CN106048693B - A kind of overcritical composite plating processing drill method based on mobile anode - Google Patents
A kind of overcritical composite plating processing drill method based on mobile anode Download PDFInfo
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- CN106048693B CN106048693B CN201610595427.XA CN201610595427A CN106048693B CN 106048693 B CN106048693 B CN 106048693B CN 201610595427 A CN201610595427 A CN 201610595427A CN 106048693 B CN106048693 B CN 106048693B
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- 238000007747 plating Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000012545 processing Methods 0.000 title claims description 16
- 238000004070 electrodeposition Methods 0.000 claims abstract description 17
- 239000002114 nanocomposite Substances 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 230000033001 locomotion Effects 0.000 claims abstract description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 36
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 22
- 238000000429 assembly Methods 0.000 claims description 20
- 230000000712 assembly Effects 0.000 claims description 20
- 239000001569 carbon dioxide Substances 0.000 claims description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 16
- 150000001875 compounds Chemical class 0.000 claims description 15
- 239000002105 nanoparticle Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 13
- 239000000654 additive Substances 0.000 claims description 11
- 230000000996 additive effect Effects 0.000 claims description 11
- 239000011159 matrix material Substances 0.000 claims description 11
- 229910000831 Steel Inorganic materials 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 239000010959 steel Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 8
- -1 ether compound Chemical class 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 5
- 150000002815 nickel Chemical class 0.000 claims description 5
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 5
- 239000010432 diamond Substances 0.000 claims description 4
- 229910003460 diamond Inorganic materials 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- 229910002056 binary alloy Inorganic materials 0.000 claims description 2
- 239000000839 emulsion Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000012805 post-processing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 10
- 238000013019 agitation Methods 0.000 abstract description 2
- 239000002103 nanocoating Substances 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 239000012530 fluid Substances 0.000 description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 13
- 229910052802 copper Inorganic materials 0.000 description 13
- 239000010949 copper Substances 0.000 description 13
- 238000005323 electroforming Methods 0.000 description 11
- 239000000243 solution Substances 0.000 description 8
- 238000009413 insulation Methods 0.000 description 6
- 239000002113 nanodiamond Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 5
- 239000004327 boric acid Substances 0.000 description 5
- 238000009713 electroplating Methods 0.000 description 5
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 4
- 239000002202 Polyethylene glycol Substances 0.000 description 4
- 229920006351 engineering plastic Polymers 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- 230000005684 electric field Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005055 memory storage Effects 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
- 125000006850 spacer group Chemical group 0.000 description 2
- 238000013268 sustained release Methods 0.000 description 2
- 239000012730 sustained-release form Substances 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 229910000997 High-speed steel Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000002048 anodisation reaction Methods 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 235000008434 ginseng Nutrition 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
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000002604 ultrasonography Methods 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
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- 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
- C25D21/10—Agitating of electrolytes; Moving of racks
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
-
- 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
-
- 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
Abstract
The present invention provides a kind of overcritical composite plating tool bit method based on mobile anode, and the key step of this method includes：The basis material of drill bit is pre-processed, is allowed to the ability for having electro-deposition nano-composite plate；The electroplate liquid being configured is added in into reactor, after sealing, is passed through CO2Gas adds in surfactant, forms the plating system under super critical condition；Setting meets the parameters such as electric current, temperature and the mechanical agitation speed of electro-deposition requirement；The relative position between anode and cathode is adjusted, anode movement speed and stroke is set, powers on, nano-composite plate is enable fully to deposit to the processed bit face as cathode body；Drill bit after electro-deposition is removed it is clean, obtain surface have high-performance composite Nano coating drill bit.Bit face tissue made from the method for the present invention is fine and closely woven, and wearability and hardness all have a distinct increment, and service life increases.
Description
The application is application No. is 201410412652.6, and the applying date is August in 2014 20 days, and invention and created name is
The divisional application of the application for a patent for invention of " method of the overcritical composite plating processing drill based on mobile anode ".
Technical field
The present invention relates to electrochemical deposition processing technique fields, and in particular to a kind of based on the overcritical compound of mobile anode
The method of processing drill is electroplated.
Background technology
Supercritical fluid（Supercritical Fluid）Refer to that pure substance is in critical point（Critical pressure and critical
Temperature）More than when, showed one kind between liquid and gaseous fluid.In Near The Critical Point, supercritical fluid it is close
The phenomenon that change dramatically, occurs for the physical property of all fluids such as degree, viscosity, solubility, thermal capacity, dielectric constant.CO2Gas has
Environmentally friendly, non-ignitable, nontoxic, inertia, deposit enriches and critical pressure（7.39MPa）With temperature (31.1 DEG C) it is less high the advantages that, because
This supercritical CO2Fluid is widely used.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 electroforming system for mass transfer.
The moulding material of industry drill bit is often using titanium alloy, diamond or Special steel material etc., these materials at present
The drill bit of material prepares complex process, high expensive and performance is not excellent enough, and uses nanocomposite can be preferably
Make up these shortcomings.Industrial drill bit often uses high-speed steel and special steel etc., and as basis material, the basis material is generally difficult to
Electrochemical deposition processing is directly carried out, and after the method for using chemical plating pre-processes basis material, then so that in the base
Nano compound electroplating is carried out on body to be possibly realized.When nano particle uniformly is compounded in metal matrix material, nano particle exists
The problem of reunion occurred during electroforming and poor macro-uniformity, is very prominent.It is shaken mostly using stirring, ultrasound at present
It moves, add the modes such as dispersant to handle the agglomeration of nano particle, but because of former mould（Metal parts）It is different, during plating
Electric field, flow field uniformity are difficult to control, and can still be caused nanoparticle agglomerates in nano composite electroforming deposit and are unevenly distributed.It receives
The reunion of rice grain and being unevenly distributed will cause the cast layer mechanical property difference of different parts huge, seriously affects its use
Performance.
At present, the process and device of electrodeposited nanocrystalline composite material and micro-workpiece be under supercritical environment
There is finding.Chinese patent literature if Authorization Notice No. is CN 101092716B discloses a kind of subtle plating of supercritical fluid
Moulding process and its device, with SCF-CO2The molding of micro-structure part, the gold as obtained by this method are carried out for plating environment
Belong to plating layer surface depositing homogeneous, without buildup, and cast layer tissue is fine and closely woven smooth, but gained cast layer is single metal, is not suitable for
Composite plating molding containing nano particle；For another example publication No. is that the Chinese patent literature of CN 102146573A proposes one kind
The method of preparing nano composite material by supercritical fluid electroforming, the electro-deposition system mainly under mechanical agitation subsidiary conditions
Standby metal-base nanometer composite material, electric field distribution is fixed, from the point of view of its parameter setting and anode and cathode setting, it is impossible to column
Or tubulose class cathode carries out effective deposition nano-composite plate.
Invention content
The purpose of the present invention is：Agglomeration of the nano particle in electroplating process is controlled, is being electroplated for cathode drill bit
Nanocomposite cannot be coated with well in the process, using the overcritical composite plating method based on the mobile anode of matching,
Composite deposite enable cathode bit face becomes to be uniformly dispersed, surfacing, dense structure, crystal grain is tiny, performance is excellent
It is different.
The technical scheme is that：The side of the overcritical composite plating processing drill based on mobile anode of the present invention
Method is implemented using the overcritical composite plating device based on mobile anode, should the overcritical composite plating dress based on mobile anode
It puts including reactor, DC power supply component, mechanical agitator, carbon dioxide gas steel cylinder and high-pressure pump；DC power supply component packet
Include power supply, anode stub and cathode bar；Its main feature is that：The above-mentioned overcritical composite plating device based on mobile anode further includes shifting
Dynamic anode assemblies, drive component and the processed drill bit as cathode body；
Above-mentioned mobile anode assemblies include fixed connecting plate and mobile anode；Mobile anode is fixed with fixed connecting plate to be connected
It connects；Drive component includes servo motor, driving leading screw and connecting rod；Driving leading screw is built-in with the elastic conducting electric wire being insulated from
Circle；Servo motor is connect with driving lead screw transmission；The left end of connecting rod is fixedly connected with fixed connecting plate；The right end of connecting rod with
Driving leading screw is fixedly connected；Mobile anode by the elastic conduction coil built in fixed connecting plate, connecting rod, driving leading screw and
Anode stub is electrically connected with the anode of power supply；Be processed drill bit upper end be fixedly connected with the lower end of cathode bar and pass through cathode bar with
The cathode electrical connection of power supply；The mobile anode of above-mentioned mobile anode assemblies can be processed relatively under the driving of drive component
Drill bit upward and downward moves back and forth；
The mobile anode of above-mentioned mobile anode assemblies is equipped with 4；This 4 mobile anodes are fixed at fixed connecting plate
Four corners；It is processed drill bit and is equipped with 4, which corresponds to each setting 1 respectively with 4 mobile anodes；
The method of processing drill, includes the following steps：
1. carrying out chemical plating in advance to the matrix for being processed drill bit, last layer is plated in the matrix surface for being processed drill bit
It is easy to carry out the metal of electro-deposition；
2. the binary system electroplate liquid of prepared hard particles containing nanometer and compound additive is added in reactor, Gu
It is set for the processed drill bit for cathode body；The position for adjusting the mobile anode of mobile anode assemblies so that mobile anode can be opposite
It is moved up and down in processed drill bit；Above-mentioned electroplate liquid is sulfur acid nickel and the nickel salt solution of nickel chloride；Nanometer hard particles be
The diamond nano-particles of 30~60nm of diameter；Compound additive is made of dodecane base class compound and ether compound
Additive；
3. carbon dioxide gas is passed through into reactor, control temperature in reactor 35~70 DEG C, pressure 8~
In the range of 20MPa, form the ternary using supercritical carbon dioxide emulsion as carrier and system is electroplated；
4. set mobile anode relative to the processed drill bit as cathode body move up and down maximum single direction stroke as
5cm；Using at the uniform velocity or the move mode of simple harmonic motion, average speed is controlled in 1-20mm/s；Electrodeposition time is 1-3 hours；
Nano-composite plate is obtained under the stirring auxiliary of mechanical agitator；
5. electro-deposition finishes, by post processing, the drill bit with nano-composite plate of required performance requirement is obtained.
Further embodiment is：The reactor of the above-mentioned overcritical composite plating device based on mobile anode includes main body
And liner；Liner is set on the internal perisporium of main body；Air inlet is equipped on the left of the upper end of the main body of reactor；The main body of reactor
Leakage fluid dram is equipped on the right side of upper end；The body interior of reactor is equipped with heating coil；Mechanical agitator is arranged in reactor；Machinery
Blender is worked using horizontal direction intermittent stirring mode；High-pressure pump is used for the carbon dioxide of carbon dioxide gas steel cylinder memory storage
The air inlet for the main body that gas passes through reactor takes out pressure into main body；
The fixed connecting plate of above-mentioned mobile anode assemblies is the plate body part being integrally square, four angles of fixed connecting plate
Portion is equipped with the notch of arc；Fixed connecting plate is by carrying out insulation, high pressure resistant, acidproof engineering plastics system outside copper frame structure
Into；Mobile anode is metallic conductor part；On the arc notch of four corners that mobile anode is fixed at fixed connecting plate and
It is electrically connected with the copper frame structure of fixed connecting plate；
The driving leading screw of drive component is hollow leading screw；Above-mentioned elastic conduction coil is arranged on the hollow of driving leading screw
In position；And the left side of driving leading screw is stretched out in the lower end of the elastic conduction coil；Driving is stretched out in the upper end of the elastic conduction coil
The upper end of leading screw；The elastic conduction coil is insulated with driving leading screw by insulation spacer；Leading screw is driven by its underpart and servo electricity
Machine is sequentially connected；Above-mentioned connecting rod outside copper post by carrying out insulation, high pressure resistant, acidproof engineering plastics are made.
Further embodiment is：The cylindric pure nickel that above-mentioned mobile anode is high 2cm, diameter 3cm, thickness are 2mm is thin
Wall ring；It is 1cm to be processed the distance between the outer wall of drill bit and the inner wall of mobile anode.
Further embodiment is：A concentration of 300~450g/L of above-mentioned nickel salt solution；The concentration of Nano diamond particle
For 1~20g/L；A concentration of 0.1~2g/L of compound additive.
Further embodiment is：Above-mentioned step 1. in chemical plating in advance is carried out to the matrix for being processed drill bit,
The metal that the matrix surface of processed drill bit is plated is fine copper or pure nickel；Step 2. in electroplate liquid further include a concentration of 30g/L
The boric acid as electro-deposition sustained release agent of~60g/L.
Further embodiment is：The current density of the power supply output of above-mentioned DC power supply component is 7A/dm2；Above-mentioned
Mechanical agitator is arranged in reactor；Mechanical agitator horizontal direction intermittent stirring, stir speed (S.S.) are 200~500rpm.
Further embodiment also has：Above-mentioned compound additive is by lauryl sodium sulfate and polyethylene glycol trimethyl nonyl
Base ether；A concentration of 0.2g/L of lauryl sodium sulfate, a concentration of 0.8g/L of polyethylene glycol trimethyl nonyl ethers.
The present invention has positive effect：（1）The present invention is by using mobile anodization method, as cathode body
It is processed drill bit and ensure that each to uniformity of its surface in plating so that be electrodeposited in nano combined on processed drill bit
Coating can be smooth, uniform；Simultaneously using horizontal direction intermittent stirring mode, so that nano particle has sedimentation in electroplating solution
Trend further improves uniformity and consistency during nano combined electroforming.(2) present invention can be in non-smooth metal
The excellent nano-composite plate of forming properties on piece surface.(3) present invention can be according to use demand, by nano particle
Processing, form the nano-composite plate of different performance on metal parts using different nanometer hard materials.（4）The present invention
Can overcritical nano compound electroplating be carried out to multiple processed drill bits as cathode body simultaneously, can prepared efficiently, in batches
Go out the drill bit for the nanocomposite haveing excellent performance.
Description of the drawings
Fig. 1 is the schematic diagram of electrotyping forming device of the present invention；
Fig. 2 is the structure diagram of mobile anode in Fig. 1, and mobile anode and the quilt as cathode body are also shown in figure
The position matching of processing drill.
Reference numeral in above-mentioned attached drawing is as follows：
Reactor 1, main body 11, air inlet 11-1, leakage fluid dram 11-2, heating coil 11-3, liner 12；
Mobile anode assemblies 2, fixed connecting plate 21, mobile anode 22；
Drive component 3, servo motor 31；Drive leading screw 32, connecting rod 33；
DC power supply component 4, power supply 41, anode stub 42, cathode bar 43；
Mechanical agitator 5；
Carbon dioxide gas steel cylinder 6；
High-pressure pump 7,
It is processed drill bit 8.
Specific embodiment
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
（Embodiment 1）
See Fig. 1 and Fig. 2, the overcritical composite plating processing drill method based on mobile anode of the present embodiment, using base
Implement in the overcritical composite plating device of mobile anode, the overcritical composite plating device based on mobile anode is mainly by reacting
Device 1, mobile anode assemblies 2, drive component 3, DC power supply 4, mechanical agitator 5, carbon dioxide gas steel cylinder 6 and high-pressure pump 7
Composition.
Reactor 1 is mainly made of main body 11 and liner 12.Air inlet is equipped on the left of the upper end of the main body 11 of reactor 1
11-1；Leakage fluid dram 11-2 is equipped on the right side of the upper end of reactor 1；The main body 11 of reactor 1 is internally provided with heating coil 11-3.Liner
12 are set on the internal perisporium of main body 11.
Mobile anode assemblies 2 are made of fixed connecting plate 21 and mobile anode 22.Fixed connecting plate 21 is square to be whole
Plate body part, the four corners of fixed connecting plate 21 are equipped with the notch of arc.Fixed connecting plate 21 be by copper frame structure outside
Carry out insulation, high pressure resistant, acidproof engineering plastics are made.Mobile 22, anode preferably uses high 2cm, diameter 3cm, thickness in implementing
Cylindric pure nickel thin-walled ring for 2mm；Preferably using 4 in 22 the present embodiment of mobile anode, this 4 mobile fixations of anode 22 are set
It puts on the arc notch of the four corners of fixed connecting plate 21 and is electrically connected with the copper frame structure of fixed connecting plate 21.
Drive component 3 mainly includes servo motor 31, driving leading screw 32 and connecting rod 33.In 31 the present embodiment of servo motor
It is preferred that the DC servo motor using model KT290-A6-50.Driving leading screw 32 is hollow leading screw, is driven in leading screw 32
Empty position is built-in with elastic conduction coil；The left side of driving leading screw 32 is stretched out in the lower end of the elastic conduction coil；The elastic conduction
The upper end of driving leading screw 32 is stretched out in the upper end of coil；And the elastic conduction coil is insulated with driving leading screw 32 by insulation spacer；
Driving leading screw 32 is sequentially connected by its underpart and servo motor 31.Connecting rod 33 outside copper post by carrying out insulation, high pressure resistant, acidproof work
Engineering plastics are made.The right end of connecting rod 33 is fixedly connected with driving leading screw 32；And connecting rod 33 is by the right end of its internal copper post
It is electrically connected with the lower end of the elastic conduction coil in driving leading screw 32；The fixation of the left end of connecting rod 33 and mobile anode assemblies 2
The right side central of connecting plate 21 is fixedly connected；And connecting rod 33 is by the left end of its internal copper post and the copper of fixed connecting plate 21
Frame structure is electrically connected.
DC power supply component 4 is made of power supply 41, anode stub 42 and cathode bar 43.The upper end of anode stub 42 and power supply 41
Anode is electrically connected, and the lower end of anode stub 42 is electrically connected with the upper end of the elastic conduction coil in the driving leading screw 32 of drive component 3；
So as to by anode stub 42, driving leading screw 32 in elastic conduction coil, connecting rod 33, fixed connecting plate 21 copper frame knot
Mobile anode 22 is electrically connected by structure with the anode of power supply 41.The upper end of cathode bar 43 is electrically connected with the cathode of power supply 41, is processed
The upper end of drill bit 8 is fixed with the lower end of cathode bar 43 and is electrically connected.It is processed drill bit 8 and is used as cathode body.Drill bit 8 is processed to set
In on the central axes in the mobile anode 22 of mobile anode assemblies 2；And it is processed the inner wall of the outer wall and mobile anode 22 of drill bit 8
The distance between be 1cm.
Mechanical agitator 5 is arranged in reactor 1；Mechanical agitator 5 is worked using horizontal direction intermittent stirring mode, so that
Obtain nano particle has Subsidence trend in electroplating solution, improves uniformity and consistency during nano combined electroforming.Machinery
Horizontal direction intermittent stirring is stirred, stir speed (S.S.) is 200~500rpm.
Carbon dioxide gas steel cylinder 6 is used to store carbon dioxide gas.
High-pressure pump 7 is used for the main body 11 that the carbon dioxide gas of 6 memory storage of carbon dioxide gas steel cylinder is passed through reactor 1
Air inlet 11-1 pressure is taken out into main body 11.
The mobile anode 22 of aforementioned mobile anode assemblies 2 under the driving of drive component 3, surround be processed drill bit 8 into
The movement of row upward and downward；In the present embodiment, the maximum single direction stroke that mobile anode 22 is processed drill bit 8 relatively is 5cm；Using even
Speed or the move mode of simple harmonic motion, average speed are controlled in 1-20mm/s.
The overcritical composite plating processing drill method based on mobile anode of the present embodiment, with Ni-based benefit processing drill 8
It is illustrated for electro-deposition Nano diamond composite material, processing method mainly includes the following steps that：
1. carrying out chemical plating in advance to the matrix for being processed drill bit 8, one is plated in the matrix surface for being processed drill bit 8
Layer is easy to carry out the metal of electro-deposition；Fine copper or pure nickel may be selected in the metal.In the present embodiment, it is preferred to use in processed drill bit
8 matrix surface plates the uniform copper layer of about 10 μ m-thicks.
2. it is molten to add in nickel salt into the reactor 1 of the overcritical composite plating device based on mobile anode of the present embodiment
Liquid, boric acid, Nano diamond particle and compound additive stir 30 minutes, make that it is sufficiently mixed and nano particle uniformly divides
It dissipates.Boric acid is optionally added, a concentration of 30g/L~60g/L of boric acid as electro-deposition sustained release agent.
Nickel salt solution is sulfur acid nickel and the solution of nickel chloride；Wherein nickel sulfate dosage is 300~400g/L, and nickel chloride is used
It measures as 30~50g/L；Diamond nano-particles, a diameter of 30~60nm, dosage are 5~15g/L；The compound additive
It is formed for dodecane base class compound and ether compound, wherein dodecane base class compound amount is 0.1~2g/L, ethers
It is 0.1~1g/L to close object dosage.
In the present embodiment, additive preferably uses lauryl sodium sulfate and polyethylene glycol trimethyl nonyl ethers.Each substance
Concentration be preferably:Nickel sulfate 300g/L, nickel chloride 35g/L, boric acid 40g/L, Nano diamond particle 15g/L, dodecyl
Sodium sulphate 0.2g/L, polyethylene glycol trimethyl nonyl ethers 0.8g/L.
3. start high-pressure pump 7, by the carbon dioxide gas in carbon dioxide gas steel cylinder 6 from the main body 11 of reactor 1
Air inlet 11-1 pumpings are pressed onto in the main body 11 of reactor；Control pressure is 13MPa；Alternating current is made to pass through adding for main body 11 simultaneously
Heat coil 11-3 is heated under the action of electromagnetic induction, will by the control of the size of the current strength to alternating current
Temperature is controlled at 35~70 DEG C, preferably 50 DEG C in the present embodiment, under above-mentioned pressure and temperature, is carried out by mechanical agitator 5
It stirs and forms the supercritical fluid electroforming solution containing Nano diamond particle.In the present embodiment, carbon dioxide gas is close
Test pressure in the main body 11 of the reactor 1 closed is 8~20MPa.
4. consolidate as the lower end of the cathode bar 43 of the upper end and DC power supply component 4 of the processed drill bit 8 of cathode body
Fixed electrical connection；The upper end of the cathode bar 43 of DC power supply component 4 is electrically connected with the cathode of the power supply 41 of DC power supply component 4；
The upper end of the anode stub 42 of DC power supply component 4 is electrically connected with the anode of power supply 41；By the lower end of anode stub 42 and driving group
The driving leading screw 32 of part 3 is fixedly connected；Driving leading screw 32 and the servo motor 31 of drive component 3 are sequentially connected；By driving group
The connecting rod 33 of part 3 is fixedly connected with the fixed connecting plate 21 of mobile anode assemblies 2；It is processed drill bit 8 and is set on mobile anode unit
On central axes in the mobile anode 22 of part 2；And make to be processed the distance between the outer wall of drill bit 8 and the inner wall of mobile anode 22
For 1cm；
It is 1~13A/dm to set the current density that the power supply 41 of DC power supply component 4 exports2, preferably adopt in the present embodiment
Use 7A/dm2；The maximum single direction stroke that the mobile anode 22 of the mobile anode assemblies 2 of setting is processed drill bit 8 relatively is 5cm；It is mobile
Mode uses at the uniform velocity or simple harmonic motion, average speed are controlled in 1~20mm/s, so that electric field distribution is more uniform during electroforming.
5. starting the servo motor 31 of drive component 3, the mobile anode 21 of mobile anode assemblies 2 is controlled according to the ginseng of setting
Number moves up and down；Mechanical agitator 5 is synchronized using horizontal direction intermittent stirring；Connect the power supply 41 of DC power supply component 4；Make
Nickel ion is obtained quickly and efficiently to deposit on the processed drill bit 8 as cathode body with Nano diamond particle.The present embodiment
In, electrodeposition time is 1~3 hour.
6. after electroforming, supercritical fluid electroforming solution is led by the leakage fluid dram 11-2 in the main body 11 of reactor 1
Enter in gas-liquid separator, the carbon dioxide gas and electroforming solution of separation, which are separately recovered in retracting device, to be recycled.
7. processed drill bit 8 is taken out from reactor 1, by wash air-dry again by pickling totally to get to quilt
The nano particle that the matrix of processing drill 8 is combined closely is evenly distributed, dense structure, crystal grain is tiny, surfacing, has excellent performance
Nanocomposite electroformed layer.
Above example is the explanation rather than limitation of the present invention to the specific embodiment of the present invention, related technology
The technical staff in field without departing from the spirit and scope of the present invention, can also make various transformation and variation and obtain
To corresponding equivalent technical solution, therefore all equivalent technical solutions should be included into the patent protection model of the present invention
It encloses.
Claims (1)
1. a kind of overcritical composite plating processing drill method based on mobile anode, using based on the overcritical multiple of mobile anode
Electroplanting device is closed to implement；The overcritical composite plating device based on mobile anode includes reactor（1）, DC power supply group
Part（4）, mechanical agitator（5）, carbon dioxide gas steel cylinder（6）And high-pressure pump（7）；The DC power supply component（4）Including
Power supply（41）, anode stub（42）And cathode bar（43）；It is characterized in that：The overcritical composite plating based on mobile anode
Device further includes mobile anode assemblies（2）, drive component（3）With the processed drill bit as cathode body（8）；
The mobile anode assemblies（2）Including fixed connecting plate（21）With mobile anode（22）；Mobile anode（22）With fixation
Connecting plate（21）It is fixedly connected；Drive component（3）Including servo motor（31）, driving leading screw（32）And connecting rod（33）；Driving
Leading screw（32）It is built-in with the elastic conduction coil being insulated from；Servo motor（31）With driving leading screw（32）It is sequentially connected；Connection
Bar（33）Left end and fixed connecting plate（21）It is fixedly connected；Connecting rod（33）Right end with driving leading screw（32）It is fixedly connected；
Mobile anode（22）Pass through fixed connecting plate（21）, connecting rod（33）, driving leading screw（32）Built-in elastic conduction coil and
Anode stub（42）With power supply（41）Anode electrical connection；It is processed drill bit（8）Upper end and cathode bar（43）Lower end fix connect
It connects and passes through cathode bar（43）With power supply（41）Cathode electrical connection；The mobile anode assemblies（2）Mobile anode（22）
In drive component（3）Driving under, drill bit can be processed relatively（8）Upward and downward moves back and forth；
The mobile anode assemblies（2）Mobile anode（22）Equipped with 4；This 4 mobile anodes（22）It is fixed at
Determine connecting plate（21）Four corners；It is processed drill bit（8）Equipped with 4,4 processed drill bits（8）With 4 mobile anodes
（22）Each setting 1 is corresponded to respectively；
The method of processing drill, includes the following steps：
1. to being processed drill bit（8）Matrix carry out chemical plating in advance, in processed drill bit（8）Matrix surface plate one
Layer is easy to carry out the metal of electro-deposition；
2. the binary system electroplate liquid of prepared hard particles containing nanometer and compound additive is added in into reactor（1）In, Gu
It is set for the processed drill bit for cathode body（8）；Adjust mobile anode assemblies（2）Mobile anode（22）Position to move
Anode（22）It can be relative to processed drill bit（8）It moves up and down；The electroplate liquid is molten for the nickel salt of sulfur acid nickel and nickel chloride
Liquid；The diamond nano-particles that nanometer hard particles are 30~60nm of diameter；Compound additive is by dodecane base class compound
With the additive of ether compound composition；
3. to reactor（1）In be passed through carbon dioxide gas, control reactor（1）Interior temperature 35~70 DEG C, pressure 8~
In the range of 20MPa, form the ternary using supercritical carbon dioxide emulsion as carrier and system is electroplated；
4. the mobile anode of setting（22）Relative to the processed drill bit as cathode body（8）Moving up and down maximum single direction stroke is
5cm；Using at the uniform velocity or the move mode of simple harmonic motion, average speed is controlled in 1-20mm/s；Electrodeposition time is 1-3 hours；
In mechanical agitator（5）Stirring auxiliary under obtain nano-composite plate；
5. electro-deposition finishes, by post processing, the drill bit with nano-composite plate of required performance requirement is obtained.
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| CN201610592998.8A Active CN106087008B (en) | 2014-08-20 | 2014-08-20 | Overcritical composite plating processing drill method of the effect preferably based on mobile anode |
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| CN110257882B (en) * | 2019-06-26 | 2021-06-18 | 高国有 | Drill bit for supercritical composite electroplating processing based on moving cathode and use method |
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| CN111910224A (en) * | 2020-08-10 | 2020-11-10 | 深圳市广诚达电路技术有限公司 | PCB electroplating layer manufacturing process |
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| CN106087008A (en) | 2016-11-09 |
| CN106222729B (en) | 2018-02-06 |
| CN104141161B (en) | 2016-08-17 |
| CN106087008B (en) | 2017-11-21 |
| CN106048693A (en) | 2016-10-26 |
| CN106222729A (en) | 2016-12-14 |
| CN104141161A (en) | 2014-11-12 |
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