CN109763163A - The device and method of functional composite material is prepared under super critical condition - Google Patents
The device and method of functional composite material is prepared under super critical condition Download PDFInfo
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- CN109763163A CN109763163A CN201910141774.9A CN201910141774A CN109763163A CN 109763163 A CN109763163 A CN 109763163A CN 201910141774 A CN201910141774 A CN 201910141774A CN 109763163 A CN109763163 A CN 109763163A
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Abstract
The present invention relates to electrical-chemistry method technical field, the device and method of functional composite material, including reaction kettle component, pedestal, feed system, extraction system are prepared under especially a kind of super critical condition；Reaction kettle component includes reaction kettle ontology, kettle cover and fixture, pedestal and magnetic stirring apparatus；Feed system includes liquid reserve tank, inlet tube, electrically operated valve, high-pressure pump, counterbalance valve, check-valves, controller etc.；Extraction system includes electrically operated valve, high-pressure pump, counterbalance valve, check-valves, liquid reserve tank, outlet tube, bottom valve, ionometer and controller.Processing method mainly includes parent metal cationic electrodeposition, the reaction remaining liq in abstraction reaction kettle, two layers of metal ions solution of addition, outer layer metal cationic electrodeposition.The compound ladder plating that can be realized multilayer material on substrate using the device, also can be used for realizing real-time addition, monitoring and the sampling under the conditions of high-temperature high-voltage reaction to solution in kettle, extends the use scope of overcritical electro-deposition.
Description
Technical field
The present invention relates to electrical-chemistry method technical field, specific field is to prepare function and service material under a kind of super critical condition
The device and method of material.
Background technique
Supercritical fluid refers to that temperature and pressure is in the fluid of critical-temperature and critical pressure or more, physics and chemically
Can have superior mass transfer performances and compatibility between liquids and gases.
Electro-deposition techniques be it is a kind of based on low cost prepare important one of the method for high-performance metal based composites, because of it
The performances such as high rigidity, excellent wearability and corrosion resistance that coating has and receive much attention.Electricity based on supercritical fluid is heavy
Product technology is that supercritical fluid technique is applied to an emerging electrical-chemistry method technology of electrodeposition, be can effectively solve
The problems such as second phase additive is unevenly distributed provides a kind of new side to promote surface quality and the mechanical property of composite deposite
Method.
Currently, preparing the process and device of metal-base nanometer composite material and micro-workpiece under supercritical fluid environment
Seen in existing.Chinese patent literature if Authorization Notice No. is CN 101092716B discloses a kind of subtle electricity of supercritical fluid
Moulding process and its device are plated, the preferably single coating of mass can be prepared by this method, many productions, practice can be met
It is required that.But in certain fields, such as space shuttle, carrier rocket, outer surface will bear the high temperature of thousands of degree, and inside has again
There are good mechanical strength and thermal conductivity, single coating is difficult to meet the requirements, and the functionalization for needing to produce a kind of more coating is multiple
Condensation material.
There are many ways to manufacturing functionalization composite material, most complex technical process, working condition are harsh.It has only compound
Electro-deposition techniques have unique advantage, thus design device and the processing that functional composite material is prepared under a kind of super critical condition
Method has a very important significance.
Summary of the invention
The purpose of the present invention is to provide the device and methods that functional composite material is prepared under a kind of super critical condition, with solution
Certainly complex technical process, the problems such as working condition is harsh in the prior art.
To achieve the above object, the invention provides the following technical scheme:
Prepare the device of functional composite material under a kind of super critical condition, including reaction kettle component, pedestal, feed system and
Extraction system；The reaction kettle component includes reaction kettle autoclave body, kettle cover and fixture；The pedestal includes the magnetic embedded in chassis interior
Power agitating device and external user interface.
The device of functional composite material is prepared under super critical condition of the present invention, wherein the feed system includes
From top to bottom setting and by inlet tube be connected to the first liquid reserve tank, the first electrically operated valve, the first high-pressure pump, the first counterbalance valve and
First check-valve；The first liquid reserve tank bottom is inserted into described inlet tube one end, and the other end is connected in reaction kettle；The feed system is also
The first controller including being separately connected the first electrically operated valve and the first high-pressure pump, the first controller control the first electrically operated valve and
The operation of first high-pressure pump.
The device of functional composite material is prepared under super critical condition of the present invention, wherein first high-pressure pump will
Solution in first liquid reserve tank is delivered in reaction kettle；First check-valve can prevent the reflux of solution.
The device of functional composite material is prepared under super critical condition of the present invention, wherein first counterbalance valve
Pressure is set slightly larger than pressure in kettle；When first counterbalance valve the first high-pressure pump do not open or the first high-pressure pump open but
When feed liquor pipe pressure is not up to the first counterbalance valve setting value, the first counterbalance valve blocks pipeline；It is set when the feed liquor pipe pressure is greater than
When definite value, pipeline is connected.
The device of functional composite material is prepared under super critical condition of the present invention, wherein first electrically operated valve
It opens and is closed through the control of the first controller.
The device of functional composite material is prepared under super critical condition of the present invention, wherein first liquid reserve tank is used
It is provided with the first inlet in temporarily storage experiment reagent, the upper end, lower-left end is provided with the first liquid outlet.
The device of functional composite material is prepared under super critical condition of the present invention, wherein the inlet tube is reacting
Part in kettle is equipped with the first anticorrosion casing.
The device of functional composite material is prepared under super critical condition of the present invention, wherein the extraction system includes
Second electrically operated valve, the second high-pressure pump, the second counterbalance valve, second check-valve, the second liquid reserve tank, outlet tube, bottom valve, ion concentration
Meter and second controller, the second liquid reserve tank outside reaction kettle are connected to second check-valve, the second back by outlet tube from top to bottom
Pressure valve, the second high-pressure pump and the second electrically operated valve, the outlet tube bottom inside reaction kettle are provided with bottom valve and ionometer.
The device of functional composite material is prepared under super critical condition of the present invention, wherein second high-pressure pump will
Solution in reaction kettle is pumped to the second liquid reserve tank；Second check-valve prevents solution from flowing back.
The device of functional composite material is prepared under super critical condition of the present invention, wherein the setting of the second counterbalance valve
Slightly larger than pressure in kettle, the second electrically operated valve cannot be turned directly in kettle in solution to the second liquid reserve tank pressure when opening, and only be existed
Second high-pressure pump is opened, and pressure reaches setting value, and solution enters the second liquid reserve tank by the second counterbalance valve.
The device of functional composite material is prepared under super critical condition of the present invention, wherein the second electrically operated valve is by
The control of two controllers is opened and closure.
The device of functional composite material is prepared under super critical condition of the present invention, wherein the second liquid reserve tank is for facing
When store experiment reagent, bottom righthand side is provided with the second liquid outlet.
The device of functional composite material is prepared under super critical condition of the present invention, wherein outlet tube is in a kettle
Part be furnished with the second anticorrosion casing.
The method that material is prepared using the device for preparing functional composite material under super critical condition of the present invention, including
Following steps:
(1) parent metal cationic electrodeposition: the prepared electrolyte containing parent metal ion is poured into reaction kettle,
Surfactant is added, clamping reaction kettle produces super critical condition, prepares base's electroplated layer；
(2) the reaction remaining liq in abstraction reaction kettle: after the completion of base's plating, by extraction system by residual solution in kettle
Body extraction；
(3) add outer layer metal ions solution: preparatory prepared outer layer metal ion electrolyte is poured into power-off
Liquid reserve tank is squeezed into liquid in reservoir in reaction kettle by feed system.
(4) it outer layer metal cationic electrodeposition: is powered, prepares two layers of electroplated layer.
The functional composite material for using the method for the present invention to prepare is two layers or two layers or more.
Compared with prior art, the beneficial effects of the present invention are: (1) of the invention device for preparing functional composite material can
High temperature resistant, anti abrasive functional composite material are prepared, there is excellent structure and performance.(2) present invention also can be used as high temperature
Under the conditions of high pressure is anti-in reaction process solution addition, solve because electrodeposit reaction carry out cause certain ion concentrations to subtract
The problem of causing quality of coating to be unevenly distributed less.(3) the compound ladder plating of multilayer material can be realized on substrate using the device,
Also it can be used for realizing real-time addition, monitoring and the sampling under the conditions of high-temperature high-voltage reaction to solution in kettle, extend overcritical
The use scope of electro-deposition.
Detailed description of the invention
Fig. 1 is the main view that the device of functional composite material is prepared under super critical condition of the invention；
Fig. 2 is the schematic perspective view that the device of functional composite material is prepared under super critical condition of the invention；
Fig. 3 is the schematic diagram of internal structure that the device of functional composite material is prepared under super critical condition of the invention；
Reaction kettle component internal structural schematic diagram Fig. 4 of the invention；
Feed system schematic diagram of internal structure Fig. 5 of the invention；
Extraction system schematic diagram of internal structure Fig. 6 of the invention；
Fig. 5 and Fig. 6 does not illustrate control centre's component；
In figure, 1, reaction kettle component, 11, reaction kettle ontology, 12, air inlet and venthole, 13, kettle cover, 14, fixture, 2,
Pedestal, 21, magnetic stirring apparatus, 22, customer center, 3, feed system, the 31, first high-pressure pump, the 32, first counterbalance valve, 33,
One check-valves, the 34, first electrically operated valve, the 35, first liquid reserve tank, the 351, first inlet, the 352, first liquid outlet, 36, feed liquor
Pipe, the 361, first anticorrosion casing, the 37, first control centre, 4, extraction system, the 41, second electrically operated valve, the 42, second high pressure
Pump, the 43, second counterbalance valve, 44, second check-valve, the 45, second liquid reserve tank, the 451, second leakage fluid dram；46, outlet tube, 461,
Two anticorrosion casings, 47, bottom valve, 48, ionometer, the 49, second control centre.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
In conjunction with Fig. 1-6, the device of functional composite material, including reaction kettle component 1, pedestal are prepared under a kind of super critical condition
2, feed system 3 and extraction system 4；The reaction kettle component 1 includes reaction kettle autoclave body 11, kettle cover 13 and fixture 14；The bottom
Seat 2 includes the magnetic stirring apparatus 21 and external user interface 22 embedded in chassis interior.Kettle cover 13 is equipped with air inlet and outlet
Hole 12.
The feed system 3 includes first the 35, first electricity of liquid reserve tank for being arranged from top to bottom and being connected to by inlet tube 36
Movable valve 34, the first high-pressure pump 31, the first counterbalance valve 32 and first check-valve 33；The first liquid storage is inserted into described 36 one end of inlet tube
35 bottom of case, the other end are connected in reaction kettle；The feed system 1 further includes that be separately connected the first electrically operated valve 34 and first high
First controller 37 of press pump 31, the first controller 37 control the operation of the first electrically operated valve 34 and the first high-pressure pump 31.
Solution in first liquid reserve tank 35 is delivered in reaction kettle 1 by first high-pressure pump 31；First check-valve 33 can
Prevent the reflux of solution.
The setting pressure of first counterbalance valve 32 is slightly larger than pressure in kettle；When first counterbalance valve 32 is in the first high pressure
When pump 31 is not opened or the first high-pressure pump 31 is opened but 36 pressure of inlet tube is not up to the first 32 setting value of counterbalance valve, the first back
Pressure valve 32 blocks pipeline；When 36 pressure of inlet tube is greater than the set value, pipeline is connected.
First electrically operated valve 34 is opened through the control of the first controller 37 and closure, liquid when only electrically operated valve is opened
Pipeline could be passed through.First liquid reserve tank 35 is provided with the first inlet 351 for temporarily storing experiment reagent, the upper end, left
Lower end is provided with the first liquid outlet 352.The part of the inlet tube 36 in a kettle is equipped with the first anticorrosion casing 361.
The extraction system 4 includes the second electrically operated valve 41, the second high-pressure pump 42, the second counterbalance valve 43, second check-valve
44, the second liquid reserve tank 45, outlet tube 46, bottom valve 47, ionometer 48 and second controller 49, the second storage outside reaction kettle
Liquid case 45 is connected to second check-valve 44, the second counterbalance valve 43, the second high-pressure pump 42 and the second electricity by outlet tube 46 from top to bottom
Movable valve 4, the outlet tube bottom inside reaction kettle are provided with bottom valve 47 and ionometer 48.
Second high-pressure pump 42 pumps the solution in reaction kettle 1 to the second liquid reserve tank 45；Second check-valve 44 prevents
Solution reflux.
For the setting pressure of second counterbalance valve 43 slightly larger than pressure in kettle, the second electrically operated valve 41 cannot be directly by kettle when opening
Interior solution is beaten to the second liquid reserve tank 45, is only opened in the second high-pressure pump 42, and pressure reaches setting value, and solution passes through the second back pressure
Valve 43 enters the second liquid reserve tank 45.
Second electrically operated valve 41 is opened and is closed by the control of second controller 49, liquid ability when only electrically operated valve is opened
Pipeline can be passed through.Second liquid reserve tank 45 is provided with the second liquid outlet 451 for temporarily storing experiment reagent, bottom righthand side.Outlet tube
It is furnished with the second anticorrosion casing 461 in 46 part in a kettle.
The method that material is prepared using the device for preparing functional composite material under super critical condition, comprising the following steps:
(1) parent metal cationic electrodeposition: the prepared electrolyte containing parent metal ion is poured into reaction kettle,
Surfactant is added, clamping reaction kettle produces super critical condition, prepares base's electroplated layer；
(2) the reaction remaining liq in abstraction reaction kettle: after the completion of base's plating, by extraction system by residual solution in kettle
Body extraction；
(3) add outer layer metal ions solution: preparatory prepared outer layer metal ion electrolyte is poured into power-off
Liquid reserve tank is squeezed into liquid in reservoir in reaction kettle by feed system.
(4) it outer layer metal cationic electrodeposition: is powered, prepares two layers of electroplated layer.
Prepared functional composite material is two layers or two layers or more.
Embodiment 2
Using the device of embodiment 1, for accurate, complex three-dimensional parts machining, using copper base Shang Du base as nickel layer,
To be illustrated for nickel cobalt (alloy), processing method mainly comprises the steps that outer layer
(1) parent metal cationic electrodeposition: the prepared electrolyte containing nickel metal ion is poured into reaction kettle, is added
Enter surfactant, clamping reaction kettle, wherein fixture anode is nickel plate, and cathode is same plate.Magnetic stirring apparatus is opened, is passed through
CO2, 50 DEG C are heated to, 10MPa is forced into, reaches super critical condition, dual-pulse power supply is loaded, prepares nickel coating；
(2) the reaction remaining liq in abstraction reaction kettle: after the completion of electronickelling, the pulse power in cutting, pause reaction, the right side
In the extraction system of side, user issues controller by user interface and instructs, and controller opens electrically operated valve and high-pressure pump, by kettle
Interior liquid is extracted into liquid reserve tank, and liquid is discharged by leakage fluid dram；
(3) add outer layer metal ions solution: in feed system, will it is prepared in advance containing nickel ion and cobalt from
The electrolyte of son pours into liquid reserve tank, and user issues controller by user interface and instructs, and controller opens electrically operated valve and height
Press pump squeezes into electrolyte in liquid reserve tank in reaction kettle.
(4) outer layer metal cationic electrodeposition: be powered, at this time due to squeeze into liquid and before extract out liquid it is suitable, kettle internal pressure
Power keeps substantially and unanimously, loads dual-pulse power supply before, prepare outer layer electroplated layer.
Embodiment 3
Using the device of embodiment 1, using copper base Shang Du base as nickel layer, middle layer is nickel cobalt (alloy), and outer layer is nickel Gao Meng
It is illustrated for alloy, processing method mainly comprises the steps that
(1) parent metal cationic electrodeposition: the prepared electrolyte containing nickel metal ion is poured into reaction kettle, is added
Enter surfactant, clamping reaction kettle, wherein fixture anode is nickel plate, and cathode is same plate.Magnetic stirring apparatus is opened, is passed through
CO2, 50 DEG C or so are heated to, 10MPa is forced into, reaches super critical condition, dual-pulse power supply is loaded, prepares nickel coating；
(2) the reaction remaining liq in abstraction reaction kettle: after the completion of electronickelling, the pulse power in cutting, pause reaction, the right side
In the extraction system of side, user issues controller by user interface and instructs, and controller opens electrically operated valve and high-pressure pump, by kettle
Interior liquid is extracted into liquid reserve tank, and liquid is discharged by leakage fluid dram；
(3) add middle layer metal ions solution: in feed system, will it is prepared in advance containing nickel ion and cobalt from
The electrolyte of son pours into liquid reserve tank, and user issues controller by user interface and instructs, and controller opens electrically operated valve and height
Press pump squeezes into electrolyte in liquid reserve tank in reaction kettle.
(4) middle layer metal cationic electrodeposition: be powered, at this time due to squeeze into liquid and before extract out liquid it is similar, in kettle
Pressure is kept and consistent before, load dual-pulse power supply, preparation middle layer electroplated layer substantially.
(5) the reaction remaining liq in abstraction reaction kettle: after the completion of nickel-cobalt alloy plating, the pulse power in cutting, pause
It reacts, in the extraction system of right side, user issues controller by user interface and instructs, and controller opens electrically operated valve and high pressure
Pump, liquid in kettle is extracted into liquid reserve tank, liquid is discharged by leakage fluid dram；
(6) add outer layer metal ions solution: in feed system, will it is prepared in advance containing nickel ion and manganese from
The electrolyte of son pours into liquid reserve tank, and user issues controller by user interface and instructs, and controller opens electrically operated valve and height
Press pump squeezes into electrolyte in liquid reserve tank in reaction kettle.
(4) outer layer metal cationic electrodeposition: be powered, at this time due to squeeze into liquid and before extract out liquid it is similar, in kettle
Pressure keeps substantially and unanimously, loads dual-pulse power supply before, prepare outer layer electroplated layer.
Advantage as combined electro-deposition uniqueness in embodiment 2-3, manufacturing process is simple, changeability is strong, and preparing can be full
Sufficient product using in terms of function requirement, adapt to the advanced material that environment is strong and controllability is strong, sharpest edges are can
The advantages of multiple material, is combined, has many advantages, such as that conventional composite materials are incomparable.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (15)
1. preparing the device of functional composite material under a kind of super critical condition, it is characterised in that: including reaction kettle component (1), bottom
Seat (2), feed system (3) and extraction system (4)；The reaction kettle component (1) include reaction kettle autoclave body (11), kettle cover (13) and
Fixture (14)；The pedestal (2) includes the magnetic stirring apparatus (21) and external user interface (22) embedded in chassis interior.
2. preparing the device of functional composite material under super critical condition according to claim 1, it is characterised in that: it is described into
It include the first liquid reserve tank (35), the first electrically operated valve for being arranged from top to bottom and being connected to by inlet tube (36) to system (3)
(34), the first high-pressure pump (31), the first counterbalance valve (32) and first check-valve (33)；Inlet tube (36) one end insertion first
Liquid reserve tank (35) bottom, the other end are connected in reaction kettle；The feed system (1) further includes being separately connected the first electrically operated valve
(34) and the first controller (37) of the first high-pressure pump (31), the first controller (37) control the first electrically operated valve (34) and first
The operation of high-pressure pump (31).
3. preparing the device of functional composite material under super critical condition according to claim 2, it is characterised in that: described
Solution in first liquid reserve tank (35) is delivered in reaction kettle (1) by one high-pressure pump (31)；First check-valve (33) can prevent molten
The reflux of liquid.
4. preparing the device of functional composite material under super critical condition according to claim 2, it is characterised in that: described
The setting pressure of one counterbalance valve (32) is slightly larger than pressure in kettle；When first counterbalance valve (32) is not opened in the first high-pressure pump (31)
It opens or the first high-pressure pump (31) is opened but inlet tube (36) pressure is when being not up to the first counterbalance valve (32) setting value, the first back pressure
Valve (32) blocks pipeline；When the inlet tube (36) pressure is greater than the set value, pipeline is connected.
5. preparing the device of functional composite material under super critical condition according to claim 2, it is characterised in that: described
One electrically operated valve (34) is opened through the first controller (37) control and closure.
6. preparing the device of functional composite material under super critical condition according to claim 2, it is characterised in that: described
One liquid reserve tank (35) is provided with the first inlet (351) for temporarily storing experiment reagent, the upper end, and lower-left end is provided with first and goes out liquid
Mouth (352).
7. preparing the device of functional composite material under super critical condition according to claim 2, it is characterised in that: it is described into
The part of liquid pipe (36) in a kettle is equipped with the first anticorrosion casing (361).
8. preparing the device of functional composite material under super critical condition according to claim 1, it is characterised in that: the pumping
Taking system (4) includes the second electrically operated valve (41), the second high-pressure pump (42), the second counterbalance valve (43), second check-valve (44), the
Two liquid reserve tanks (45), outlet tube (46), bottom valve (47), ionometer (48) and second controller (49), outside reaction kettle
Second liquid reserve tank (45) is connected to second check-valve (44), the second counterbalance valve (43), second high by outlet tube (46) from top to bottom
Press pump (42) and the second electrically operated valve (41), the outlet tube bottom inside reaction kettle are provided with bottom valve (47) and ionometer
(48)。
9. preparing the device of functional composite material under super critical condition according to claim 8, it is characterised in that: described
Two high-pressure pumps (42) pump the solution in reaction kettle (1) to the second liquid reserve tank (45)；Second check-valve (44) prevents solution from returning
Stream.
10. preparing the device of functional composite material under super critical condition according to claim 8, it is characterised in that: second
The setting pressure of counterbalance valve (43) cannot directly beat solution in kettle when opening slightly larger than pressure in kettle, the second electrically operated valve (41)
It in the second liquid reserve tank (45), is only opened in the second high-pressure pump (42), pressure reaches setting value, and solution passes through the second counterbalance valve
(43) enter the second liquid reserve tank (45).
11. preparing the device of functional composite material under super critical condition according to claim 8, it is characterised in that: second
Electrically operated valve (41) is opened and is closed by the control of second controller (49).
12. preparing the device of functional composite material under super critical condition according to claim 8, it is characterised in that: second
Liquid reserve tank (45) is provided with the second liquid outlet (451) for temporarily storing experiment reagent, bottom righthand side.
13. preparing the device of functional composite material under super critical condition according to claim 8, it is characterised in that: go out liquid
It manages the part of (46) in a kettle and is furnished with the second anticorrosion casing (461).
14. preparing material using the device for preparing functional composite material under any super critical condition of claim 1-13
Method, it is characterised in that: the following steps are included:
(1) parent metal cationic electrodeposition: the prepared electrolyte containing parent metal ion is poured into reaction kettle, is added
Surfactant, clamping reaction kettle produce super critical condition, prepare base's electroplated layer；
(2) the reaction remaining liq in abstraction reaction kettle: after the completion of base's plating, residual liquid in kettle is taken out by extraction system
Out；
(3) add outer layer metal ions solution: preparatory prepared outer layer metal ion electrolyte is poured into liquid storage by power-off
Case is squeezed into liquid in reservoir in reaction kettle by feed system.
(4) it outer layer metal cationic electrodeposition: is powered, prepares two layers of electroplated layer.
15. according to preparation method described in claims 14, it is characterised in that: prepared functional composite material be two layers or
Two layers or more.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910141774.9A CN109763163B (en) | 2019-02-26 | 2019-02-26 | Device and method for preparing functional composite material under supercritical condition |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910141774.9A CN109763163B (en) | 2019-02-26 | 2019-02-26 | Device and method for preparing functional composite material under supercritical condition |
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| CN109763163B CN109763163B (en) | 2021-02-09 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113061966A (en) * | 2021-03-26 | 2021-07-02 | 江苏理工学院 | Supercritical electrodeposition device for preparing composite material and use method thereof |
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