WO2012073501A1 - Electrolytic solution, electrolysis case, electropolishing system, and electropolishing method using these - Google Patents
Electrolytic solution, electrolysis case, electropolishing system, and electropolishing method using these Download PDFInfo
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- WO2012073501A1 WO2012073501A1 PCT/JP2011/006691 JP2011006691W WO2012073501A1 WO 2012073501 A1 WO2012073501 A1 WO 2012073501A1 JP 2011006691 W JP2011006691 W JP 2011006691W WO 2012073501 A1 WO2012073501 A1 WO 2012073501A1
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- electrolytic
- electrolytic solution
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F7/00—Constructional parts, or assemblies thereof, of cells for electrolytic removal of material from objects; Servicing or operating
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
Definitions
- the present invention relates to electropolishing, and particularly relates to an electrolytic solution, an electrolysis case, an electropolishing system, and an electropolishing method used for electropolishing.
- Electrolytic polishing is often used as a method for removing metal rust and dirt.
- the metal (workpiece) and the cathode are immersed in an electrolyte solution at a predetermined distance, and a positive current is applied to the metal and a negative current is applied to the cathode to flow a predetermined current, so that the metal element on the workpiece surface is dissolved and the surface is modified.
- a pre-process of this treatment it is usual to perform buffing and mechanical polishing.
- the metal workpiece is made of stainless steel
- phosphoric acid or phosphoric acid and sulfuric acid are usually used as the electrolyte, and the distance between the electrodes is about 10 cm, and the current is 10 A to 20 A.
- This buffing is a harsh work because workers are forced to enter directly into a can in a hot and humid environment. In addition to that, buffing alone destroys the surface structure and tends to cause rusting and deterioration, so that an electrolytic polishing treatment is being tried after this buffing.
- JP 2010-209423 a frame and an electrode are assembled along the inner surface of the can body, and the inner surface of the can body is electrolytically polished with a small amount of electrolyte.
- JP 2010-209423 Even if the method disclosed in JP 2010-209423 is used, until the frame and the electrode are assembled, the operator needs to act inside the can body, even if it is not as much as the buffing work, The work is not comfortable. Further, the method of holding the electrolytic solution in the felt or the like increases the resistance between the electrodes, and a large current cannot flow. Therefore, the working time becomes long, and it is impossible to use this method for large-scale electrolytic polishing, in particular, electrolytic polishing of the inner surface of the can body as the main purpose of the present application even in consideration of the working environment.
- the present invention has been proposed in view of the above-described conventional circumstances, and there is no need to assemble a frame or an electrode, and an electropolishing method and an electrolysis used therefor that make it extremely easy for an operator to work inside the can.
- An object is to provide a liquid, an electrolytic case, and an electrolytic polishing system.
- the electrolytic solution used in the present invention is made to have a predetermined viscosity by bringing a gelling agent into contact with an inorganic acid which is an electrolytic solution usually used for electrolytic polishing.
- the inorganic acid used as the electrolytic solution for electropolishing is usually a phosphoric acid aqueous solution or a mixed aqueous solution of phosphoric acid and sulfuric acid, and this point is not different from conventional ones.
- Silicon gel is used as the gelling agent. Silicon dioxide in contact with the inorganic acid dissolves in a gel state and gives viscosity to the electrolytic solution. This viscosity can be adjusted by changing the amount of silicon dioxide added.
- This electrolytic solution is introduced into the following electrolytic case, the introduction is continued, and the previously introduced electrolytic solution is discharged so that the electrolytic polishing proceeds.
- a cathode having a predetermined size and a predetermined depth is provided with a cathode at a predetermined height from the lower opening end, and an electrolytic solution having a predetermined viscosity is introduced above the cathode. And an outlet for discharging the electrolytic solution introduced into the annular frame from the electrolytic case frame.
- the introduction port When a net is used as the cathode, the introduction port includes a pipe disposed along the net having a large number of small holes with respect to the net of the net, and the electrolyte is supplied to the pipe. It can be. Further, it is possible to adopt a configuration using a mesh as the discharge port. Furthermore, it is good also as a structure filled with the holding material which hold
- an electrolytic case having this configuration, an electrolytic solution storage tank storing the electrolytic solution, a pump for pumping out the electrolytic solution from the electrolytic solution storage tank at a predetermined discharge amount, and the pumped electrolytic solution
- the flow rate is adjusted to a predetermined flow rate per unit volume of the electrolysis case, and a negative voltage is applied to the flow rate adjustment valve for flowing the electrolytic solution to the introduction port, the cathode of the electrolysis case, and the positive voltage to the work
- the electropolishing system may be configured in combination with a DC power source that applies each of.
- the electrolyte solution is always transferred to the electrolytic case at a predetermined flow rate per unit volume of the electrolytic case, so that the electrolyte solution is always fresh between the cathode of the electrolytic case and the workpiece. Therefore, the workpiece can be subjected to high-quality electropolishing with few defects.
- the open end under the annular frame of the electrolytic case having this configuration is placed facing the workpiece surface, and an electrolytic solution having a predetermined viscosity is introduced between the workpiece and the cathode of the annular frame through the small hole, so When a predetermined negative voltage is applied to the cathode side to allow a predetermined current to flow, electropolishing proceeds. At this time, since oxygen is generated on the workpiece side, the previously introduced electrolytic solution is discharged from the discharge port while continuing to introduce the electrolytic solution from the introduction port. As a result, the generated oxygen is expelled and does not hinder the electropolishing operation.
- electrolytic solution is introduced between the workpiece and the cathode at a predetermined flow rate per unit volume between the workpiece and the cathode, high-quality electrolytic polishing can be performed as described above. It can be realized.
- the electrolytic solution having viscosity can be easily held, and the cathode of the electrolytic case has a small distance from the opening end where the workpiece surface is located (for example, 5 to 20 mm). )can do.
- the resistance of the electrolytic solution can be kept low, so that a large current (for example, 30 to 100 A / dm 2 ) can flow, and the working time can be shortened.
- electrolyte Since the electrolyte is viscous, when current is passed, bubbles (oxygen generated from the anode (work)) accumulate in the electrolyte, but the electrolyte is introduced into the annular frame through the inlet and discharged. The air bubbles can be expelled from the outlet. As a result, the work of the worker who has entered the can is only to move the electrolytic case, and the amount of work is extremely reduced. Furthermore, by moving the electrolytic case along the workpiece by automatic control in a state where the electrolytic case is in contact with the workpiece surface, electropolishing inside the can can can be performed even without an operator.
- an electrolytic polishing system that constantly supplies a predetermined amount of electrolytic solution to the electrolytic case, it is possible to realize high-quality electrolytic polishing for the workpiece.
- FIG. 1 is a perspective view of the electrolytic case used in the present invention as viewed from above.
- FIG. 2 is a perspective view of the electrolytic case used in the present invention as viewed from below.
- 3 is a cross-sectional view taken along the line AA in FIG.
- FIG. 4 is a surface photograph of the samples (a) to (b) of Example 1 using an electron microscope.
- FIG. 5 is a surface photograph of the samples (d) to (f) of Example 1 using an electron microscope.
- FIG. 6 is a conceptual diagram of the electropolishing system of the present invention.
- the electrolytic solution used in the present invention is made to have a predetermined viscosity by bringing a gelling agent into contact with an inorganic acid which is a normal polishing electrolytic solution.
- the inorganic acid is usually a phosphoric acid aqueous solution or a mixed aqueous solution of phosphoric acid and sulfuric acid, and silicon dioxide is used as a gelling agent. Silicon dioxide in contact with the inorganic acid dissolves in a gel state and gives viscosity to the electrolytic solution. This viscosity can be adjusted by changing the amount of silicon dioxide added.
- the polishing function does not work sufficiently when the amount of phosphoric acid is 500 mL / L or less. Even with the total amount of phosphoric acid, the object of the present application can be achieved, but there is no room for adding sulfuric acid to be described later, and the gloss is not high.
- sulfuric acid for example, concentration 98%) at 0 mL / L to 500 mL / L.
- Sulfuric acid has a function to give gloss to the finished surface, and is added when gloss is required.
- the sulfuric acid is 500 mL / L or more, the amount of phosphoric acid is reduced, and the polishing function is not sufficient.
- a surfactant is added for the purpose of ensuring the wettability of the above-mentioned viscous electrolytic solution to the workpiece.
- the surfactant is 0.001% or less, the wettability is insufficient, and even when it is 0.01% or more, the wettability returns and falls.
- FIGS. 1 is a perspective view seen from the upper side of the electrolytic case
- FIG. 2 is a perspective view seen from the lower side
- FIG. 3 is a cross-sectional view taken along the line AA in FIG.
- the cathode 12 is disposed at a predetermined height position from the lower opening end 11o of the annular frame 11 surrounding the periphery, and the introduction port 13 for introducing the electrolyte solution having the predetermined viscosity above the cathode 12;
- the discharge port 14 for discharging the electrolytic solution introduced into the annular frame 11 from the annular frame 11 is provided.
- an introduction pipe 13p having a large number of small holes 13h open to the mesh of the mesh body is disposed along the mesh body, and the viscous pipe is electrolyzed with respect to the introduction pipe 13p.
- the introduction port 13 can be configured by erecting a guide pipe 13g for guiding the liquid, and the mesh of the mesh body 12 can be used as the discharge port 14e.
- the lead 16 of the cathode 12 is provided.
- the shape and size of the annular frame 11 are not particularly limited, but in the following embodiments, the shape and size are such that they can be freely moved on the workpiece surface by hand. is there. This point can be appropriately changed according to the application scene.
- the annular frame 11 having a relatively small strength is a support pair of the cathode, the distance between the open end 11o (work surface) under the annular frame 11 and the cathode is extremely small, for example, 5 mm to 20 mm. As a result, a large current (for example, 30 to 100 A / dm 2 ) can be obtained, and the electrolytic treatment time can be significantly shortened.
- the annular frame 11 may be filled with an artificial turf-shaped holding material 15 so that the electrolytic solution can be easily held.
- an artificial turf-shaped holding material 15 so that the electrolytic solution can be easily held.
- FIG. 2 some of the turf leaves of the holding material 5 are drawn and the others are omitted.
- the open end 11o under the annular frame 11 of the electrolytic case 10 having this configuration is placed toward the surface of the workpiece W (see FIG. 3), and an electrolyte solution having a predetermined viscosity is supplied from the inlet 13 to the workpiece W and the cathode of the annular frame 11.
- electrolytic polishing on the workpiece W proceeds.
- the electrolytic solution since the electrolytic solution has a viscosity, the electrolytic solution is held by the annular frame 11 and the holding material 15 and does not flow out of the electrolytic case 10 rapidly. The function of the liquid will be maintained. Further, since the distance between the workpiece W and the cathode 12 is small, the electric resistance is small, and a large current can be passed, so that polishing at a high speed is possible.
- the place on the workpiece of the electrolytic case is sequentially moved, and the entire workpiece or a predetermined portion of the workpiece W is subjected to the electrolytic treatment.
- Example 1 ⁇ Electrolyte> First, the following electrolytic solution was prepared. (1) Electrolytic solutions for comparative examples (b), (c), (f) (hereinafter referred to as normal solutions) 85% -phosphoric acid 750 ml / L 98% -Sulfuric acid 250ml / L (2) Electrolytic solution of the present invention (hereinafter referred to as high viscosity liquid) 85% -phosphoric acid 750 ml / L 98% -Sulfuric acid 250ml / L SiO2 / XH2O 200g / L ⁇ Electrolytic polishing> The following polishing treatment was performed on a SUS316L (30 ⁇ 30 ⁇ 3) mm test piece.
- the coating type electrolytic polishing of (b) and (c) below is a method in which an electrolytic solution is soaked in a felt or chemical resistant cloth, and current is passed between the workpiece and the cathode with the felt (cloth) sandwiched between them. It is. Further, the following (d) and (e) are the systems of the present application using an electrolysis case (distance 10 mm between the workpiece and the cathode).
- Ry is the sum of the maximum peak height and maximum valley depth in the measured range.
- Rz is the sum of the average value of the maximum mountain height and the fifth highest mountain height and the average value of the maximum valley depth and the fifth highest valley depth.
- Table 1 shows the measurement results of the surface roughness.
- austenite is generated on the surface as in the test piece (f), and surface modification occurs. It can be understood that this makes it possible to perform electropolishing with higher durability.
- Example 2 ⁇ Electrolyte> Both the normal solution and the high viscosity solution are the same as the electrolyte solutions (1) and (2) shown in Example 1.
- Example 1 Compared with Example 1, the voltage at the test pieces (d) and (e) of the present invention was increased. As a result, the current also increases, but conversely, it is evaluated that the current can flow up to here. In (d) and (e), the current has a width of 50 to 70 A / dm 2 . It is the current fluctuation when moving the electrolytic case.
- the surface roughness of the test pieces (d) and (e) of the present invention is markedly improved from that of Example 1 (e) (processing time 2 minutes).
- Example 1 processing time 2 minutes
- it is excellent in gloss on appearance and shows the superiority of the present invention.
- austenite is generated on the surface as in the test piece (f)
- surface modification occurs, and electropolishing with high durability can be performed.
- FIG. 6 is a conceptual diagram showing an electrolysis system to which the electrolysis case is applied.
- the electrolytic solution L stored in the electrolytic solution storage tank 3 is pumped by the pump 4 to the inlet 13 of the electrolytic case 2 through the flow rate adjusting valve 5. Further, a negative voltage from a DC power source 6 is applied to the cathode 12 of the electrolytic case 2 via a lead 16, and a positive voltage from the DC power source 6 is applied to the work W, respectively. It has become.
- the electrolytic solution storage tank 3 stores the electrolytic solution L having a predetermined viscosity described above.
- the pump 4 is configured to pump out the electrolytic solution L from the electrolytic solution storage tank 3 with a predetermined discharge amount.
- the pump 4 since the electrolytic solution L is strongly acidic and highly viscous, the pump 4 has excellent chemical resistance and a high discharge amount (high head) corresponding to the electrolytic solution L.
- a synthetic resin diaphragm pump is used.
- the maximum discharge amount is 50 L / min or more, or the maximum self-priming lift is 2.0 m or more.
- the diaphragm pump 4 having a maximum discharge amount of 54.5 L / min and a maximum self-priming lift of 2.4 m is applied.
- the flow rate adjusting valve 5 is provided between the pump 4 and the electrolytic case 2, and the flow rate of the electrolytic solution L pumped from the pump 4 is set to a volume (1000 cm 3 ) of the electrolytic case 2.
- the electrolytic solution L is adjusted to a predetermined flow rate per unit volume (1 cm 3 ) of the electrolytic case 2 and the electrolytic solution L flows through the inlet 13.
- the electrolyte solution L is always transferred to the electrolytic case 2 at a predetermined flow rate per unit volume of the electrolytic case 2, so that the space between the cathode 12 of the electrolytic case 2 and the workpiece W is increased. Therefore, it is possible to always supply fresh electrolytic solution L, and it is possible to subject the workpiece W to high-quality electrolytic polishing with few defects.
- the predetermined flow rate per unit volume of the electrolytic case 2 corresponds to the predetermined flow rate per unit volume between the workpiece W and the cathode 12 in other words.
- the predetermined flow rate of the electrolytic solution L per unit volume of the electrolytic case 2 is determined by the flow rate adjusting valve 5 when, for example, the dimensions of the electrolytic case 2 are 20 cm long, 10 cm wide, and 5 cm high. Since the volume of the electrolysis case 2 is 1000 cm 3 , the flow rate is in the range of 20 to 100 mL / min per unit volume (1000 cm 3 ) of the electrolysis case 2 and per unit volume (1 cm 3 ) of the electrolysis case 2. A range of 0.020 to 0.100 mL / min is preferable.
- the DC power supply 6 is configured to apply a negative voltage to the cathode 12 of the electrolytic case 2 via the lead 16 and a positive voltage to the work W, respectively.
- the voltage to be applied is a large value within the range of 11V to 20V, for example, as described above. If the distance between the cathode 12 and the workpiece W in the electrolytic case 2 is 5 mm to 20 mm, the current flowing between the two can be set to 30 to 100 A / dm 2 as described above. Become.
- the electrolytic case 2 the electrolytic solution storage tank 3, the pump 4, the flow rate adjustment valve 5, and the direct current power source 6 are assembled to the electrolytic case 2. Since the electrolytic solution L is constantly supplied at a predetermined flow rate per unit volume of the electrolytic case 2, fresh electrolysis is always performed between the cathode 12 of the electrolytic case 2 and the workpiece W. The liquid L flows and the workpiece W can be subjected to high-quality electrolytic polishing.
- an operator can freely move the cathode 12 (bottom surface) of the electrolysis case 2 onto the surface of the workpiece W by holding the electrolysis case 2 by hand ( Scanning), the workpiece W is subjected to electrolytic polishing.
- the electrolytic polishing is performed by allowing the electrolytic case 2 to stand on the surface of the workpiece W for a predetermined processing time.
- the reciprocal of this processing time corresponds to, for example, a scanning speed for moving (scanning) the electrolytic case 2 to the workpiece W.
- the processing time is not particularly limited.
- the processing time is within the range of 5 min / m 2 to 15 min / m 2 , specifically 10 min / m 2 , the workpiece W is substantially immersed in the electrolytic polishing. A similar gloss can be obtained, which is preferable.
- the processing time can be appropriately changed in design according to the shape of the workpiece W, the current density of the current by the DC power supply 6, and the purpose of the electrolytic polishing process.
- the purpose of the electrolytic polishing treatment is to degrease or slightly dissolve the surface of the workpiece W (dissolve several ⁇ m in thickness relative to the surface of the workpiece W)
- the treatment time is within the above range.
- the purpose of the electrolytic polishing treatment is large-scale dissolution equivalent to immersion electrolytic polishing (dissolution of several tens of ⁇ m on the surface of the workpiece W)
- the processing time Can be within the above range or more.
- the present invention can perform electropolishing with a large current, the working time is shortened, and a small amount of electrolytic solution can be easily held, so that the electrolytic treatment becomes extremely simple.
- the present invention can realize high-quality electrolytic polishing, the industrial applicability is extremely large.
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Abstract
Description
<電解液>
まず、以下の電解液を用意した。
(1)比較例用(b)、(c)、(f)の電解液(以下通常液という)
85%-燐酸 750ml/L
98%-硫酸 250ml/L
(2)本発明の電解液(以下高粘液という)
85%-燐酸 750ml/L
98%-硫酸 250ml/L
SiO2・XH2O 200g/L
<電解研磨>
SUS316L(30×30×3)mmの試験片に対して以下の研磨処理をした。下記(b)、(c)の塗布式電解研磨とは、フェルト、あるいは耐薬品性の布に電解液を滲みこませ、当該フェルト(布)を挟んで、ワークとカソード間に電流を流す方式である。また、下記(d)、(e)が、電解ケース(ワークとカソード間の距離10mm)を用いた本願の方式である。 Example 1
<Electrolyte>
First, the following electrolytic solution was prepared.
(1) Electrolytic solutions for comparative examples (b), (c), (f) (hereinafter referred to as normal solutions)
85% -phosphoric acid 750 ml / L
98% -Sulfuric acid 250ml / L
(2) Electrolytic solution of the present invention (hereinafter referred to as high viscosity liquid)
85% -phosphoric acid 750 ml / L
98% -Sulfuric acid 250ml / L
SiO2 / XH2O 200g / L
<Electrolytic polishing>
The following polishing treatment was performed on a SUS316L (30 × 30 × 3) mm test piece. The coating type electrolytic polishing of (b) and (c) below is a method in which an electrolytic solution is soaked in a felt or chemical resistant cloth, and current is passed between the workpiece and the cathode with the felt (cloth) sandwiched between them. It is. Further, the following (d) and (e) are the systems of the present application using an electrolysis case (distance 10 mm between the workpiece and the cathode).
(b) 通常液(上記電解液(1))による塗布式電解研磨(1分)
電圧11V、電流0.1A/dm2
(c) 通常液(上記電解液(1))による塗布式電解研磨(2分)
電圧11V、電流0.1A/dm2
(d) 高粘液(上記電解液(2))による塗布式電解研磨(1分)
電圧11V、電流35A/dm2
(e) 高粘液(上記電解液(2))による塗布式電解研磨(2分)
電圧11V、電流35A/dm2
(f) 通常液による浸漬電解研磨(5分)
電圧11V、電流10A/dm2
上記(b)から(e)は液循環実施
<性能評価方法>
(1) 表面粗さの測定
ミツトヨ製SJ-301による5点粗さ測定
ここで粗さパラメータRaは測定した範囲の平均粗さ。Ryは測定した範囲の最大山高さと最大谷深さの和。Rzは最大山高さと五番目までの山高さの平均値と最大谷深さと五番目までの谷深さの平均値の和。
(2)表面観察
日本電子製操作顕微鏡JCM-5700による。 (A) Buffing only (b) Application type electrolytic polishing (1 minute) with normal solution (the above electrolyte (1))
Voltage 11V, current 0.1A / dm 2
(C) Application type electropolishing (2 minutes) with normal solution (the above electrolyte (1))
Voltage 11V, current 0.1A / dm 2
(D) Application type electropolishing with high viscosity liquid (the above electrolytic solution (2)) (1 minute)
Voltage 11V, current 35A / dm 2
(E) Application type electropolishing with high viscosity liquid (the above electrolytic solution (2)) (2 minutes)
Voltage 11V, current 35A / dm 2
(F) Immersion electropolishing with normal solution (5 minutes)
Voltage 11V, current 10A / dm 2
Above (b) to (e) are liquid circulation <Performance evaluation method>
(1) Measurement of surface roughness Five-point roughness measurement with Mitutoyo SJ-301 The roughness parameter Ra is the average roughness of the measured range. Ry is the sum of the maximum peak height and maximum valley depth in the measured range. Rz is the sum of the average value of the maximum mountain height and the fifth highest mountain height and the average value of the maximum valley depth and the fifth highest valley depth.
(2) Surface observation According to JEOL operation microscope JCM-5700.
(1)上記表面粗さの測定結果を表1に示す。 <Result>
(1) Table 1 shows the measurement results of the surface roughness.
図4に示す写真(b)、(c)(上記試験片(b)、(c)に対応)ではバフ研磨のみによる試験片(a)に見られる横の筋が消えていないが、図5に示す、本願発明に対応の試験片(d)、(e)、特に(e)に対応する写真ではそれが消え、写真(f)(浸漬品)に近くなっている。 <Evaluation>
In the photographs (b) and (c) shown in FIG. 4 (corresponding to the above test pieces (b) and (c)), the horizontal streak seen in the test piece (a) by buffing alone is not erased. The test pieces (d) and (e) corresponding to the present invention shown in (2), particularly, the photo corresponding to (e) disappears, and is close to the photo (f) (immersion product).
<電解液>
前記、通常液、高粘液とも実施例1に示す電解液(1)(2)に同じ。 (Example 2)
<Electrolyte>
Both the normal solution and the high viscosity solution are the same as the electrolyte solutions (1) and (2) shown in Example 1.
実施例1と略同じであるが、本願発明に対応する下記(c)、(d)の電圧を大きくしている。従って、当然電流も大きくなっている。また、(c)、(e)では処理時間を3分としている。 <Electrolytic polishing>
Although it is substantially the same as Example 1, the voltage of following (c) and (d) corresponding to this invention is enlarged. Accordingly, the current is naturally increased. In (c) and (e), the processing time is 3 minutes.
(b) 通常液(上記電解液(1))による塗布式電解研磨(1分)
電圧11V、電流0.1A/dm2
(c) 通常液(上記電解液(1))による塗布式電解研磨(3分)
電圧11V、電流0.1A/dm2
(d) 高粘液(上記電解液(2))による塗布式電解研磨(1分)
電圧20V、電流50~70A/dm2
(e) 高粘液(上記電解液(2))による塗布式電解研磨(3分)
電圧20V、電流50~70A/dm2
(f) 通常液による浸漬電解研磨(5分)
電圧11V、電流10A/dm2
上記(b)から(e)は液循環実施
<性能評価方法>
実施例1に同じ、但し、外観評価は目視
<結果>
表2に表面粗さの結果を示し、表3に目視での外観評価の結果を示す。 (A) Buffing only (b) Application type electrolytic polishing (1 minute) with normal solution (the above electrolyte (1))
Voltage 11V, current 0.1A / dm 2
(C) Application type electropolishing (3 minutes) with normal solution (the above electrolyte (1))
Voltage 11V, current 0.1A / dm 2
(D) Application type electropolishing with high viscosity liquid (the above electrolytic solution (2)) (1 minute)
Voltage 20V, current 50-70A / dm 2
(E) Application type electropolishing with high viscosity liquid (the above electrolytic solution (2)) (3 minutes)
Voltage 20V, current 50-70A / dm 2
(F) Immersion electropolishing with normal solution (5 minutes)
Voltage 11V, current 10A / dm 2
Above (b) to (e) are liquid circulation <performance evaluation method>
Same as Example 1, except that the appearance evaluation is visual <result>
Table 2 shows the results of surface roughness, and Table 3 shows the results of visual appearance evaluation.
実施例1と比して、本願発明の試験片(d)、(e)での電圧を大きくした。その結果、電流も大きくなっているが、逆に、電流をここまで流せるという評価となる。(d)、(e)において、電流が50~70A/dm2と幅を持っている。電解ケースを移動するときの電流変動である。 <Evaluation>
Compared with Example 1, the voltage at the test pieces (d) and (e) of the present invention was increased. As a result, the current also increases, but conversely, it is evaluated that the current can flow up to here. In (d) and (e), the current has a width of 50 to 70 A / dm 2 . It is the current fluctuation when moving the electrolytic case.
図6は、前記電解ケースを適用した電解システムを示す概念図である。 <Electrolytic polishing system>
FIG. 6 is a conceptual diagram showing an electrolysis system to which the electrolysis case is applied.
12 カソード
13 導入口
14 排出口
15 保持材
Claims (10)
- 無機酸にゲル化剤を接触させて、所定の粘度を持たせた、電解液。 An electrolytic solution in which a gelling agent is brought into contact with an inorganic acid to have a predetermined viscosity.
- 上記無機酸が、リン酸水溶液または、リン酸と硫酸の混合水溶液であり、ゲル化剤が二酸化珪素である請求項1に記載の電解液。 The electrolytic solution according to claim 1, wherein the inorganic acid is a phosphoric acid aqueous solution or a mixed aqueous solution of phosphoric acid and sulfuric acid, and the gelling agent is silicon dioxide.
- 85%リン酸500mL/L~1000mL/L
98%硫酸0mL~500mL/L
水0mL~500mL/L
二酸化珪素100g/L~200g/L
を含む請求項2に記載の電解液。 85% phosphoric acid 500mL / L to 1000mL / L
98% sulfuric acid 0mL ~ 500mL / L
Water 0mL-500mL / L
Silicon dioxide 100g / L ~ 200g / L
The electrolytic solution according to claim 2, comprising: - 更に、界面活性剤0.001%~0.01%を含む請求項3に記載の電解液。 The electrolytic solution according to claim 3, further comprising 0.001% to 0.01% of a surfactant.
- 環状枠と、
上記環状枠の下の開口端から所定の高さの位置に配設したカソードと、
上記開口端の位置のワークとカソードの間に所定粘度の電解液を導入する導入口と、
上記環状枠内に導入された電解液を環状枠から排出する排出口と、
を備えたことを特徴とする電解ケース。 An annular frame;
A cathode disposed at a predetermined height from the opening end under the annular frame;
An inlet for introducing an electrolyte of a predetermined viscosity between the work at the position of the opening end and the cathode;
A discharge port for discharging the electrolyte introduced into the annular frame from the annular frame;
Electrolytic case characterized by comprising. - 上記カソードを網体とし、当該網体の網目に対応して小穴を備えた導入パイプを、網体上に沿って配設し、当該導入パイプを介して所定粘度の電解液を、前記開口端に位置するワークとカソードの間に導入する構成とした導入口を備え、上記排出口として網目を利用した、請求項5に記載の電解ケース。 An introduction pipe having a small hole corresponding to the mesh of the mesh body is provided along the mesh body, and an electrolyte solution having a predetermined viscosity is passed through the introduction pipe. The electrolysis case according to claim 5, further comprising an introduction port configured to be introduced between the workpiece positioned at the cathode and the cathode, and using a mesh as the discharge port.
- 前記環状枠の下の開口端とカソードとで構成される空間に前記所定粘度の電解液を保持する保持材を充填した請求項6に記載の電解ケース。 The electrolytic case according to claim 6, wherein a holding material for holding the electrolytic solution having the predetermined viscosity is filled in a space formed by the open end under the annular frame and the cathode.
- 請求項5~7のいずれか一項に記載の電解ケースと、
前記電解液を貯留した電解液貯留槽と、
前記電解液貯留槽から、前記電解液を所定の吐出量で汲み出すポンプと、
前記汲み出された電解液の流量を、前記電解ケースの単位体積当たりの所定の流量に調整して、当該電解液を前記導入口に流す流量調整弁と、
前記電解ケースのカソードに負の電圧を、前記ワークに正の電圧をそれぞれ印加する直流電源と
を備えた電解研磨システム。 Electrolytic case according to any one of claims 5 to 7,
An electrolytic solution storage tank storing the electrolytic solution;
A pump for pumping out the electrolytic solution from the electrolytic solution storage tank at a predetermined discharge amount;
A flow rate adjusting valve for adjusting the flow rate of the pumped electrolyte solution to a predetermined flow rate per unit volume of the electrolytic case, and flowing the electrolyte solution to the inlet;
An electropolishing system comprising: a DC power source that applies a negative voltage to the cathode of the electrolytic case and a positive voltage to the workpiece. - 環状枠の下の開口端から所定高さの位置にカソードを配置した電解ケースの上記環状枠の下端を、ワーク表面に向けて置き、
所定粘度の電解液を前記ワークとカソードの間に継続して導入し、先に導入された電解液を排出しつつ、
ワーク側に正、カソード側に負の所定電圧を印加して所定電流を流すとともに、
上記環状枠のワーク上の位置を移動させて、ワーク上の目的の領域を電解研磨する
電解研磨方法。 Place the lower end of the annular frame of the electrolytic case in which the cathode is disposed at a predetermined height from the opening end under the annular frame toward the work surface,
While continuously introducing an electrolytic solution of a predetermined viscosity between the workpiece and the cathode, while discharging the previously introduced electrolytic solution,
While applying a positive predetermined voltage on the work side and negative predetermined voltage on the cathode side,
An electropolishing method in which a position of the annular frame on the work is moved to electropolish a target region on the work. - 前記電解液を、前記ワークとカソードの間の単位体積当たりの所定の流量で、当該ワークとカソードとの間に導入する
請求項9に記載の電解研磨方法。 The electrolytic polishing method according to claim 9, wherein the electrolytic solution is introduced between the workpiece and the cathode at a predetermined flow rate per unit volume between the workpiece and the cathode.
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JP2012546699A JP5889799B2 (en) | 2010-12-01 | 2011-11-30 | Electrolytic case |
US13/991,203 US20130319878A1 (en) | 2010-12-01 | 2011-11-30 | Electrolytic solution, electrolysis case, electropolishing system, and electropolishing method using these |
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