CN110499522A - A kind of interior preparation method for flowing electric deposition device and electro-deposition porous structure of pipe - Google Patents
A kind of interior preparation method for flowing electric deposition device and electro-deposition porous structure of pipe Download PDFInfo
- Publication number
- CN110499522A CN110499522A CN201910897746.XA CN201910897746A CN110499522A CN 110499522 A CN110499522 A CN 110499522A CN 201910897746 A CN201910897746 A CN 201910897746A CN 110499522 A CN110499522 A CN 110499522A
- Authority
- CN
- China
- Prior art keywords
- storage device
- liquid storage
- electrolyte
- solution
- concentration
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000151 deposition Methods 0.000 title claims abstract description 24
- 230000008021 deposition Effects 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000004070 electrodeposition Methods 0.000 title claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 191
- 239000003792 electrolyte Substances 0.000 claims abstract description 111
- 238000003860 storage Methods 0.000 claims abstract description 106
- 229910052751 metal Inorganic materials 0.000 claims description 37
- 239000002184 metal Substances 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 150000001768 cations Chemical class 0.000 claims description 22
- 239000000126 substance Substances 0.000 claims description 15
- 239000004020 conductor Substances 0.000 claims description 13
- RPAJSBKBKSSMLJ-DFWYDOINSA-N (2s)-2-aminopentanedioic acid;hydrochloride Chemical compound Cl.OC(=O)[C@@H](N)CCC(O)=O RPAJSBKBKSSMLJ-DFWYDOINSA-N 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 229920006395 saturated elastomer Polymers 0.000 claims description 11
- 230000005684 electric field Effects 0.000 claims description 6
- 238000004064 recycling Methods 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 3
- 238000001802 infusion Methods 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 claims 2
- 238000007689 inspection Methods 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 7
- 229910002804 graphite Inorganic materials 0.000 abstract description 7
- 239000010439 graphite Substances 0.000 abstract description 7
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 62
- 238000010438 heat treatment Methods 0.000 description 10
- 239000010410 layer Substances 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 235000011299 Brassica oleracea var botrytis Nutrition 0.000 description 7
- 240000003259 Brassica oleracea var. botrytis Species 0.000 description 7
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 7
- 238000010586 diagram Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 230000005611 electricity Effects 0.000 description 5
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 4
- 210000001787 dendrite Anatomy 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 238000004062 sedimentation Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000004891 communication Methods 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000001413 cellular effect Effects 0.000 description 2
- 229910000365 copper sulfate Inorganic materials 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 244000132059 Carica parviflora Species 0.000 description 1
- 235000014653 Carica parviflora Nutrition 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- -1 ammonium chloride Chemical class 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 230000005574 cross-species transmission Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910000939 field's metal Inorganic materials 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
- C25D17/02—Tanks; Installations therefor
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
- C25D17/10—Electrodes, e.g. composition, counter electrode
- C25D17/12—Shape or form
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
- C25D21/14—Controlled addition of electrolyte components
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/04—Tubes; Rings; Hollow bodies
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Automation & Control Theory (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The application provides a kind of interior preparation method for flowing electric deposition device and electro-deposition porous structure of pipe.The device includes: liquid storage device, sleeve cathode, anode and power supply；Wherein, the sleeve cathode is connect with the cathode of the power supply；The anode is set to inside the pipe of the sleeve cathode, and the anode is connect with the anode of the power supply；The liquid storage device is connect by conduit with the first nozzle of the sleeve cathode for storing electrolyte, the liquid storage device.Electric deposition device provided by the embodiments of the present application can prepare the sedimentary of the micro-nano structure of different-shape in pipe, not need the molds such as graphite rod auxiliary, the sedimentary that can be formed in the tube the porous structure of different-thickness by adjusting technological parameter.
Description
Technical field
This application involves heat and mass technical fields, heavy in particular to flowing electric deposition device in a kind of pipe and electricity
The preparation method of product porous structure.
Background technique
Porous structure is prepared in round tube, has heat and mass field to have important application.Porous knot is such as prepared in pipe
After structure, it can be processed into heat pipe, become a kind of phase transformation by totally-enclosed shell internal working medium to transmit the device of heat.
This porous structure is the capillary wick of heat pipe, and working medium in heat pipe can be promoted to flow back, make heat pipe cycle operation.Wherein, lead to
It crosses graphite rod production mold sintered metal particle in pipe and obtains the porous structure of better performances.This is also most common side
Method.But the complex process of this sample loading mode, and be difficult to prepare some relatively thin porous structures.
Summary of the invention
The embodiment of the present application is designed to provide a kind of interior system for flowing electric deposition device and electro-deposition porous structure of pipe
Preparation Method, to solve to prepare the sedimentary complex process of porous structure in managing in the prior art and be difficult to prepare the porous knot of micro-nano
The problem of sedimentary of structure.
In a first aspect, the embodiment of the present application, which provides, flows electric deposition device in a kind of pipe, comprising: liquid storage device, sleeve cathode,
Anode and power supply；
Wherein, the sleeve cathode is connect with the cathode of the power supply；
The anode is set to inside the pipe of the sleeve cathode, and the anode is connect with the anode of the power supply；
The liquid storage device is connected for storing electrolyte, the liquid storage device by the first nozzle of conduit and the sleeve cathode
It connects.
Electric deposition device provided by the embodiments of the present application can prepare the deposition of the micro-nano structure of different-shape in pipe
Layer, does not need the molds such as graphite rod auxiliary, the porous structure that can be formed in the tube different-thickness by adjusting technological parameter
Sedimentary.
Further, described device includes solution recover, and the solution recover passes through conduit and the sleeve cathode
The second nozzle connection；The solution recover is used for the solution after storage reaction.It is molten after reaction so as to sufficiently recycle
Liquid, it is therefore prevented that the random discharge of electrolyte pollutes the environment.
Further, the solution recover is connect by conduit with the liquid storage device；
Described device further include: the pump on the channel between the solution recover and the liquid storage device is set, is used for
Solution in the solution recover is transported in the liquid storage device.Electrolyte is made full use of to realize.
Further, described device includes liquid replenisher；The liquid replenisher is connect by conduit with the liquid storage device, the benefit
Liquid device is for storing make-up solution.So as to provide sufficient electrolyte, and it can guarantee the concentration of electrolyte.
Further, described device further includes liquid level sensor, the first controller and the first valve；The liquid level sensor
It is connect with first controller with first valve；The liquid level sensor is set to inside the liquid storage device, is used for
Detect the liquid level information in the liquid storage device；Leading for the connection liquid storage device and the sleeve cathode is arranged in first valve
Guan Shang；First controller is used to receive the liquid level information that the liquid level sensor is sent, and is believed according to the liquid level
The aperture of breath the first valve of control.To realize automatic liquid supply, it is not necessarily to artificial fluid infusion.
Further, described device further includes concentration detector, and the concentration detector is set to inside the liquid storage device,
The concentration information is sent for detecting the concentration information of electrolyte in the liquid storage device, and to first controller；It is described
First controller controls the aperture of first valve according to the concentration information.By detecting the concentration of electrolyte automatically, from
And it ensure that the concentration of electrolyte flowed into sleeve cathode is identical.
Further, device further includes switch and second controller, the switch setting the power supply, sleeve cathode and
On the circuit that anode is constituted；The second controller includes timer, and the second controller is used to control institute according to timer
It states and switches on-off.The accurate control to sedimentation time is realized by second controller and switch.
Further, described device further include: second the second valve of nozzle of the sleeve cathode is set；And pass through
The drain pipe that second valve is connect with the second nozzle.Electrolyte can be controlled inside sleeve cathode by the second valve
Flow velocity.
Further, described device further includes heater, and described device further includes thermostat, and the thermostat is used for institute
The temperature for stating the electrolyte in liquid storage device is controlled.Due to electrolyte temperature difference, the sedimentary of different structure can produce,
It is controlled by the temperature to electrolyte, meets some preparation demands.
Further, the shape of the sleeve cathode is round tube, semi-circular tube or polygonal tube.
Further, the material of the sleeve cathode includes the metal simple-substance not reacted with the electrolyte, inertia
The mixture of conductor or the metal simple-substance not reacted with the electrolyte and inert conductor.
Further, the material of the anode includes the mixed of metal simple-substance, inert conductor or metal simple-substance and inert conductor
Close object.
Second aspect, the embodiment of the present application provide a kind of preparation method of electro-deposition porous structure, comprising:
Electrolyte in liquid storage device is introduced by conduit in the pipe of sleeve cathode；
It is driven in electrolyte by the electric field that the anode being arranged in the pipe of the sleeve cathode and the sleeve cathode applies
Metal cation deposited on the inner wall of the sleeve cathode, obtain the sedimentary of porous structure.
The embodiment of the present application is deposited in the pipe of sleeve cathode by electrolyte, it is only necessary to control relevant deposition ginseng
Number, it is easy to operate without the molds such as graphite rod auxiliary, and can be realized the sedimentary of different structure.
Further, after the sedimentary for obtaining porous structure, the method also includes:
The sedimentary of the porous structure is sintered in vacuum or protective atmosphere environment.It is more strong to obtain
Sedimentary.
Further, the method also includes:
Solution after reaction is discharged into solution recover by conduit, and will be anti-in the solution recover by pump
Solution after answering is delivered in the liquid storage device.It realizes and electrolyte is made full use of.
Further, the method also includes:
Make-up solution in liquid replenisher is introduced into the liquid storage device.So as to provide sufficient electrolyte, and can protect
Demonstrate,prove the concentration of electrolyte.
Further, the method also includes:
The liquid level information of electrolyte is detected by the liquid level sensor being arranged in liquid storage device, and is sent to the first controller
The liquid level information；First controller controls the aperture of the first valve between liquid replenisher and liquid storage device according to liquid level information, with
Adjust the fluid infusion to liquid storage device.By detecting the concentration of electrolyte automatically, to ensure that the electrolyte flowed into sleeve cathode
Concentration is identical.
Further, the method also includes:
The second valve is adjusted, to control flow velocity of the electrolyte in the pipe of sleeve cathode；Wherein, the second valve setting
At the second nozzle of the sleeve cathode.
Further, hydrionic concentration range is the saturated concentration of 0.001mol/L~first in the electrolyte, described
The concentration range of metal cation is the saturated concentration of 0.001mol/L~second；First saturated concentration be comprising the hydrogen from
The solution of son reaches hydrionic concentration when saturation, and second saturated concentration is the solution comprising the metal cation
Reach the concentration of metal cation when saturation.
Further, the voltage range of the power supply is 0.1V~300V, and the current density range is 0.001A/cm2
~10A/cm2, the electrodeposition time range is 1s~2h.
Further, the temperature range of sintering is 100 DEG C~2000 DEG C, and sintering time scope is 1min~30h.
Other feature and advantage of the application will be illustrated in subsequent specification, also, partly be become from specification
It is clear that by implementing the embodiment of the present application understanding.The purpose of the application and other advantages can be by written theorys
Specifically noted structure is achieved and obtained in bright book, claims and attached drawing.
Detailed description of the invention
Technical solution in ord to more clearly illustrate embodiments of the present application will make below to required in the embodiment of the present application
Attached drawing is briefly described, it should be understood that the following drawings illustrates only some embodiments of the application, therefore should not be seen
Work is the restriction to range, for those of ordinary skill in the art, without creative efforts, can be with
Other relevant attached drawings are obtained according to these attached drawings.
Fig. 1 is to flow electric deposition device structural schematic diagram in a kind of pipe provided by the embodiments of the present application；
Fig. 2 is another electric deposition device structural schematic diagram provided by the embodiments of the present application；
Fig. 3 is another electric deposition device structural schematic diagram provided by the embodiments of the present application；
Fig. 4 is a kind of preparation method flow diagram of electro-deposition porous structure provided by the embodiments of the present application；
Fig. 5 is a kind of electron microscope of porous structure provided by the embodiments of the present application；
Fig. 6 is the electron microscope of another porous structure provided by the embodiments of the present application；
Fig. 7 is the electron microscope of another porous structure provided by the embodiments of the present application.
Icon: 101- liquid storage device；102- sleeve cathode；103- anode；104- power supply；105- solution recover；106- pump；
107- liquid replenisher.
Specific embodiment
Below in conjunction with the attached drawing in the embodiment of the present application, technical solutions in the embodiments of the present application carries out clear, complete
Site preparation description.
In the description of the present application, it should be noted that the orientation or positional relationship of the instructions such as term "inner", "outside" is base
In orientation or positional relationship shown in the drawings or this application product using when the orientation or positional relationship usually put, only
It is the application and simplified description for ease of description, rather than the device or element of indication or suggestion meaning must have specifically
Orientation is constructed and operated in a specific orientation, therefore should not be understood as the limitation to the application.In addition, term " first ", " the
Two " etc. are only used for distinguishing description, are not understood to indicate or imply relative importance.
It should also be noted that, unless otherwise clearly defined and limited, term " setting ", " connection " should do broad sense reason
Solution, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can be directly connected, it can also be with
Indirectly connected through an intermediary, it can be the connection inside two elements.For the ordinary skill in the art, may be used
The concrete meaning of above-mentioned term in this application is understood with concrete condition.
Fig. 1 is to flow electric deposition device structural schematic diagram in a kind of pipe provided by the embodiments of the present application, as shown in Figure 1, should
Device includes liquid storage device 101, sleeve cathode 102, anode 103 and power supply 104, in which:
Sleeve cathode 102 can be connect by conducting wire with the cathode of power supply 104, and anode 103 passes through conducting wire and power supply 104
Anode connection, and anode 103 is located inside the tubular structure of sleeve cathode 102.Wherein it is possible to by anode 103 along sleeve cathode
102 axis direction fixed setting, such as: connector can be used, anode is fixed, connector can for metallic rod or
Person's plastic bar, but one end of bar and anode 103 are fixed, and the other end and the sleeve cathode of bar are fixed, to realize anode 103 in pipe
The hanging setting in 102 inside of shape cathode.It should be noted that the material of connector needs significant reaction not to occur with electrolyte
Material.The length of anode 103 can the slightly short length with sleeve cathode 102, the electro-deposition that also can according to need acquisition is porous
The length of structure determines.Since conduit is connect with the first nozzle of sleeve cathode 102, if the second of sleeve cathode 102 manages
Mouth is in opening-wide state, then the conducting wire of 104 anode of connection power supply and anode 103 can be from the second nozzle of sleeve cathode 102
It passes through.If having conduit connection at the first nozzle and the second nozzle, can be opened on conduit or above the pipe of sleeve cathode 102
Hole passes through the conducting wire of 104 anode of connection power supply and anode from tapping.It should be noted that position of opening can be with
Guarantee that electrolyte is not leaked, the embodiment of the present application is not specifically limited position of opening.In addition, power supply 104 can be
D.C. regulated power supply, be also possible to square wave, oblique wave, pulsed voltage or electric current, can also be other kinds of voltage or
Electric current can be configured, the embodiment of the present application is not especially limited this according to the actual situation in actually preparation.
Liquid storage device 101 is connect for storing electrolyte, and by conduit with the first nozzle of sleeve cathode 102, liquid storage device
Electrolyte in 101 is entered by conduit in the pipe of sleeve cathode 102, under the action of electric field, metal sun in electrolyte from
Son adheres on the inner wall of sleeve cathode 102, to obtain the sedimentary of porous structure.Solution after reaction is from sleeve cathode
102 the second nozzle outflow can place recycling bin in the lower section of sleeve cathode 102, so that the solution after reaction flows into recycling
In bucket.It should be noted that liquid storage device 101 and conduit are the material that significant reaction does not occur with electrolyte at normal temperature.
In addition, the shape of sleeve cathode 102 can be round tube, semi-circular tube, rectangular tube, triangle tube, hexagonal tube, and
Other polygonal tubes etc..The material of sleeve cathode 102 includes the metal simple-substance not reacted with electrolyte, inert conductor or not
The mixture of the metal simple-substance and inert conductor that react with the electrolyte can also be that surface passes through the methods of chemical plating
It is nonmetallic to generate silicon, plastics of conductive layer etc..Such as can be the inert conductors such as graphite, can also according to electrolyte select not with
The material that electrolyte reacts.
The material for constituting anode 103 may include metal simple-substance, inert conductor either metal simple-substance and inert conductor
Mixture.Wherein, metal simple-substance can be metal simple-substance to be deposited, be also possible to other metal simple-substances such as silver, platinum, and inertia is led
Body can be graphite.The embodiment of the present application is not specifically limited the selection of the material of sleeve cathode 102 and anode 103.
It should be noted that sleeve cathode 102 is also a factor for influencing Structure of the deposits at a distance from anode 103,
Therefore, the sleeve cathode 102 of respective diameters can be selected according to different needs.It is uniformly deposited to allow to generate structure
Layer, anode 103 can be configured along the axle center of sleeve cathode 102, thus guarantee anode 103 to sleeve cathode 102 away from
It is equal from radially.Certainly, for some sedimentaries, anode 103 can not also be arranged in the axle center of sleeve cathode 102,
Specifically the position inside sleeve cathode 102 can be adjusted anode 103 according to actual needs, the embodiment of the present application to this not
Make specific limit.
Electrolyte is revealed in order to prevent, and the bore of conduit can be identical as the caliber size of sleeve cathode 102, and passes through company
Fitting is by sealing joint, wherein connector can be plastic adhesive tape etc..It is also possible that the bore of conduit is less than sleeve cathode
102 bore protrudes into conduit in the first nozzle of sleeve cathode 102.
Electric deposition device provided by the embodiments of the present application can prepare the deposition of the micro-nano structure of different-shape in pipe
Layer, does not need the molds such as graphite rod auxiliary, the porous structure that can be formed in the tube different-thickness by adjusting technological parameter
Sedimentary.
On the basis of the above embodiments, the solution after recycling is reacted for convenience, which further includes solution recover
105, solution recover 105 is connect by conduit with the second nozzle of sleeve cathode 102.It should be noted that conduit is normal
The material for significant reaction not occurring with electrolyte under temperature is made.Solution leakage after reacting in order to prevent, the bore of conduit can be with
It is identical as the caliber size of the second nozzle of sleeve cathode 102, it is connect conduit to be aligned with the second nozzle of sleeve cathode 102
Afterwards, it is sealed against by connector.The bore of conduit can also be greater than the bore of the second nozzle of sleeve cathode 102, at this point, pipe
Second nozzle of shape cathode 102 protrudes into the second conduit.
On the basis of the above embodiments, Fig. 2 is another electric deposition device structural representation provided by the embodiments of the present application
Figure, as shown in Figure 2.After electrolyte flows through in the pipe of sleeve cathode 102, metal ion therein will not all with anode 103 into
Row reaction, therefore may further include metal cation to be deposited in the solution after reaction, in order to make full use of electrolyte,
Solution recover 105 is connect by conduit with liquid storage device, and the device further includes pump 106, and pump 106 can be set in conduit
On, the effect for pumping 106 is that the solution after the reaction in solution recover 105 is imported into liquid storage device 101, to realize liquid
The recycling of (solution after electrolyte and reaction).It is understood that another effect of pump 106 can control liquid
The speed of flowing.When carrying out the preparation of porous structure using the device, the switch of pump can be manually controlled, and adjust pump
Relevant parameter, to control the speed of the solution after conveying reaction.
Fig. 3 is another electric deposition device structural schematic diagram provided by the embodiments of the present application, as shown in figure 3, in order to guarantee
The concentration for flowing into the electrolyte in 102 pipe of sleeve cathode, can be set liquid replenisher 107, and liquid replenisher 107 passes through conduit and liquid storage device
101 connections, liquid replenisher 107 is for storing make-up solution, it is to be understood that the concentration of make-up solution can be with liquid storage device 101
The concentration of middle electrolyte is identical, can also be different, and can specifically be configured according to the actual situation.
On the basis of the above embodiments, in order to automatic liquid supply, which further includes liquid level sensor,
One controller and the first valve.Liquid level sensor is arranged inside liquid storage device, for detecting the liquid level information in liquid storage device 101,
And liquid level information is sent to the first controller, the conduit of connection liquid storage device 101 and liquid replenisher 107 is arranged in the first valve
On.First controller can control the aperture of the first valve according to liquid level information.Such as: it can preset in liquid storage device 101
Minimum liquid level and highest liquid level, when the liquid level information that the first controller receives is less than the aperture of minimum liquid level then control valve
Increase, so that the make-up solution in liquid replenisher 107 flows into liquid storage device 101.When the liquid level information that the first controller receives reaches
When to highest liquid level, the first valve of control is closed.
The liquid of the electrolyte in automatic adjustment liquid storage device is realized by liquid level sensor, the first controller and the first valve
Position.
On the basis of the above embodiments, the concentration of electrolyte can have an impact the structure of deposition layer, for some
The preparation of deposition layer needs to keep concentration constant during the preparation process, Concentration Testing can be arranged inside liquid storage device 101
Device, concentration detector is used to detect the concentration information in liquid storage device 101, and concentration information is sent to the first controller.Generally
In the case of, with the recycling of solution, the concentration of the electrolyte in liquid storage device 101 is being reduced, therefore can be in liquid replenisher 107
In be stored with the make-up solution higher than preset concentration.Preset concentration can be set in the controller, if concentration information is lower than default
Concentration then controls the first valve opening, so that make-up solution flows into liquid storage device 101.It is understood that concentration detector can
By be conductance type densimeter, in terms of electromagnetic type thickness, density type densimeter or nuclear radiation formula densimeter etc..
The embodiment of the present application more accurately control can prepare the concentration of deposition layer by setting concentration detector.
On the basis of the above embodiments, in order to accurately control the reaction time, which can also include switch
And second controller.Switch is arranged on the circuit that power supply 104, sleeve cathode 102 and anode 103 are constituted.Second controller
In include timer, and second controller can control the opening and closing of switch.It, can be in second controller before preparation starts
Reaction time is set, and when preparing beginning, timer starts simultaneously at timing, meets the reaction time of setting when the real reaction time
When, second controller control switch disconnects.
It should be noted that the first valve can be electrically operated valve, the first controller and second controller may each be 51
Single-chip microcontroller, also concentration sensor is connect with the I/O port of 51 single-chip microcontrollers liquid level sensor, and the information that will test is sent to first
Controller, the first valve are also connect with the I/O port of 51 single-chip microcontrollers, control instruction are sent to the first valve by I/O port, with realization pair
The control of first valve opening.Switch is connect with the I/O port of second controller, and second controller passes through the logical of I/O port control switch
It is disconnected.It should be noted that the first controller can also be that electric valve controller etc., second controller are also possible to other models
Single-chip microcontroller.
On the basis of the above embodiments, the structure that the flow velocity of electrolyte can also treat sedimentary has an impact, therefore, can
The second valve, and the drain pipe connected by the second valve to be arranged at the second nozzle of sleeve cathode 102, pass through adjusting
The flow velocity of the aperture control electrolyte of second valve, and the solution after reaction can be discharged by drain pipe.It is understood that
, the second valve can be manually-operated gate, is also possible to solenoid valve etc..
On the basis of the above embodiments, which includes thermostat, it is to be appreciated that thermostat for pair
The temperature of electrolyte in liquid storage device 101 is controlled, and can be heater, is also possible to refrigerator.The temperature of electrolyte
Also deposition layer structure can be had an impact, when other conditions (referring to the factors such as voltage, sedimentation time) are constant, increases electrolyte
Temperature, it will usually accelerate the diffusion velocity of cathode reaction speed and metal cation, reduce cathodic polarization effect, thus also can
Make to crystallize thicker.Therefore, when the temperature that electrolyte needs is higher than room temperature, heater can be set, heater is in liquid storage device
Electrolyte heated.Such as: heater can be electric heating wire or alcolhol burner, by heating wire or alcolhol burner as liquid storage device
Lower section, by realizing the heating to the electrolyte in liquid storage device to liquid storage device bottom-heated.In addition, heater can also be
Heating rod, heating rod do not react with electrolyte, and heating rod is placed on inside liquid storage device, and electrolyte contacts, to realize pair
Electrolyte directly heats.It should be noted that heater can also be arranged, inside sleeve cathode to realize to electrolyte
Heating.In addition, when the temperature that electrolyte needs is lower than room temperature, refrigerator can be set in the preparation of some sedimentaries.Example
Such as: refrigerator, which can be, cools down to liquid storage device by liquid nitrogen, to realize the control to electrolyte temperature.Also, this Shen
Please embodiment the selection of control temp (heater or refrigerator) is not specifically limited, as long as can reach to the electricity in liquid storage device
Solution liquid is heated or is cooled down.
In addition, temperature sensor can be set inside liquid storage device in order to guarantee that the temperature of electrolyte in liquid storage device is constant,
The temperature of electrolyte is detected by temperature sensor, and is heated according to temperature control heater.
Fig. 4 is a kind of preparation method flow diagram of electro-deposition porous structure provided by the embodiments of the present application, such as Fig. 4 institute
Show, comprising:
Step 401: the electrolyte in liquid storage device being introduced by conduit in the pipe of sleeve cathode.
When introducing electrolyte in the pipe of sleeve cathode, liquid storage device be can be set in the top of sleeve cathode, pass through weight
The effect of power is so that electrolyte flows via a conduit in the pipe of sleeve cathode.Furthermore it is also possible to which pump is arranged at conduit, pass through pump
Electrolyte is transported in the pipe of sleeve cathode.It is understood that including certain density hydrogen ion and centainly in electrolyte
The metal cation of concentration, which is well prepared in advance, and the electrolyte prepared is poured into liquid storage device.Pass through pump
The benefit of the mode of importing is the flow velocity that can control electrolyte.
Wherein, hydrionic concentration range be the saturated concentration of 0.001mol/L~first, such as can for 0.001mol/L,
0.01mol/L, 11mol/L, 3mol/L and 6mol/L etc..First saturated concentration is hydrogen when reaching saturation comprising hydrionic solution
The concentration of ion.It is different when reaching saturation containing hydrionic solution, it includes hydrogen ion concentration it is different.And it is hydrionic
Source can be acid, such as: sulfuric acid can also derive from strong acid weak base salt, such as ammonium chloride, can also be other contain hydrogen from
The solution of son.The concentration range of metal cation is the saturated concentration of 0.001mol/L~second；Second saturated concentration is to include gold
The concentration of metal cation when the solution for belonging to cationic reaches saturation.Different solution containing metal cation, reach full
With when included the concentration of metal cation it is different.It should be noted that the concentration difference meeting of hydrogen ion and metal cation
Obtain the sedimentary of different porous structures.And hydrionic concentration can also be adjusted according to the actual situation, such as maximum
Concentration can also be 10mol/L, 15mol/L etc..
Step 402: being driven by the electric field that the anode being arranged in the sleeve cathode and the pipe of the sleeve cathode applies
Metal cation in electrolyte deposits on the inner wall of the sleeve cathode, obtains the sedimentary of porous structure.
Sleeve cathode connects the cathode of power supply, and anode connects the volume anode of power supply, passes through power supply, sleeve cathode and anode structure
At circuit, sleeve cathode and anode produce electric field, when electrolyte flows into the pipe of sleeve cathode, under the action of electric field
Metal cation is deposited on the inner wall of sleeve cathode, to obtain the sedimentary of porous structure.
The embodiment of the present application by by anode be arranged inside sleeve cathode, by electrolyte import sleeve cathode pipe in from
And the sedimentary of porous structure is obtained, and it only needs to adjust relevant parameter when preparing, it is easy to operate, and can be formed a variety of
Structure, the sedimentary of multi-thickness.
In addition, the preparation of deposition layer can be divided into galvanostatic method and constant voltage method by the supply mode of electric energy used in it.
Galvanostatic method is using constant-current electrolysis.Constant voltage method is that electrode voltage when will be electrolysed is constant in a certain value, is made in electrolyte
Metal cation occur electrochemical reduction and be precipitated.It should be noted that other methods, such as current increase can also be used
Method, the embodiment of the present application is not especially limited this.
Voltage, current density and electrodeposition time can all have an impact porous structure, also, the voltage range of power supply
For 0.1V~300V, such as: it can be 0.1V, 100V, 200V, 300V etc..Current density range is 0.001A/cm2~10A/
cm2, such as: it can be 0.001A/cm2、1A/cm2、5A/cm2、10A/cm2Deng.Electrodeposition time range is 1s~2h, such as can
To be 1s, 30min, 1h, 2h etc..Can according to actual needs, regulating power source voltage, current density or electrodeposition time.
In order to obtain more strong porous structure, after completing preparation, the sedimentary of porous structure can be put
Enter and is sintered in vacuum or protective atmosphere.Wherein, protective atmosphere can be nitrogen or nitrogen hydrogen mixeding gas etc..The temperature of sintering
Be 100 DEG C~2000 DEG C, such as: can be 100 DEG C, 500 DEG C, 1000 DEG C, 1500 DEG C or 2000 DEG C, sintering time be 1min~
30h, such as: it can be 1min, 30min, 1h, 5h, 10h, 20h or 30h.
On the basis of the above embodiments, due to being likely present metal cation in the solution after reaction, in order to
Electrolyte is made full use of, the solution after reaction can be imported in solution recover, and will be anti-in solution recover by pump
Solution after answering, which is transported in liquid storage device, to be continued to use.It is Ke Yitong by pumping the benefit conveyed to the solution after reaction
The running parameter of control pump is crossed to control the amount of the solution after reaction is added into liquid storage device, is unlikely to the electricity so that in liquid storage device
It is too small to solve liquid concentration.
On the basis of the above embodiments, it will lead to the dense of the metal cation in electrolyte since electrolyte is recycled
Degree and the decline of hydrionic concentration, at this point it is possible to supplement electrolyte into liquid storage device by liquid replenisher.It is understood that
Make-up solution in liquid replenisher also includes certain density hydrogen ion and metal cation, and concentration can be more initial than in liquid storage device
Electrolyte concentration it is high.It is of course also possible to identical as the concentration of electrolyte initial in liquid storage device.
On the basis of the above embodiments, in the pipe in order to guarantee the electrolyte inflow sleeve cathode for having sufficient, can make
Make-up solution is carried out to liquid storage device with liquid replenisher, but needs to guarantee that electrolyte does not spill over liquid storage device again, it at this time can be in liquid storage
Liquid level sensor is set in device, and liquid level sensor can monitor the liquid level information of liquid storage device electrolyte inside, and by liquid level information
It is sent to the first controller, the first controller can be controlled according to aperture of the liquid level information to the first valve.Such as: first
Controller judges whether liquid level information is too high or too low, and judgment basis can be to set liquid storage device in the first controller in advance
In highest liquid level and minimum liquid level.If liquid level information is greater than highest liquid level, illustrate that the electrolyte in liquid storage device is excessive, in order to
It prevents from overflowing, connection liquid storage device is arranged in the control of the first controller and supravasal first valve of liquid replenisher is closed.If liquid level
Information is less than minimum liquid level, then illustrates that the electrolyte in liquid storage device is very few, in order to guarantee the electrolyte for having sufficient, the first controller
The first valve opening is controlled, the make-up solution in liquid replenisher is introduced into liquid storage device by conduit.It is understood that liquid level passes
Sensor can be contact liquid level sensor, including single flange static pressure, double flange differential pressure liquid level sensors, floating ball type liquid level sensing
Device, magnetic liquid level sensor, capacitance level transducer；It can also be noncontacting proximity sensor, such as: supersonic liquid level sensing
Device, radar level sensor etc..
In some embodiments, it is desirable to by flow into sleeve cathode in concentration of electrolyte be maintained at one it is metastable
Value, can be arranged concentration sensor inside liquid storage device, and the concentration letter of electrolyte in liquid storage device is detected by concentration sensor
Breath, and concentration information is sent to the first controller, the first controller controls the aperture of the first valve according to concentration information.And
Third valve can also be set between liquid recovery device and liquid storage device, and the first controller can also be according to the same time control of concentration information
The aperture of the first valve and third valve is made, so that the concentration of the electrolyte in liquid storage device is maintained at metastable value.
In some embodiments, the temperature of electrolyte can also have an impact porous structure, therefore, for need temperature compared with
When high electrolyte, can use heater and electrolyte heated, wherein heater can be alcolhol burner, be also possible to electricity plus
Hot pin etc. when if alcolhol burner, can heat liquid storage device bottom, carry out indirect heating to electrolyte by heat-conduction principle.If
When heater is electrically heated rod, electrically heated rod can be put into liquid storage device, directly electrolyte is heated.In order to enable electrolysis
Liquid is heated evenly, and stirring rod can be used and be stirred to electrolyte.
In order to more precisely control the temperature of electrolyte, temperature sensor can be set in liquid storage device, it can be with
The temperature of electrolyte is checked by temperature sensor, operator can manually control the parameters such as heating time according to temperature.Into
One step, in order to realize automatic heating, by taking heater is electrically heated rod as an example, temperature sensor can connect with the first controller
It connects, the first controller is also connect with electrically heated rod, also, the first controller can control the heating parameters of electrically heated rod.Temperature
The temperature information that sensor will test is sent to the first controller, and the first controller carries out electrically heated rod according to temperature information
Control.
In some embodiments, flow velocity of the electrolyte in the pipe of sleeve cathode can have an impact to obtained porous structure,
Therefore, for coutroi velocity, the second valve can be set in the second nozzle of sleeve cathode, by the aperture of the second valve come real
Now to the control of electrolyte flow rate.
In some embodiments, the metal to be deposited of various concentration deposits if other conditions are the same, obtains
The porous structure of sedimentary is different, is 1A/cm in current density by experiment2When, the pattern on cellular porous surface is with sulfuric acid
Concentration of copper sulfate situation of change.When the concentration for controlling sulfuric acid is 1.84M, with the increase of concentration of copper sulfate in solution,
Cellular porous surface evolves as the cellular structures of single layer from double-deck honeycomb.When control copper sulphate it is dense
When degree is 0.8M, the reduction meeting of sulfuric acid concentration is so that the hole wall on porous structure surface is thinning.
In some embodiments, the reaction time of electro-deposition is also an influence factor for influencing sedimentary pattern.Respectively
It is 150s, 300s, 450s, 600s that sedimentation time, which is arranged,.Control CuSO in electrolyte4Concentration be 0.6M, H2SO4Concentration is chosen
0.4M, current rise rate are 0.67mA/ (cm2S), anode and cathode spacing is controlled in 3.5cm when reaction.Experimental result is, with
The growth of sedimentation time, the thickness on fakement surface has apparent increase, and the dendrite arm of sedimentary becomes larger.
Several groups of specific application examples are described below:
In some embodiments, referring to Fig. 3, the electrolyte stored in liquid storage device is the H of 3mol/L2SO4, 0.5mol/L
CuSO4, connect on the positive and negative anodes of power supply, compensated by conducting wire respectively as anode as sleeve cathode, silver-colored stick using copper tube
Device is provided with the (H of 6mol/L2SO4, 1mol/L CuSO4) mixed solution.After opening pump, solution is flowed out from liquid storage device, is passed through
Conduit flows through sleeve cathode, then reaches solution recover by conduit, and come back to liquid storage device by conduit and pump.It opens
Power supply, in 0.5A/cm2Current density under electro-deposition 200s, porous structure sedimentary is obtained on cathode.The porous structure
Electron microscope is as shown in Figure 5.Fig. 5 is the electron microscope picture for amplifying 3000 times, shows the micro-nano porous structure being prepared into coral
Shape dendrite arm structure, the size of dendrite arm are about 1um, and many micron orders and nanoscale hole are formd between dendrite arm.Terminate in reaction
Afterwards, 5ml mixed electrolytic solution, the copper ion and hydrogen ion consumed in supplement reaction are supplemented to liquid storage device using liquid replenisher, then carried out
It tests next time.
In some embodiments, referring to fig. 2, the electrolyte stored in liquid storage device is the H of 3mol/L2SO4, 0.5mol/L
CuSO4, conducting wire is passed through as anode as sleeve cathode, stainless steel using copper tube respectively and is connect on the positive and negative anodes of power supply.It opens
After opening pump, solution is flowed out from liquid storage device, flows through sleeve cathode by conduit, then reaches solution recover by conduit, and lead to
It crosses conduit and pump comes back to liquid storage device.Power supply is opened, in 0.3A/cm2Current density under electro-deposition 240s, in sleeve cathode
On obtain porous structure sedimentary.The electron microscope of the porous structure is as shown in Figure 6.Fig. 6 is the electron microscope for amplifying 1000 times
Figure shows the micro-nano porous structure that is prepared into cauliflower shape, and the size of cauliflower is some tens of pm, on each cauliflower again there are many
Several microns of small particles.
In some embodiments, referring to Fig. 1, the electrolyte stored in liquid storage device is the H of 3mol/L2SO4, 0.5mol/L
CuSO4, connect on the positive and negative anodes of power supply by conducting wire respectively as sleeve cathode, copper rod as anode using copper tube.It opens
After power supply, solution is flowed out from liquid storage device, flows through sleeve cathode by conduit, then reaches solution recover, In by conduit
0.5A/cm2Current density under electro-deposition 120s, porous structure sedimentary is obtained on sleeve cathode.The electricity of the porous structure
Mirror figure is as shown in Figure 7.Fig. 7 is the electron microscope picture for amplifying 1000 times, shows that the micro-nano porous structure being prepared into is in cauliflower shape,
The size of cauliflower is some tens of pm, and there are many several microns of small particles again on each cauliflower.But since the time of reaction is partially short,
Its cauliflower structure is not as good as the abundant of Fig. 6.
In embodiment provided herein, it should be understood that disclosed device and method, it can be by others side
Formula is realized.The apparatus embodiments described above are merely exemplary, for example, the division of the unit, only one kind are patrolled
Function division is collected, there may be another division manner in actual implementation, in another example, multiple units or components can combine or can
To be integrated into another system, or some features can be ignored or not executed.Another point, shown or discussed is mutual
Coupling, direct-coupling or communication connection can be INDIRECT COUPLING or communication link by some communication interfaces, device or unit
It connects, can be electrical property, mechanical or other forms.
In addition, unit may or may not be physically separated as illustrated by the separation member, as unit
The component of display may or may not be physical unit, it can and it is in one place, or may be distributed over more
In a network unit.Some or all of unit therein can be selected to realize this embodiment scheme according to the actual needs
Purpose.
Furthermore each functional module in each embodiment of the application can integrate one independent portion of formation together
Point, it is also possible to modules individualism, an independent part can also be integrated to form with two or more modules.
Herein, relational terms such as first and second and the like be used merely to by an entity or operation with it is another
One entity or operation distinguish, and without necessarily requiring or implying between these entities or operation, there are any this reality
Relationship or sequence.
The above description is only an example of the present application, the protection scope being not intended to limit this application, for ability
For the technical staff in domain, various changes and changes are possible in this application.Within the spirit and principles of this application, made
Any modification, equivalent substitution, improvement and etc. should be included within the scope of protection of this application.
Claims (21)
1. flowing electric deposition device in a kind of pipe characterized by comprising liquid storage device, sleeve cathode, anode and power supply；
Wherein, the sleeve cathode is connect with the cathode of the power supply；
The anode is set to inside the pipe of the sleeve cathode, and the anode is connect with the anode of the power supply；
The liquid storage device is connect by conduit with the first nozzle of the sleeve cathode for storing electrolyte, the liquid storage device.
2. the apparatus according to claim 1, which is characterized in that described device includes solution recover, the solution recycling
Device is connect by conduit with the second nozzle of the sleeve cathode；The solution recover is used for the solution after storage reaction.
3. the apparatus of claim 2, which is characterized in that the solution recover is connected by conduit and the liquid storage device
It connects；
Described device further include: the pump on the channel between the solution recover and the liquid storage device is set, is used for institute
The solution in solution recover is stated to be transported in the liquid storage device.
4. the apparatus of claim 2, which is characterized in that described device includes liquid replenisher；The liquid replenisher is by leading
Pipe is connect with the liquid storage device, and the liquid replenisher is for storing make-up solution.
5. device according to claim 4, which is characterized in that described device further includes liquid level sensor, the first controller
With the first valve；The liquid level sensor and first valve are connect with first controller；The liquid level sensor
It is set to inside the liquid storage device, for detecting the liquid level information in the liquid storage device；The first valve setting is in connection institute
On the conduit for stating liquid storage device and the sleeve cathode；First controller is used to receive the described of the liquid level sensor transmission
Liquid level information, and according to the aperture of the liquid level information the first valve of control.
6. device according to claim 5, which is characterized in that described device further includes concentration detector, the concentration inspection
It surveys device to be set to inside the liquid storage device, be controlled for detecting the concentration information of electrolyte in the liquid storage device, and to described first
Device processed sends the concentration information；First controller controls the aperture of first valve according to the concentration information.
7. the apparatus according to claim 1, which is characterized in that device further includes switch and second controller, the switch
It is arranged on the circuit that the power supply, sleeve cathode and anode are constituted；The second controller includes timer, second control
Device processed be used for according to timer control described in switch on-off.
8. the apparatus according to claim 1, which is characterized in that described device further include:
Second the second valve of nozzle of the sleeve cathode is set；And
The drain pipe being connect by second valve with the second nozzle.
9. the apparatus according to claim 1, which is characterized in that described device further includes thermostat, and the thermostat is used for
The temperature of electrolyte in the liquid storage device is controlled.
10. the apparatus according to claim 1, which is characterized in that the shape of the sleeve cathode is round tube, semi-circular tube or more
Side shape pipe.
11. -10 described in any item devices according to claim 1, which is characterized in that the material of the sleeve cathode include not with
Metal simple-substance, inert conductor or the metal simple-substance not reacted with the electrolyte and inertia that the electrolyte reacts
The mixture of conductor.
12. -10 described in any item devices according to claim 1, which is characterized in that the material of the anode includes metal list
The mixture of matter, inert conductor or metal simple-substance and inert conductor.
13. a kind of preparation method of electro-deposition porous structure characterized by comprising
Electrolyte in liquid storage device is introduced by conduit in the pipe of sleeve cathode；
The gold in electrolyte is driven by the electric field that the anode being arranged in the pipe of the sleeve cathode and the sleeve cathode applies
Belong to cation to deposit on the inner wall of the sleeve cathode, obtains the sedimentary of porous structure.
14. according to the method for claim 13, which is characterized in that after the sedimentary for obtaining porous structure, the side
Method further include:
The sedimentary of the porous structure is sintered in vacuum or protective atmosphere environment.
15. according to the method for claim 13, which is characterized in that the method also includes:
Solution after reaction is discharged into solution recover by conduit, and will be after the reaction in the solution recover by pump
Solution be delivered in the liquid storage device.
16. according to the method for claim 13, which is characterized in that the method also includes:
Make-up solution in liquid replenisher is introduced into the liquid storage device.
17. according to the method for claim 13, which is characterized in that the method also includes:
The liquid level information of electrolyte is detected by the liquid level sensor being arranged in liquid storage device, and to described in the transmission of the first controller
Liquid level information；
First controller controls the aperture of the first valve between liquid replenisher and liquid storage device according to liquid level information, to adjust to liquid storage
The fluid infusion of device.
18. according to the method for claim 13, which is characterized in that the method also includes:
The second valve is adjusted, to control flow velocity of the electrolyte in the pipe of sleeve cathode；Wherein, second valve is arranged in institute
It states at the second nozzle of sleeve cathode.
19. according to the method for claim 13, which is characterized in that hydrionic concentration range is in the electrolyte
The saturated concentration of 0.001mol/L~first, the concentration range of the metal cation are the saturated concentration of 0.001mol/L~second；
First saturated concentration is hydrionic concentration when reaching saturation comprising the hydrionic solution, second saturation
Concentration is the concentration that the solution comprising the metal cation reaches metal cation when saturation.
20. the described in any item methods of 3-19 according to claim 1, which is characterized in that the voltage range of power supply be 0.1V~
300V, current density range 0.001A/cm2~10A/cm2, electrodeposition time range is 1s~2h.
21. according to the method for claim 14, which is characterized in that the temperature range of sintering is 100 DEG C~2000 DEG C, sintering
Time range is 1min~30h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910897746.XA CN110499522A (en) | 2019-09-20 | 2019-09-20 | A kind of interior preparation method for flowing electric deposition device and electro-deposition porous structure of pipe |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910897746.XA CN110499522A (en) | 2019-09-20 | 2019-09-20 | A kind of interior preparation method for flowing electric deposition device and electro-deposition porous structure of pipe |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110499522A true CN110499522A (en) | 2019-11-26 |
Family
ID=68592375
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910897746.XA Pending CN110499522A (en) | 2019-09-20 | 2019-09-20 | A kind of interior preparation method for flowing electric deposition device and electro-deposition porous structure of pipe |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110499522A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114214702A (en) * | 2021-12-20 | 2022-03-22 | 鸿富锦精密电子（成都）有限公司 | Method and apparatus for etching alloy plate having slot |
| CN114507888A (en) * | 2022-01-20 | 2022-05-17 | 江苏大学 | Electro-deposition preparation method and device for super-hydrophobic structure on inner wall of pipeline |
| CN115979382A (en) * | 2023-03-17 | 2023-04-18 | 山东省地质矿产勘查开发局八〇一水文地质工程地质大队(山东省地矿工程勘察院) | A drilling water level measuring device for hydrogeological survey |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4675085A (en) * | 1985-07-31 | 1987-06-23 | Adalberto Vasquez | Method and apparatus for recovery of metal from solution |
| US5200044A (en) * | 1989-04-24 | 1993-04-06 | Ephraim S. Greenberg | Method for measuring oxygen content |
| JPH0688285A (en) * | 1992-09-04 | 1994-03-29 | Iketsukusu Kogyo:Kk | Electrodeposition method of metal |
| KR20010094833A (en) * | 2000-04-07 | 2001-11-03 | 유주현 | Preparation of ceramic tube by electrophoretic deposition processing |
| JP2004059948A (en) * | 2002-07-25 | 2004-02-26 | Mishima Kosan Co Ltd | Method and apparatus for recovering metal from metal dissolution liquid |
| US20110233069A1 (en) * | 2010-03-24 | 2011-09-29 | Rasirc | Method and system for electrochemical hydrogen generation |
| CN103046088A (en) * | 2012-12-20 | 2013-04-17 | 华南理工大学 | Micro-nano composite porous copper surface structure and preparation method and device thereof |
| CN202968258U (en) * | 2012-12-13 | 2013-06-05 | 成都飞创科技有限公司 | Electrolysis scale removal device convenient to disassemble |
| CN107287650A (en) * | 2017-08-14 | 2017-10-24 | 江东电子材料有限公司 | A kind of electrolyte automatic regulating system and adjusting method |
| CN109023459A (en) * | 2018-08-04 | 2018-12-18 | 中山大学 | A kind of multiple dimensioned surface texture and preparation method thereof for strengthening boiling of bilayer |
| CN211005669U (en) * | 2019-09-20 | 2020-07-14 | 中山大学 | In-tube flowing electrodeposition device |
-
2019
- 2019-09-20 CN CN201910897746.XA patent/CN110499522A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4675085A (en) * | 1985-07-31 | 1987-06-23 | Adalberto Vasquez | Method and apparatus for recovery of metal from solution |
| US5200044A (en) * | 1989-04-24 | 1993-04-06 | Ephraim S. Greenberg | Method for measuring oxygen content |
| JPH0688285A (en) * | 1992-09-04 | 1994-03-29 | Iketsukusu Kogyo:Kk | Electrodeposition method of metal |
| KR20010094833A (en) * | 2000-04-07 | 2001-11-03 | 유주현 | Preparation of ceramic tube by electrophoretic deposition processing |
| JP2004059948A (en) * | 2002-07-25 | 2004-02-26 | Mishima Kosan Co Ltd | Method and apparatus for recovering metal from metal dissolution liquid |
| US20110233069A1 (en) * | 2010-03-24 | 2011-09-29 | Rasirc | Method and system for electrochemical hydrogen generation |
| CN202968258U (en) * | 2012-12-13 | 2013-06-05 | 成都飞创科技有限公司 | Electrolysis scale removal device convenient to disassemble |
| CN103046088A (en) * | 2012-12-20 | 2013-04-17 | 华南理工大学 | Micro-nano composite porous copper surface structure and preparation method and device thereof |
| CN107287650A (en) * | 2017-08-14 | 2017-10-24 | 江东电子材料有限公司 | A kind of electrolyte automatic regulating system and adjusting method |
| CN109023459A (en) * | 2018-08-04 | 2018-12-18 | 中山大学 | A kind of multiple dimensioned surface texture and preparation method thereof for strengthening boiling of bilayer |
| CN211005669U (en) * | 2019-09-20 | 2020-07-14 | 中山大学 | In-tube flowing electrodeposition device |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114214702A (en) * | 2021-12-20 | 2022-03-22 | 鸿富锦精密电子（成都）有限公司 | Method and apparatus for etching alloy plate having slot |
| CN114507888A (en) * | 2022-01-20 | 2022-05-17 | 江苏大学 | Electro-deposition preparation method and device for super-hydrophobic structure on inner wall of pipeline |
| CN114507888B (en) * | 2022-01-20 | 2023-09-26 | 江苏大学 | Electrodeposition preparation method and device for pipeline inner wall super-hydrophobic structure |
| CN115979382A (en) * | 2023-03-17 | 2023-04-18 | 山东省地质矿产勘查开发局八〇一水文地质工程地质大队(山东省地矿工程勘察院) | A drilling water level measuring device for hydrogeological survey |
| CN115979382B (en) * | 2023-03-17 | 2023-06-20 | 山东省地质矿产勘查开发局八〇一水文地质工程地质大队(山东省地矿工程勘察院) | Drilling water level measuring device for hydrogeology investigation |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110499522A (en) | A kind of interior preparation method for flowing electric deposition device and electro-deposition porous structure of pipe | |
| CN211005669U (en) | In-tube flowing electrodeposition device | |
| US5630932A (en) | Tip etching system and method for etching platinum-containing wire | |
| US2571709A (en) | Apparatus for electroplating articles | |
| CN106811778A (en) | The preparation and palladium-copper alloy film and application of component and the controllable palladium-copper alloy film of thickness | |
| EP2664692A2 (en) | Plating apparatus and plating solution management method | |
| Chen et al. | Electrodeposition and characterization of nanocrystalline CoNiFe films | |
| CN104032339A (en) | Method for controlling electro-deposition nickel-tungsten alloy coating structure | |
| CN108666526A (en) | A kind of lithium ion cell positive and prepare the device of lithium ion cell positive, method | |
| CN100595578C (en) | Method for preparing platinum nano-perforated electrode by evaporation deposition | |
| CN208829786U (en) | A kind of electroplanting device | |
| CN110118793A (en) | Electrochemical in-situ experimental provision in a kind of electrochemistry sample clamp and scanning electron microscope | |
| CN116837424A (en) | Electrochemical additive manufacturing device and method for improving quality of workpiece | |
| CN104818512A (en) | Device and method for preparing magnetically soft alloy continuous films through electric deposition of soluble separated anodes | |
| CN108536197A (en) | A kind of porous air inlet Markov bottle and application method | |
| BJ | Thermal diffusivity of iron at high temperature in both the liquid and solid states | |
| Cai et al. | Non-Cyanide Thick Silver Electrodeposition Base on Instantaneous Nucleation for 3D Microstructures with High Performance | |
| CN206188913U (en) | Electroplating experiment platform that can realize undercurrent and can carry out high accuracy regulation and control | |
| CN108866582A (en) | A kind of technique of electrodeposition process preparation roughening nickel foil | |
| CN105648477A (en) | Preparation method of template-free electro-deposition SmCo nanowires | |
| CN108441911B (en) | The method that cathodic electrodeposition prepares manganese cobalt composite material | |
| Booking | High speed selective jet electrodeposition | |
| CN209247480U (en) | A kind of metallographic sample preparation electrolyzing and corroding device | |
| CN207498477U (en) | A kind of electron anode protection erosion protection system of phase-transition heat-storage equipment | |
| CN211005664U (en) | Copper foil electroplating experimental device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |