CN109763163B - Device and method for preparing functional composite material under supercritical condition - Google Patents

Device and method for preparing functional composite material under supercritical condition Download PDF

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CN109763163B
CN109763163B CN201910141774.9A CN201910141774A CN109763163B CN 109763163 B CN109763163 B CN 109763163B CN 201910141774 A CN201910141774 A CN 201910141774A CN 109763163 B CN109763163 B CN 109763163B
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valve
reaction kettle
storage tank
liquid
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CN109763163A (en
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雷卫宁
邓瑶
张文杰
王剑桥
彭勇
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Jiangsu University of Technology
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Abstract

The invention relates to the technical field of electrochemical machining, in particular to a device and a method for preparing a functional composite material under a supercritical condition, which comprises a reaction kettle assembly, a base, a feeding system and an extraction system, wherein the reaction kettle assembly is arranged on the base; the reaction kettle component comprises a reaction kettle body, a kettle cover, a clamp, a base and a magnetic stirring device; the feeding system comprises a liquid storage tank, a liquid inlet pipe, an electric valve, a high-pressure pump, a back pressure valve, a check valve, a controller and the like; the extraction system comprises an electric valve, a high-pressure pump, a back pressure valve, a check valve, a liquid storage tank, a liquid outlet pipe, a bottom valve, an ion concentration meter and a controller. The processing method mainly comprises the steps of base layer metal ion electrodeposition, extraction of reaction residual liquid in a reaction kettle, addition of two layers of deposition metal ion solutions, outer layer metal ion electrodeposition and the like. The device can realize composite ladder plating of multilayer materials on the substrate, and can also be used for realizing real-time addition, monitoring and sampling of the solution in the kettle under the high-temperature and high-pressure reaction condition, thereby expanding the application range of the supercritical electrodeposition.

Description

Device and method for preparing functional composite material under supercritical condition
Technical Field
The invention relates to the technical field of electrochemical machining, in particular to a device and a method for preparing a functional composite material under a supercritical condition.
Background
The supercritical fluid is a fluid with the temperature and the pressure above the critical temperature and the critical pressure, has the physical and chemical properties between those of liquid and gas, and has excellent mass transfer property and miscibility.
Electrodeposition is one of the important methods for preparing high-performance metal matrix composites based on low cost, and has attracted attention because of the high hardness, excellent wear resistance and corrosion resistance of the coating. The supercritical fluid-based electrodeposition technology is a novel electrochemical processing technology which applies the supercritical fluid technology to the field of electrodeposition, can effectively solve the problems of uneven distribution of second-phase additives and the like, and provides a new method for improving the surface quality and the mechanical property of a composite coating.
At present, the process and the device for preparing the metal-based nano composite material and the micro parts under the supercritical fluid environment are known. For example, chinese patent publication No. CN 101092716B discloses a supercritical fluid fine micro-electroplating forming process and apparatus, by which a single plating layer with good quality can be prepared, and many requirements for production and practice can be satisfied. However, in some fields, such as space shuttles and launch vehicles, the outer surface of the composite material needs to bear thousands of high temperatures, the inner side of the composite material needs to have good mechanical strength and thermal conductivity, a single coating is difficult to meet the requirements, and a multi-coating functionalized composite material needs to be manufactured.
The method for manufacturing the functional composite material has various methods, most of which have complex process and harsh production conditions. Only the composite electrodeposition technology has unique advantages, so that the design of a device and a processing method for preparing the functional composite material under the supercritical condition has very important significance.
Disclosure of Invention
The invention aims to provide a device and a method for preparing a functional composite material under a supercritical condition, so as to solve the problems of complex process, harsh production conditions and the like in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
a device for preparing functional composite material under supercritical condition comprises a reaction kettle assembly, a base, a feeding system and an extraction system; the reaction kettle assembly comprises a reaction kettle body, a kettle cover and a clamp; the base includes a magnetic stirring device embedded within the base and an external user interface.
The device for preparing the functional composite material under the supercritical condition comprises a feeding system, a first liquid storage tank, a first electric valve, a first high-pressure pump, a first back pressure valve and a first check valve, wherein the feeding system is arranged from bottom to top and is communicated with the first liquid storage tank through a liquid inlet pipe; one end of the liquid inlet pipe is inserted into the bottom of the first liquid storage tank, and the other end of the liquid inlet pipe is communicated with the reaction kettle; the feeding system further comprises a first controller which is respectively connected with the first electric valve and the first high-pressure pump, and the first controller controls the first electric valve and the first high-pressure pump to operate.
The device for preparing the functional composite material under the supercritical condition comprises a first high-pressure pump, a second high-pressure pump, a third high-pressure pump and a fourth high-pressure pump, wherein the first high-pressure pump conveys a solution in a first liquid storage tank into a reaction kettle; the first check valve may prevent backflow of the solution.
The device for preparing the functional composite material under the supercritical condition, disclosed by the invention, is characterized in that the set pressure of the first back pressure valve is slightly greater than the pressure in the kettle; when the first backpressure valve is not opened at the first high-pressure pump or the first high-pressure pump is opened but the pressure of the liquid inlet pipe does not reach the set value of the first backpressure valve, the first backpressure valve blocks the pipeline; and when the pressure of the liquid inlet pipe is greater than a set value, the pipeline is connected.
The device for preparing the functional composite material under the supercritical condition is characterized in that the first electric valve is controlled to be opened and closed by the first controller.
The device for preparing the functional composite material under the supercritical condition is characterized in that the first liquid storage tank is used for temporarily storing the experimental reagent, a first liquid inlet is formed in the upper end of the first liquid storage tank, and a first liquid outlet is formed in the left lower end of the first liquid storage tank.
The device for preparing the functional composite material under the supercritical condition is characterized in that a first anti-corrosion sleeve is arranged on the part of the liquid inlet pipe in the reaction kettle.
The device for preparing the functional composite material under the supercritical condition comprises a first electric valve, a first high-pressure pump, a first back pressure valve, a first check valve, a first liquid storage tank, a liquid outlet pipe, a bottom valve, an ion concentration meter and a first controller, wherein the first liquid storage tank outside a reaction kettle is communicated with the first check valve, the first back pressure valve, the first high-pressure pump and the first electric valve from bottom to top through the liquid outlet pipe, and the bottom valve and the ion concentration meter are arranged at the bottom of the liquid outlet pipe inside the reaction kettle.
The device for preparing the functional composite material under the supercritical condition is characterized in that the second high-pressure pump pumps the solution in the reaction kettle to the second liquid storage tank; the second check valve prevents the solution from flowing back.
The device for preparing the functional composite material under the supercritical condition, disclosed by the invention, is characterized in that the set pressure of the second back pressure valve is slightly larger than the pressure in the kettle, the solution in the kettle cannot be directly pumped into the second liquid storage tank when the second electric valve is opened, only the second high-pressure pump is opened, the pressure reaches the set value, and the solution enters the second liquid storage tank through the second back pressure valve.
The device for preparing the functional composite material under the supercritical condition is characterized in that the second electric valve is controlled by the second controller to open and close.
The device for preparing the functional composite material under the supercritical condition is characterized in that the second liquid storage tank is used for temporarily storing the experimental reagent, and the right lower end of the second liquid storage tank is provided with a second liquid outlet.
The device for preparing the functional composite material under the supercritical condition is characterized in that a second anti-corrosion sleeve is arranged on the part of the liquid outlet pipe in the reaction kettle.
The method for preparing the material by adopting the device for preparing the functional composite material under the supercritical condition comprises the following steps:
(1) electrodeposition of base metal ions: pouring the prepared electrolyte containing the base metal ions into a reaction kettle, adding a surfactant, clamping the reaction kettle, manufacturing a supercritical condition, and preparing a base electroplated layer;
(2) extracting reaction residual liquid in the reaction kettle: after the base electroplating is finished, pumping out residual liquid in the kettle through a pumping system;
(3) adding an outer layer deposition metal ion solution: and (3) powering off, pouring the prepared outer-layer metal ion electrolyte into the liquid storage tank, and pumping the liquid in the liquid storage tank into the reaction kettle through the feeding system.
(4) Outer layer metal ion electrodeposition: electrifying to prepare a two-layer electroplated layer.
The functional composite material prepared by the method has two or more layers.
Compared with the prior art, the invention has the beneficial effects that: (1) the device for preparing the functional composite material can prepare the high-temperature-resistant and wear-resistant functional composite material, and has excellent structure and performance. (2) The invention can also be used for adding solution in the reaction process under the high-temperature and high-pressure reaction condition, and solves the problem of uneven distribution of the coating quality caused by the reduction of certain ion concentration due to the progress of the electrodeposition reaction. (3) The device can realize composite ladder plating of multilayer materials on the substrate, and can also be used for realizing real-time addition, monitoring and sampling of the solution in the kettle under the high-temperature and high-pressure reaction condition, thereby expanding the application range of the supercritical electrodeposition.
Drawings
FIG. 1 is a front view of an apparatus for preparing a functional composite material under supercritical conditions according to the present invention;
FIG. 2 is a schematic perspective view of an apparatus for preparing a functional composite material under supercritical conditions according to the present invention;
FIG. 3 is a schematic view showing the internal structure of an apparatus for preparing a functional composite material under supercritical conditions according to the present invention;
FIG. 4 is a schematic view of the internal structure of a reactor assembly according to the present invention;
FIG. 5 is a schematic view of the internal structure of the feeding system of the present invention;
FIG. 6 is a schematic diagram of the internal structure of the extraction system of the present invention;
FIGS. 5 and 6 do not illustrate the control center components;
in the figure, 1, a reaction kettle assembly, 11, a reaction kettle body, 12, an air inlet and an air outlet, 13, a kettle cover, 14, a clamp, 2, a base, 21, a magnetic stirring device, 22, a user center, 3, a feeding system, 31, a first high-pressure pump, 32, a first backpressure valve, 33, a first check valve, 34, a first electric valve, 35, a first liquid storage tank, 351, a first liquid inlet, 352, a first liquid outlet, 36, a liquid inlet pipe, 361, a first corrosion-resistant sleeve, 37, a first control center, 4, an extraction system, 41, a second electric valve, 42, a second high-pressure pump, 43, a second backpressure valve, 44, a second check valve, 45, a second liquid storage tank, 451, and a second liquid outlet; 46. a liquid outlet pipe 461, a second anti-corrosion sleeve 47, a bottom valve 48, an ion concentration meter 49 and a second control center.
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.
Example 1
With reference to fig. 1-6, an apparatus for preparing a functional composite material under supercritical conditions comprises a reaction kettle assembly 1, a base 2, a feeding system 3 and an extraction system 4; the reaction kettle assembly 1 comprises a reaction kettle body 11, a kettle cover 13 and a clamp 14; the base 2 includes a magnetic stirring device 21 embedded inside the base and an external user interface 22. An air inlet and an air outlet 12 are arranged on the kettle cover 13.
The feeding system 3 comprises a first liquid storage tank 35, a first electric valve 34, a first high-pressure pump 31, a first back pressure valve 32 and a first check valve 33 which are arranged from bottom to top and communicated through a liquid inlet pipe 36; one end of the liquid inlet pipe 36 is inserted into the bottom of the first liquid storage tank 35, and the other end is communicated with the reaction kettle; the feed system 1 further comprises a first controller 37 connected to the first electric valve 34 and the first high-pressure pump 31, respectively, the first controller 37 controlling the operation of the first electric valve 34 and the first high-pressure pump 31.
The first high-pressure pump 31 conveys the solution in the first liquid storage tank 35 into the reaction kettle 1; the first check valve 33 prevents the backflow of the solution.
The set pressure of the first back pressure valve 32 is slightly larger than the pressure in the kettle; when the first backpressure valve 32 is not opened at the first high-pressure pump 31 or the first high-pressure pump 31 is opened but the pressure of the liquid inlet pipe 36 does not reach the set value of the first backpressure valve 32, the first backpressure valve 32 blocks a pipeline; when the pressure of the liquid inlet pipe 36 is larger than a set value, the pipeline is connected.
The first electrically operated valve 34 is controlled to open and close by a first controller 37, and liquid can only pass through the pipeline when the electrically operated valve is opened. The first liquid storage tank 35 is used for temporarily storing the experiment reagent, and has a first liquid inlet 351 at the upper end thereof and a first liquid outlet 352 at the left lower end thereof. The part of the liquid inlet pipe 36 in the reaction kettle is provided with a first anti-corrosion casing 361.
Extraction system 4 includes second electric valve 41, second high-pressure pump 42, second backpressure valve 43, second check valve 44, second liquid reserve tank 45, drain pipe 46, bottom valve 47, ion concentration meter 48 and second controller 49, and outside second liquid reserve tank 45 of reation kettle communicates second check valve 44, second backpressure valve 43, second high-pressure pump 42 and second electric valve 4 from the bottom up through drain pipe 46, and the inside drain pipe bottom of reation kettle is provided with bottom valve 47 and ion concentration meter 48.
The second high-pressure pump 42 pumps the solution in the reaction kettle 1 to a second liquid storage tank 45; the second check valve 44 prevents the solution from flowing back.
The set pressure of the second backpressure valve 43 is slightly larger than the pressure in the kettle, when the second electric valve 41 is opened, the solution in the kettle cannot be directly pumped into the second liquid storage tank 45, only when the second high-pressure pump 42 is opened, the pressure reaches the set value, and the solution enters the second liquid storage tank 45 through the second backpressure valve 43.
The second electrically operated valve 41 is controlled by a second controller 49 to open and close, and liquid can only pass through the conduit when the electrically operated valve is open. The second liquid storage tank 45 is used for temporarily storing the experiment reagent, and a second liquid outlet 451 is formed at the lower right end of the second liquid storage tank. The portion of the effluent pipe 46 in the reactor is fitted with a second corrosion protection sleeve 461.
The method for preparing the material by adopting the device for preparing the functional composite material under the supercritical condition comprises the following steps:
(1) electrodeposition of base metal ions: pouring the prepared electrolyte containing the base metal ions into a reaction kettle, adding a surfactant, clamping the reaction kettle, manufacturing a supercritical condition, and preparing a base electroplated layer;
(2) extracting reaction residual liquid in the reaction kettle: after the base electroplating is finished, pumping out residual liquid in the kettle through a pumping system;
(3) adding an outer layer deposition metal ion solution: and (3) powering off, pouring the prepared outer-layer metal ion electrolyte into the liquid storage tank, and pumping the liquid in the liquid storage tank into the reaction kettle through the feeding system.
(4) Outer layer metal ion electrodeposition: electrifying to prepare a two-layer electroplated layer.
The prepared functional composite material has two or more layers.
Example 2
The device of the embodiment 1 is used for processing precise and complex three-dimensional parts, and the processing method mainly comprises the following steps of:
(1) electrodeposition of base metal ions: pouring the prepared electrolyte containing nickel metal ions into a reaction kettle, adding a surfactant, and clamping the reaction kettle, wherein the anode of the clamp is a nickel plate, and the cathode of the clamp is the same plate. Opening the magnetic stirring device and introducing CO2Heating to 50 ℃, pressurizing to 10MPa to reach a supercritical condition, and loading a double-pulse power supply to prepare a nickel coating;
(2) extracting reaction residual liquid in the reaction kettle: after the nickel electroplating is finished, cutting off a pulse power supply, suspending the reaction, sending an instruction to a controller by a user through a user interface in a right-side pumping system, opening an electric valve and a high-pressure pump by the controller, pumping the liquid in the kettle into a liquid storage tank, and discharging the liquid through a liquid discharge port;
(3) adding an outer layer deposition metal ion solution: in the feeding system, electrolyte containing nickel ions and cobalt ions prepared in advance is poured into the liquid storage tank, a user sends an instruction to the controller through a user interface, the controller opens the electric valve and the high-pressure pump, and the electrolyte in the liquid storage tank is pumped into the reaction kettle.
(4) Outer layer metal ion electrodeposition: and electrifying, wherein the liquid is pumped into the kettle and the liquid is pumped out before the kettle, the pressure in the kettle is basically consistent with the pressure in the kettle, and a double-pulse power supply is loaded to prepare an outer-layer electroplated layer.
Example 3
By adopting the device of embodiment 1, the copper substrate is plated with the nickel layer as the base layer, the nickel-cobalt alloy as the middle layer and the nickel-manganese alloy as the outer layer, and the processing method mainly comprises the following steps:
(1) electrodeposition of base metal ions: pouring the prepared electrolyte containing nickel metal ions into a reaction kettle, adding a surfactant, and clamping the reaction kettle, wherein the anode of the clamp is a nickel plate, and the cathode of the clamp is the same plate. Opening the magnetic stirring device and introducing CO2Heating to about 50 ℃, pressurizing to 10MPa to reach a supercritical condition, and loading a double-pulse power supply to prepare a nickel coating;
(2) extracting reaction residual liquid in the reaction kettle: after the nickel electroplating is finished, cutting off a pulse power supply, suspending the reaction, sending an instruction to a controller by a user through a user interface in a right-side pumping system, opening an electric valve and a high-pressure pump by the controller, pumping the liquid in the kettle into a liquid storage tank, and discharging the liquid through a liquid discharge port;
(3) adding a middle layer deposition metal ion solution: in the feeding system, electrolyte containing nickel ions and cobalt ions prepared in advance is poured into the liquid storage tank, a user sends an instruction to the controller through a user interface, the controller opens the electric valve and the high-pressure pump, and the electrolyte in the liquid storage tank is pumped into the reaction kettle.
(4) And (3) intermediate layer metal ion electrodeposition: and electrifying, wherein the pressure in the kettle is basically consistent with the pressure in the kettle because the injected liquid is almost the same as the liquid extracted before, and loading a double-pulse power supply to prepare the middle-layer electroplated layer.
(5) Extracting reaction residual liquid in the reaction kettle: after the nickel-cobalt alloy is electroplated, cutting off a pulse power supply, suspending the reaction, sending an instruction to a controller by a user through a user interface in a right-side pumping system, opening an electric valve and a high-pressure pump by the controller, pumping the liquid in the kettle into a liquid storage tank, and discharging the liquid through a liquid discharge port;
(6) adding an outer layer deposition metal ion solution: in the feeding system, electrolyte containing nickel ions and manganese ions prepared in advance is poured into the liquid storage tank, a user sends an instruction to the controller through a user interface, the controller opens the electric valve and the high-pressure pump, and the electrolyte in the liquid storage tank is pumped into the reaction kettle.
(4) Outer layer metal ion electrodeposition: and electrifying, wherein the pressure in the kettle is basically consistent with the pressure in the kettle because the liquid is pumped in almost the same as the liquid pumped out before, and loading a double-pulse power supply to prepare an outer-layer electroplated layer.
For example, the embodiment 2 to 3 combines the unique advantages of electrodeposition, has a simple manufacturing process and strong variability, and prepares an advanced material that can satisfy the requirements of the product in terms of use functions, has strong environmental suitability and strong controllability, and has the greatest advantage of combining the advantages of a plurality of materials, and has many advantages that the conventional composite material cannot compare with.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (13)

1. An apparatus for preparing functional composite material under supercritical conditions, characterized in that: comprises a reaction kettle component (1), a base (2), a feeding system (3) and an extraction system (4); the reaction kettle assembly (1) comprises a reaction kettle body (11), a kettle cover (13) and a clamp (14); the base (2) comprises a magnetic stirring device (21) embedded inside the base and an external user interface (22);
the extraction system (4) comprises a second electric valve (41), a second high-pressure pump (42), a second backpressure valve (43), a second check valve (44), a second liquid storage tank (45), a liquid outlet pipe (46), a bottom valve (47), an ion concentration meter (48) and a second controller (49), the second liquid storage tank (45) outside the reaction kettle is communicated with the second check valve (44), the second backpressure valve (43), the second high-pressure pump (42) and the second electric valve (41) from bottom to top through the liquid outlet pipe (46), and the bottom valve (47) and the ion concentration meter (48) are arranged at the bottom of the liquid outlet pipe inside the reaction kettle;
the set pressure of the second backpressure valve (43) is slightly larger than the pressure in the kettle, when the second electric valve (41) is opened, the solution in the kettle cannot be directly pumped into the second liquid storage tank (45), only the second high-pressure pump (42) is opened, the pressure reaches a set value, and the solution enters the second liquid storage tank (45) through the second backpressure valve (43).
2. The apparatus for preparing a functional composite under supercritical conditions according to claim 1, wherein: the feeding system (3) comprises a first liquid storage tank (35), a first electric valve (34), a first high-pressure pump (31), a first back pressure valve (32) and a first check valve (33), which are arranged from bottom to top and are communicated through a liquid inlet pipe (36); one end of the liquid inlet pipe (36) is inserted into the bottom of the first liquid storage tank (35), and the other end of the liquid inlet pipe is communicated with the reaction kettle; the feeding system (1) further comprises a first controller (37) which is respectively connected with the first electric valve (34) and the first high-pressure pump (31), and the first controller (37) controls the operation of the first electric valve (34) and the first high-pressure pump (31).
3. The apparatus for preparing a functional composite under supercritical conditions according to claim 2, wherein: the first high-pressure pump (31) conveys the solution in the first liquid storage tank (35) into the reaction kettle (1); the first check valve (33) prevents backflow of the solution.
4. The apparatus for preparing a functional composite under supercritical conditions according to claim 2, wherein: the set pressure of the first back pressure valve (32) is slightly larger than the pressure in the kettle; when the first backpressure valve (32) is not opened at the first high-pressure pump (31) or the first high-pressure pump (31) is opened but the pressure of the liquid inlet pipe (36) does not reach the set value of the first backpressure valve (32), the first backpressure valve (32) blocks a pipeline; when the pressure of the liquid inlet pipe (36) is larger than a set value, the pipeline is connected.
5. The apparatus for preparing a functional composite under supercritical conditions according to claim 2, wherein: the first electric valve (34) is controlled to open and close by a first controller (37).
6. The apparatus for preparing a functional composite under supercritical conditions according to claim 2, wherein: the first liquid storage tank (35) is used for temporarily storing the experimental reagent, and is provided with a first liquid inlet (351) at the upper end and a first liquid outlet (352) at the left lower end.
7. The apparatus for preparing a functional composite under supercritical conditions according to claim 2, wherein: the part of the liquid inlet pipe (36) in the reaction kettle is provided with a first anti-corrosion sleeve (361).
8. The apparatus for preparing a functional composite under supercritical conditions according to claim 1, wherein: the second high-pressure pump (42) pumps the solution in the reaction kettle (1) to a second liquid storage tank (45); a second check valve (44) prevents backflow of the solution.
9. The apparatus for preparing a functional composite under supercritical conditions according to claim 1, wherein: the second electric valve (41) is controlled by a second controller (49) to open and close.
10. The apparatus for preparing a functional composite under supercritical conditions according to claim 1, wherein: the second liquid storage tank (45) is used for temporarily storing the experimental reagent, and the right lower end of the second liquid storage tank is provided with a second liquid outlet (451).
11. The apparatus for preparing a functional composite under supercritical conditions according to claim 1, wherein: the part of the liquid outlet pipe (46) in the reaction kettle is provided with a second corrosion-proof sleeve (461).
12. A method for preparing a material using the apparatus for preparing a functional composite material under supercritical conditions according to any one of claims 1 to 11, wherein: the method comprises the following steps:
(1) electrodeposition of base metal ions: pouring the prepared electrolyte containing the base metal ions into a reaction kettle, adding a surfactant, clamping the reaction kettle, manufacturing a supercritical condition, and preparing a base electroplated layer;
(2) extracting reaction residual liquid in the reaction kettle: after the base electroplating is finished, pumping out residual liquid in the kettle through a pumping system;
(3) adding an outer layer deposition metal ion solution: when the power is cut off, pouring the prepared outer layer metal ion electrolyte into a liquid storage tank, and pumping the liquid in the liquid storage tank into the reaction kettle through a feeding system;
(4) outer layer metal ion electrodeposition: electrifying to prepare a two-layer electroplated layer.
13. The method of claim 12, wherein: the prepared functional composite material has two or more layers.
CN201910141774.9A 2019-02-26 2019-02-26 Device and method for preparing functional composite material under supercritical condition Active CN109763163B (en)

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