CN114875470A - Automatic circulating electrolyte concentration compensation device and method - Google Patents
Automatic circulating electrolyte concentration compensation device and method Download PDFInfo
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- CN114875470A CN114875470A CN202210569449.4A CN202210569449A CN114875470A CN 114875470 A CN114875470 A CN 114875470A CN 202210569449 A CN202210569449 A CN 202210569449A CN 114875470 A CN114875470 A CN 114875470A
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- 238000004070 electrodeposition Methods 0.000 claims abstract description 28
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
- C25D21/14—Controlled addition of electrolyte components
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention relates to a device and a method for compensating concentration of automatic circulating electrolyte, comprising the following steps: the electrolytic cell is provided with an electrolyte inlet and an electrolyte outlet; the electrolyte circulating water tank is provided with a circulating electrolyte recycling port and a circulating electrolyte outlet, the circulating electrolyte recycling port is communicated with the electrolyte outlet, and the circulating electrolyte outlet is communicated with the electrolyte inlet; and the electrolyte compensation system is communicated with the electrolyte circulating water tank and is used for performing concentration compensation on the electrolyte in the electrolyte circulating water tank according to the concentration of the electrolyte. According to the invention, the concentration compensation is carried out on the electrolyte in the electrolyte circulating water tank by using the electrolyte compensation system, so that the ion concentration in the electrolyte is always in a control range, and the electrolyte can also drive the electrolyte to flow in the circulating process, thereby generating a stirring effect, helping ions near a cathode to diffuse, and solving the problem of low concentration of the ions attached to the cathode in the electrodeposition process.
Description
Technical Field
The invention relates to the technical field of 3D printing, in particular to a device and a method for compensating concentration of an automatic circulating electrolyte.
Background
Electrochemical deposition, also referred to as electrodeposition, is a technique in which a current is transferred by positive and negative ions in an electrolyte solution under the action of an external electric field, and an oxidation-reduction reaction of electrons is generated at an electrode to form a plating layer. Electrochemical deposition techniques are widely used in industry and are also well established. Electroplating, electroforming, anodizing, etc. coatings and part fabrication methods are typical applications for electrochemical deposition techniques. The electrochemical deposition process has very low heat input, which is equivalent to a non-thermal process, so that the residual stress of the obtained product or coating is very low, and the problem of oxidation can be avoided under normal pressure. In addition, the electrochemical deposition has excellent microstructure regulation and control performance, and crystal grain structures with different sizes and orientations can be obtained by regulating and controlling process parameters, so that the mechanical properties of the crystal grain structures are controlled. Therefore, attempts have been made to develop additive manufacturing techniques for metal three-dimensional structures and parts using electrochemical deposition. For example, patent [ ZL201710351130.3] proposes an electrochemical metal needle tip 3D printer, which implements localized scanning using a metal needle tip to implement electrochemical metal needle tip deposition 3D printing; CN201711387048.2 discloses a method for manufacturing a micro-mold by electroforming with a metalized jet on the surface of a substrate, which utilizes a machine tool to drive an electroforming nozzle connected with an anode to perform selective scanning electroforming on the surface of a metal substrate connected with a cathode, thereby obtaining the electroforming micro-mold. The electrochemical 3D printing technology effectively avoids the problems of thermal stress and high-temperature oxidation of the workpiece of the existing metal 3D printing technology, and has the advantages of low manufacturing cost, simple equipment process and good compactness of the workpiece. In addition, due to these characteristics, the electrochemical 3D printing technology is very suitable for the fabrication of miniature articles.
The main limitations of current electrochemical 3D printing technologies are in two aspects. Firstly, along with the reaction of the electrolyte, the concentration and the content of specific metal ions are suddenly reduced, and other products are increased, so that the printing time (reaction time) is greatly shortened, and the electrolyte needs to be frequently replaced, so that the processing efficiency of parts is low; secondly, although the deposition reaction is carried out in a sufficient amount of the electrolyte, the ion diffusion concentration cannot satisfy the ion consumption rate without stirring or circulation, and thus there is a certain ion concentration difference between the vicinity of the cathode and the edge region.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide an automatic circulating electrolyte concentration compensation device and method.
In order to achieve the purpose, the invention provides the following scheme:
an automatic circulating electrolyte concentration compensating apparatus comprising:
the electrolytic bath is provided with an electrolyte inlet and an electrolyte outlet;
the electrolyte circulating water tank is provided with a circulating electrolyte recycling port and a circulating electrolyte outlet, the circulating electrolyte recycling port is communicated with the electrolyte outlet, and the circulating electrolyte outlet is communicated with the electrolyte inlet;
the baume degree measuring instrument is arranged inside the electrolyte circulating water tank and is used for detecting the concentration of the electrolyte;
and the electrolyte compensation system is communicated with the electrolyte circulating water tank and is used for performing concentration compensation on the electrolyte in the electrolyte circulating water tank according to the concentration of the electrolyte.
Preferably, an electrolyte heater, a first baffle and a second baffle are further arranged in the electrolyte circulating water tank;
the lower extreme of first baffle has first breach, the upper end of second baffle has the second breach, electrolyte heater sets up in the passageway that first breach and second breach constitute.
Preferably, an electrolyte tank temperature measuring instrument is further arranged on one side of the circulating electrolyte outlet.
Preferably, the electrolyte compensation system comprises:
the electrolyte tank is provided with an electrolyte tank liquid outlet, and the electrolyte tank liquid outlet is communicated with the electrolyte circulating water tank; a new electrolyte is arranged in the electrolyte water tank;
and the electromagnetic valve is arranged on one side of the liquid outlet of the electrolyte tank and used for regulating and controlling the valve according to the concentration of the electrolyte and enabling new electrolyte to flow into the electrolyte circulating tank so as to enable the concentration of the electrolyte in the electrolyte circulating tank to be unchanged.
Preferably, the electrolytic cell comprises:
the bottom of the electrolytic cell box body is made of optical high-transmittance glass;
and the liquid level limiting water outlet is arranged on one side of the electrolytic tank body.
Preferably, an electrolyte inlet flow sensor is arranged on the electrolyte inlet; and an electrolyte outlet flow sensor is arranged on the electrolyte outlet.
Preferably, the method further comprises the following steps:
a 3D printing system for completing 3D printing using an electrolytic bath; the 3D printing system comprises a Z-direction movement device, an anode substrate and a laser; the Z-direction movement device is connected with the cathode substrate and is used for controlling the cathode substrate to lift; the anode substrate is arranged inside the electrolytic cell; the laser is arranged at the bottom of the electrolytic tank and used for irradiating the cathode substrate with laser to carry out electrochemical deposition.
Preferably, the method further comprises the following steps:
an electrochemical processing power supply, wherein the negative electrode of the electrochemical processing power supply is connected with the cathode substrate, and the positive electrode of the electrochemical processing power supply is connected with the anode substrate;
the invention also provides an automatic circulating electrolyte concentration compensation method, which comprises the following steps:
step 1: introducing electrolyte into the electrolytic cell by using an electrolyte circulating water tank;
step 2: judging whether the difference between the inflow amount of the electrolyte inlet and the outflow amount of the electrolyte outlet is within a preset range;
and step 3: when the difference between the inflow and outflow is in a preset range, adjusting the focal length of the laser to enable the focal point of the laser to fall on the surface of the cathode substrate;
and 4, step 4: heating the electrolyte to a preset temperature by using an electrolyte heater;
and 5: the 3D printing system performs 3D printing by using an electrolytic bath;
step 6: in the 3D printing process, the electrolyte concentration in the electrolyte is monitored in real time, when the electrolyte concentration is lower than a set lower limit value, the electromagnetic valve is opened, and the high-concentration electrolyte is injected into the circulating water tank to compensate the concentration of the electrolyte; when the electrolyte concentration is not lower than the lower limit value, the electromagnetic valve keeps a closed state, and no high-concentration electrolyte is injected into the water tank.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the automatic circulating electrolyte concentration compensation device and method provided by the invention have the beneficial effects that: compared with the prior art, the concentration compensation of the electrolyte in the electrolyte circulating water tank is carried out by using the electrolyte compensation system, so that the ion concentration in the electrolyte is always in a control range, and the electrolyte can drive the electrolyte to flow in the circulating process, thereby generating a stirring effect, helping ions near a cathode to diffuse, and solving the problem of low concentration of cathode attached ions in the electrodeposition process.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a schematic diagram of an external structure of an automatic circulating electrolyte concentration compensation apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of an internal structure of an automatic circulating electrolyte concentration compensation apparatus according to an embodiment of the present invention;
FIG. 3 is a schematic view of an electrolytic cell in an embodiment provided by the present invention;
FIG. 4 is a flow chart of electrolyte circulation and concentration compensation provided by the present invention;
FIG. 5 is a schematic three-dimensional structure diagram of a part to be machined according to example 1 of the present invention;
FIG. 6 is a schematic three-dimensional structure diagram of a part to be processed according to example 2 of the present invention;
FIG. 7 is a schematic three-dimensional structure diagram of a part to be machined according to embodiment 3 of the present invention;
fig. 8 is a schematic three-dimensional structure diagram of a part to be processed in embodiment 4 of the present invention.
Description of the symbols:
1-electrolyte tank outlet, 2-solenoid valve, 3-electrolyte compensation water tank port, 4-electrolyte heater, 5-electrolyte filling and observing port, 6-circulating electrolyte recovery port, 7-high concentration electrolyte filling and observing port, 8-electrolyte water tank, 9-high concentration electrolyte water tank strut, 10-electrolyte circulating water tank, 11-baume measuring instrument, 12-circulating electrolyte outlet, 13-high concentration electrolyte conveying hose, 14-electrolyte heater, 15-electrolyte water tank cover, 16-circulating electrolyte, 17-high concentration electrolyte water tank cover, 18-high concentration electrolyte, 19-electrolyte tank temperature measuring instrument, 20-second baffle; 101-cathode substrate, 102-temperature measuring meter, 103-electrolytic tank end cover, 104-electrolytic tank body, 105-liquid level limiting drain outlet, 106-electrolyte, 107-electrolyte inlet, 108-electrolyte inlet flow sensor, 109-cathode substrate level adjusting silica gel column, 1010-electrodeposition processing power supply cathode line, 1011-cathode substrate clamp, 1012-anode substrate, 1013-optical high-transmittance glass, 1014-electrolyte outlet, 1015-electrolyte outlet flow sensor and 1016-laser.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Referring to fig. 1, an apparatus for compensating the concentration of an automatically circulating electrolyte includes: the device comprises an electrolytic bath, an electrolyte circulating water tank 10, a baume degree measuring instrument 11 and an electrolyte compensation system.
An electrolyte inlet 107 and an electrolyte outlet 1014 are arranged on the electrolytic cell; electrolyte circulation tank 10 is equipped with circulation electrolyte and retrieves mouth 6 and circulation electrolyte liquid outlet 12, circulation electrolyte retrieve mouth 6 with electrolyte liquid outlet 1014 intercommunication, circulation electrolyte liquid outlet 12 with electrolyte inlet 107 intercommunication. It should be noted that, the electrolyte in the electrolytic cell can be conveyed into the electrolyte circulation water tank 10 by the liquid discharge pump, and the electrolyte in the electrolyte circulation water tank 10 can be conveyed into the electrolytic cell by the input pump; a baume degree measuring instrument 11 disposed inside the electrolyte circulation water tank 10 for detecting the concentration of the electrolyte; and the electrolyte compensation system is communicated with the electrolyte circulating water tank 10 and is used for compensating the concentration of the electrolyte in the electrolyte circulating water tank 10 according to the concentration of the electrolyte.
Further, an electrolyte heater 14, a first baffle, a second baffle 20 and an electrolyte tank temperature measuring instrument 19 are arranged in the electrolyte circulation water tank 10; the lower end of the first baffle plate is provided with a first notch, the upper end of the second baffle plate 20 is provided with a second notch, and the electrolyte heater 14 is arranged in a passage formed by the first notch and the second notch; the electrolyte tank temperature measuring instrument 19 is arranged at one side of the circulating electrolyte outlet 12.
In an embodiment of the present invention, an electrolyte compensation system includes: electrolyte tank 8 and solenoid valve 2.
The electrolyte tank 8 is provided with an electrolyte tank liquid outlet 1, and the electrolyte tank liquid outlet 1 is communicated with the electrolyte circulating water tank 10; a new electrolyte (high-concentration electrolyte) is arranged in the electrolyte water tank 8; and the electromagnetic valve 2 is arranged on one side of the liquid outlet 1 of the electrolyte tank and used for regulating and controlling a valve according to the concentration of the electrolyte and enabling new electrolyte to flow into the electrolyte circulating water tank 10 to enable the concentration of the electrolyte in the electrolyte circulating water tank 10 to be unchanged.
Further, the electrolytic cell includes: an electrolytic tank body 104 and a liquid level limiting drain opening 105.
The bottom of the electrolytic cell box 104 is made of optical high-transparent glass 1013; and a liquid level limiting drain opening 105 provided on one side of the electrolytic cell case 104.
The automatic circulating electrolyte concentration compensation device is provided with a flow sensor on a liquid inlet pipe and a liquid outlet pipe of an electrolytic bath respectively, and is responsible for monitoring the inflow and outflow of electrolyte of the electrolytic bath; besides the liquid inlet and the liquid outlet, a liquid level limiting water outlet is also arranged, so that the specified liquid level can be conveniently and quickly reached; on the cell end cover plate 103, there is a temperature meter for measuring the real-time temperature condition of the feedback cell. A small water tank containing high-concentration electrolyte is arranged on the electrolyte water tank 8, a liquid outlet of the small water tank is connected with the electrolyte water tank 8, and the opening and closing of a pipeline are controlled by an electromagnetic valve in the middle; the high concentration electrolyte is collected near the recycling port of the electrolyte tank 8, and the baume measuring instrument is installed near the outlet of the electrolyte tank 8. Two baffles are arranged in the middle of the water tank, and are distributed at intervals from top to bottom, so that the electrolyte reaches the liquid outlet from the recovery port again and must pass through the electrolyte heater, and the constant temperature state of the electrolyte is realized, as shown in fig. 2.
In the embodiment of the invention, the electrolytic cell can finish the processing of parts by means of a 3D printing system. The electrolytic cell is fixed above the laser 1016 and below the cathode substrate 101, a piece of high-transparent glass 12 is left in the middle of the cell bottom, and the laser can irradiate onto the cathode substrate 101 through the high-transparent glass 12 and the electrolyte. Except for a window with the same size as the cathode substrate 101, the other parts of the electrolytic cell are covered by an electrolytic cell end cover 103, and a liquid inlet and a liquid outlet are arranged in the electrolytic cell, so that the circulation of the electrolyte is facilitated, as shown in fig. 3, the 3D printing system comprises a Z-direction movement device, an anode substrate 1012 and a laser; the Z-direction movement device is connected with the cathode substrate 101 through a cathode substrate horizontal adjustment silica gel column 109 and a cathode substrate clamp 1011 and is used for controlling the cathode substrate 101 to lift; the anode substrate 1012 disposed inside the electrolytic cell; the laser 1016 is positioned at the bottom of the cell for use in irradiating the cathode substrate with laser light for electrochemical deposition. The cathode of the electrochemical machining power supply is connected to the cathode substrate 101, and the anode of the electrochemical machining power supply is connected to the anode substrate. The laser head is driven by the high-precision motion platform to move in the X/Y direction to the plane direction, and the cathode substrate 101 is driven by the high-precision Z-direction motion device to move in a height lifting mode. The specific processing process is as follows:
(1) CAD modeling of parts: modeling a part to be processed on three-dimensional modeling software;
(2) and (3) model slicing treatment: importing the built three-dimensional model into slicing software, and slicing according to the thickness as required to obtain slicing data;
(3) generating a processing track: planning a processing track scanned by the laser by using the obtained slice data, and producing a numerical control code or a processing file which can be identified by a 3D printer;
(4)3D printing process simulation: simulating the processing process of the generated numerical control code or processing file by using simulation software, verifying whether the generated numerical control code or processing file meets the design and processing requirements, returning to a model slicing processing link if the generated numerical control code or processing file does not meet the design and processing requirements, and resetting and generating slicing and processing track data again; if the requirement is met, entering the next link, importing the processing file into a 3D printing system, and preparing for actual processing;
(5) electrolyte preparation: preparing electrolyte with reasonable components and concentration according to the material requirements of a workpiece, filling the electrolyte into an electrolyte circulating filter water tank, and preparing the electrolyte with the same components and high concentration and placing the electrolyte into an electrolyte compensation water tank;
(6) setting electrodeposition parameters: setting parameters of electrochemical deposition according to processing requirements, wherein the parameters mainly comprise electrolyte flow, electrodeposition current, electrodeposition voltage, electrodeposition frequency, electrodeposition pulse width, electrolyte concentration compensation, upper and lower limits for stopping compensation and the like;
(7) laser tool setting: slowly descending the cathode plate, detecting the current generated by a loop once the cathode touches the electrolyte, and braking the cathode plate by a control card to complete the positioning of the cathode plate; adjusting the focal length of the laser to enable the focal point of the laser to fall on the surface of the cathode substrate;
(8) laser parameter setting: setting laser scanning parameters including power, scanning speed and the like according to processing requirements;
(9)3D printing and processing: and starting a laser, an electrodeposition power supply and the like to perform layer-by-layer printing and processing of the workpiece. After the printing of the workpiece is completed, the surface of the workpiece needs to be passivated and finished, so that the surface quality and precision of the workpiece are ensured.
In the process of printing parts, because the ion concentration in the electrolyte is gradually reduced, the invention needs to utilize an automatic circulating electrolyte concentration compensation device to keep the ion concentration in the plating solution unchanged, and the specific compensation process is as follows:
an automatic circulating electrolyte concentration compensation method, comprising:
step 1: introducing electrolyte into the electrolytic cell by using an electrolyte circulating water tank;
step 2: judging whether the difference between the inflow amount of the electrolyte inlet and the outflow amount of the electrolyte outlet is within a preset range;
and step 3: when the difference between the inflow and outflow is in a preset range, adjusting the focal length of the laser to enable the focal point of the laser to fall on the surface of the cathode substrate;
and 4, step 4: heating the electrolyte to a preset temperature by using an electrolyte heater;
and 5: the 3D printing system performs 3D printing by using an electrolytic bath;
step 6: in the 3D printing process, the electrolyte concentration in the electrolyte is monitored in real time, when the electrolyte concentration is lower than a set lower limit, the electromagnetic valve is opened, and the high-concentration electrolyte is injected into the circulating water tank to compensate the concentration of the electrolyte; when the electrolyte concentration is not lower than the lower limit, the electromagnetic valve keeps a closed state, and no high-concentration electrolyte is injected into the water tank.
Referring to fig. 4, in practical applications, the compensation process of the present invention is as follows:
(1) setting a displacement starting input pump: setting the flow of the electrolytic cell according to the process requirement, setting the discharge amount according to the flow, and opening the input pump to quickly fill the electrolytic cell with electrolyte;
(2) raising to the liquid level, limiting and starting a liquid discharge pump: when the electrolyte rises to the liquid level limit position, the electrolyte overflow can be observed, at the moment, the liquid discharge pump is started, and the discharge capacity is set to be gradually increased;
(3) observing inflow and outflow: setting a range value a according to the flow of the electrolytic cell, and when the data of the observation flow meter meets 0ml < inflow-outflow < aml, considering that the electrolyte in the electrolytic cell realizes dynamic balance and entering the next link; if not, continuing to wait for the increase of the discharge capacity of the liquid discharge pump;
(4) keeping the discharge capacity of the two pumps, and zeroing the negative plate: when the electrolytic bath realizes dynamic balance, the discharge capacity of the two pumps is kept unchanged. Slowly descending the cathode plate, detecting the current generated by a loop once the cathode touches the electrolyte, and braking the cathode plate by a control system to finish the zero resetting and positioning of the cathode plate; adjusting the focal length of the laser to enable the focal point of the laser to fall on the surface of the cathode substrate;
(5) setting the working temperature t of electrolyte: and setting the working temperature t of the electrolyte according to the process requirement.
(6) Starting a heating mode: and after the working temperature of the electrolyte is set, controlling the heater to enter a heating mode, and starting heating the electrolyte by the heater.
(7) Observing the temperature T of the plating solution in the electrolytic bath: and when the temperature T of the electrolyte in the electrolytic cell meets T >0.95T, the electrolyte is considered to basically reach the working temperature, and if the temperature T of the electrolyte does not meet the working temperature, the next link can be started, and the heating mode is continued.
(8) Starting a heat preservation mode: and when the electrolyte reaches the basic working temperature, controlling the heater to enter a heat preservation mode, and beginning to preserve heat of the electrolyte by the heater.
(9)3D printing and processing: starting a laser, a 3D printing system, an electrodeposition power supply and the like, and performing layer-by-layer printing processing on the workpiece;
(10) concentration compensation system: the printing is started to trigger the density compensation system, and the electromagnetic valve has two states in the compensation process. After the 3D printing process is started, the ion concentration in the electrolyte gradually decreases as the printing process progresses. Monitoring the electrolyte concentration in the electrolyte in real time by using a baume degree measuring instrument, wherein when the electrolyte concentration is higher than a set lower limit value, the electromagnetic valve keeps a closed state, and the printing process is continuously carried out; when the electrolyte concentration is lower than the set lower limit value, the electromagnetic valve is opened to carry out concentration compensation, and the printing process is interrupted. The electrolyte concentration in the electrolyte water tank is increased along with the addition of the high-concentration electrolyte, and if the electrolyte concentration does not reach the set upper limit value, the electromagnetic valve is kept in an open state, and concentration compensation is continuously carried out; when the electrolyte concentration reaches the set upper limit value, the electromagnetic valve is closed, the concentration compensation is stopped, and the laser beam resumes the printing process from the breakpoint. The two states of the electromagnetic valve are circularly carried out, so that the concentration of the electrolyte in the electrolyte is always in a control range.
The concentration compensation process of the present invention is further illustrated below with reference to specific examples:
example 1:
the concentration compensation method of the invention is explained in detail by taking the preparation of a cuboid three-dimensional nickel structure with the length of 12mm, the width of 8mm and the height of 1mm as an example shown in figure 5.
1. Setting a displacement starting input pump: setting the flow of the electrolytic cell to be 400ml/min according to the process requirement, and opening the input pump to quickly fill the electrolytic cell with electrolyte;
2. raising to the liquid level, limiting and starting a liquid discharge pump: when the electrolyte rises to the liquid level limit position, the electrolyte overflow can be observed, at the moment, the liquid discharge pump is started, and the discharge capacity is set to be gradually increased;
3. observing inflow and outflow: when the data of the flow meter is observed to meet the condition that 0ml < inflow-outflow <4ml, the electrolyte in the electrolytic cell is considered to realize dynamic balance, and the next link can be entered; if not, continuing to wait for the increase of the discharge capacity of the liquid discharge pump;
4. keeping the negative plate of the discharge capacity of the two pumps to zero: when the electrolytic bath realizes dynamic balance, the discharge capacity of the two pumps is kept unchanged. Slowly descending the cathode plate, contacting the cathode with the electrolyte, and braking the cathode plate by the control card; adjusting the focal length of the laser to enable the focal point of the laser to fall on the surface of the cathode substrate;
5. setting the working temperature of the electrolyte: setting the working temperature of the electrolyte to be 38 ℃ according to the process requirement;
6. starting a heating mode: and after the working temperature of the electrolyte is set, controlling the heater to enter a heating mode, and starting heating the electrolyte by the heater.
7. Observing the temperature of the plating solution in the electrolytic bath: when the temperature of the electrolyte in the electrolytic cell is higher than 36.1 ℃, the electrolyte is considered to basically reach the working temperature, and the next link can be entered; if not, the heating mode is continued.
8. Starting a heat preservation mode: and when the electrolyte reaches the basic working temperature, controlling the heater to enter a heat preservation mode, and beginning to preserve heat of the electrolyte by the heater.
9.3D printing: starting a laser, a 3D printer, an electrodeposition power supply and the like, and performing layer-by-layer printing and processing on the workpiece;
10. concentration compensation: the compensated process solenoid valve includes two states: after 3D printing processing is started, the concentration of NiSiO4 in the electrolyte is gradually reduced, and when the concentration of NiSiO4 is lower than 160g/L, the solenoid valve is opened to compensate the concentration, and the printing process is interrupted; if the pressure is not lower than 160g/L, the electromagnetic valve keeps a closed state. With the addition of high-concentration electrolyte, the ion concentration in the solution is increased, when the concentration of NiSiO4 is higher than 190g/L, the electromagnetic valve is closed to stop concentration compensation, and the laser beam resumes printing processing from the breakpoint; if the pressure is not higher than 190g/L, the electromagnetic valve is kept in an open state. Two states of the electromagnetic valve are carried out in sequence, so that the concentration of NiSiO4 in the electrolyte is always 160 g/L-190 g/L.
Example 2:
the concentration compensation method of the present invention will be described in detail by taking the preparation of a three-dimensional nickel structure with a circular ring pattern having a height of 1mm, an inner diameter of 10mm and an outer diameter of 11mm as an example shown in FIG. 6.
1. Setting a displacement starting input pump: setting the flow of the electrolytic cell to be 350ml/min according to the process requirements, and opening the input pump to quickly fill the electrolytic cell with electrolyte;
2. raising to the liquid level, limiting and starting a liquid discharge pump: when the electrolyte rises to the liquid level limit position, the electrolyte overflow can be observed, at the moment, the liquid discharge pump is started, and the discharge capacity is set to be gradually increased;
3. observing inflow and outflow: when the data of the flow meter is observed to meet the condition that 0ml < inflow-outflow <3.5ml, the electrolyte in the electrolytic cell is considered to realize dynamic balance, and the next link can be entered; if not, continuing to wait for the increase of the discharge capacity of the liquid discharge pump;
4. keeping the negative plate of the discharge capacity of the two pumps to zero: when the electrolytic bath realizes dynamic balance, the discharge capacity of the two pumps is kept unchanged. Slowly descending the cathode plate, contacting the cathode with the electrolyte, and braking the cathode plate by the control card; adjusting the focal length of the laser to enable the focal point of the laser to fall on the surface of the cathode substrate;
5. setting the working temperature of the electrolyte: setting the working temperature of the electrolyte to be 38 ℃ according to the process requirement;
6. starting a heating mode: and after the working temperature of the electrolyte is set, controlling the heater to enter a heating mode, and starting heating the electrolyte by the heater.
7. Observing the temperature of the plating solution in the electrolytic bath: when the temperature of the electrolyte in the electrolytic cell is higher than 36.1 ℃, the electrolyte is considered to basically reach the working temperature, and the next link can be entered; if not, the heating mode is continued.
8. Starting a heat preservation mode: and when the electrolyte reaches the basic working temperature, controlling the heater to enter a heat preservation mode, and beginning to preserve heat of the electrolyte by the heater.
9.3D printing: starting a laser, a 3D printer, an electrodeposition power supply and the like, and performing layer-by-layer printing and processing on the workpiece;
10. concentration compensation: the compensated process solenoid valve includes two states: after 3D printing processing is started, the concentration of NiSiO4 in the electrolyte is gradually reduced, when the concentration of NiSiO4 is lower than 160g/L, the electromagnetic valve is opened to compensate the concentration, and the printing process is interrupted at the moment; if the pressure is not lower than 160g/L, the electromagnetic valve keeps a closed state. With the addition of high-concentration electrolyte, the ion concentration in the solution is increased, when the concentration of NiSiO4 is higher than 190g/L, the electromagnetic valve is closed to stop concentration compensation, and the laser beam resumes printing processing from the breakpoint; if the pressure is not higher than 190g/L, the electromagnetic valve is kept in an open state. The two states of the electromagnetic valve are carried out in sequence, so that the concentration of NiSiO4 in the electrolyte is always 160 g/L-190 g/L.
Example 3:
the concentration compensation method of the present invention will be described in detail by taking the preparation of a hemispherical three-dimensional copper structure with a radius of 10mm as an example shown in fig. 7.
1. Setting a displacement starting input pump: setting the flow of the electrolytic tank to be 250ml/min according to the process requirements, and opening the input pump to quickly fill the electrolytic tank with electrolyte;
2. raising to the liquid level, limiting and starting a liquid discharge pump: when the electrolyte rises to the liquid level limit position, the electrolyte overflow can be observed, at the moment, the liquid discharge pump is started, and the discharge capacity is set to be gradually increased;
3. observing inflow and outflow: when the data of the flow meter is observed to meet the conditions that the flow rate is more than 0ml and the inflow rate is less than 3ml, the electrolyte in the electrolytic cell is considered to realize dynamic balance, and the next link can be entered; if not, continuing to wait for the increase of the discharge capacity of the liquid discharge pump;
4. keeping the negative plate of the discharge capacity of the two pumps to zero: when the electrolytic bath realizes dynamic balance, the discharge capacity of the two pumps is kept unchanged. Slowly descending the cathode plate, contacting the cathode with the electrolyte, and braking the cathode plate by the control card; adjusting the focal length of the laser to enable the focal point of the laser to fall on the surface of the cathode substrate;
5. setting the working temperature of the electrolyte: setting the working temperature of the electrolyte to be 40 ℃ according to the process requirement;
6. starting a heating mode: and after the working temperature of the electrolyte is set, controlling the heater to enter a heating mode, and starting heating the electrolyte by the heater.
7. Observing the temperature of the plating solution in the electrolytic bath: when the temperature of the electrolyte in the electrolytic cell is higher than 38 ℃, the electrolyte is considered to basically reach the working temperature, and the next link can be entered; if not, the heating mode is continued.
8. Starting a heat preservation mode: and when the electrolyte reaches the basic working temperature, controlling the heater to enter a heat preservation mode, and beginning to preserve heat of the electrolyte by the heater.
9.3D printing: starting a laser, a 3D printer, an electrodeposition power supply and the like, and performing layer-by-layer printing and processing on the workpiece;
10. concentration compensation: the compensation process comprises two steps: after 3D printing processing is started, the concentration of CuSiO4 in the electrolyte is gradually reduced, when the concentration of CuSiO4 is lower than 140g/L, an electromagnetic valve is opened for concentration compensation, and the printing process is interrupted at the moment; if the pressure is not lower than 140g/L, the electromagnetic valve keeps a closed state. With the addition of the high-concentration electrolyte, the ion concentration in the solution is increased, when the concentration of CuSiO4 is higher than 170g/L, the electromagnetic valve is closed to stop concentration compensation, and the laser beam resumes printing processing from the breakpoint; if the pressure is not higher than 170g/L, the electromagnetic valve is kept in an open state. The two steps are carried out in sequence, so that the concentration of CuSiO4 in the electrolyte is 140 g/L-170 g/L all the time.
Example 4:
the concentration compensation method of the present invention is described in detail by taking the preparation of a three-dimensional copper structure with a cylindrical and spherical copper hollow sealed cavity with an outer diameter of 10mm and a height of 8mm, a wall thickness of 1mm and a bottom thickness of 1mm as an example, as shown in fig. 8.
1. Setting a displacement starting input pump: setting the flow of the electrolytic cell to be 280ml/min according to the process requirement, and opening the input pump to quickly fill the electrolytic cell with electrolyte;
2. raising to the liquid level, limiting and starting a liquid discharge pump: when the electrolyte rises to the liquid level limit position, the electrolyte overflow can be observed, at the moment, the liquid discharge pump is started, and the discharge capacity is set to be gradually increased;
3. observing inflow and outflow: when the data of the flow meter is observed to meet the conditions that the flow rate is more than 0ml and the inflow rate is less than 3ml, the electrolyte in the electrolytic cell is considered to realize dynamic balance, and the next link can be entered; if not, continuing to wait for the increase of the discharge capacity of the liquid discharge pump;
4. keeping the negative plate of the discharge capacity of the two pumps to zero: when the electrolytic bath realizes dynamic balance, the discharge capacity of the two pumps is kept unchanged. Slowly descending the cathode plate, contacting the cathode with the electrolyte, and braking the cathode plate by the control card; adjusting the focal length of the laser to enable the focal point of the laser to fall on the surface of the cathode substrate;
5. setting the working temperature of the electrolyte: setting the working temperature of the electrolyte to be 40 ℃ according to the process requirement;
6. starting a heating mode: and after the working temperature of the electrolyte is set, controlling the heater to enter a heating mode, and starting heating the electrolyte by the heater.
7. Observing the temperature of the plating solution in the electrolytic bath: when the temperature of the electrolyte in the electrolytic cell is higher than 38 ℃, the electrolyte is considered to basically reach the working temperature, and the next link can be entered; if not, the heating mode is continued.
8. Starting a heat preservation mode: and when the electrolyte reaches the basic working temperature, controlling the heater to enter a heat preservation mode, and beginning to preserve heat of the electrolyte by the heater.
9.3D printing: starting a laser, a 3D printer, an electrodeposition power supply and the like, and performing layer-by-layer printing and processing on the workpiece;
10. concentration compensation: the compensation process comprises two steps: after 3D printing processing is started, the concentration of CuSiO4 in the electrolyte is gradually reduced, when the concentration of CuSiO4 is lower than 140g/L, an electromagnetic valve is opened for concentration compensation, and the printing process is interrupted at the moment; if the pressure is not lower than 140g/L, the electromagnetic valve keeps a closed state. With the addition of the high-concentration electrolyte, the ion concentration in the solution is increased, when the concentration of CuSiO4 is higher than 170g/L, the electromagnetic valve is closed to stop concentration compensation, and the laser beam resumes printing processing from the breakpoint; if the pressure is not higher than 170g/L, the electromagnetic valve is kept in an open state. The two steps are carried out in sequence, so that the concentration of CuSiO4 in the electrolyte is 140 g/L-170 g/L all the time.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the concentration compensation mode adopted by the invention has the advantages of rapid ion concentration supplement and no impurity generation in the supplement process.
Secondly, the electrolyte circulation of the invention can drive the electrolyte to flow, thereby generating stirring effect, helping the ions near the cathode to diffuse, and solving the problem of low concentration of the cathode attached ions in the electrodeposition process.
The invention controls the liquid level of the electrolyte, and leads the cathode to be always in contact with only the bottom surface of the electrolyte, and only the bottom surface of the settled layer is in contact with the electrolyte in the printing process, thereby realizing the manufacture of the closed hollow part and reducing the deposition in the non-processing area.
The processing area of the workpiece printing mode is positioned in the electrolyte, inert gas is not needed to be introduced for protection, and the equipment and the process are simpler;
the invention mainly realizes printing in an electrodeposition mode, has low heat input and small heat influence, so that the internal stress of a workpiece is lower and the workpiece is not easy to deform and crack;
sixthly, the 3D printing scheme adopted by the invention is based on the reduction reaction of the electrolyte, and a powder laying link is not needed in the printing process, so that the processing efficiency is greatly improved;
the electrochemical deposition mode adopted by the invention has more excellent microstructure regulation and control performance, and crystal grain structures with different sizes and orientations can be obtained by regulating and controlling process parameters, so that the mechanical performance of the crystal grain structures is controlled;
and the parts adopted by the invention are printed in an inverted mode, so that the manufacturing of the closed hollow parts can be realized.
In the present specification, the embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The principle and the embodiment of the present invention are explained by applying specific examples, and the above description of the embodiments is only used to help understanding the method and the core idea of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (9)
1. An automatic circulating electrolyte concentration compensating device, comprising:
the electrolytic bath is provided with an electrolyte inlet and an electrolyte outlet;
the electrolyte circulating water tank is provided with a circulating electrolyte recycling port and a circulating electrolyte outlet, the circulating electrolyte recycling port is communicated with the electrolyte outlet, and the circulating electrolyte outlet is communicated with the electrolyte inlet;
the baume degree measuring instrument is arranged inside the electrolyte circulating water tank and used for detecting the concentration of the electrolyte;
and the electrolyte compensation system is communicated with the electrolyte circulating water tank and is used for performing concentration compensation on the electrolyte in the electrolyte circulating water tank according to the concentration of the electrolyte.
2. The automatic circulating electrolyte concentration compensating device of claim 1 wherein an electrolyte heater, a first baffle and a second baffle are further disposed in the electrolyte circulating tank;
the lower extreme of first baffle has first breach, the upper end of second baffle has the second breach, electrolyte heater sets up in the passageway that first breach and second breach constitute.
3. The automatic circulating electrolyte concentration compensating device of claim 1, wherein an electrolyte tank temperature measuring instrument is further arranged on one side of the circulating electrolyte outlet.
4. The automatic circulating electrolyte concentration compensating apparatus of claim 1 wherein the electrolyte compensating system comprises:
the electrolyte tank is provided with an electrolyte tank liquid outlet, and the electrolyte tank liquid outlet is communicated with the electrolyte circulating water tank; a new electrolyte is arranged in the electrolyte water tank;
and the electromagnetic valve is arranged on one side of the liquid outlet of the electrolyte tank and used for regulating and controlling the valve according to the concentration of the electrolyte and enabling new electrolyte to flow into the electrolyte circulating tank so as to enable the concentration of the electrolyte in the electrolyte circulating tank to be unchanged.
5. The automatic circulating electrolyte concentration compensating apparatus of claim 1 wherein the electrolytic cell comprises:
the bottom of the electrolytic cell box body is made of optical high-transmittance glass;
and the liquid level limiting water outlet is arranged on one side of the electrolytic tank body.
6. The automatic circulating electrolyte concentration compensating device of claim 1 wherein the electrolyte inlet is provided with an electrolyte inlet flow sensor; and an electrolyte outlet flow sensor is arranged on the electrolyte outlet.
7. The automatic circulating electrolyte concentration compensating apparatus of claim 1, further comprising:
a 3D printing system for completing 3D printing using an electrolytic bath; the 3D printing system comprises a Z-direction movement device, an anode substrate and a laser; the Z-direction movement device is connected with the cathode substrate and is used for controlling the cathode substrate to lift; the anode substrate is arranged inside the electrolytic cell; the laser is arranged at the bottom of the electrolytic tank and used for irradiating the cathode substrate with laser to carry out electrochemical deposition.
8. The automatic circulating electrolyte concentration compensating apparatus of claim 7, further comprising:
and the cathode of the electrochemical machining power supply is connected with the cathode substrate, and the anode of the electrochemical machining power supply is connected with the anode substrate.
9. An automatic circulating electrolyte concentration compensation method is characterized by comprising the following steps:
step 1: introducing electrolyte into the electrolytic cell by using an electrolyte circulating water tank;
step 2: judging whether the difference between the inflow amount of the electrolyte inlet and the outflow amount of the electrolyte outlet is within a preset range;
and step 3: when the difference between the inflow and outflow is in a preset range, adjusting the focal length of the laser to enable the focal point of the laser to fall on the surface of the cathode substrate;
and 4, step 4: heating the electrolyte to a preset temperature by using an electrolyte heater;
and 5: the 3D printing system performs 3D printing by using an electrolytic bath;
step 6: in the 3D printing process, the electrolyte concentration in the electrolyte is monitored in real time, when the electrolyte concentration is lower than a set lower limit, the electromagnetic valve is opened, and the high-concentration electrolyte is injected into the circulating water tank to compensate the concentration of the electrolyte; when the electrolyte concentration is not lower than the lower limit, the electromagnetic valve keeps a closed state, and no high-concentration electrolyte is injected into the water tank.
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