CN106086961B - Method based on supercritical fluid 3D electro-deposition process components - Google Patents
Method based on supercritical fluid 3D electro-deposition process components Download PDFInfo
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- CN106086961B CN106086961B CN201610592776.6A CN201610592776A CN106086961B CN 106086961 B CN106086961 B CN 106086961B CN 201610592776 A CN201610592776 A CN 201610592776A CN 106086961 B CN106086961 B CN 106086961B
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- 238000004070 electrodeposition Methods 0.000 title claims abstract description 75
- 239000012530 fluid Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 39
- 230000008569 process Effects 0.000 title claims abstract description 14
- 238000012545 processing Methods 0.000 claims abstract description 29
- 238000000429 assembly Methods 0.000 claims abstract description 16
- 230000000712 assembly Effects 0.000 claims abstract description 16
- 238000000151 deposition Methods 0.000 claims abstract description 15
- 230000008021 deposition Effects 0.000 claims abstract description 13
- 238000007747 plating Methods 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 4
- 239000011159 matrix material Substances 0.000 claims description 30
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 20
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- 239000000654 additive Substances 0.000 claims description 13
- 230000000996 additive effect Effects 0.000 claims description 13
- 239000001569 carbon dioxide Substances 0.000 claims description 10
- 229920006351 engineering plastic Polymers 0.000 claims description 9
- 238000009413 insulation Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 239000010949 copper Substances 0.000 claims description 8
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000013268 sustained release Methods 0.000 claims description 7
- 239000012730 sustained-release form Substances 0.000 claims description 7
- -1 ether compound Chemical class 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000033001 locomotion Effects 0.000 claims description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004327 boric acid Substances 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- 150000002815 nickel Chemical class 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 230000033228 biological regulation Effects 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 230000003068 static effect Effects 0.000 claims description 3
- 229910002056 binary alloy Inorganic materials 0.000 claims description 2
- 239000000839 emulsion Substances 0.000 claims description 2
- 238000012805 post-processing Methods 0.000 claims description 2
- 238000003672 processing method Methods 0.000 abstract description 4
- 238000005323 electroforming Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 230000005684 electric field Effects 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000012266 salt solution Substances 0.000 description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000001879 copper Chemical class 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
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- 238000004062 sedimentation Methods 0.000 description 1
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- 238000003860 storage Methods 0.000 description 1
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- 229910052717 sulfur Inorganic materials 0.000 description 1
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- 238000002604 ultrasonography Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/003—3D structures, e.g. superposed patterned layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y30/00—Apparatus for additive manufacturing; Details thereof or accessories 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
-
- 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
-
- 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
- C25D5/003—Electroplating using gases, e.g. pressure influence
-
- 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
- C25D5/04—Electroplating with moving electrodes
Abstract
Present invention offer is a kind of by the method for the process component implemented based on supercritical fluid 3D electro-deposition processing unit (plant), and device includes dioxide bottle, high-pressure pump, CNC controller, reactor, mobile anode assemblies, swap cathode component, dc source and the cathode base as processed parts；Mechanical agitator is set in reactor；Mobile anode assemblies include Z-direction linear electric motors, driving leading screw, anode connecting rod and mobile anode；Swap cathode component includes X to the linear electric motors with Y-direction, guide rail, movable block and fixture；In use, mobile anode and cathode base electrically connect with the both positive and negative polarity of dc source respectively.Processing method mainly include cathode base in advance chemical plating, cathode base is installed, prepares supercritical fluid, electro-deposition processing and post-treating and other steps.The present invention can effectively improve electrodeposition rate, improve deposition quality, prepare complicated, precision metallic parts by electro-deposition in three dimensions, widen electro-deposition techniques application field.
Description
The application is Application No. 201410762856.2, and the applying date is on December 11st, 2014, and invention and created name is
The divisional application of the application for a patent for invention of " based on supercritical fluid 3D electro-deposition processing unit (plant) and method ".
Technical field
The present invention relates to electrochemical deposition processing technique field, and in particular to one kind is based on supercritical fluid 3D（It is three-dimensional）Electricity
The device and method of deposition process part.
Background technology
Electro-deposition techniques are the current focuses studied both at home and abroad under supercritical environment.Supercritical fluid
（Supercritical Fluid）Refer to that pure material is in critical point（Critical pressure and critical-temperature）During the above, showed
One kind out is between liquid and gaseous fluid.In Near The Critical Point, density, viscosity, solubility, the thermal capacitance of supercritical fluid
Phenomenon jumpy occurs for the physical property of all fluids such as amount, dielectric constant.CO2Gas has environmentally friendly, non-ignitable, nontoxic, lazy
Property, deposit is abundant and critical pressure（7.39MPa）With temperature (31.1 DEG C) it is less high the advantages that, therefore supercritical CO2Fluid quilt
Extensive utilization.Due to supercritical CO2With relatively low viscosity（0.03-0.1 MPa·s）Higher diffusion coefficient（10- 4
cm2·s-1）, good condition can be provided in electro-deposition system for mass transfer.At present Metal Substrate is prepared under supercritical fluid environment
The existing finding of the process and device of nano composite material and micro-workpiece.As Authorization Notice No. is CN 101092716B
Chinese patent literature discloses a kind of trickle electroforming technique of supercritical fluid and its device, and it is with SCF-CO2To electroplate ring
Border carries out the shaping of micro-structure part, metal plating layer surface depositing homogeneous as obtained by this method, without buildup, and cast layer group
Knit fine and closely woven smooth, but gained cast layer part is advance photoetching（Internal model）The part of shape, flexible it can not prepare different types of 3D
Parts；The Chinese patent literature that and for example publication No. is CN 102146573A proposes a kind of supercritical fluid electrotyping forming system
The method of standby nano composite material, mainly the electro-deposition under mechanical agitation subsidiary conditions prepares metal-based nano composite wood for it
Material, Electric Field Distribution is fixed, from the point of view of its parameter setting and anode and cathode are set, it is impossible to effectively carry out to parts in three-dimensional
Space is processed preparation by electro-deposition.Thus, by three-dimensionally shaped and motor in currently very popular 3D printing technique
Reason is applied in overcritical electro-deposition processing skill, and design one kind can carry out electro-deposition processing to parts in three dimensions and prepare
Device and processing method, it appears it is very necessary.
The content of the invention
The purpose of the present invention is：In view of the shortcomings of the prior art, there is provided one kind can effectively improve electrodeposition rate, improve and sink
Accumulate quality, complicated, precision metallic parts are prepared by electro-deposition in three dimensions, and electro-deposition techniques application field can be widened
Based on supercritical fluid 3D electro-deposition processing unit (plant) and using the device process component method.
The technical scheme is that：The method based on supercritical fluid 3D electro-deposition process components of the present invention, by
Based on supercritical fluid 3D electro-deposition processing unit (plant) implement, the device include dioxide bottle, high-pressure pump, CNC controller,
Reactor, dc source and the cathode base as processed parts；Above-mentioned reactor includes body and mechanical agitator；
Body is provided with air inlet, leakage fluid dram and heating coil；To reaction when above-mentioned dioxide bottle and high-pressure pump are used to use
Device provides carbon dioxide；It is characterized in that：Also include mobile anode assemblies and swap cathode component；
Above-mentioned mobile anode assemblies include Z-direction linear electric motors, driving leading screw, anode connecting rod and mobile anode；Z-direction is straight
Line motor is fixedly mounted on the top of the body of reactor；Leading screw is driven to be connected with Z-direction linear electric motors；Anode connecting rod with
Driving leading screw is fixedly connected；Driving leading screw is built-in with the elastic conduction coil being insulated from；Mobile anode anode connecting rod is fixed
Connection；The positive pole that mobile anode passes through the elastic conduction coil external direct current power supply built in anode connecting rod and driving leading screw；Move
The mobile anode of dynamic anode assemblies by Z-direction linear electric motors by driving the transmission of leading screw and anode connecting rod, can be in reactor
Pumped in body；
Above-mentioned swap cathode component is led including X to linear electric motors, X direction guiding rails, X to movable block, Y-direction linear electric motors, Y-direction
Rail, Y-direction movable block and fixture；X is fixedly mounted on the body of reactor to linear electric motors；X direction guiding rails point are front and rear to be provided with 2；X
Direction guiding rail is fixedly mounted on the intrinsic lower surface of reactor；X is arranged on X direction guiding rails to movable block and in X to straight line
X direction guiding rails or so can be relied under the driving of motor to linear slide；
Y-direction linear electric motors are fixedly mounted on X on the upper surface of movable block；Y-direction guide rail point or so is provided with 2；Y-direction guide rail
X is fixedly mounted on on the upper surface of movable block and Y-direction guide rail is vertically arranged with X direction guiding rails；On the upper surface of Y-direction movable block 66
Coated with insulation engineering plastics；Y-direction movable block is arranged in Y-direction guide rail and Y-direction can be relied on to lead under the driving of Y-direction linear electric motors
Rail is front and rear to linear slide；
The material of fixture is acidproof, high pressure resistant and high rigidity insulation engineering plastics；Fixture is arranged on the upper of Y-direction movable block
Cathode base is clamped on end face, during for using；In use, cathode base electrically connects with the negative pole of dc source.
The X of swap cathode component is to the Z-direction linear electric motors of linear electric motors and Y-direction linear electric motors and mobile anode assemblies
Operation controls by CNC controller；
The material of above-mentioned driving leading screw is stainless steel, inner hollow；Anode connecting rod is built-in copper framework and outer shoe
Insulation, the body of rod part of acidproof, high voltage bearing engineering plastics；Junction and anode of the above-mentioned driving leading screw with anode connecting rod
Connecting rod and the junction of mobile anode are sealed with high-pressure seal ring；
Above-mentioned mobile anode includes matrix and electrode；The material of matrix is glass, and matrix is by upper cylinder portion and lower circle
Trunk portion integrally forms, and the diameter in the upper cylinder portion of matrix is less than the diameter in lower cylinder portion, the upper cylinder portion of matrix with
Anode connecting rod is fixedly connected；Electrode is arranged in matrix and on the axial line of matrix.
Using the above-mentioned method based on supercritical fluid 3D electro-deposition processing unit (plant) process components, including following step
Suddenly：
1. cathode base chemical plating in advance：On the surface of the cathode base as processed parts, plating last layer is easy
In the uniform copper layer for about 10 μ m-thicks for carrying out electro-deposition；
2. cathode base is installed：Cathode base is fixed on to the upper end of Y-direction movable block by the fixture of swap cathode component
On face；The upward and downward position of the mobile anode of regulation, makes it not interference with swap cathode component；
3. prepare supercritical fluid：Two containing surface additive and electro-deposition sustained release agent configured are added in the reactor
First system plating solution；Binary system electroplate liquid containing surface additive and electro-deposition sustained release agent is nickel salt or copper salt solution；Surface
Additive is the additive being made up of dodecane base class compound and ether compound；Above-mentioned nickel salt or the concentration of copper salt solution
For 300~500g/L；The concentration of surface additive is 0.1~2g/L；Electro-deposition sustained release agent is concentration 30g/L~60g/L boron
Acid, bath pH values are controlled 2~6；After closed, carbon dioxide is passed through into reactor, controls the temperature in reactor
In 35~70 DEG C, pressure in the range of 8~20MPa, it is heavy as the ternary electricity of carrier using supercritical carbon dioxide emulsion to be formed
Product system；
4. electro-deposition is processed：Switch on power, the position of setting electro-deposition parameter and mobile anode opposing cathode matrix；In number
Control and carry out electro-deposition under the control of controller and the stirring auxiliary of mechanical agitator to obtain institute in the outer surface of cathode base
The deposition layer needed；The mobile anode of CNC controller control and swap cathode component are moved by the track of setting；Mobile anode phase
The maximum single direction stroke that moves up and down for the cathode base as cathode body is 5cm；Electro-deposition process is added by multiple
In series between work area, each processing interval is divided into deposition section and cutter lifting section；Electrodeposition time is 2~5 hours, Mei Gechen
Product section duration control is 30min, and duration control in cutter lifting section is 2min；In cutter lifting section, swap cathode component is static；
5. electro-deposition completion of processing post-processes：After electro-deposition completion of processing, by post processing, that is, required performance and shape are obtained
The parts of shape.
Further scheme is：During above-mentioned electro-deposition section, the bottom of mobile anode and the spacing of cathode base control
For 1cm.
Further scheme is：Above-mentioned step 4. in, mechanical agitator or so is to horizontal intermittent stirring；Mechanical agitator
Stir speed (S.S.) be 200~500rpm；The current density of dc source output is 1~13 A/dm2, preferably current density is 7A/
dm2。
Further scheme is：A diameter of 5mm in the lower cylinder portion of above-mentioned matrix；Under the lower cylinder portion of matrix
End is provided with angle of inclination control concane gap or the lower circle of periphery away from matrix provided with bottom indent in 60 ° of upward inclined-plane
The outer peripheral face 1mm of trunk portion arc concave shape breach；Above-mentioned electrode is diameter 1-2mm insoluble Pt silks.
Further scheme also has：Above-mentioned X to movable block and Y-direction movable block be the hollow square of stainless steel
Body part；And the size of Y-direction movable block is less than sizes of the X to movable block.
The present invention has positive effect：（1）It is of the present invention to be based on supercritical fluid 3D electro-deposition processing unit (plant)s,
It can effectively improve electrodeposition rate, improve deposition quality, prepare complicated, essence by electro-deposition in three dimensions when in use
Close metallic element, and electro-deposition techniques application field can be widened.（2）The present invention overcritical electro-deposition system in, metal from
Son mass transfer performances are more several ten times larger than in conventional electrodeposition system or even hundreds of times.This high mass transfer rate can supplement rapidly
The metal ion of cathode surface, significantly reduces concentration polarization, it is possible to is entered with the current density higher than conventional electrodeposition
Row electro-deposition, the problem of so as to overcome long processing time existing for traditional electro-deposition method.Supercritical fluid has pole simultaneously
Good compatibility, can effectively absorb hydrogen caused by cathode surface, avoid deposition cell surface and inside from defect occur.（3）This
Invention can carry out 3D electro-deposition incessantly on non-smooth base part surface.（4）The present invention can be according to depositing zero
Part shape need, programmed by digitizing the mobile anode of setting and swap cathode component motion track and processing interval when
It is long, effectively control the accuracy of form and position and sedimentary quality of deposition layer, it is not necessary to the complicated negative electrode master mold of traditional electroforming.（5）This
Equivalent to one point of electrode of the electro-deposition movement anode of invention, under the constraint of the glass basis of mobile anode, diverse location
When, the electric-field intensity and current density of corresponding cathode base surface region are all almost equal, so as to improve cathode base table
The Electric Field Distribution in face, improve deposition layer quality.
Brief description of the drawings
Fig. 1 is the structural representation of the present invention based on supercritical fluid 3D electro-deposition processing unit (plant)s；
Fig. 2 is the planar structure schematic diagram of the swap cathode component in Fig. 1；
Fig. 3 is a kind of structural representation of the mobile anode in Fig. 1, and it is cuing open along the axis upward and downward for moving anode
View；
Fig. 4 is another structural representation of the mobile anode in Fig. 1, and it is along the axis upward and downward for moving anode
Sectional view.
Reference in above-mentioned accompanying drawing is as follows：
Dioxide bottle 1；
High-pressure pump 2；
CNC controller 3；
Reactor 4, body 41, air inlet 41-1, leakage fluid dram 41-2, heating coil 41-3, mechanical agitator 42；
Mobile anode assemblies 5, Z-direction linear electric motors 51, driving leading screw 52, anode connecting rod 53, mobile anode 54, matrix
54-1, electrode 54-2, concane gap 54-3, arc concave shape breach 54-4 in inclined-plane；
Swap cathode component 6, X is to linear electric motors 61, and X direction guiding rails 62, X is to movable block 63, and Y-direction linear electric motors 64, Y-direction is led
Rail 65, Y-direction movable block 66, fixture 67；
Cathode base 7；
Dc source 8.
Embodiment
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
（Embodiment 1）
The present embodiment when travel direction describes, using Fig. 1 left and right directions as X to, using Fig. 1 towards direction the back side as Y-direction,
Using Fig. 1 upward and downward as Z-direction.
See Fig. 1 to Fig. 4, the method based on supercritical fluid 3D electro-deposition process components of the present embodiment, by based on super
Critical fluids 3D electro-deposition processing unit (plant) is implemented, and the device is mainly by dioxide bottle 1, high-pressure pump 2, CNC controller 3, anti-
Device 4, mobile anode assemblies 5, swap cathode component 6, dc source 8 and cathode base 7 is answered to form.
Dioxide bottle 1 is used for the CO that storage prepares supercritical fluid2Gas；To anti-when high-pressure pump 2 is used to need
Answer and pressure CO is taken out in device 42Gas.
CNC controller 3 is the control controller of existing Numeric Control Technology, and when digital control implement 3 is used for electro-deposition processing, control moves
Dynamic anode assemblies 5 and swap cathode component 6 are moved according to track set in advance.
Reactor 4 is mainly made up of body 41 and mechanical agitator 42.Body 41 is provided with air inlet 41-1, leakage fluid dram
41-2 and heating coil 41-3.Air inlet 41-1 is used to input CO by high-pressure pump 22Gas；Leakage fluid dram 41-2 is used to use
After supercritical fluid electroforming solution import gas-liquid separator in, the carbon dioxide and electroforming solution of separation return respectively
Receive in retracting device and recycle；Heating coil 41-3 is used for the temperature for controlling supercritical fluid electroforming solution in reactor 4.
Mechanical agitator 42 is arranged in body 41；Mechanical agitator 42 is worked using level to intermittent stirring mode, and stir speed (S.S.) is
200~500rpm, to improve the uniformity and uniformity during electroforming.
Mobile anode assemblies 5 are mainly by Z-direction linear electric motors 51, driving leading screw 52, anode connecting rod 53 and mobile anode 54
Composition.
Z-direction linear electric motors 51 are fixedly mounted on the top of the body 41 of reactor 4；Drive leading screw 52 and Z-direction linear electric motors
51 drive connections；Anode connecting rod 53 is fixedly connected with driving leading screw 52.The material for driving leading screw 52 is stainless steel, in internal
Sky, driving leading screw 52 are built-in with the elastic conduction coil being insulated from, for mobile anode 54 to be connected into power supply.Anode connecting rod
53 be built-in copper framework and outer shoe insulation, the body of rod part of acidproof, high voltage bearing engineering plastics；Drive the elasticity built in leading screw 52
One end of conductive coil is electrically connected by the built-in copper framework of anode connecting rod 53 with mobile anode 54；Drive built in leading screw 52
The other end of elastic conduction coil electrically connected with the positive pole of dc source 8.All junctions are carried out close with high-pressure seal ring
Envelope.
Referring to Fig. 3 and Fig. 4, mobile anode 54 is made up of matrix 54-1 and electrode 54-2.Matrix 54-1 material is glass,
Matrix 54-1 is integrally made up of upper cylinder portion and lower cylinder portion, and the diameter in matrix 54-1 upper cylinder portion is less than lower cylinder
The diameter in body portion, matrix 54-1 upper cylinder portion are connected with anode connecting rod 53；Matrix 54-1 lower cylinder portion it is straight
Footpath is 5mm or so；There are 2 kinds of structures in matrix 54-1 lower cylinder portion, and a kind of is in the lower end in matrix 54-1 lower cylinder portion
Provided with concane gap 54-3 in upward inclined-plane；Angle of inclination is controlled at 60 ° or so；Another kind is provided with arc concave shape breach 54-
4, the circumference of bottom indent is away from insulating glass external boundary 1mm or so.Electrode 54-2 is insoluble Pt silks, and a diameter of 1-2mm is electric
Pole 54-2 is arranged in matrix 54-1 and on matrix 54-1 axial line.Concane gap 54-3 or arc concave shape in inclined-plane are set
Breach 54-4 purpose is the concentration for contributing to electric field line, can be very good to control deposition region in electrodeposition process, carries
High current efficiency and cast layer quality.
The mobile anode 54 of mobile anode assemblies 5 is by Z-direction linear electric motors 51 by driving leading screw 52 and anode connecting rod 53
Transmission, can be pumped in the body 41 of reactor 4.
Still see Fig. 2, swap cathode component 6 is mainly straight to linear electric motors 61, X direction guiding rails 62, X to movable block 63, Y-direction from X
Line motor 64, Y-direction guide rail 65, Y-direction movable block 66 and fixture 67 form.
X is fixedly mounted on the body 41 of reactor 4 to linear electric motors 61；X direction guiding rails 62 divide front and rear provided with 2；Guide X
Rail 62 is fixedly mounted on the lower surface in the body 41 of reactor 4；X to movable block 63 be the hollow square of stainless steel
Body part.X is arranged on X direction guiding rails 62 to movable block 63 and in X to can rely on X direction guiding rails 62 or so under the driving of linear electric motors 61
To linear slide.
Y-direction linear electric motors 64 are fixedly mounted on X on the upper surface of movable block 63；Y-direction guide rail 65, which is divided or so, is provided with 2；Y
Direction guiding rail 65 is fixedly mounted on X on the upper surface of movable block 63 and Y-direction guide rail 65 and X direction guiding rails 62 are vertically arranged；But do not exist
In same plane.The size of Y-direction movable block 66 is less than X to movable block 63；Y-direction movable block 66 is the hollow side of stainless steel
Body part；One layer of acidproof, high pressure resistant and high rigidity insulation engineering plastics are coated with the upper surface of Y-direction movable block 66.Y-direction is moved
Motion block 66 is arranged in Y-direction guide rail 65 and can rely on Y-direction guide rail 65 is front and rear to be slided to straight line under the driving of Y-direction linear electric motors 64
It is dynamic.
The material of fixture 67 is acidproof, high pressure resistant and high rigidity insulation engineering plastics.Fixture 67 is arranged on Y-direction movable block
On 66 upper surface.Cathode base 7 of the clamping as part to be processed when fixture 67 is used to use.During work, cathode base 7 with
The negative pole electrical connection of dc source 8.
All gap locations of swap cathode component 6 are sealed with high-pressure seal ring.
The X of swap cathode component 6 is to linear electric motors 61 and Y-direction linear electric motors 64 and the Z-direction straight line of mobile anode assemblies 5
The operation of motor 51 is controlled by CNC controller 3.
The present embodiment based on supercritical fluid 3D electro-deposition processing unit (plant)s, it is used for accurate, complex three-dimensional parts and added
The processing method of work, illustrated by taking Ni-based electroplate liquid and stainless steel cathode matrix 7 as an example, its processing method mainly includes following
Step：
1. the chemical plating in advance of cathode base 7：On the surface of cathode base 7, plating last layer is easy to carry out the gold of electro-deposition
Belong to, the optional fine copper of the metal or pure nickel, in the present embodiment, it is preferred to use about 10 μ m-thicks are plated on the surface of cathode base 7
Uniform copper layer；
2. cathode base is installed：Cathode base 7 is fixed on Y-direction movable block 66 by the fixture 67 of swap cathode component 6
Upper surface on；The upward and downward position of the mobile anode 54 of regulation, makes it not interference with swap cathode component 6.
3. prepare supercritical fluid：Nickel salt solution, boric acid and additive are added in the reactor 4, are stirred under ultrasound environments
Mix 60 minutes, be sufficiently mixed it；Boric acid is optionally added as electro-deposition sustained release agent, the concentration of boric acid for 30g/L~
60g/L.Nickel salt solution is the solution of sulfur acid nickel and nickel chloride；Wherein nickel sulfate dosage is 300~400g/L, nickel chloride dosage
For 30~50g/L；Additive is made up of dodecane base class compound and ether compound, wherein dodecane base class compound amount
For 0.1~2g/L, ether compound dosage is 0.1~1g/L.In the present embodiment, additive preferably uses lauryl sodium sulfate
With polyethylene glycol trimethyl nonyl ethers.The concentration of each material is preferably:Nickel sulfate 300g/L, nickel chloride 35g/L, boric acid 40g/L,
Lauryl sodium sulfate 0.2g/L, polyethylene glycol trimethyl nonyl ethers 0.8g/L.
Start high-pressure pump 2, the air inlet for the body 41 that carbon dioxide is passed through into reactor 4 from dioxide bottle 1
41-1 is taken out in the body 41 for being pressed onto reactor 4；Control pressure is 8 ~ 20MPa；Alternating current is set to pass through heating coil 41-3 simultaneously
Heated in the presence of electromagnetic induction, temperature control is existed by the control of the size of the current strength to alternating current
35~70 DEG C, preferably 50 DEG C in the present embodiment, under above-mentioned pressure and temperature, it is stirred by mechanical agitator 42 to be formed
Supercritical fluid ternary electro-deposition system.
In the present embodiment, pressure of the carbon dioxide in the body 41 of closed reactor 4 is 13MPa；Machinery stirs
The stir speed (S.S.) for mixing device 42 is 200~500rpm；Mechanical agitation speed is preferably used in the present embodiment as 400rmp.Mechanical agitation
Device 42 is worked using left and right to horizontal intermittent stirring mode.
4. electro-deposition is processed：Switch on power, under the control that CNC controller 3 adopts existing Numeric Control Technology, mobile anode
54 and swap cathode component 6 moved by predetermined track；Mobile anode 54 is relative to the upper of the cathode base 7 as cathode body
The lower maximum single direction stroke of movement is 5cm；Cathode and anode is controlled to move using timing electro-deposition mode；Electro-deposition process is by more
Individual processing interval is in series, and each processing interval is divided into deposition section and cutter lifting section；Mobile anode 54 and negative electrode base simultaneously
Body 7 discharges, and forms the electric field of relative constancy；Nickel ion in solution deposits to the surface of cathode base 7 under electric field action；Electricity
Sedimentation time is 2~5 hours, and deposition section duration is 30min or so, and cutter lifting section is 2min；In cutter lifting section, swap cathode
Component 6 is static.Preferred electrodeposition time is 3 hours, deposition process section 28min, cutter lifting section duration 2min in the present embodiment.
The current density that dc source 8 exports is 1~13 A/dm2；Current density is preferably used in the present embodiment as 7A/
dm2。
5. electro-deposition completion of processing post-processes：After electro-deposition completion of processing, pass through the leakage fluid dram on the body 41 of reactor 4
41-2 imports supercritical fluid electroforming solution in gas-liquid separator, and the carbon dioxide and electroforming solution of separation are separately recovered
Recycled into retracting device.
6. cathode base post-processes：Cathode base 7 is taken out from reactor 4, done again by pickling by washing to air-dry
Only, that is, the dense structure that obtains combining closely with the stainless steel of cathode base 7, crystal grain are tiny, surfacing, excellent performance and shape
The preferable precision metal of shape, fine parts.
Above example is the explanation to the embodiment of the present invention, rather than limitation of the present invention, relevant technology
The technical staff in field without departing from the spirit and scope of the present invention, can also make various conversion and change and obtain
To corresponding equivalent technical scheme, therefore all equivalent technical schemes should be included into the patent protection model of the present invention
Enclose.
Claims (1)
- A kind of 1. method based on supercritical fluid 3D electro-deposition process components, it is characterised in that：By based on supercritical fluid 3D electro-deposition processing unit (plant) is implemented, and described supercritical fluid 3D electro-deposition processing unit (plant) includes dioxide bottle（1）, high pressure Pump（2）, CNC controller（3）, reactor（4）, mobile anode assemblies（5）, swap cathode component（6）, dc source（8）And work To be processed the cathode base of parts（7）；Described reactor（4）Including body（41）And mechanical agitator（42）；Body （41）It is provided with air inlet（41-1）, leakage fluid dram（41-2）And heating coil（41-3）；Described dioxide bottle（1）And height Press pump（2）To reactor during for using（4）Carbon dioxide is provided；Described mobile anode assemblies（5）Including Z-direction straight line Motor（51）, driving leading screw（52）, anode connecting rod（53）With mobile anode（54）；Z-direction linear electric motors（51）It is fixedly mounted on Reactor（4）Body（41）Top；Drive leading screw（52）With Z-direction linear electric motors（51）Drive connection；Anode connecting rod （53）With driving leading screw（52）It is fixedly connected；Drive leading screw（52）It is built-in with the elastic conduction coil being insulated from；Mobile anode （54）With anode connecting rod（53）It is fixedly connected；Mobile anode（54）Pass through anode connecting rod（53）With driving leading screw（52）It is built-in Elastic conduction coil external direct current power supply（8）Positive pole；Mobile anode assemblies（5）Mobile anode（54）By Z-direction straight-line electric Machine（51）By driving leading screw（52）With anode connecting rod（53）Transmission, can be in reactor（4）Body（41）It is interior past up and down Multiple motion；Described swap cathode component（6）Including X to linear electric motors（61）, X direction guiding rails（62）, X is to movable block（63）, Y-direction it is straight Line motor（64）, Y-direction guide rail（65）, Y-direction movable block（66）And fixture（67）；X is to linear electric motors（61）It is fixedly mounted on reaction Device（4）Body（41）On；X direction guiding rails（62）2 are provided with before and after point；X direction guiding rails（62）It is fixedly mounted on reactor（4）Sheet Body（41）On interior lower surface；X is to movable block（63）Installed in X direction guiding rails（62）It is upper and in X to linear electric motors（61）Driving Under can rely on X direction guiding rails（62）Left and right is to linear slide；Y-direction linear electric motors（64）X is fixedly mounted on to movable block（63）Upper surface on；Y-direction guide rail（65）Point or so be provided with 2 Root；Y-direction guide rail（65）X is fixedly mounted on to movable block（63）Upper surface on and Y-direction guide rail（65）With X direction guiding rails（62）Vertically Set；Coated with insulation engineering plastics on the upper surface of Y-direction movable block 66；Y-direction movable block（66）Installed in Y-direction guide rail（65）On And in Y-direction linear electric motors（64）Driving under can rely on Y-direction guide rail（65）It is front and rear to linear slide；Fixture（67）Material be acidproof, high pressure resistant and high rigidity insulation engineering plastics；Fixture（67）It is arranged on Y-direction movable block （66）Upper surface on, clamp cathode base during for using（7）；In use, cathode base（7）With dc source（8）It is negative Pole electrically connects；Swap cathode component（6）X to linear electric motors（61）With Y-direction linear electric motors（64）And mobile anode assemblies（5）Z-direction Linear electric motors（51）Operation by CNC controller（3）Control；Described driving leading screw（52）Material be stainless steel, inner hollow；Anode connecting rod（53）For built-in copper framework and It is outer to carry out insulation, the body of rod part of acidproof, high voltage bearing engineering plastics；Described driving leading screw（52）With anode connecting rod（53）Company Connect place and anode connecting rod（53）With mobile anode（54）Junction sealed with high-pressure seal ring；Described mobile anode（54）Including matrix（54-1）And electrode（54-2）；Matrix（54-1）Material be glass, matrix （54-1）Integrally it is made up of upper cylinder portion and lower cylinder portion, matrix（54-1）The diameter in upper cylinder portion be less than lower cylinder The diameter in body portion, matrix（54-1）Upper cylinder portion and anode connecting rod（53）It is fixedly connected；Electrode（54-2）It is arranged on base Body（54-1）It is interior and be located at matrix（54-1）Axial line on；The method of process component, comprises the following steps：1. cathode base chemical plating in advance：In the cathode base as processed parts（7）Surface plating last layer it is easy In the uniform copper layer for 10 μ m-thicks for carrying out electro-deposition；2. cathode base is installed：By cathode base（7）Pass through swap cathode component（6）Fixture（67）It is fixed on Y-direction movable block （66）Upper surface on；The mobile anode of regulation（54）Upward and downward position, make its not with swap cathode component（6）Interference；3. prepare supercritical fluid：In reactor（4）It is middle to add two containing surface additive and electro-deposition sustained release agent configured First system plating solution；The described binary system electroplate liquid containing surface additive and electro-deposition sustained release agent is that nickel salt or mantoquita are molten Liquid；Surface additive is the additive being made up of dodecane base class compound and ether compound；Described nickel salt or mantoquita is molten The concentration of liquid is 300~500g/L；The concentration of surface additive is 0.1~2g/L；Electro-deposition sustained release agent be concentration 30g/L~ 60g/L boric acid, bath pH values are controlled 2~6；After closed, to reactor（4）In be passed through carbon dioxide, control is anti- Answer device（4）Interior temperature in 35~70 DEG C, pressure in the range of 8~20MPa, formed using supercritical carbon dioxide emulsion as The ternary electro-deposition system of carrier；4. electro-deposition is processed：Switch on power, setting electro-deposition parameter and mobile anode（54）Opposing cathode matrix（7）Position； In CNC controller（3）Control and mechanical agitator（42）Stirring auxiliary lower carry out electro-deposition with cathode base（7） Outer surface obtain required deposition layer；CNC controller（3）The mobile anode of control（54）With swap cathode component（6）By setting Fixed track motion；Mobile anode（54）Relative to the cathode base as cathode body（7）Move up and down maximum unidirectional row Journey is 5cm；Electro-deposition process is in series by multiple processing intervals, and each processing interval is divided into deposition section and cutter lifting area Between；Electrodeposition time is 2~5 hours, and each deposition section duration control is 30min, and duration control in cutter lifting section is 2min；Lift In knife section, swap cathode component（6）It is static；5. electro-deposition completion of processing post-processes：After electro-deposition completion of processing, by post processing, that is, required performance and shape are obtained Parts.
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| WO2022023647A1 (en) * | 2020-07-30 | 2022-02-03 | Safran | Device and method for depositing thick metal nitride coatings by the supercritical fluid route |
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| CN106191933B (en) | 2017-11-21 |
| CN106086961A (en) | 2016-11-09 |
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| CN106191933A (en) | 2016-12-07 |
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| CN106222707B (en) | 2018-02-06 |
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