 2 is a scanning electron microscope photograph (magnification of 200 times) of the tungsten-based wire rods after electrolytic polishing, and fig. 3 is a scanning electron microscope photograph (magnification of 500 times) of the tungsten-based wire rods after electrolytic polishing; fig. 4 is an atomic force topography of the tungsten-based wire rod after electropolishing in example 1 of the present invention, with surface roughness Ra =0.06 μm.
As can be seen from FIG. 1, the tungsten-based wire before treatment had rough and uneven surface, and marked scratches and grooves resulted from the treatment. As can be seen from fig. 2 to 4, the tungsten-based wire processed in example 1 has a smooth and bright surface, a low roughness Ra =0.06 μm, and no scratches or grooves generated by machining, so that when the tungsten-based wire is polished by using the electrolytic polishing solution and the method of this example, the surface flatness of the tungsten-based wire can be improved, and the tungsten-based wire has a smooth and bright surface, a low roughness, and no scratches or grooves generated by machining.
Example 2
The embodiment provides an electrolytic polishing solution for tungsten-based wires or sheets and an electrolytic polishing method thereof, wherein the electrolytic polishing solution for tungsten-based wires or sheets is prepared by mixing tetraethylammonium hydroxide quaternary ammonium hydroxide, absolute ethyl alcohol, 2-methyl-1-hexene, sodium sulfate and water, and in the prepared electrolytic polishing solution, the concentration of quaternary ammonium hydroxide is 25g/L, the concentration of absolute ethyl alcohol is 30g/L, the concentration of 2-methyl-1-hexene is 5g/L, and the concentration of sodium sulfate is 75g/L.
The surface area of the electrolytic polishing solution used in the present example was about 30mm 2 The electrolytic polishing is carried out on the tungsten-based wire, and the specific process is as follows: placing a tungsten-based wire to be treated in an electrolytic polishing solution as an anode, taking a nickel rod as a cathode, separating a cathode and an anode by 30mm, controlling the stirring speed of the electrolytic polishing solution to be 10r/s, and adjusting the current density of a direct-current stabilized power supply to be 2.0A/cm 2 And performing electrolytic polishing on the surface of the tungsten-based wire, wherein the polishing time of the electrolytic polishing is 150s, cleaning the tungsten-based wire with deionized water after the electrolytic polishing is completed, and blow-drying with cold air to obtain the tungsten-based wire with a bright surface.
Fig. 5 is a scanning electron microscope photograph (magnification 500 times) of the tungsten-based wire rod after the electrolytic polishing in example 2, and fig. 6 is an atomic force topography map of the tungsten-based wire rod after the electrolytic polishing in example 2, wherein the surface roughness Ra =0.08 μm, so that it can be seen that the tungsten-based wire rod treated in example 2 has a bright and flat surface, a low roughness Ra =0.08 μm, and no scratches and grooves generated by the processing.
Example 3
The embodiment provides an electrolytic polishing solution for tungsten-based wire or sheet and an electrolytic polishing method thereof, the electrolytic polishing solution for tungsten-based wire or sheet is prepared by mixing tetrapropylammonium hydroxide, absolute ethyl alcohol, 2-methyl-1-hexene, sodium sulfate and water, and in the prepared electrolytic polishing solution, the concentration of quaternary ammonium hydroxide is 20g/L, the concentration of absolute ethyl alcohol is 10g/L, the concentration of 2-methyl-1-hexene is 2g/L, and the concentration of sodium sulfate is 100g/L.
Electrolysis using this exampleThe surface area of the polishing solution is about 30mm 2 The electrolytic polishing is carried out on the tungsten-based wire, and the specific process is as follows: placing the tungsten-based wire to be treated in an electrolytic polishing solution as an anode, taking a nickel rod as a cathode, and keeping the distance between the anode and the cathode at 30mm, controlling the stirring speed of the electrolytic polishing solution at 5r/s, and adjusting the current density of a direct-current stabilized power supply to be 1.5A/cm 2 And performing electrolytic polishing on the surface of the tungsten-based wire, wherein the polishing time of the electrolytic polishing is 350s, cleaning the tungsten-based wire with deionized water after the electrolytic polishing is completed, and blow-drying with cold air to obtain the tungsten-based wire with a bright surface.
Fig. 7 is a scanning electron microscope photograph (magnification 500 times) of the tungsten-based wire rod after electropolishing in example 3, from which it can be seen that the tungsten-based wire rod treated in example 3 has a smooth and bright surface, a low roughness Ra =0.10 μm, and no scratches and grooves due to machining, and therefore, when the tungsten-based wire rod is polished by using the electropolishing solution and method of this example, the smoothness of the tungsten-based wire rod surface can be improved, and the tungsten-based wire rod has a smooth and bright surface, a low roughness, and no scratches and grooves due to machining.
Example 4
The embodiment provides an electrolytic polishing solution for tungsten-based wire or sheet and an electrolytic polishing method thereof, the electrolytic polishing solution for tungsten-based wire or sheet is prepared by mixing tetrabutylammonium hydroxide quaternary ammonium hydroxide, absolute ethyl alcohol, 2-methyl-1-hexene, sodium sulfate and water, and the concentration of the quaternary ammonium hydroxide, the absolute ethyl alcohol, the 2-methyl-1-hexene and the sodium sulfate in the prepared electrolytic polishing solution is 40g/L, 50g/L, 1g/L and 50g/L.
The surface area of the electrolytic polishing solution used in the present example was about 30mm 2 The electrolytic polishing is carried out on the tungsten-based wire, and the specific process is as follows: placing the tungsten-based wire to be treated in an electrolytic polishing solution as an anode, taking a nickel rod as a cathode, and keeping the distance between the anode and the cathode at 30mm, controlling the stirring speed of the electrolytic polishing solution at 20r/s, and adjusting the current density of a direct-current stabilized power supply to be 4A/cm 2 Carrying out electrolytic polishing on the surface of the tungsten-based wire, wherein the polishing time of the electrolytic polishing is 60s, cleaning the tungsten-based wire with deionized water after the electrolytic polishing is finished, and drying the tungsten-based wire with cold air to obtain the surfaceA bright tungsten-based wire.
Fig. 8 is a scanning electron micrograph (magnification 500 times) of the tungsten-based wire rod after electropolishing in example 4, from which it can be seen that the tungsten-based wire rod treated in example 3 has a smooth and bright surface, exhibits a low roughness Ra =0.09 μm, and is free of scratches and grooves due to machining, and therefore, when the tungsten-based wire rod is polished by using the electropolishing solution and the method according to this example, the smoothness of the tungsten-based wire rod surface can be improved, and the tungsten-based wire rod has a smooth and bright surface, exhibits a low roughness, and is free of scratches and grooves due to machining.
Comparative example 1
The difference from example 1 is that: the electrolytic polishing solution of the tungsten-based wire or sheet does not contain 2-methyl-1-hexene, namely the electrolytic polishing solution of the tungsten-based wire or sheet is prepared by mixing quaternary ammonium hydroxide, absolute ethyl alcohol, sodium sulfate and water.
The rest is the same as in example 1.
Fig. 9 is a scanning electron microscope photograph (magnification of 200 times) of the tungsten-based wire rod of comparative example 1 after electropolishing, and fig. 10 is an atomic force topography of the tungsten-based wire rod of comparative example 1 after electropolishing, in which the surface roughness Ra =5.2 μm, from which it can be seen that the tungsten-based wire rod after treatment of comparative example 1 has an uneven and rough surface, and has scratches and grooves.
Comparative example 2
The difference from example 1 is that: the electrolytic polishing solution of the tungsten-based wire or sheet does not contain sodium sulfate, namely the electrolytic polishing solution of the tungsten-based wire or sheet is prepared by mixing quaternary ammonium hydroxide, absolute ethyl alcohol, 2-methyl-1-hexene and water.
The rest is the same as in example 1.
Fig. 11 is a scanning electron microscope photograph (magnification of 200 times) of the tungsten-based wire rod of comparative example 2 after electropolishing, and fig. 12 is an atomic force topography of the tungsten-based wire rod of comparative example 1 after electropolishing, in which the surface roughness Ra =2.5 μm, from which it can be seen that the tungsten-based wire rod after treatment of comparative example 2 has an uneven and rough surface, and has scratches and grooves.
Comparing examples 1-5 with comparative example 1 (the electrolytic polishing solution lacks 2-methyl-1-hexene), and comparative example 2 (the electrolytic polishing solution lacks sodium sulfate), it can be seen that the tungsten-based wire rod treated in examples 1-5 has a bright and flat surface, low roughness and no scratches and grooves generated by machining, while the tungsten-based wire rod treated in comparative examples 1-2 has an uneven surface, high roughness and certain scratches and grooves, thus it is shown that the lack of 2-methyl-1-hexene and sodium sulfate in the electrolytic polishing solution directly affects the polishing effect, therefore, the electrolytic polishing solution of the present invention uses the common action of the raw materials such as quaternary ammonium base, absolute ethyl alcohol, 2-methyl-1-hexene, sodium sulfate, etc., so as to make the treated tungsten-based wire rod have a bright and flat surface, low roughness and no scratches and grooves generated by machining, and good polishing effect.
The above are merely characteristic embodiments of the present invention, and do not limit the scope of the present invention in any way. All technical solutions formed by equivalent exchanges or equivalent substitutions fall within the protection scope of the present invention.
Claims (8)
1. An electrolytic polishing solution for tungsten-based wires or sheets is characterized by comprising the following components: quaternary ammonium base, absolute ethyl alcohol, 2-methyl-1-hexene, sodium sulfate and water, wherein the concentration of the quaternary ammonium base in the electrolytic polishing solution is 20-40 g/L, the concentration of the absolute ethyl alcohol is 10-50 g/L, the concentration of the 2-methyl-1-hexene is 1-5 g/L, and the concentration of the sodium sulfate is 50-100 g/L;
the quaternary ammonium hydroxide is one or more of tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide and trimethylethylammonium hydroxide.
2. The electrolytic polishing solution for tungsten-based wires or sheets according to claim 1, wherein the concentration of quaternary ammonium hydroxide is 25 to 35g/L, the concentration of absolute ethyl alcohol is 30 to 40g/L, the concentration of 2-methyl-1-hexene is 2 to 4g/L, and the concentration of sodium sulfate is 70 to 80g/L.
3. The electrolytic polishing solution for tungsten-based wires or sheets according to claim 2, wherein the concentration of quaternary ammonium hydroxide is 35g/L, the concentration of absolute ethyl alcohol is 35g/L, the concentration of 2-methyl-1-hexene is 3g/L, and the concentration of sodium sulfate is 80g/L.
4. The electrolytic polishing solution for tungsten-based wires or sheets according to claim 2, wherein the concentration of quaternary ammonium hydroxide is 25g/L, the concentration of absolute ethyl alcohol is 35g/L, the concentration of 2-methyl-1-hexene is 5g/L, and the concentration of sodium sulfate is 75g/L.
5. A method for electrolytic polishing of tungsten-based wire or sheet by using the electrolytic polishing solution as claimed in any one of claims 1 to 4, characterized in that the tungsten-based wire or sheet to be treated is placed in the electrolytic polishing solution as an anode, nickel is used as a cathode, the current density of a DC stabilized power supply is adjusted to 1.0-4.0A/cm 2, the stirring speed of the electrolytic polishing solution is controlled to 5-40 r/s, and the electrolytic polishing is carried out on the surface of the tungsten-based wire or sheet.
6. The method of electropolishing tungsten-based wire or sheet according to claim 5, wherein the electropolishing time is not less than 30 seconds.
7. The method of electropolishing a tungsten-based wire or sheet according to claim 5, wherein the current density is 2.0-3.0A/cm 2.
8. The method for electropolishing tungsten-based wires or sheets according to claim 5, wherein the electropolishing solution stirring speed is 10-20 r/s.
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