CN114214702B - Etching method and etching device for alloy plate with slotted hole - Google Patents

Etching method and etching device for alloy plate with slotted hole Download PDF

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Publication number
CN114214702B
CN114214702B CN202111566508.4A CN202111566508A CN114214702B CN 114214702 B CN114214702 B CN 114214702B CN 202111566508 A CN202111566508 A CN 202111566508A CN 114214702 B CN114214702 B CN 114214702B
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alloy plate
electrolyte
conduit
etching apparatus
etching
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CN114214702A (en
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马磊
王路
张果
赖建昌
阳高
许兵
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Hongfujin Precision Electronics Chengdu Co Ltd
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Hongfujin Precision Electronics Chengdu Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/26Anodisation of refractory metals or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00Electrolytic etching or polishing
    • C25F3/02Etching
    • C25F3/08Etching of refractory metals
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • ing And Chemical Polishing (AREA)
  • Fuel Cell (AREA)

Abstract

The application provides an etching method and an etching device for an alloy plate with a slotted hole. The etching method comprises the following steps: an alloy plate is provided, the alloy plate having slots. Providing an electrolyte, and inserting a cathode into the electrolyte. And taking the alloy plate as an anode, and controlling the electrolyte to flow through the slotted hole. And electrifying between the cathode and the anode to enable the inner wall of the slotted hole to form an oxidation layer after anodic oxidation. By adopting the etching method, a uniform oxide layer can be formed on the inner wall of the slot hole, and the universality is strong.

Description

Etching method and etching device for alloy plate with slotted hole
Technical Field
The present disclosure relates to the field of metal alloy cationization, and more particularly, to an etching method and an etching apparatus for an alloy plate having a slot.
Background
In the existing electronic product housing, in order to realize the transmission of electronic signals of the electronic product, an injection molding piece is required to be arranged on a metal shell. In the existing process of combining the titanium alloy and the injection molding, in order to improve the combining capability of the injection molding in the titanium alloy slot hole, the hole wall of the titanium alloy needs to be treated. The existing treatment mode mainly comprises the steps of forming an oxide film on the hole wall of the titanium alloy through a low-voltage anodic oxidation process, wherein the titanium alloy can form a closed loop in a slot hole, and a uniform oxide film cannot be formed on the inner wall of the slot hole, so that a titanium alloy workpiece cannot be stably connected with an injection molding piece.
Disclosure of Invention
In view of the above, the present application provides an etching method and an etching apparatus for an alloy plate with slots, which are used for solving the above problems.
The application provides an etching method of an alloy plate with a slot hole, which comprises the following steps: an alloy plate is provided, the alloy plate having slots. Providing an electrolyte, and inserting a cathode into the electrolyte. And taking the alloy plate as an anode, and controlling the electrolyte to flow through the slotted hole. And electrifying between the cathode and the anode to enable the inner wall of the slotted hole to form an oxidation layer after anodic oxidation.
In some possible implementations, the energizing voltage is 30-40V and the current density is 0.8-1.5A/dm 2
In some possible implementations, the flow rate of the electrolyte through the slots is 150-180mL/s.
In some possible implementations, the electrolyte includes 50% -70% glacial acetic acid and 5% -15% chloride salt including one of sodium chloride or potassium chloride, by volume fraction.
In some possible implementations, the electrolyte further includes 15% -20% propylene glycol and 1% -3% aluminum sulfate by volume fraction.
The application also provides an etching device for executing the etching method of the alloy plate with the slotted hole, wherein the etching device comprises a fixing component and a liquid pump. The fixing component is used for fixing the alloy plate. The liquid pump is used for communicating the electrolyte, and the liquid pump is used for controlling the electrolyte to flow through the slotted hole.
In some possible implementations, the fixing assembly includes a first fixing block and a second fixing block disposed opposite to each other, a receiving cavity for mounting the alloy plate is formed between the first fixing block and the second fixing block, the first fixing block has a first through hole, and the second fixing block has a second through hole, and the first through hole and the second through hole are used for communicating with the slot and allowing the electrolyte to pass through.
In some possible implementations, the fixing assembly further includes a first seal ring and a second seal ring, the first fixing block has a first surface facing the second fixing block, the first surface is partially concave to form a first accommodating groove, and the first seal ring is accommodated in the first accommodating groove;
the second fixed block is provided with a second surface facing the first fixed block, a second accommodating groove is formed in the second surface in a partially concave mode, the second sealing ring is accommodated in the second accommodating groove, and the first sealing ring and the second sealing ring are oppositely arranged to seal the joint of the first fixed block, the second fixed block and the alloy plate.
In some possible implementations, the central axes of the first and second perforations are parallel and non-collinear.
In some possible implementations, the etching apparatus further includes an electrolytic cell for containing the electrolyte, and the alloy plate is located outside the electrolytic cell.
In some possible implementations, the electrolytic cell includes a sealed cavity.
In some possible implementations, the etching device further includes a first conduit and a second conduit, the first conduit and the second conduit are communicated with the electrolytic tank and are respectively communicated with two ends of the slot, the liquid pump is communicated with the first conduit, and the electrolyte forms a continuously closed loop through the first conduit, the second conduit and the electrolytic tank.
Compared with the prior art, the method has the advantages that the inner walls of the slots in the alloy plate can be etched only by completely immersing the alloy plate in the electrolyte for anodic oxidation, so that the inner walls of the slots are uniformly oxidized to form a uniform oxide layer, other positions of the alloy plate are protected from being etched, the appearance is not affected, and the universality is strong; meanwhile, the aging frequency of the electrolytic tank for containing the electrolyte can be reduced, and the power-on energy consumption is also reduced.
Drawings
Fig. 1 is a schematic structural diagram of an etching apparatus provided in the present application.
FIG. 2 is a schematic diagram of a portion of an etching apparatus according to an embodiment shown in FIG. 1.
Fig. 3 is a schematic structural view of an alloy sheet in the present application.
FIG. 4 is a partial exploded view of the etching apparatus of one embodiment shown in FIG. 2.
FIG. 5 is a partial exploded view of another view of the etching apparatus of the embodiment shown in FIG. 4.
FIG. 6 is a schematic diagram showing a connection structure between the etching apparatus and the alloy plate in the embodiment shown in FIG. 1.
FIG. 7 is a schematic cross-sectional view of the etching apparatus along VI-VI in one embodiment of FIG. 6.
Fig. 8 is a schematic structural diagram of an anodic oxidation process according to an embodiment of the present disclosure.
FIG. 9 is a scanning electron microscope image of a titanium alloy plate without etching the slot in example 1 of the present application.
FIG. 10 is a scanning electron microscope image of the titanium alloy slot of example 1 of the present application after etching.
Description of the main reference signs
Etching apparatus 100
Console 10
Securing assembly 20
First fixed block 21
First through hole 211
First surface 212
First receiving groove 213
Positioning column 214
Fixing hole 215
Second fixed block 22
Second through hole 221
Second surface 222
Second accommodation groove 223
Mounting hole 224
Accommodation chamber 30
First seal ring 41
Second seal ring 42
Fastener 50
Fastening nail 51
Spacing assembly 60
First limiting block 61
Third receiving groove 611
Second limiting block 62
Fourth receiving groove 621
Conductive block 70
Limiting groove 71
First conduit 81
Second conduit 82
First support table 83
Recess 831
Second support table 84
Pump 90
Electrolytic cell 200
Alloy plate 300
Slot 310
Through hole 320
Power supply 400
Anode 410
Cathode 420
Detailed Description
Embodiments of the present invention are described in detail below. The embodiments described below by referring to the drawings are illustrative only and are not to be construed as limiting the invention.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Referring to fig. 1, 2 and 3, the present application provides an etching apparatus 100, wherein the etching apparatus 100 is used for fixing an alloy plate 300 and etching slots 310 in the alloy plate 300 through an anodic oxidation process. The etching device 100 comprises an operation table 10, a fixing assembly 20, a limiting assembly 60 and a liquid pump 90, wherein the fixing assembly 20 and the limiting assembly 60 are arranged on the operation table 10, and the limiting assembly 60 is arranged on the side face of the fixing assembly 20. The fixing member 20 is used to fix the alloy plate 300 and allow the electrolyte to sufficiently infiltrate the slots 310 of the alloy plate 300. The spacing assembly 60 is used to define the position of the alloy plate 300. The liquid pump 90 is used to convey the electrolyte into the slots 310 of the alloy plate 300.
Referring to fig. 3, 4 and 5, the fixing assembly 20 includes a first fixing block 21 and a second fixing block 22 detachably coupled with the second fixing block 22. A receiving cavity 30 for receiving the alloy plate 300 is formed between the first and second fixing blocks 21 and 22 to fix the alloy plate 300 by the first and second fixing blocks 21 and 22. The first fixing block 21 has a first through hole 211, the second fixing block 22 has a second through hole 221, when the alloy plate 300 is accommodated in the accommodating cavity 30, the first fixing block 21 and the second fixing block 22 are located at two sides of the alloy plate 300 and clamp the alloy plate 300 in the etching device 100, and the first through hole 211, the slot 310 and the second through hole 221 are communicated, wherein the aperture of the slot 310 is larger than the inner diameters of the first through hole 211 and the second through hole 221. The electrolyte can flow in through the first through holes 211, flow through the slots 310 to completely infiltrate the inner walls of the slots 310, and then flow out through the second through holes 221.
Referring to fig. 3, 4 and 5, in some embodiments, the fixing assembly 20 further includes a first sealing ring 41 and a second sealing ring 42, a surface of the first fixing block 21 facing the second fixing block 22 is defined as a first surface 212, a portion of the first surface 212 is concave inward to form a first receiving groove 213, and the first sealing ring 41 is received in the first receiving groove 213 and partially protrudes out of the first receiving groove 213. The surface of the second fixing block 22 facing the first fixing block 21 is defined as a second surface 222, a part of the second surface 222 is concave inward to form a second accommodating groove 223, the second sealing ring 42 is accommodated in the second accommodating groove 223 and partially extends out of the second accommodating groove 223, wherein the first accommodating groove 213 and the second accommodating groove 223 are oppositely arranged and correspond to the slotted hole 310 of the alloy plate 300.
Referring to fig. 6 and 7, when the alloy plate 300 is disposed between the first fixing block 21 and the second fixing block 22, the arrangement of the first seal ring 41 and the second seal ring 42 can prevent the electrolyte flowing into the slot 310 from leaking from the connection between the first fixing block 21 and the slot 310 in the alloy plate 300 or the connection between the second fixing block 22 and the slot 310 in the alloy plate 300. In some embodiments, the first seal ring 41 and the second seal ring 42 may be made of silicone rubber.
Referring to fig. 6 and 7, in some embodiments, the central axes of the first perforation 211 and the second perforation 221 are parallel and non-collinear, such that the electrolyte flows into the slot 310 from the first perforation 211, and the buffer flows out of the second perforation 221 for a period of time, such that the electrolyte can sufficiently infiltrate the inner wall of the slot 310. For example, when the central axes of the first through holes 211 and the second through holes 221 are parallel to the upper surface of the console 10, the height of the central axis of the first through holes 211 is smaller than the height of the central axis of the second through holes 221, so that the electrolyte flowing into the slots 310 can fully infiltrate the inner walls of the entire slots 310. In some embodiments, the entire etching apparatus 100 may be disposed not only horizontally, as in fig. 6. In other embodiments, the entire etching apparatus 100 may be vertically disposed, that is, the operation table 10 is vertically disposed, and the central axes of the first and second through holes 211 and 221 are vertically disposed. Preferably, the first through holes 211 and the second through holes 221 are respectively communicated with both end portions of the slot 310, so that partial electrolyte is prevented from directly flowing out due to incomplete infiltration of the partial electrolyte on the inner wall of the slot 310.
Referring to fig. 3, 4 and 5, in some embodiments, the first surface 212 of the first fixing block 21 is further provided with a positioning post 214, and the second fixing block 22 is provided with a mounting hole 224 at a position corresponding to the positioning post 214 so as to facilitate the positioning post 214 to pass through. Through holes 320 are formed in the alloy plate 300 at positions corresponding to the positioning posts 214. In the present embodiment, two positioning posts 214 are provided, each positioning post 214 extends along the direction from the first surface 212 to the second surface 222, and the two positioning posts 214 are disposed near the edge of the first surface 212 and are disposed at two opposite sides of the first surface 212 at intervals. When the alloy plate 300 is provided, the two positioning posts 214 respectively pass through the through holes 320, so that the quick and accurate alignment of the alloy plate 300, the first fixing block 21 and the second fixing block 22 can be realized, and the alignment of the slotted holes 310 of the alloy plate 300 with the first sealing ring 41 and the second sealing ring 42 is prevented from being deviated, so that the electrolyte in the slotted holes 310 is prevented from leaking. In the case of multiple alloy plates 300 in the same batch, the positioning columns 214 can also realize rapid positioning of the positions of the alloy plates 300, so that the production efficiency is improved.
Referring to fig. 3, 4 and 5, in some embodiments, the securing assembly 20 further includes a fastener 50, the fastener 50 being used to fasten the first securing block 21 and the second securing block 22. The fastener 50 includes four fastening nails 51, wherein two fastening nails 51 are disposed near the upper end of the second fixing block 22 at a distance, and the other two fastening nails 51 are disposed near the lower end of the second fixing block 22 at a distance such that the alloy plate 300 is located between the upper and lower sets of fastening nails 51. The first fixing block 21 is provided with fixing holes 215 at positions corresponding to the fastening nails 51. One end of a fastening pin 51, such as a bolt, passes through the fixing holes 215 of the second fixing block 22 and the first fixing block 21 to fasten both.
Referring to fig. 3, 4 and 5, in some embodiments, the limiting assembly 60 is fixed on the console 10, the limiting assembly 60 includes a first limiting block 61 and a second limiting block 62 corresponding to the first limiting block 61, the first fixing block 21 and the second fixing block 22 are disposed between the first limiting block 61 and the second limiting block 62, the first limiting block 61 and the second limiting block 62 are disposed on two sides of a side surface of the first fixing block 21 and the second fixing block 22, the surface of the first limiting block 61 facing the second limiting block 62 is concave to form a third accommodating groove 611, the surface of the second limiting block 62 facing the first limiting block 61 is concave to form a fourth accommodating groove 621, and two sides of the alloy plate 300 are disposed in the third accommodating groove 611 and the fourth accommodating groove 621, respectively. The third receiving groove 611 and the fourth receiving groove 621 are provided to prevent the alloy plate 300 and the fixing assembly 20 from being offset after the alloy plate 300 is mounted or fastened to the first and second fixing blocks 21 and 22.
Referring to fig. 3, 4 and 5, in some embodiments, the first limiting block 61 is further provided with a conductive block 70, where the conductive block 70 has a limiting groove 71, and the limiting groove 71 is opened toward the first limiting block 61. The conductive block 70 is electrically connected to the power supply 400 through an electric wire. The conductive block 70 is mounted on the alloy plate 300 through the limit groove 71 to realize electrical conduction to the alloy plate 300.
Referring to fig. 4, 5 and 6, in applying the etching apparatus 100, first, the positioning posts 214 of the first fixing block 21 pass through the through holes 320 of the alloy plate 300 and the mounting holes 224 of the second fixing block 22 to achieve the pre-positioning of the first fixing block 21, the alloy plate 300 and the second fixing block 22, and then, the first fixing block 21 and the second fixing block 22 are fastened by the fastening members 50 and both sides of the alloy plate 300 fixed between the first fixing block 21 and the second fixing block 22 are placed in the third receiving groove 611 and the fourth receiving groove 621 to define the position of the alloy plate 300, preventing the tilting or shifting from occurring.
Referring to fig. 6 and 7, the etching apparatus 100 further includes a first conduit 81 and a second conduit 82, the first conduit 81 being connected to the first fixing block 21 and communicating with the first through-holes 211, and the electrolyte being supplied through the first through-holes 211 to the slots 310 of the alloy plate 300 by the first conduit 81. The second conduit 82 is connected to the second fixing block 22 and communicates with the second through hole 221, and the electrolyte in the slot 310 flows out through the second through hole 221 and the second conduit 82. The operation table 10 is further provided with a first supporting table 83 for supporting the first conduit 81 and a second supporting table 84 for supporting the second conduit 82, the first supporting table 83 is close to the joint of the first conduit 81 and the first fixed block 21, and liquid leakage at the joint of the first fixed block 21 and the first conduit 81 due to the fact that the joint of the first conduit 81 and the first fixed block 21 is pulled by the gravity of the first conduit 81 and the electrolyte is avoided. In some embodiments, the top surface of the first support 83 is concavely formed with a recess 831, and the center of the recess 831 is collinear with the center of the first conduit 81 to define the position of the first conduit 81 on the first support 83, so as to avoid the first conduit 81 sliding or twisting from the first support 83 to pull the connection between the first conduit 81 and the first fixing block 21. Similarly, the second support table 84 has the same structure as the first support table 83, and will not be described here.
Referring to fig. 1 and 3, in some embodiments, the inlet of the pump 90 extends into the electrolyte of the cell 200, and the outlet of the pump 90 communicates with the first conduit 81 to deliver electrolyte to the slots 310 in the alloy plate 300. In some embodiments, the liquid pump 90 is an air pump.
Referring to fig. 8, the present application also provides an etching method of an alloy plate 300 with slots 310, for etching slots 310 in the alloy plate 300 by using the etching apparatus 100 (see fig. 3). The etching method comprises the following steps:
s1, providing an alloy plate 300, wherein the alloy plate 300 is provided with a slot 310.
Alloy plate 300 may be a titanium alloy or other alloy.
S2, the alloy plate 300 is mounted in the etching device 100.
The fixing of the alloy plate 300 is achieved by the etching apparatus 100.
S3, providing an electrolytic tank 200, wherein the electrolytic tank 200 is provided with electrolyte, and a cathode 420 is inserted into the electrolyte. The alloy plate 300 is disposed outside the electrolytic cell 200 and serves as an anode 410, and the anode 410 and the cathode 420 are respectively connected to the positive and negative poles of the power supply 400. The first conduit 81 and the second conduit 82 of the etching apparatus 100 are each extended into the electrolyte in the electrolytic bath 200.
In step S3, the liquid pump 90 is started so that the electrolyte forms a continuous reflux through the electrolytic cell 200, the first conduit 81, the slot 310 and the second conduit 82. The power supply 400 is then activated to effect etching of the inner walls of the slots 310 by an anodic oxidation process.
Compared with the prior anodic oxidation process, the alloy plate 300 is arranged outside the electrolytic tank 200, and the flowing electrolyte fully infiltrates the inner walls of the slotted holes 310 by transferring the electrolyte in the electrolytic tank 200 into the slotted holes 310, so that the slotted holes 310 of the alloy plate 300 are etched in a non-soaking mode, and a uniform oxide layer is formed on the inner walls of the slotted holes 310. In this method, on the one hand, the etching can be performed for the various slots 310 on the alloy plate 300, and the problem of uneven etching of the slots 310 of the alloy plate 300 can be solved by immersing the alloy plate 300 in the electrolyte. On the other hand, this method can also realize surface treatment in the slot 310 of complex structure. Meanwhile, the number of times of aging and replacing the electrolyte is reduced, the power consumption is reduced, and the etching amount of the alloy plate 300 is reduced. In particular, this partially selective immersion etching method can protect information (e.g., two-dimensional code information, etc.) attached to other positions on the alloy plate 300.
In some embodiments, the electrolytic cell 200 is a sealed cavity, so that the electrolyte is isolated from air during the output and input flow processes, and some solvents with pungent odor or volatile solvents are prevented from overflowing from the electrolytic cell 200, for example, high-concentration acetic acid, so that the health of operators is ensured. On the other hand, the gas generated in the process of electrifying the anode and the volatile gas can be conveyed to the waste gas treatment device together in a sealing way, so that the unified recovery of waste gas is realized.
The application also provides an electrolyte for etching the titanium alloy, which comprises, by volume, 50% -70% of glacial acetic acid, 5% -15% of chloride salt, 15% -20% of passivating agent, 1% -3% of aluminum sulfate and deionized water, wherein the chloride salt is one of sodium chloride and potassium chloride, and the passivating agent comprises one of propylene glycol and glycerol.
In the anodic oxidation process, the high-concentration glacial acetic acid can increase the resistance of the electrolyte and control the current, so that the electrolyte can sufficiently and uniformly etch the inner walls of the slots 310 of the titanium alloy plate 300.
In some embodiments, the alloy plate 300 may be a titanium alloy or an aluminum alloy, or the like. In the present embodiment, the titanium alloy plate 300 is selected as the alloy plate 300 for illustration, but the present invention is not limited thereto.
The chloride salt acts as an etchant to form an oxide layer on the inner walls of the slots 310 in the titanium alloy plate 300. The passivating agent can also increase the resistance of the electrolyte, and further improve the uniformity of the oxide layer on the inner wall of the slot 310 of the titanium alloy plate 300. Aluminum sulfate serves as a stabilizer to improve the stability of the inner walls of the anodized slots 310.
The electrolyte provided by the application can form micron-sized etching apertures in the slotted holes 310 of the titanium alloy plate 300, so that the bonding strength of the titanium alloy plate 300 and plastic with low fluidity (such as AV651 plastic) can be molded in an injection manner is greatly improved, and the electrolyte does not contain toxic substances such as fluorine, chromium, methanol and the like and is environment-friendly.
In some embodiments, the power supply 400 has a voltage of between 30-40V and a current density of 0.8-1.5A/dm 2 Within this range of voltage and current density, the slots 310 of the titanium alloy plate 300 are enabled to be etched.
In some embodiments, the flow rate of the electrolyte through the slots is 150-180mL/s for 40-45min, which is arranged to allow the slots 310 to be fully wetted. If the flow rate is too low or the time is too short, the etching of the inner wall of the slot 310 is insufficient; if the flow rate is too high or the flow time is long, the inner wall of the slot 310 is excessively etched, and the production cost is increased.
In some embodiments, the titanium alloy sheet 300 may also be subjected to degreasing and pretreatment prior to the anodic oxidation process of the titanium alloy sheet 300, the degreasing treatment specifically being:
immersing the titanium alloy plate 300 in a degreasing agent, wherein the temperature of the degreasing agent is 34-36 ℃, the immersing time is 4-6min, and oil stains or dirt on the surface of the titanium alloy plate 300 can be removed through degreasing treatment. In some embodiments, the degreasing agent may be an alkaline degreasing agent, such as model R105 degreasing agent.
The specific pretreatment is as follows: in immersing the degreasing-treated titanium alloy sheet 300 in a nitric acid solution having a volume fraction of 30%, the immersing time was 1min. The nitric acid solution can further clean the surface of the titanium alloy plate 300, and on the other hand, can remove the degreasing agent remained on the surface of the titanium alloy, so that the degreasing agent is prevented from affecting the subsequent anodic oxidation to act on the titanium alloy plate 300.
In some embodiments, the titanium alloy plate 300 is subjected to a current-carrying anodic oxidation treatment, and then is immersed in a nitric acid solution having a volume fraction of 3% for 1min. The 3% nitric acid solution can remove impurities from the etched titanium alloy plate 300, and can also remove glacial acetic acid in the energized anodic oxidation process. The titanium alloy plate 300 treated with 3% nitric acid solution is dried at 70-80 deg.c for 15min to obtain the micro-sized slots 310.
The scheme of the present invention will be explained below with reference to examples. It will be appreciated by those skilled in the art that the following examples are for illustrative purposes only and are not to be construed as limiting the invention. Unless otherwise indicated, the reagents, software and instrumentation involved in the examples below are all conventional commercial products or open source.
Example 1
Step 1. The titanium alloy plate 300 (model TC 4) was immersed in a degreasing agent (model R105) at 35℃for 5min.
And 2, immersing the titanium alloy plate 300 degreased in the step 1 into a nitric acid solution with the volume fraction of 30%, wherein the temperature is 25 ℃, and the immersion time is 1min.
And 3, fixing the titanium alloy plate 300 processed in the step 2 in the etching device 100, wherein the titanium alloy plate 300 is used as an anode 410, a cathode 420 is made of graphite/stainless steel, the cathode 420 is inserted into electrolyte, and a liquid pump 90 is started to enable the electrolyte to form a continuous closed loop so as to fully soak the slotted holes 310.
The electrolyte comprises 60% of glacial acetic acid, 10% of sodium chloride, 20% of propylene glycol, 2% of aluminum sulfate and the balance of deionized water according to volume fraction.
Step 4, starting the power supply 400, regulating the voltage of the power supply 400 to be between 35V and the current density to be 1A/dm 2 The flow rate of the liquid pumped by the liquid pump 90 is 150-180mL/s, such as 166mL/s. The power supply 400 is operated for 43 minutes so that the electrolyte is sufficiently immersed in and acts on the inner walls of the slots 310 in the titanium alloy plate 300 to form a uniform oxide layer on the inner walls of the slots 310.
And 5, placing the titanium alloy plate 300 treated in the step 4 into a nitric acid solution with the volume fraction of 3%, soaking for 1min, and then placing into a baking oven with the temperature of 70-80 ℃ for baking for 15min to obtain the titanium alloy plate 300 with the micron-sized oxide layer on the surface.
Referring to fig. 9 and 10, in embodiment 1, the slots 310 in the titanium alloy plate 300 were subjected to sem test before and after etching, respectively.
Referring to fig. 9, before the anodic oxidation process is performed on the slots 310 of the titanium alloy plate, that is, before the slots 310 are etched, the inner walls of the slots 310 have smooth surfaces and regular lines are formed along the same direction. Referring to fig. 10, after etching, the inner walls of the slots 310 form a uniform porous surface structure, and the majority of the holes have a pore diameter in the micrometer range. This means that a uniform oxide layer can be formed on the inner wall of the slot 310 by the etching method provided in the present application.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention.

Claims (10)

1. An etching apparatus, characterized in that the etching apparatus comprises:
the fixing assembly is used for fixing the alloy plate, and the alloy plate is provided with a slotted hole;
the liquid pump is used for communicating electrolyte, taking the alloy plate as an anode, and controlling the electrolyte to flow through the slotted hole;
the electrolyte is used for accommodating the electrolyte, a cathode is inserted into the electrolyte, and the alloy plate is positioned outside the electrolyte;
and the power supply is used for electrifying between the cathode and the anode, so that the inner wall of the slotted hole forms an oxide layer after anodic oxidation.
2. The etching apparatus according to claim 1, wherein the fixing assembly includes a first fixing block and a second fixing block disposed opposite to each other, a receiving chamber for mounting the alloy plate is formed between the first fixing block and the second fixing block, the first fixing block has a first through hole, the second fixing block has a second through hole, and the first through hole and the second through hole are for communicating with the slot and passing the electrolyte.
3. The etching apparatus of claim 2, wherein the securing assembly further comprises a first seal ring and a second seal ring, the first securing block having a first surface facing the second securing block, the first surface portion being recessed to form a first receiving groove, the first seal ring being received in the first receiving groove;
the second fixed block is provided with a second surface facing the first fixed block, a second accommodating groove is formed in the second surface in a partially concave mode, the second sealing ring is accommodated in the second accommodating groove, and the first sealing ring and the second sealing ring are oppositely arranged to seal the joint of the first fixed block, the second fixed block and the alloy plate.
4. The etching apparatus of claim 2, wherein central axes of the first and second perforations are parallel and non-collinear.
5. The etching apparatus of claim 1, wherein the electrolytic cell comprises a sealed cavity.
6. The etching apparatus according to claim 1, further comprising a first conduit and a second conduit, wherein the first conduit and the second conduit are communicated with the electrolytic cell and are respectively communicated with both ends of the slot, wherein the liquid pump is communicated with the first conduit, and wherein the electrolyte forms a continuously closed circuit via the first conduit, the second conduit and the electrolytic cell.
7. The etching apparatus according to claim 1, wherein the power supply has a supply voltage of 30 to 40V and a current density of 0.8 to 1.5A/dm 2
8. An etching method using the etching apparatus according to any one of claims 1 to 7, wherein a flow rate of the electrolyte flowing through the slot is 150 to 180mL/s.
9. The etching method according to claim 8, wherein the electrolytic solution comprises, in volume fraction, 50% -70% glacial acetic acid and 5% -15% chloride salt, the chloride salt comprising one of sodium chloride or potassium chloride.
10. The etching method according to claim 9, wherein the electrolyte further comprises 15% to 20% of propylene glycol and 1% to 3% of aluminum sulfate in terms of volume fraction.
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Publication number Priority date Publication date Assignee Title
JP2008192838A (en) * 2007-02-05 2008-08-21 Tokyo Electron Ltd Etching apparatus, etching method, and manufacturing method of electronic device
CN101307480A (en) * 2008-02-05 2008-11-19 哈尔滨工业大学 Titanium alloy surface high temperature oxidation corrosion resistance coatings preparation method
CN101724879B (en) * 2009-12-16 2011-07-20 中国科学院力学研究所 Brush-plating and film-forming device for ceramic coating through plasma electrolytic oxidation (PEO) and method thereof
CN102330136B (en) * 2011-09-06 2013-12-25 上海瑞尔实业有限公司 Auxiliary cathode and method for carrying out anodic oxidation on blind hole by using same
CN105696052B (en) * 2016-03-31 2017-12-05 浙江工业大学 Differential arc oxidation reaction unit
CN105755516B (en) * 2016-04-26 2018-04-20 重庆协成汽车零部件有限公司 Piston ring groove rapid anodization device
CN206872969U (en) * 2017-07-04 2018-01-12 湖南江滨机器(集团)有限责任公司 A kind of piston limit oxidation unit
CN107313095A (en) * 2017-08-30 2017-11-03 重庆协成汽车零部件有限公司 Anodic oxidation device and piston anodic oxidation processing technology
CN109468672A (en) * 2019-01-23 2019-03-15 李运 A kind of Aluminium alloy anode oxidation device
CN110499522A (en) * 2019-09-20 2019-11-26 中山大学 A kind of interior preparation method for flowing electric deposition device and electro-deposition porous structure of pipe
CN212865024U (en) * 2020-06-10 2021-04-02 上海宝敦金属表面处理厂(普通合伙) Local anodic oxidation equipment for valve body
CN212669822U (en) * 2020-06-28 2021-03-09 山东哈船船舶装备制造有限公司 Light metal anticorrosive treatment and oxidation device
CN112609209B (en) * 2020-11-28 2022-06-07 欧之萌(武汉)国际贸易有限公司 Electrolytic bath device for preparing colloid nano silver by low-current mobile phase
CN113201776A (en) * 2021-05-08 2021-08-03 深圳市蓝海永兴实业有限公司 Aluminum alloy anodic oxidation surface treatment process
CN113416955A (en) * 2021-06-25 2021-09-21 浙江天力机车部件有限公司 Titanium alloy fastener anodic oxidation and magnetron sputtering surface composite treatment method

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