CN114910114A - Online in-situ monitoring device for internal stress of plating layer and pH of plating solution in electroforming process - Google Patents
Online in-situ monitoring device for internal stress of plating layer and pH of plating solution in electroforming process Download PDFInfo
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- CN114910114A CN114910114A CN202110169482.3A CN202110169482A CN114910114A CN 114910114 A CN114910114 A CN 114910114A CN 202110169482 A CN202110169482 A CN 202110169482A CN 114910114 A CN114910114 A CN 114910114A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
- G01D21/00—Measuring or testing not otherwise provided for
- G01D21/02—Measuring two or more variables by means not covered by a single other subclass
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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
- C25D1/00—Electroforming
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- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D27/00—Simultaneous control of variables covered by two or more of main groups G05D1/00 - G05D25/00
- G05D27/02—Simultaneous control of variables covered by two or more of main groups G05D1/00 - G05D25/00 characterised by the use of electric means
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- Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
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Abstract
The invention provides an in-situ online monitoring device for coating internal stress and bath pH in an electroforming process, which comprises a measuring electroforming tank, a real-time stress observation platform, a pH measuring device and a circulating liquid flow path, wherein the measuring electroforming tank is provided with a bottom plate, a cathode chamber, an anode chamber and a connecting channel; the real-time stress observation platform is arranged on the side face right facing the cathode chamber, and the pH measuring device is communicated with the anode chamber through a pH real-time monitoring passage. The invention can eliminate the influence of edge effect to the maximum extent by improving the coating stress electroforming tank, and can realize the online in-situ monitoring of the coating stress and the pH value of the plating solution by matching with the in-situ stress test platform and the liquid flow pipeline passage.
Description
Technical Field
The invention belongs to the field of electroforming chemistry, and particularly relates to an online in-situ monitoring device for internal stress of a coating and pH of a plating solution in an industrial electroforming process.
Background
With the rapid development of deep space exploration technology, pulsar navigation and astronomical observation technology, people have increasingly greater demands on high-efficiency and high-performance X-ray telescopes. At present, the lens of an X-ray telescope mainly adopts a Wolter-I type electroformed lens, and the main preparation process comprises the steps of processing an aluminum mandrel, chemically plating Ni-P alloy on the surface of the mandrel, ultra-fine cutting and polishing the surface of the mandrel, sputtering a gold film on the surface, electroforming a zero-stress nickel or nickel-cobalt alloy lens, separating the lens from the mandrel and the like. One of the difficulties is the high precision, low stress electroforming nickel cobalt lens technology.
After a gold film is plated on the surface of the super-smooth core mould through magnetron sputtering, the super-smooth core mould needs to be immersed into nickel or nickel-cobalt electroplating solution for electroforming, and the electroformed lens needs to meet the requirements of low stress, high precision and high strength. If the stress of the electroforming layer (lens) is overlarge in the electroforming process, on one hand, the lens is deformed, and the surface accuracy cannot meet the design requirement; on the other hand, the mechanical properties of the lens are affected by excessive stress. It is therefore important to control the electroforming layer (lens) stress during electroforming.
In conventional industrial electroforming stress control, a stress test is usually performed by taking out a part of an electroforming solution from an industrial electroforming tank before electroforming, and the stress is not measured on-line. On one hand, the precision of the stress control of the method is poor, the time of the industrial electroforming is usually more than 24h, and the time of the stress test is usually 1h, so that the stress test can only represent the stress condition in the early stage of the industrial electroforming, and the stress change in the later stage of the industrial electroforming can only be predicted through experience; on the other hand, as the electroforming solution is analyzed after each electroforming is finished, the electroforming of the next mandrel can be carried out only after the stress test result is obtained; secondly, the flexibility of the stress test is poor, and the method can not monitor the stress in the electroforming process in real time and can not properly correct the electroforming parameters in the electroforming process.
Meanwhile, the current common online stress testing method is mainly a cathode bending method, in-situ observation is carried out on a cathode test piece by an auxiliary means, and stress calculation is carried out on the observed data by applying a Stoney formula. However, in many methods, the effect of edge effects on the cathode stress test is not considered. In fact, in the electroforming process, due to the influence of the edge effect, the electric lines of force at the edge of the cathode test piece are denser, the current density is higher, and the measurement of the cathode stress is greatly influenced, and the influence is larger when the coating thickness is thicker.
In addition, the pH value of the electrocasting solution is constantly changing during electrocasting. Generally, although the electroforming solution contains a buffer, the surface area of the cathode mandrel is large, hydrogen ions are consumed in the hydrogen evolution reaction of the cathode, and the pH of the electroforming solution increases. And in each electroforming process, the surface areas of the cathode mandrels are different, the adopted current densities are different, and the rising speeds of the pH value are different. In order to maintain the pH of the electrocasting solution constant, it is necessary to monitor the pH of the electrocasting solution in real time during the electrocasting process. However, the electric field in the electrocasting solution affects the zero point potential of the pH electrode, so that the measured value of the pH electrode is greatly fluctuated and deviated, and thus the pH electrode cannot be directly inserted into the electrocasting solution for measurement, and the electrocasting solution needs to be taken out and then measured.
Disclosure of Invention
In view of the above, the present invention is directed to provide an online in-situ monitoring device for internal stress of a plating layer and pH of a plating solution during electroforming, which can eliminate the influence of edge effect to the maximum extent by improving a plating layer stress electroforming tank, and can realize online in-situ monitoring for the plating layer stress and the pH of the plating solution by matching with an in-situ stress testing platform and a liquid flow pipeline passage.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
an in-situ monitor for the internal stress of plating layer and pH value of plating solution in electrocasting procedure includes a measuring electrocasting tank with bottom plate, cathode chamber, anode chamber and connecting channel, a real-time stress observation platform for capturing the dynamic change of cathode specimen, a pH measuring device for real-time pH monitoring, and a circulating liquid flow path for connecting the measuring electrocasting tank with industrial electrocasting tank; the real-time stress observation platform is arranged on the side face right facing the cathode chamber, and the pH measuring device is communicated with the anode chamber through a pH real-time monitoring passage.
Furthermore, the main body of the measuring electroforming tank is in a convex shape, wherein the small end of the convex shape is a cathode chamber, the large end of the convex shape is an anode chamber, the side surface of the cathode chamber is also connected with a fixed plate, and the real-time stress observation platform is arranged on the fixed plate; a concave socket is formed in the upper end face of the cathode chamber, a cathode clamp is matched at the concave socket and comprises a short-edge T-shaped plate and a long-edge T-shaped plate with a square through hole, and the cathode test piece and the two T-shaped plates are inserted into the concave socket to be fixed in a sandwich interlayer mode; the side of the cathode chamber is provided with scales, and two ends of each scale are respectively provided with a long vertical line mark.
Furthermore, a square groove and a step are formed in the communication position of the cathode chamber and the anode chamber on the bottom plate, the square groove is a fixing groove of the connecting channel, the step and the connecting channel form a bottom fixing groove of the long-side T-shaped plate, and a square ring fixing frame is further arranged on the inner side wall, far away from the cathode chamber, of the anode chamber and used for fixing the anode plate; the connecting channel is a square channel, and the shape of a square through hole of the square channel is the same as that of the cathode test piece; the cathode test piece substrate is a silicon wafer, and one surface of the silicon wafer is deposited with a layer of gold film in a magnetron sputtering mode.
Furthermore, the upper part of the long-side T-shaped plate is T-shaped, the shape and the size of the upper part of the long-side T-shaped plate are consistent with those of the short-side T-shaped plate, the lower part of the long-side T-shaped plate is U-shaped, and the thickness of the lower part of the long-side T-shaped plate extends outwards to be twice of the thickness of the upper part; one side of the short-side T-shaped plate is pasted with a titanium sheet, one side of the titanium sheet extends out of the T-shaped plate, the cathode test piece is arranged on the long-side T-shaped plate, the square deposition area of the cathode test piece and the square through hole of the long-side T-shaped plate are in a coincident state, and the side edge of the cathode test piece is not in contact with the side wall of the square through hole of the long-side T-shaped plate.
Furthermore, the real-time stress observation platform comprises a circular light source, a lens, a CCD camera, an L-shaped connecting plate and a computer, wherein a circular observation port is formed in the short edge of the L-shaped connecting plate, an arc-shaped hole and a plurality of through holes are formed in the long edge of the L-shaped connecting plate, the L-shaped connecting plate is adjusted through the arc-shaped hole and the through holes and is fixed on a fixing plate on the side face of the cathode chamber, the lens is connected with the CCD camera and is installed on the long edge of the L-shaped plate, and the lens points to the circular observation port; the circular light source is arranged on the outer side of the short side of the L-shaped connecting plate and is coaxially arranged with the circular observation port, and image data of the cathode test piece observed by the CCD camera is transmitted to the computer through the data line.
Furthermore, the stress observation platform is positioned and calibrated through the long vertical line on the side surface of the cathode chamber; the image data observed by the stress observation platform is the displacement value of each point on the side edge of the lower half part of the cathode test piece; and fitting the displacement value by software to obtain a curvature value.
Further, pH measuring device includes overflow joint, pH electrode, stock solution overflow ware and first circulating pump, the lower extreme of stock solution overflow ware is the feed liquor end, and the middle-end is the overflow end, and the upper end is pH measurement port, the pH electrode is inserted at pH measurement port, is equipped with the overflow joint at the overflow end, stock solution overflow ware lower extreme with first circulating pump intercommunication, first circulating pump passes through pH real-time supervision route and anode chamber intercommunication.
Furthermore, three bottom through openings and three square grooves are formed in one side of a bottom plate of the electroplating bath, each bottom through opening corresponds to one square groove, the bottom through openings are communicated with the corresponding square grooves, two upper through openings are formed in the side wall of the anode chamber, and the through openings are connected in a sealing mode through silica gel plugs with different apertures;
the upper port of the anode chamber close to the cathode and the bottom port of the bottom plate close to the anode are connected with the industrial electroforming tank; an upper port close to the anode on the anode chamber is connected with a bottom opening close to the cathode on the bottom plate and a pH real-time monitoring passage; and a heating rod is inserted into the opening at the bottom in the middle of the bottom plate and is connected with a temperature controller.
Further, the pH real-time monitoring passage comprises a valve and a plurality of silicone tubes, a first threaded pagoda joint of the valve is connected with a second threaded pagoda joint of the pH measuring device through the silicone tubes, and an overflow joint of the pH measuring device is connected with an upper port, close to the anode, of the side wall of the anode chamber through a liquid inlet joint and the silicone tubes to form the pH real-time monitoring passage.
Furthermore, the circulation liquid flow path comprises a second valve, a second circulating pump and a plurality of silicone tubes, a third threaded pagoda joint of the second valve is connected with a fourth threaded pagoda joint through the silicone tubes, the fourth threaded pagoda joint is connected with the water outlet end of the second circulating pump, the water inlet end of the second circulating pump is connected with a fifth threaded pagoda joint, the fifth threaded pagoda joint is connected with the industrial electroforming tank through the silicone tubes, meanwhile, the industrial electroforming tank is connected with an overflow joint through the silicone tubes, the overflow joint is communicated with an upper opening, close to the cathode, of the side wall of the anode chamber, and the circulation path for measuring electroforming liquid of the electroforming tank and the industrial electroforming tank is formed.
Compared with the prior art, the online in-situ monitoring device for the internal stress of the plating layer and the pH value of the plating solution in the electroforming process has the following advantages:
the device can be used as a device for testing the in-situ stress and the pH value in real time, can be matched with an automatic control system, automatically adjusts the current and the pH value in the electroforming process through a controller and software according to the tested stress and the pH value, adjusts process parameters at any time, and stably controls the product quality.
When the real-time in-situ stress and pH online measuring device is used, the second circulating pump pumps the electroforming solution in the industrial electroforming tank into the measuring electroforming tank, the electroforming solution in the measuring electroforming tank flows into the industrial electroforming tank again from the overflow port after being filled with the electroforming solution, and the temperature control system in the measuring electroforming tank is used for auxiliary heating, so that the temperature in the measuring electroforming tank is kept consistent with the temperature of the industrial electroforming tank; simultaneously, the first circulating pump starts to work, and electroforming liquid in the measurement electroforming tank returns to the measurement electroforming tank through the first circulating pump in sequence through a water inlet at the lower end of the liquid storage overflow device, the liquid storage cavity and a middle-end overflow port; an opening at the upper end of the liquid storage overflow device is a pH electrode socket for measuring pH; after the whole testing device is in a stable state, assembling the cathode test piece and the cathode clamp in a sandwich manner, and inserting the cathode test piece into the concave socket at the upper end of the cathode chamber for fixing; and switching on a power supply, observing the bending deformation condition of the cathode sheet at any time through a CCD (charge coupled device) camera on the side surface when the cathode is turned on, and calculating the in-situ stress through a computer.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention, illustrate embodiments of the invention and together with the description serve to explain the invention and do not constitute a limitation of the invention. In the drawings:
FIG. 1 is a schematic structural diagram of an in-situ online monitoring device for in-plating stress and plating solution pH during electroforming, according to an embodiment of the present invention;
FIG. 2 is a schematic view of a measuring electroforming tank in an online in-situ monitoring device for internal stress of a plating layer and pH of a plating solution during electroforming according to an embodiment of the present invention;
FIG. 3 is an exploded view of an in-situ online monitoring device for the in-plating stress and the pH of the plating solution during electroforming (excluding a pH measuring device) according to an embodiment of the present invention;
fig. 4 is an exploded view of a pH measurement device in an online in-situ monitoring device for the internal stress of the plating layer and the pH of the plating solution during electroforming according to an embodiment of the present invention.
Description of reference numerals:
10-measuring the size of the electroforming bath,
11-cathode chamber, 111-cathode test block, 112-short side T-shaped plate, 113-long side T-shaped plate, 12-anode chamber, 121-anode plate, 13-connecting channel, 14-first valve, 141-first threaded pagoda joint, 142-connecting valve, 144-port silica gel plug I, 15-second valve, 151-third threaded pagoda joint, 16-liquid inlet joint, 17-overflow joint, 171-straight joint, 172-port silica gel plug II, 18-fixing plate and 181-threaded through hole; 101-concave socket, 102-bottom port one, 103-bottom port two, 104-bottom port three, 105-upper port one, 106-upper port two, 107-step, 108-square groove, 109-square ring holder, 1010-bottom plate;
20-heating rod;
30-a pH measuring device for measuring the pH value,
31-an overflow joint, 32-a second threaded pagoda joint, 33-a pH electrode, 34-an annular top cover, 35-a liquid storage overflow device and 36-a first circulating pump;
40-a second circulating pump, 41-a fifth threaded pagoda joint, 42-a fourth threaded pagoda joint;
50-a real-time stress observation platform,
51-annular light source, 52-L-shaped connecting plate, 521-arc-shaped hole, 522-through hole, 53-lens and 54-CCD camera.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
In addition, the industrial electroforming cell mentioned in the embodiment of the present invention is generally specially designed according to its production task, and the present invention is focused on the measurement electroforming cell, which has no special requirement for the industrial electroforming cell, and is an existing structure, so the drawing does not give a schematic view of the industrial electroforming cell.
The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
As shown in fig. 1 to 4, an in-situ online monitoring device for internal stress of plating layer and pH of plating solution during electroforming process comprises a measuring electroforming tank 10 having a bottom plate 1010, a cathode chamber 11, an anode chamber 12 and a connecting channel 13, a real-time stress observation platform 50 capable of capturing dynamic changes of a cathode test piece 111, a pH measuring device 30 capable of realizing real-time pH monitoring, and a circulating fluid passage for communicating the measuring electroforming tank 10 with an industrial production electroforming tank; the real-time stress observation platform 50 is arranged at the side opposite to the cathode chamber 11, and the pH measuring device 30 is communicated with the anode chamber 12 through a pH real-time monitoring passage;
the main body of the measuring electroforming tank 10 is in a convex shape, wherein the small end of the convex shape is a cathode chamber 11, the large end of the convex shape is an anode chamber 12, the side surface of the cathode chamber 11 is also connected with a fixing plate 18, and the real-time stress observation platform 50 is arranged on the fixing plate 18; a concave socket 101 is formed in the upper end face of the cathode chamber 11, a cathode clamp is matched with the concave socket 101 and comprises a short-side T-shaped plate 112 and a long-side T-shaped plate 113 with a square through hole, and a cathode test block 111 and the two T-shaped plates are inserted into the concave socket to be fixed in a sandwich interlayer mode; the surface of the T-shaped plate with the titanium sheet is contacted with the conductive surface of the cathode sheet. The titanium sheet mainly serves as a lead, current is connected and conducted with a cathode wire on a power supply through the titanium sheet with the length of 1cm extending out of the T-shaped plate, and the corrosion of the cathode wire of the power supply can be effectively prevented due to the fact that the connecting position is located on the outer side of the electroforming tank; the side of the cathode chamber 11 is provided with scales, and two ends of each scale are respectively provided with a long vertical line mark for positioning and measuring an industrial CCD camera, the positions of the scales are flush with the lower end of the cathode test piece, and the scales or the cathode test piece are prevented from exceeding the visual angle range when the camera is used for observing.
The material of the measurement electroforming tank 10 can adopt polyvinyl chloride, tetrafluoroethylene, organic glass and the like, preferably, the organic glass has high hardness, high corrosion resistance and easy adhesion; meanwhile, the organic glass has various colors and varieties and can meet different requirements. Preferably, the cathode chamber 11 can be made of transparent organic glass, so that on one hand, the light-transmitting effect is good, and the observation is easy; on the other hand, the price is cheap and the processing is easy. The side wall of the cathode chamber can adopt organic glass with the thickness of 5mm and 10mm, preferably 5mm, and can have higher light transmission under the condition of meeting the strength requirement. The selected material can be processed by laser cutting, milling cutter cutting and linear cutting. Taking the organic glass as an example, the processing mode of 'wire cutting' is preferred, and the organic glass processed by the wire cutting has higher precision. The processed and formed organic glass is bonded into the measuring electroforming tank 10 by the special glue for the organic glass.
One side of the bottom plate 1010 of the measurement electroforming tank 10 is provided with three bottom ports and three corresponding square grooves, namely a first bottom port 102, a second bottom port 103 and a third bottom port 104, wherein the square groove distance corresponding to the first bottom port 102 and the third bottom port 104 is short, so that the effect of the electric casting liquid diversion is achieved, and the square groove distance corresponding to the second bottom port 103 is long and is used as a socket of a heating rod.
Two upper part ports are arranged on the side wall of the anode chamber, and the ports are connected in a sealing way through silica gel plugs with different apertures;
the upper port of the anode chamber close to the cathode and the bottom port of the bottom plate close to the anode are connected with the industrial electroforming tank; an upper port close to the anode on the anode chamber is connected with a bottom opening close to the cathode on the bottom plate and a pH real-time monitoring passage; and a heating rod is inserted into the bottom port in the middle of the bottom plate and is connected with the temperature controller.
The bottom plate 1010 of the measuring electroforming tank 10 is provided with a square groove 108 and a step 107, the square groove 108 is a fixing groove for the connecting channel 13, and the step 107 and the connecting channel 13 form a bottom fixing groove for the long-side T-shaped plate 113. The connecting channel 13 is a square channel, the length of the connecting channel is larger than 10cm, and the size and the shape of a square through hole of the connecting channel 13 are completely the same as those of a square cathode window of the long-side T-shaped plate. The connecting channel 13 has two main functions: firstly, the influence of the edge effect on the cathode plate during electroforming is weakened; and secondly, the disturbance of the electroforming liquid to the cathode test piece during circulation is reduced. The connecting channel is arranged in the square groove of the bottom plate, and the square channels with different square through holes are replaced, so that the connecting channel can be suitable for cathode test pieces with different sizes. The channel corresponds to the cathode strip, and a wider range of applications can be used.
The bottom plate 1010 of the measuring electroforming tank 10 is provided with a fixing plate 18 for fixing the real-time stress observation platform 50, and the fixing plate 18 is provided with a plurality of threaded through holes 181 with the spacing of 20mm, which correspond to the through holes 522 and the arc-shaped holes 521 on the connecting plate 52.
The measuring electroforming tank 10 includes a cathode chamber 11 having a symmetrical female socket 101 at an upper end thereof, serving as an upper end fixing groove for a short side T-shaped plate 112 and a long side T-shaped plate 113.
The side wall of the anode chamber 12 of the measuring electroforming tank 10 is provided with a first upper port 105 and a second upper port 106, wherein the second upper port 106 serves as an overflow port, and the first upper port 105 serves as a liquid inlet; the measuring electrocasting tank 10 includes an anode chamber having a square ring holder 109 for fixing an anode plate 121.
The first valve 14 is connected with a first bottom port 102 of the bottom plate 1010, the first valve 14 is composed of a first port silicone plug 144, a connecting valve 142 and two first threaded pagoda connectors 141, the first port silicone plug 144 is screwed into the first bottom port 102, a pagoda end of one first threaded pagoda connector is connected with the first port of the first port silicone plug 144, a threaded end is connected with one end of the connecting valve 142, the other end of the connecting valve 142 is connected with a threaded end of the other first threaded pagoda connector 141, and the first valve 14 is connected with the first bottom port 102. The second bottom port 103 of the bottom plate 1010 is connected with the heating rod 20, and the third bottom port 104 of the bottom plate 1010 is connected with the second valve 15 in the same way as the first valve 14.
And the second upper port 106 of the anode chamber 12 is connected with the overflow joint 17, the overflow joint 17 consists of a second through-hole silica gel plug 172 and a straight joint 171, the second through-hole silica gel plug 172 is rotatably plugged into the second upper port 106, and then the straight joint 171 is rotatably plugged into the second through-hole of the second through-hole silica gel plug 172 to complete connection. The first upper port 105 of the anode chamber 12 is connected to the inlet connection 16 in a manner consistent with the overflow connection 17. The square ring fixing frame 109 of the anode chamber 12 is used for installing the anode plate 121.
The cathode test piece 111 is a strip-shaped silicon oxide wafer with the thickness of 0.01mm, one surface of the silicon oxide wafer is deposited with a 50nm gold film in a magnetron sputtering mode, and the cathode test piece is divided into an upper flow guide area and a lower square deposition area by using insulating glue with the width of 2cm as a boundary line. The anode faces to the electroforming process, and the deposition surface of the metal ions is formed. According to the characteristics of the silicon oxide wafer, the back surface of the cathode plate is not conductive, and the whole deposition process is single-side electroplating; the upper part of the long-side T-shaped plate 113 is T-shaped, the shape and size of the upper part are the same as those of the short-side T-shaped plate 112, the lower part is U-shaped, and the thickness of the lower part of the long-side T-shaped plate extends outwards to be twice of that of the upper part. One surface of the short side T-shaped plate 112 is adhered with a titanium sheet, one side of the titanium sheet extends out of the T-shaped plate by 1cm, and the rest parts are overlapped; the cathode test block 111 is arranged on the long-side T-shaped plate 113, so that the square deposition area of the cathode test block 111 and the square through hole of the long-side T-shaped plate 113 are in a superposed state, but the side edge of the cathode test block 111 is not in contact with the side wall of the square through hole of the long-side T-shaped plate 113; the size of the periphery of a rectangular cathode window extending from the lower part of the long-edge T-shaped plate is slightly larger than that of the cathode test piece, and the exceeding value is about 0.1-0.2mm, so that the edge effect generated during electroforming is reduced as much as possible.
The bottom of the long-side T-shaped plate 113 is inserted into a square groove formed by the step 107 and the connecting channel 13, the upper part of the long-side T-shaped plate is overlapped with the concave socket 101, and the thickness of the upper part of the long-side T-shaped plate 113 is half of the width of the concave groove; the side of the short side T-shaped plate 112 adhered with the titanium sheet faces the upper long side T-shaped plate, and is inserted into the concave groove 101, and is just clamped with the long side T-shaped plate 113 to play a fixing role, and meanwhile, the side of the short side T-shaped plate 112 with the titanium sheet and the side of the cathode test piece 111 with the gold film are contacted to form a conduction path.
The real-time stress observation platform 50 comprises an L-shaped connecting plate 52, a light source 51, a lens 53 and a CCD camera 54, wherein a short plate of the L-shaped connecting plate 52 is provided with a round through opening, the diameter of the round through opening is slightly wider than that of the lens, and the light source 51 is arranged on the outer side of the short plate; the lens 53 is connected to the CCD camera 54 and fixed to the L-shaped plate 52, and the L-shaped plate 52 has an arc-shaped hole 521 and a through hole 522 corresponding to the through hole 181 of the fixing plate 18. An image observed by the CCD camera 54 is transmitted to a computer through a data line, after positioning and calibration are carried out on the image by visual measurement software through two vertical lines on the side surface of the cathode chamber, the displacement of the lower part of the cathode test piece 111 at the position of 2mm is measured in real time, data is stored, then the average curvature R is obtained through data fitting, and the R is substituted into a Stoney formula to obtain a stress value;
when the lens is fixed, firstly, a through hole 522 on the L-shaped connecting plate 52 and a threaded through hole 181 on the fixing plate 18 are selected to be fixed by an M8 screw, then, according to actual conditions, the lens angle is adjusted by taking the fixing point as the center of a circle, and finally, the lens is fixed with the connecting plate 18 by an M8 screw through the arc-shaped hole 521.
The pH measuring device 30 comprises a second threaded pagoda joint 32, a first circulating pump 36, a liquid storage overflow device 35, an overflow joint 31 and an annular top cover 34, the second threaded pagoda joint 32 is connected with the water inlet end of the first circulating pump 36, the water outlet end of the first circulating pump 36 is connected with the lower end of the liquid storage overflow device 35, the upper end of the first threaded pagoda joint is connected with the annular top cover 34, a through hole of the annular top cover 34 is used for a socket of a pH electrode 33, and the middle end of the liquid storage overflow device 35 is connected with the overflow joint 31. When the electroforming machine works, electroforming liquid sequentially passes through the second threaded pagoda joint 32, the first circulating pump 36 and the lower end of the liquid storage overflow device 35 to enter the containing cavity of the liquid storage overflow device 35, and flows out through the overflow joint 31 after the containing cavity is fully stored by the electroforming liquid. The zero point value of the pH meter is affected by the electric field during electroforming, and thus direct insertion of the pH electrode into the electroforming tank causes fluctuation and deviation of the measurement result. The water inlet end of the first circulating pump is connected with the opening of the bottom plate close to the anode end, and the water outlet end of the first circulating pump is connected with the lower end of the liquid storage overflow device; the middle end of the liquid storage overflow device is an overflow port, the first circulating pump pumps the electroforming liquid into the liquid storage overflow device to reach the position of a water outlet, the electroforming liquid flows out, and the liquid level is stable; the upper end is a pH meter socket, and a pH meter is inserted into the socket to obtain a numerical value.
The first threaded pagoda joint 141 of the first valve 14 is connected with the second threaded pagoda joint 32 of the pH measuring device 30 through a silicone tube, and the overflow joint 31 of the pH measuring device 30 is connected with the first upper port 105 of the side wall of the anode chamber 12 through the liquid inlet joint 16 and the silicone tube to form a liquid flow channel for pH measurement; a third threaded pagoda joint 151 of the second valve 15 is connected with a fourth threaded pagoda joint 42 through a silicone tube, the fourth threaded pagoda joint 42 is connected with a water outlet end of a second circulating pump 40, a water inlet end of the second circulating pump 40 is connected with a fifth threaded pagoda joint 41, and then the industrial electroforming tank is connected with the silicone tube, meanwhile, the industrial electroforming tank is also connected with an overflow joint 17, and the overflow joint 17 is communicated with a second upper through hole 106, so that a circulation passage for measuring electroforming tank and industrial electroforming tank electroforming liquid is formed.
The heating rod 20 is connected with a temperature controller, so that the temperature of the electroforming bath can be controlled; because the electrocasting solution is conducted into the measuring electrocasting tank 10 from the industrial electrocasting tank, and the temperature of the measuring electrocasting tank is lower, an auxiliary temperature control system is added. The heating rod 20 is connected to a temperature controller, which measures the temperature of the electrocasting solution by a temperature probe and controls the on/off of the heating rod 20 to control the temperature. The real-time stress observation platform 50 is connected with a computer and can observe and analyze the bending stress of the cathode test piece 111 on line; a 1cm titanium sheet extending out of the side surface of the short-side T-shaped plate 112 is connected with the anode of a power supply; the anode plate 121 is connected to the positive electrode of the power supply.
The working process of the monitoring device is as follows: after the plating solution in the industrial electroforming tank is heated to a preset temperature, opening a second circulating pump 40 to guide the electroforming solution into the measurement electroforming tank 10, and after the measurement electroforming tank 10 is filled with the plating solution, starting to flow into the industrial electroplating tank from the overflow joint 17, and adjusting a second valve 15 to ensure that the plating solution flows at a proper flow rate and in a laminar flow mode;
because the heating rod 20 is connected with the temperature controller, when the plating solution flows stably, the power supply of the temperature controller is turned on to perform auxiliary temperature control. Turning on the power supply of the first circulating pump 36 and the connecting valve 142 of the pH measuring device 30, starting to store the plating solution in the storage overflow device 35, and after a certain volume of the plating solution is reached, allowing the plating solution to flow out of the overflow joint 31; adjusting the connecting valve 142 to achieve a proper flow rate of the plating solution; the pH meter 33 is inserted into the upper end of the liquid storage overflow device 35 through the annular top cover 34 to start the real-time monitoring of the pH value;
the current guiding area above the cathode test block 111 and the insulating adhesive tape serving as a boundary are clamped between the upper parts of the short-side T-shaped plate 112 and the long-side T-shaped plate 113, and the surface coated with the gold film is opposite to the surface of the short-side T-shaped plate adhered with the titanium sheet, so that the cathode current can be conducted; the deposition area below the cathode test piece 111 is embedded into the square through hole below the long-side T-shaped plate 113, the shape of the deposition area is the same as that of the square hole, the size of the deposition area is slightly smaller than that of the square hole, and the deposition area and the square hole are basically superposed but not contacted, so that the edge effect of the cathode test piece can be reduced to the greatest extent under the condition of free bending; the bottom surfaces of the assembled cathode test piece 111, the short-side T-shaped plate 112 and the long-side T-shaped plate 113 are embedded into a square groove consisting of the step 107 and the connecting channel 13, the upper part of the square groove is inserted into the concave groove 101 of the cathode chamber 11, and the whole cathode is completely installed;
the side surface of the cathode chamber 11 is provided with scales, and two ends of the cathode chamber are respectively provided with a vertical red line; the light source 51, the lens 53, the CCD camera 54 and the connecting plate 52 form an integrated stress observation platform 50; the CCD camera 54 is aligned with a graduated face of the cathode chamber 11 and is positioned in a perpendicular relationship by adjustment of the connector plate 52. Before measurement, the computer calibrates the real size and the image size through scales and red lines of fixed distance on the side surface of the cathode chamber; during measurement, the horizontal distances from the left-end vertical red line and the right-end vertical red line to the cathode test piece 111 are measured respectively; one measuring point is arranged every 2mm at the lower half part of the cathode test piece 111, and the real-time bending curvature change of the cathode test piece is obtained by fitting the data. And finally, obtaining a real-time change curve of the coating stress through a Stoney formula. It should be noted that the stress measured before electroforming needs to be zeroed.
In this embodiment, the specific processing manner of the data observed by the stress observation platform is as follows:
step 1: and fitting the obtained data through software to obtain the bending curvature R of the cathode.
Step 2: and obtaining the thickness Hf of the electroformed layer at each moment through a conversion formula of the electric quantity and the thickness.
Formula i: :
in formula I, C represents the electric quantity of electroforming at each moment; m represents the molar mass of the deposited metal; n represents the valence of the deposit metal; f represents a Faraday constant; ρ represents the density of the deposited metal; s represents the area of the cathode coupon.
And step 3: and substituting the obtained curvature R and the thickness Hf of the electroformed layer into a Stoney formula to obtain a stress numerical value.
Formula ii:
formula II is Stoney formula, wherein E s 、V s The elastic modulus and the Poisson ratio of the silicon wafer are shown; h s Is the thickness of the silicon wafer.
In the embodiment, the power supply is a battery performance testing system, and different working steps can be set so as to adjust the electroforming process; the electrocast anode 121 is the same anode as an industrial electrocasting tank.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. An online in-situ monitoring device for coating internal stress and plating solution pH in an electroforming process is characterized in that: comprises a measuring electroforming groove with a bottom plate, a cathode chamber, an anode chamber and a connecting channel; the device comprises a real-time stress observation platform capable of capturing the dynamic change of a cathode test piece, a pH measuring device capable of realizing real-time pH monitoring and a circulating liquid flow path for communicating a measuring electroforming tank and an industrial production electroforming tank; the real-time stress observation platform is arranged on the side face right facing the cathode chamber, and the pH measuring device is communicated with the anode chamber through a pH real-time monitoring passage.
2. The on-line in-situ monitoring device for the internal stress of the coating and the pH value of the plating solution in the electroforming process according to claim 1, wherein: the main body of the measuring electroforming tank is in a convex shape, wherein the small end of the convex shape is a cathode chamber, the large end of the convex shape is an anode chamber, the side surface of the cathode chamber is also connected with a fixing plate, and the real-time stress observation platform is arranged on the fixing plate; a concave socket is formed in the upper end face of the cathode chamber, a cathode clamp is matched at the concave socket and comprises a short-edge T-shaped plate and a long-edge T-shaped plate with a square through hole, and the cathode test piece and the two T-shaped plates are inserted into the concave socket to be fixed in a sandwich interlayer mode; the side of the cathode chamber is provided with scales, and two ends of each scale are respectively provided with a long vertical line mark.
3. The on-line in-situ monitoring device for the internal stress of the coating and the pH value of the plating solution in the electroforming process according to claim 2, wherein: a square groove and a step are arranged at the communication position of the cathode chamber and the anode chamber on the bottom plate, the square groove is a fixing groove of the connecting channel, the step and the connecting channel form a bottom fixing groove of a long-side T-shaped plate, and a square ring fixing frame is further arranged on the inner side wall of the anode chamber, which is far away from the cathode chamber, and is used for fixing the anode plate; the connecting channel is a square channel, and the shape of a square through hole of the square channel is the same as that of the cathode test piece; the cathode test piece substrate is a silicon wafer, and one surface of the silicon wafer is deposited with a layer of gold film in a magnetron sputtering mode.
4. The on-line in-situ monitoring device for the internal stress of the coating and the pH value of the plating solution in the electroforming process according to claim 3, wherein: the upper part of the long-side T-shaped plate is T-shaped, the shape and the size of the upper part of the long-side T-shaped plate are consistent with those of the short-side T-shaped plate, the lower part of the long-side T-shaped plate is U-shaped, and the thickness of the lower part of the long-side T-shaped plate extends outwards to be twice of the thickness of the upper part; one surface of the short-edge T-shaped plate is adhered with a titanium sheet, and one side of the titanium sheet extends out of the T-shaped plate; the cathode test piece is arranged on the long-edge T-shaped plate, the square deposition area of the cathode test piece is in a superposed state with the square through hole of the long-edge T-shaped plate, and the side edge of the cathode test piece is not in contact with the side wall of the square through hole of the long-edge T-shaped plate.
5. The on-line in-situ monitoring device for the internal stress of the coating and the pH value of the plating solution in the electroforming process according to claim 1, wherein: the real-time stress observation platform comprises a circular light source, a lens, a CCD camera, an L-shaped connecting plate and a computer; a circular observation port is arranged on the short edge of the L-shaped connecting plate, an arc-shaped hole and a plurality of through holes are arranged on the long edge of the L-shaped connecting plate, the L-shaped connecting plate is fixed on a fixing plate on the side face of the cathode chamber through the arc-shaped hole and the through holes, the lens is connected with the CCD camera and is installed on the long edge of the L-shaped plate, and the lens points to the circular observation port; the circular light source is arranged on the outer side of the short side of the L-shaped connecting plate and is coaxially arranged with the circular observation port, and image data of the cathode test piece observed by the CCD camera is transmitted to the computer through a data line.
6. The on-line in-situ monitoring device for the internal stress of the coating and the pH value of the plating solution in the electroforming process according to claim 5, wherein: the stress observation platform is positioned and calibrated through the long vertical line on the side surface of the cathode chamber; the image data observed by the stress observation platform is the displacement value of each point on the lower half part side edge of the cathode test piece; and fitting the displacement value by software to obtain a curvature value.
7. The on-line in-situ monitoring device for the internal stress of the plating layer and the pH value of the plating solution in the electroforming process according to claim 1, wherein: the pH measuring device comprises an overflow joint, a pH electrode, a liquid storage overflow device and a first circulating pump, wherein the lower end of the liquid storage overflow device is a liquid inlet end, the middle end of the liquid storage overflow device is an overflow end, the upper end of the liquid storage overflow device is a pH measuring port, the pH electrode is inserted into the pH measuring port, the overflow joint is arranged at the overflow end, the lower end of the liquid storage overflow device is communicated with the first circulating pump, and the first circulating pump is communicated with the anode chamber.
8. The on-line in-situ monitoring device for the internal stress of the plating layer and the pH value of the plating solution in the electroforming process according to claim 7, wherein: the electroplating bath comprises an anode chamber, a bottom plate, a bottom port, two upper ports and silica gel plugs, wherein the anode chamber is provided with a plurality of square grooves, the bottom plate is provided with a plurality of square grooves, the anode chamber is provided with a plurality of square grooves, the bottom port is provided with a plurality of bottom ports, the bottom port is provided with a plurality of square grooves, the square grooves are arranged in the square grooves, the anode chamber is provided with a plurality of square grooves, the bottom port is provided with a plurality of square grooves, the square grooves are provided with a plurality of square grooves, and the square grooves are arranged on the bottom plate of the electroplating bath;
the upper port of the anode chamber close to the cathode and the bottom port of the bottom plate close to the anode are connected with the industrial electroforming tank; an upper port close to the anode on the anode chamber is connected with a bottom opening close to the cathode on the bottom plate and a pH real-time monitoring passage; and a heating rod is inserted into the bottom port in the middle of the bottom plate and is connected with the temperature controller.
9. The on-line in-situ monitoring device for the internal stress of the coating and the pH value of the plating solution in the electroforming process according to claim 8, wherein: the pH real-time monitoring passage comprises a valve and a plurality of silicone tubes, a first threaded pagoda joint of the valve is connected with a second threaded pagoda joint of the pH measuring device through the silicone tubes, and an overflow joint of the pH measuring device is connected with an upper port, close to the anode, of the side wall of the anode chamber through a liquid inlet joint and the silicone tubes to form the pH real-time monitoring passage.
10. The on-line in-situ monitoring device for the internal stress of the plating layer and the pH value of the plating solution in the electroforming process according to claim 8, wherein: the circulating liquid flow path comprises a second valve, a second circulating pump and a plurality of silicone tubes, a third threaded pagoda joint of the second valve is connected with a fourth threaded pagoda joint through the silicone tubes, the fourth threaded pagoda joint is connected with the water outlet end of the second circulating pump, the water inlet end of the second circulating pump is connected with a fifth threaded pagoda joint, and the fifth threaded pagoda joint is connected with the industrial electroforming tank through the silicone tubes; meanwhile, the industrial electroforming tank is connected with an overflow joint through a silicone tube, and the overflow joint is communicated with an upper port of the side wall of the anode chamber, which is close to the cathode, so that a circulation passage for measuring the electroforming tank and the electroforming liquid of the industrial electroforming tank is formed.
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| CN1651884A (en) * | 2004-02-03 | 2005-08-10 | 株式会社山本镀金试验器 | Electrode cartridge and a system for measuring internal stress of an electroplated film |
| CN1865515A (en) * | 2006-04-12 | 2006-11-22 | 吴建明 | Improvement of gold electroforming process |
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