CN208266299U - The flexibly coating or passivation layer preparation facilities of control environmental parameter - Google Patents
The flexibly coating or passivation layer preparation facilities of control environmental parameter Download PDFInfo
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- CN208266299U CN208266299U CN201820836388.2U CN201820836388U CN208266299U CN 208266299 U CN208266299 U CN 208266299U CN 201820836388 U CN201820836388 U CN 201820836388U CN 208266299 U CN208266299 U CN 208266299U
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Abstract
The utility model belongs to material experiment research field, more precisely, is related to being electroplated and being passivated field, the especially a kind of coating or passivation layer preparation facilities of flexibly control environmental parameter.The device includes plating or Passivation Treatment system, conducting wire, power supply provider, plating or Passivation Treatment system include anode, cathode, heating magnetic stirring apparatus and plating or Passivation Treatment pond, anode, cathode bestow fixed current density or current potential by cathode and an anode conducting wire external power supply power supply unit.Using plating or modification technology, flexibly the accurate plating of control is perhaps passivated the experiment conditions such as environment temperature, uniformity, atmosphere, ingredient, current density and deposits monometallic film layer or alloy film on metallic conductor surface.The utility model is easy to operate, easy to maintain, and the good adhesive force of coating uniformity is strong, can be applied to machinery, electronics, precision instrument etc..
Description
Technical field
The utility model belongs to material experiment research field, more precisely, is related to being electroplated and is passivated field, especially
A kind of coating or passivation layer preparation facilities of flexible control environmental parameter.
Background technique
Currently, plating and passivation widely apply in various fields, other than the method for surface treatment, it is also applied to
Circuit board, film etc. are made, the thickness uniformity of superficial layer is always the important indicator of assessment plating efficiency.Influence thickness
The factor of uniformity is related to electrolyte composition, surface area of sample, electrolyte temperature, electrolyte Combination, interelectrode distance, electricity
Pole material etc..For example, the low temperature preparation method that ten thousand Jing, Zhang Yanrong of the Central China University of Science and Technology provide a kind of TiO 2 coating film (is awarded
Weigh notification number CN101608330B), entire pulse electrodeposition process heat release needs ice-water bath to provide low temperature environment.Shenzhen is difficult to understand
Wire surface described in Mei Te Science and Technology Ltd. Su Qian etc. is gold-plated or plates palladium technology (Authorization Notice No. CN102586830B),
It needs to be constantly in inert protective atmosphere in electrolyte, layer of precious metal to be plated is prevented to be oxidized.
In fact, workpiece to be plated is precisely due to the experimental situations control such as temperature, dissolved gas, electrolyte uniformity, electric field line
The not stringency of system, in protrusion region, electric field line is intensive and loose in recess area electric current, is so easily formed in uneven thickness
Coating.In consideration of it, needing with cost-effectiveness, coating uniformity is good and coating or passivation layer thickness needed for being especially suitable for exist
The electrolysis unit and method of the range of about 50nm~200nm.The utility model passes through while utilizing fixed reaction surface, uniform electric field
The ancillary measures such as intensity, cooling, heating, gas shield, concussion, adjustment solution composition, to meet above-mentioned film layer demand.
Utility model content
The utility model aim is that providing the flexible control environmental parameter of one kind obtains uniform coating coating or passivation layer system
Standby device, uniform and stable coating or passivation layer structure can be generated in the case where stablizing electrolyte or passivating solution environment, solves existing skill
The problems such as controlling present in art is poor, troublesome maintenance.
The technical solution of the utility model is as follows:
A kind of coating or passivation layer preparation facilities of flexible control environmental parameter, the device can control the accurate parameter of environment
Down be metal material surface depositing homogeneous cover film, the parameter be the temperature of experimental solutions, uniformity, atmosphere, dissolved gas,
Concentration, ion concentration, current density and anode and cathode type, experiment leakproofness, the device include plating or Passivation Treatment system,
Conducting wire, power supply provider, plating or Passivation Treatment system include anode, cathode, heating magnetic stirring apparatus and plating or passivation
Processing pond, anode, cathode bestow fixed current density or current potential by cathode and an anode conducting wire external power supply power supply unit；Its
In:
Cooling sandwith layer is arranged in plating or Passivation Treatment pond periphery, and the beneath side of cooling sandwith layer opens up a cooling water inlet,
It is opened on cooling sandwith layer and sets a cooling water outlet, the plating or Passivation Treatment pond upper cover with plating or the sealing of Passivation Treatment pond
Equipped with anode port, cathode port, air inlet, exhaust outlet and filling opening；
Heating magnetic stirring apparatus tool, there are three control window: heating time display window, temperature display and control window, magnetic
Power stirs rotor speed and controls window, and magnetic stir bar is located at the bottom in plating or Passivation Treatment pond, and the revolving speed of magnetic stir bar is defeated
Outlet is connect with magnetic agitation rotor speed control window, and temperature display and control window show and control target temperature and temperature spy
Head ambient temperature；Temp probe one end insertion plating or Passivation Treatment pond cooling sandwith layer cooling water in, temp probe it is another
One end is connect by conducting wire with temperature display and control window, and experimental temperature is in temperature display and control window real-time display；Add
Pyromagnetic force blender stablizes fixed frame in heating magnetic stirring apparatus by platform loading fixed frame, by fastening nut cooperation
On platform, the movable iron clamp position adjusted on fixed frame consolidates temp probe and plating or Passivation Treatment pond.
The coating or passivation layer preparation facilities of the flexible control environmental parameter, power supply unit pass through positive and negative anodes nut
It is U-shaped with the cathode connecting wire of the U-shaped fork of the positive connecting wire of positive connecting wire one end and cathode connecting wire one end respectively
Fork is fixed, and the positive connecting wire electric wire butt joint of the positive connecting wire other end and the cathode of the cathode connecting wire other end connect
Connect the anode and cathode that the butt joint of conducting wire electric wire is transferred to plating or Passivation Treatment system respectively.
The coating or passivation layer preparation facilities of the flexible control environmental parameter, the anode sample that anode uses are being electrolysed
Expose reaction surface in liquid or passivating solution, the other faces of anode sample are encapsulated by insulation-encapsulated insulation resin, pass through insulation-encapsulated tree
Anode sample is connect by rouge medial surface conducting wire connection welding with positive wire；The cathode sample that cathode uses is in electrolyte or passivation
Expose reaction surface in liquid, the other faces of cathode sample are encapsulated by insulation-encapsulated insulation resin, pass through insulation-encapsulated resin medial surface
Cathode sample is connect by conducting wire connection welding with cathode wire.
The coating or passivation layer preparation facilities of the flexible control environmental parameter, the programmable controller of power supply unit
PLC unit designs three parts: time record and control section, electrogram and control section and electric current record and control unit
Point.
The coating of the flexible control environmental parameter or the application method of passivation layer preparation facilities, including pre-treatment, electricity
Solution or passivation, post-processing, the specific steps are as follows:
(1) cathode and anode cleaning: cathode and anode sample welding lead post package sample obtain cathode and anode, put
It is cleaned in alcohol, and 5~10min is shaken with ultrasonic instrument；After washing the dust and grease being infected with after approved sample, deionized water
It is cleaned, the drying of hair dryer cold wind；
(2) plating or Passivation Treatment pond are fixed: the plating of 200~1000mL of volume or the production of Passivation Treatment pond periphery design
Water-bath cooling interlayer with polytetrafluoroethylene (PTFE) material or glass material, plating or Passivation Treatment pond are put into heating magnetic stirring apparatus
Fixed frame in it is fixed, plating or Passivation Treatment pond it is suitable for reading it is vertical upward；
(3) cathode and anode are placed: the cleaned anode and cathode are fixed in plating or Passivation Treatment pond
Middle position, opposite be parallel to each other of the reaction surface of anode and cathode separate the reaction distance of 2~4cm, close at plating or passivation
Manage pond upper cover；
(4) treatment fluid is to entering: pouring into pre- electrolyte or passivating solution in plating or Passivation Treatment pond, liquor capacity is being electroplated
Or the 2/3~4/5 of Passivation Treatment pond maximum volume, the anode sample of anode and the cathode sample bottom of cathode be placed in liquid level with
On；Then, the magnetic stir bar of heating magnetic stirring apparatus is added in electrolyte or passivating solution；
(5) experiment starts to judge: to be heated, cooling or protective gas source switch system reaches stable state, is rotated down
The positive wire of anode and the cathode wire of cathode, make treatment fluid cover anode sample and cathode sample 2mm or more, heat at this time
The temperature display and control window display screen temperature of magnetic stirring apparatus are stablized in experiment required temperature T；Alternatively, this is specific by energy
Reason measures electrolyte or passivating solution gas content, and it is up to standard that electrochemical workstation test judgement measures dissolved gas p in treatment fluid,
The standard corrosion potential of cathode opposite anode reaches experiment predetermined value；Anode is surveyed as reference electrode, system corrosion potential
When examination determines to measure that dissolved gas is up to standard in treatment fluid, cathode reaches experiment predetermined value with respect to corrosion potential；
(6) in experiment process: after system is stablized, positive connecting wire, cathode connecting wire and power supply unit are connected, into
The following operation of row: the positive connecting wire electric wire butt joint of positive connecting wire and the cathode connecting wire electricity of cathode connecting wire
The positive wire of anode and the cathode wire of cathode are pushed down in line butt joint respectively, then screw the positive spiral shell of power supply unit respectively
The U-shaped fork of the positive connecting wire that mother pushes down positive connecting wire with cathode nut respectively is connected with the cathode of cathode connecting wire leads
The U-shaped fork of line, then power supply is opened, adjust current density 0.02A/dm2~50A/dm2, power supply supply is closed after sample electroplating processes
Device, amount of liquid is controlled by plating or Passivation Treatment pond filling opening in experiment, the processing time by heating magnetic stirring apparatus heating when
Between display window set；If being only passivated operation, access power supply unit is not needed in the step, controls temperature, atmosphere
Condition, cathode surface passivation layer to be processed is spontaneous to be formed in passivating solution.
The coating of the flexible control environmental parameter or the application method of passivation layer preparation facilities, such as experiment need to add
Heat, cooling or adscititious gases measure, choice experiment condition perform the following operation:
A, it heats: using the temperature display and control window and its temp probe of heating magnetic stirring apparatus, adjusting and stablize temperature
5~80 DEG C of degree adjusts revolving speed control window value and controls magnetic stir bar, guarantees solution uniformity；
B, cooling: the periphery design cooling sandwith layer in sealing plating or Passivation Treatment pond, cooling sandwith layer downside open up cooling water
Import, cooling sandwith layer upside open up cooling water outlet, and the cooling water of cooling sandwith layer is connected in the cooling water source outlet of additional water bath
Import, cooling water outlet connect water bath water inlet formed cooling circuit, actual temperature by heating magnetic stirring apparatus temperature
Probes records are spent, temperature level is adjusted by water flow velocity in control cooling sandwith layer, and solution uniformity is controlled by stirring rotor speed；
C, ventilate: the upper cover in plating or Passivation Treatment pond opens up air inlet and gas vent, connects plating or Passivation Treatment pond
The additional carrier gas of the air inlet of upper cover, hose air exit immerse the underwater of 200~500mL volumetric flask；Protective gas is nitrogen
One kind of gas, argon gas or other inert gases, reaction gas are oxygen, hydrogen or ammonia；
Actual experiment selects one of aforesaid operations or two or more experiment parameters, such as reproducibility environment room temperature electricity
Plating, but the electroplating process heat release need to load three kinds of heating, cooling and ventilation addition theretos.
The coating of the flexible control environmental parameter or the application method of passivation layer preparation facilities, anode and cathode carry out
Pre-treatment and encapsulation, specific as follows:
(1) pretreatment process of anode and cathode includes: to guarantee that impressed current carries out plating or gas solubility is surveyed
Electric field line uniformity when examination process selects the size in anode example reaction face for 2~3 times of cathode sample；Cathode sample to be processed
Product: long 11~16mm × wide 11~16mm × 3~5mm of thickness, selecting purity is 99.7wt% with Anodic sample: long 21~46mm
× wide 21~46mm × 3~5mm of thickness；Sample craft edge chamfer 0.5mm × 45 °, six surfaces by slightly to carefully sequentially water mill to
800~2000#；Sample is soaked in 5.0vol.% acetone+95.0vol.% alcohol again, cooperates Supersonic Wave heating 30~80
DEG C cleaning 10~30min；Then, cleaned with deionized water, the drying of hair dryer cold wind is spare；
(2) electrolyte or passivating solution gap are penetrated into order to prevent, and fixed plating, passivation or gas solubility test
Example reaction face surface area: the long 10~15mm × wide 10~15mm of cathode sample, the long 20~45mm of anode sample × wide by 20~
45mm, sample needs are packaged processing；
The encapsulation process of sample includes: the 1.5mm of 100~300mm of clip length first2Copper conductor removes both ends each 3
The plastic insulation layer of~5mm grinds off exposed copper oxide layer with 80~150# sand paper；Then with soldering or high temperature spot welding by copper core
Conducting wire front end is fixed on the anode sample and cathode sample center side got ready, and spot size is 1~2mm；It is determined with multimeter
After the conduction of copper wire and sample, sample is fixed on mold bottom center；It is poured into after insulation-encapsulated resin agitating is mixed
Mold, only exposes the response area of anode anode and cathode sample, insulation-encapsulated resin pour into that depth is thickness of sample 3~
5 times；After room temperature 12~solidification for 24 hours, it is removed from the molds from the anode and cathode electrode prepared, corase grinding-fine grinding-polishing
Process makes the reaction surface metal of sample in specular brightness.
The coating of the flexible control environmental parameter or the application method of passivation layer preparation facilities, plating or Passivation Treatment
Pond upper cover tapping is equipped with anticorrosive plastic material Seal Kit: band inner hole stud, O-ring, solid or hollow hold-down bolt, aperture
Guarantee corresponding interpolation pipeline: anode, cathode, air inlet pipe, the stabilization and tight suture of exhaust pipe and inlet tube；At plating or passivation
The top Li Chi air inlet is inscribed bottom of the tube and is vented from plating or Passivation Treatment bottom of pond 2~3mm of end, plating or Passivation Treatment pond top
Mouth inner connecting tube 1~2mm with a distance from plating or Passivation Treatment pond upper cover, plating or the socket of Passivation Treatment pond top exhaust outlet extension tube attached
Hose, hose are connected to underwater inside swept volume bottle, and the air in electrolyte or passivating solution is discharged, make outside air without
Method enters plating or Passivation Treatment pond.
The coating of the flexible control environmental parameter or the application method of passivation layer preparation facilities, plating or Passivation Treatment
The not external flow straightener of system, is directly passivated in metallic matrix or metallic film surface；Coating or passivation layer cleaning after, then by its
20~200 DEG C of 5~60min of processing in protective atmosphere drying box are placed, its superficial layer is fixed.
The advantages of the utility model and beneficial effect are:
1, the preparation facilities of the utility model homogeneous coating, the device are equipped at power supply unit, conducting wire, plating or passivation
The composition such as reason system, the stable potential or electric current that power supply unit provides can control the time, and conducting wire plays stabilized power supply and yin
Between anode effectively conducting act on, plating or Passivation Treatment system can regulate and control the atmosphere of confined space, solute temperature, concentration and
Type, distance and the size of even property and anode and cathode.The utility model is independently reequiped by commercially available common device, low in cost, operation
Simply, stablize safety.
2, the utility model realizes power supply unit programmable control (PLC), automatically controls and acquisition current potential, electric current are timely
Half interval contour, overload-alarm is stable, securely and reliably.
3, the plating of the utility model or Passivation Treatment system can control the temperature of experimental solutions, atmosphere, the uniformity, dense
The parameters such as degree, can be added special ion according to requirement of experiment.
4, the anode and cathode of the plating of the utility model or Passivation Treatment system passes through special package, guarantees the accurate of reaction surface
Property, anode reaction face is designed as 2~3 times or so of cathode reaction face, guarantees electric field line uniformity, make to test it is more accurate, simultaneously
It is easy to Reusability.
5, the anode and cathode mounting means of the plating of the utility model or Passivation Treatment system passes through special adaptations, can comparatively fast adjust
It saves the position of sample and guarantees the leakproofness of system, quickly measure solubility of the gas in electrolyte or passivating solution, closed loop
The accuracy that sample guarantees the processing time is immersed after the conditional stability of border.
6, the utility model can guarantee that solution uniformity, cooling water and heating component control temperature by magnetic agitation,
Disengaging gas guarantees that solution dissolves atmosphere in seal, and process sampling analysis guarantees electrolyte or passivating solution concentration.
7, gas content is ingenious in the utility model electrolyte or passivating solution is demarcated by Nernst equation, and mark is made
Directrix curve simply can accurately control gas flow in electrolyte or passivating solution.
8, the lead material of the utility model connection power supply and superficial treatment system is copper wire, and connector passes through special transformation
Close connection avoids generally existing oxidation poor contact problem between connector.
9, the utility model cathode forms uniform films by processing, after over cleaning dries up, bakes under high pure nitrogen protection
Certain time surface of stability layer crystal state is sintered on furnace.
Detailed description of the invention
Fig. 1 is the utility model whole device structure chart.In figure, A, anode；B, cathode；C, plating or Passivation Treatment pond；
C1, upper cover；C2, cooling sandwith layer；C3, cooling water inlet；C4, cooling water outlet；C5, air inlet；C6, exhaust outlet；C7, liquid feeding
Mouthful；D, magnetic stirring apparatus is heated；D1, fixed frame；D2, magnetic stir bar；D3, heating time display window；D4, temperature display and
Control window；D5, revolving speed control window；D6, temp probe；D7, movable iron clamp；D8, platform；E, electrolyte or passivating solution；
F, positive connecting wire；F1, positive connecting wire electric wire butt joint；F2, the U-shaped fork of positive connecting wire；G, cathode connection is led
Line；G1, cathode connecting wire electric wire butt joint；G2, the U-shaped fork of cathode connecting wire；H, power supply unit；H1, the time record and
Control section；H2, electrogram and control section；H3, electric current record and control section.
Fig. 2 (a) is the schematic diagram of anode (A) component, and Fig. 2 (b) is the schematic diagram of cathode (B) component.In figure, A1, anode
Sample；A2, insulation-encapsulated resin；A3, conducting wire connection welding；A4, positive wire；B1, cathode sample；B2, insulation-encapsulated resin；
B3, conducting wire connection welding；B4, cathode wire.
Fig. 3 is room temperature electrogalvanizing propulsive cathode vs anode potential difference E and dissolved oxygen DO curve.In figure, abscissa log10(DO)
Dissolved oxygen (mg/L) is represented, ordinate represents EBvs.ARepresent potential difference (V).
Specific embodiment
As shown in Figure 1, the utility model provides a kind of plating for flexibly controlling the environmental parameters such as atmosphere, temperature and ion concentration
Layer prepares experimental rig, can control the accurate parameter of environment (such as: anode and cathode type, solution uniformity, temperature, dissolved gas)
It is down metal material surface depositing homogeneous cover film, the device is mainly by plating or Passivation Treatment system, conducting wire, power supply provider
Composition, plating or Passivation Treatment system mainly include anode, cathode, heating magnetic stirring apparatus and honeycomb seal plating or passivation
Processing pond, anode, two electrode of cathode bestow fixed current density or electricity by cathode and an anode conducting wire external power supply power supply unit
Position.Cathode will form a uniform monometallic or alloy-layer after a certain period of time, such as: zinc, nickel, nickel zinc alloy.The equipment
Not external flow straightener just can be directly passivated in metallic matrix or metallic film surface, such as: contain chromium or phosphorous passivation layer.Plating
After layer or passivation layer cleaning, then 20~200 DEG C of 5~30min of processing in drying box are placed, fixes its superficial layer.Plating or
Passivation Treatment system is capable of providing the accurate experiment condition of experiment process, and power supply provider provides plating or electro-deposition stable experiment
Current potential or current density, conducting wire plays good conducting between plating or Passivation Treatment pond and power supply, specific as follows:
Side opens up a cooling water inlet C3 and above opens and sets under cooling sandwith layer C2 on the outside of plating or Passivation Treatment pond C
One cooling water outlet C4, using the common water bath of peripheral large body (1000mL~5000mL) can control plating or it is blunt
Change the electrolyte or passivating solution E low-temperature electrolytic condition in processing pond C, and exothermicity electroplating process electrolyte or passivation can be taken away
Liquid E after-heat, electrolyte or passivating solution E lower temperature scale can combine water flow temperature and rate adaptation.At plating or passivation
The plating or Passivation Treatment pond upper cover C1 for managing pond C tight seal have 5 openings (anode port, cathode port, air inlet C5, exhaust outlet
C6 and filling opening C7), the anticorrosive plastic material (such as: polytetrafluoroethylene (PTFE), rubber) that upper cover C1 aperture has respective interior bores to design
Seal Kit (band inner hole stud, O-ring, solid or hollow hold-down bolt), solid bolt can direct closed function, inner hole
Guarantee the stabilization and tight suture of corresponding interpolation pipeline (anode A, cathode B, air inlet pipe, exhaust pipe and inlet tube).Plating is blunt
Change the top processing pond C air inlet C5 be inscribed bottom of the tube from plating or Passivation Treatment bottom of pond 2~3mm of end, plating or Passivation Treatment pond
The top C exhaust outlet C6 inner connecting tube 1~2mm with a distance from plating or Passivation Treatment pond upper cover C1, plating or Passivation Treatment pond top row
Port C6 extension tube attached is socketed hose, and hose connects the internal underwater of swept volume bottle (500mL~1L), can by electrolyte or
Air discharge in passivating solution E, and outside air is made to cannot be introduced into plating or Passivation Treatment pond C.
What the heating magnetic stirring apparatus D that the utility model uses was produced by Dragon Laboratory Instruments (Beijing) Co., Ltd.
Magnetic stirring apparatus is heated in MS7-H550-Pro thermostatic control, and there are three control window: heating time display window D3, temperature for tool
Display and control window D4, magnetic agitation rotor speed control window D5.Magnetic stir bar D2 is located at plating or Passivation Treatment pond C
The revolving speed output end of bottom, magnetic stir bar D2 is connect with magnetic agitation rotor speed control window D5, magnetic agitation rotor speed control
Window D5 operating rotational speed range processed is 100~1500rpm, and the revolving speed for adjusting electrolyte or passivating solution bottom magnetic stir bar D2 changes
Kind electrolyte or passivating solution uniformity.Heat magnetic stirring apparatus D heating temperature range be room temperature~280 DEG C, temperature display and
Control window D4 can show and control target temperature and temp probe D6 ambient temperature.Plating is inserted into one end of temp probe D6
Or in the cooling water of Passivation Treatment pond cooling sandwith layer C2, the other end of temp probe D6 passes through conducting wire and temperature display and control window
Mouth D4 connection, experimental temperature is in temperature display and control window D4 real-time display.According to different experiments temperature requirement (5~90
DEG C), and in view of heat release or heat absorption in electroplating process, plating or Passivation Treatment pond C periphery design have heating and cooling at this time
Device.In conjunction with the temperature and flow velocity of cooling water in the cooling sandwith layer C2 for adjusting plating or Passivation Treatment pond C, magnetic stirring apparatus is heated
The heating component help of D reaches experimental temperature.After heating magnetic stirring apparatus D repacking, pass through stainless steel platform D8 loading fixed frame
Fixed frame D1 is stablized on the platform D8 of heating magnetic stirring apparatus D by two fastening nut cooperations, adjusts fixed frame D1 by D1
On the position movable iron clamp D7 consolidate temp probe D6 and plating or Passivation Treatment pond C.
12V, the 500A high that the power supply unit H that the utility model uses is produced by Dongguan City Run Feng Electronics Co., Ltd.
Frequency switch electrolysis power, the overload protecting circuit of Switching Power Supply guarantee the safety in experimentation.Power supply unit H can journey
Formula controller (PLC) unit designs three parts: time record and control section H1, electrogram and control section H2 and electric current
Record and control section H3 need to reach different pulse potentials or electric current purpose in electroplating process electrolyte according to experiment, in advance
Setting electrolysis time equipment ends automatically experiment.
The power supply unit H that the utility model uses, anode connecting wire F and cathode connecting wire G, conducting wire are city
Sell 1.5mm2Red copper core electric wire.Power supply unit H is connect with the anode of the one end positive connecting wire F respectively by positive and negative anodes nut
The U-shaped fork F2 of conducting wire and the U-shaped fork G2 of cathode connecting wire of the one end cathode connecting wire G are securely fixed, and positive connecting wire F is another
The positive connecting wire electric wire butt joint F1 at end and the cathode connecting wire electric wire butt joint G1 of the cathode connecting wire G other end divide
It is not transferred to the anode A and cathode B of plating or Passivation Treatment system.
As shown in Fig. 2 (a)-(b), anode A provided by the utility model and cathode B component, specific structure are as follows:
The metal anode sample A1 (such as: pure noble metal copper, titanium, rubidium, platinum, gold sheet metal, 3~5mm of thickness) that anode A uses
Expose reaction surface (long 20~30mm × wide 20~30mm) in electrolyte or passivating solution, other faces are by insulation-encapsulated Resin A 2
(such as: epoxy resin) insulation-encapsulated is got up, by metal lateral conductive lines connection welding A3 in resin by sample and positive wire A4
(such as: copper conductor) connects.Dedicated MPD2-195 male and female head connects positive wire A4 and positive connecting wire electric wire respectively
After butt joint F1 connection, conducting wire and MPDFRD pin and box sub are compressed with dedicated Press Plier, dock male and female head it is ensured that anode
Conducting wire A4 and the anode benign connection of connecting wire electric wire butt joint F1 prevent port from aoxidizing or polluting.
Anode A carries out pre-treatment and encapsulation, specific as follows:
(1) pretreatment process of anode A includes: to select purity for 99.7wt% first, and long (21~46) mm of wire cutting ×
As anode sample A1, manual edge falls the sheet metal (all being described below using titanium sheet) of width (21~46) mm × thickness (3~5) mm
Angle 0.5mm × 45 °, six surfaces by slightly to carefully sequentially water mill to 800~2000#；Titanium sheet is soaked in 5.0 vol.% third again
In ketone+95.0vol.% alcohol, cooperate 30~80 DEG C of 10~30min of cleaning of Supersonic Wave heating.Then, it is cleaned with deionized water
Good, the drying of hair dryer cold wind is spare.
(2) electrolyte or passivating solution gap are penetrated into order to prevent, and fixed anode reaction surface area, titanium sheet need to insulate
Potting resin A2 encapsulation process.The encapsulation process of anode A includes: the 1.5mm of clip length about 200mm first2Copper conductor,
The plastic insulation layer for removing each 3~5mm in both ends, exposed copper oxide layer is ground off with 80# sand paper；Then with soldering or high temperature spot welding
Copper wire front end is fixed on to the titanium sheet center side got ready, spot size is 1~2mm；Copper wire and titanium sheet are determined with multimeter
After conduction, it is 25~50mm × 25~50mm mold bottom center that anode sample A1, which is fixed on area,；By asphalt mixtures modified by epoxy resin
The stirring of rouge AB glue pours into mold after being mixed, and only exposes titanium sheet 20~45mm × 20~45mm response area, pours into depth about
It is 3~5 times of thickness of sample；It after room temperature solidifies for 24 hours, is removed from the molds from the anode A prepared, corase grinding-fine grinding-throwing
Photoreduction process makes the reaction surface metal of anode sample A1 in specular brightness.
To be electroplated or Passivation Treatment cathode sample B1 (such as: Q235, No. 45 steel, 314 stainless steels) in electrolyte or
Expose reaction surface 10~15mm × 10~15mm in passivating solution, other faces are insulated by insulation-encapsulated resin B 2 (such as: epoxy resin)
It is encapsulated, is connect sample with cathode wire B4 (such as: copper conductor) by metal lateral conductive lines connection welding B3 in resin
Get up.Similarly, the use of elastic MPD2-195 male and female head can ignore external power supply cathode wire B4 and cathode connecting wire G and connect
The potential drop that mouth generates.
Cathode B carries out pre-treatment and encapsulation, specific as follows:
(1) pre-treatment of cathode B includes: to select long (11~16) mm × wide (11~16) mm × thickness (3~5) mm first
Commercially available material silicon carbide paper polishes chamfering 0.5mm × 45 ° again；Again by material piece to be processed be soaked in 5.0vol.% acetone+
In 95.0vol.% alcohol, cooperate 30~80 DEG C of 10~30min of cleaning；Then, cleaned with deionized water, hair dryer cold wind is blown
It does spare.
(2) encapsulation process of cathode B can use the encapsulation process of anode A.Reaction surface is 10~15mm × 10~15mm
Size, base material are the industrial alloys in common use such as carbon steel (Q235), titanium alloy (TC4), stainless steel (304SS).
Electrolyte or passivating solution gap are penetrated into order to prevent, and fixed negative pole reaction surface area, cathode sample need into
Row encapsulation process；The encapsulation process of cathode sample includes: the 1.5mm of clip length 200mm first2Copper conductor removes both ends
The plastic insulation layer of each 3~5mm grinds off exposed copper oxide layer with 80~150# sand paper；It then will with soldering or high temperature spot welding
Copper conductor front end is fixed on the cathode sample center side got ready, and spot size is 1~2mm；With multimeter determine copper wire and
After the conduction of cathode sample, it is 15~20mm × 15~20mm mold bottom center that cathode sample, which is fixed on area,；
Mold is poured into after insulation-encapsulated resin agitating is mixed, and only exposes cathode sample 10~15mm × 10~15mm reaction surface
Product pours into 3~5 times that depth is thickness of sample；After room temperature 12~solidification for 24 hours, it is removed from the molds from the cathode prepared,
Corase grinding-fine grinding-polishing process makes the reaction surface metal of cathode sample in specular brightness.
The utility model using flexible controls the sample coating or passivation layer preparation facilities of environmental parameter, including walks as follows
It is rapid:
(1) anode and cathode is cleaned: approved sample after cathode and anode sample welding lead obtains Fig. 2 (a)-(b) cathode B and anode A
Shape is placed in alcohol and cleans, and shakes 5~10min with ultrasonic instrument.Wash the dust and grease that may be infected with after approved sample
Afterwards, deionized water is cleaned, the drying of hair dryer cold wind.
(2) plating or Passivation Treatment pond fix: design and produce the water-bath cooling interlayer of polytetrafluoroethylene (PTFE) material 200~
The plating of 1000mL volume or Passivation Treatment pond C, pond body are put into fixed in the stainless steel fixed frame D1 of heating magnetic stirring apparatus D, electricity
Plating or Passivation Treatment pond C it is suitable for reading it is vertical upward.
(3) cathode and anode are placed: utilizing plating or the Passivation Treatment pond position upper cover C1 aperture respective anode A and cathode B
Industry commonly use polytetrafluoroethylene (PTFE) material Seal Kit, the cleaned anode A and cathode B are fixed at plating or passivation
The middle position pond C is managed, opposite be parallel to each other of reaction surface separates the reaction distance of 2~4cm, close plating or Passivation Treatment pond upper cover
C1。
(4) treatment fluid is to entering: pouring into pre- electrolyte or passivating solution E in plating or Passivation Treatment pond C, liquor capacity is in electricity
Plating or Passivation Treatment pond C maximum volume 2/3~4/5, the bottom cathode sample B1 of the anode sample A1 and cathode B of anode A are set
More than liquid level.Then, the magnetic stir bar D2 of heating magnetic stirring apparatus D is added in electrolyte or passivating solution E.
(5) optional experiment condition:, can if experiment needs to heat, cooling or adscititious gases (protection or reagentia) measure
The following operation of choosing:
A, it heats: using the temperature display and control window D4 and its temp probe D6 of heating magnetic stirring apparatus D, being adjusted
It 5~80 DEG C of equilibrium temperature, adjusts revolving speed and controls window D5 Numerical Control magnetic stir bar D2, guarantee solution uniformity；
B, it cooling: is opened up on the downside of the periphery design cooling sandwith layer C2 of sealing plating or Passivation Treatment pond C, cooling sandwith layer C2 cold
But cooling water outlet C4 is opened up on the upside of water inlet C3, cooling sandwith layer C2, the cooling water source outlet of additional 5L and the above water bath connects
The cooling water inlet C3 of logical cooling sandwith layer, cooling water outlet C4 connect water bath water inlet and form cooling circuit, practical temperature
Degree by heating magnetic stirring apparatus D temp probe D6 record, temperature level adjusted by water flow velocity in control cooling sandwith layer (5~
20 DEG C), solution uniformity is controlled by stirring rotor speed；
C, ventilate: the upper cover C1 of plating or Passivation Treatment pond C open up air inlet C5 and gas vent C6, connect plating or passivation
The additional carrier gas of air inlet C5 of processing pond upper cover C1, hose air exit immerse the underwater of 200~500mL volumetric flask.It protects
Shield gas is one kind of nitrogen, argon gas or other inert gases, and reaction gas is oxygen, hydrogen, ammonia etc..
Actual experiment may select one of aforesaid operations, or wherein several experiment parameters, such as reproducibility environment room temperature
Plating, but the electroplating process heat release it is necessary to load heating, cooling and ventilation three kinds of attachment devices.
(6) experiment starts to judge: to be heated, cooling or protective gas source switch system reaches stable state, is rotated down
The cathode wire B4 of the positive wire A4 and cathode B of anode A must make treatment fluid cover sample strip (anode sample A1, cathode sample
Product B1) 2mm or more, the temperature display and control window D4 display screen temperature for heating magnetic stirring apparatus D at this time, which are stablized, is testing institute
Need temperature T.Alternatively, measuring electrolyte or passivating solution gas content, electrochemical workstation test judgement by Nernst theorem
It is up to standard (according to Nernst equation E=Eo+2.3 RT/Fln (p/p to measure dissolved gas p in treatment fluidθ), cathode B is relatively positive
The standard corrosion potential of pole A reaches experiment predetermined value.Anode A is surveyed as reference electrode, system corrosion potential test judgement
When dissolved gas is up to standard in treatment fluid, cathode B reaches experiment predetermined value with respect to corrosion potential.
(7) in experiment process: after system is stablized, connecting positive connecting wire F, cathode connecting wire G and power supply unit H
(galvanostat power supply), proceeds as follows: the positive connecting wire electric wire butt joint F1 of positive connecting wire F is connected with cathode
The cathode connecting wire electric wire butt joint G1 of conducting wire G pushes down the cathode wire B4 of the positive wire A4 and cathode B of anode A respectively,
Then the anode connection that the positive nut and cathode nut for screwing power supply unit H respectively push down positive connecting wire F respectively is led
The U-shaped fork G2 of cathode connecting wire of the U-shaped fork F2 and cathode connecting wire G of line, then power supply is opened, adjust current density 0.02A/
dm2~50A/dm2, sample electroplating processes close power supply unit H after a certain period of time, and amount of liquid can be by plating or blunt in experiment
Change processing pond filling opening C7 control, the processing time can be set by the heating time display window D3 of heating magnetic stirring apparatus D.
If being only passivated operation, access power supply unit H is not needed in the step, the conditions such as control certain temperature, atmosphere are to be processed
Cathode B surface passivation layer is spontaneous to be formed in passivating solution.
It is worth noting that, if there is obvious sediment or color change in electrolyte or passivating solution E in experimentation, usually
Closing electrolytic cell filling opening C7 can assemble pH value meter probe or sampling, sampling analysis add related solute component again.Again it adjusts
After whole solution composition closing electrolytic cell, load is cooling or heats according to temperature display and control window D4 again stable experiment temperature
Degree, load is outer to add body according to anode and cathode potential difference again stablizing solution concentration.
(8) stop experiment: closing and remove exhaust heat insulation device, open plating or Passivation Treatment pond upper cover C1, remove subsidiary
The facilities such as heating, cooling, degasification, take out cathode B and simultaneously rinse the surface metallic cathode sample B1 with ethyl alcohol, with deionized water ultrasound
Rinse room temperature drying after, place bulk purity 99.9% 50~200 DEG C of dryings 5 of nitrogen atmosphere oven or drying box~
60min processing takes out sample for surface quality detection.
In the following, being further elaborated on by embodiment and attached drawing to the utility model.
Embodiment 1
The current potential E of cathode B vs anode A and the measurement of dissolved oxygen standard curve are as follows in 25 DEG C of electrogalvanizing liquid of room temperature:
The experimental material of cathode B to be processed is domestic commercially available Q235 carbon steel, and anode A material is that commercially available 99.99wt% is high-purity
Titanium sheet.Commercially available alkali formula is 10g/L ZnCl without cyanogen room temperature electrolytic zinc ingredient2, 120g/L NaCl, 850 type alkali formula electrogalvanizings lights
Agent A, the agent B and cleanser C that walks are respectively 6mL/L, 1mL/L and 2mL/L, remaining is water, and pH value control is 3.0.According to can this
Specific rule E=E0+2.3RT/F·ln(p/pθ), E and DO are in logarithmic relationship.It is previously obtained the standard curve of the E ∝ DO of B vs A,
The dissolved oxygen DO of the solution can be conveniently indirectly controlled by E later.The measurement of experiment E passes through 2273 electrification of PARSTAT
It learns work station (Princeton instrument), the measurement of DO passes through HI9143 dissolved oxygen instrument (Italian Kim Yong-jin), pH value
By the desk-top pH meter (Mettler Toledo Inc. of Switzerland) of EF28, experimental procedure is as follows for test:
(1) preparing experiment: 300mL zinc plating electrolyte is added into 500mL plating or Passivation Treatment pond, places magnetic in solution
Power stirrer immerses in solution after connecting cathode and anode.Dissolved oxygen instrument is installed in former filling opening position, and dissolved oxygen instrument dissolves at this time
Oxygen saturation 8.2ppm (mg/L).Air inlet connects High Purity Nitrogen gas tank, and exhaust outlet connects seal protecting device, places at plating or passivation
Pond body is sealed after managing the upper cover in pond.Then, magnetic agitation is heated on heating magnetic stirring apparatus in fixed plating or Passivation Treatment pond
In the temp probe access plating of device or the cooling water of Passivation Treatment pond cooling sandwith layer C2, set temperature shows and controls window D4
25 DEG C of equilibrium temperature.Then, electrochemical workstation working electrode line connects cathode wire by conducting wire pin and box sub, to electrode wires and
Cathode wire is connect by conducting wire pin and box sub after reference electrode wire docking.
(2) current potential-solubility test experiment: window D5 is controlled by magnetic agitation rotor speed and adjusts solution uniformity, is beaten
High Purity Nitrogen bottle is opened into valve, exhaust outlet bubble is got after stablizing by current potential record portion on electrochemical workstation and dissolved oxygen instrument
Standard E ∝ DO data.
(3) stop experiment: closing and remove electrochemical recording part, dissolved oxygen instrument device, open plating or Passivation Treatment pond
Upper cover C1 removes the facilities such as subsidiary exhaust, heating, cooling, takes out cathode anode and is cleaned and dried preservation.
As shown in figure 3, room temperature electrogalvanizing propulsive cathode vs anode potential E and dissolved oxygen DO curve, E ∝ DO meets can this special formula
Journey E=-0.52+0.13log10(DO).Therefore, after logical High Purity Nitrogen 2h is stablized in laboratory (occur in swept volume bottle 2 bubbles/
S), B vs A corrosion potential E is -0.65V, and dissolved oxygen is 0.1mol/L (100ppb) at this time.
Embodiment 2
Electrogalvanizing+trivalent chromium passivation process is such as in the electrolyte of room temperature, plating or Passivation Treatment pond C for domestic Q235 steel
Under:
The experimental material of cathode to be processed is domestic commercially available Q235 carbon steel, and selection anode material is commercially available 99.99wt% high
Pure titanium sheet.Test galvanizing technique: electrolyte such as example 1, temperature T are 25 DEG C, and dissolved oxygen DO is 0.1mol/L (ppm).Experiment
The U.S. finish materials Co., Ltd of the Suzhou Ji of selection sells FC-85 trivalent blue-white chromating liquid, and temperature is 25 DEG C, pH value
Control is 2.0, and experimental procedure is as follows:
(1) electroplating experiments prepare: 300mL zinc plating electrolyte being added into 500mL plating or Passivation Treatment pond, puts in solution
Magnetic stir bar is set, cathode is connected and anode sample bottom is placed on right above solution.Air inlet connects High Purity Nitrogen gas tank, exhaust
Mouth connects seal protecting device, seals pond body after placing plating or Passivation Treatment pond upper cover.Then, fixed plating or Passivation Treatment pond
Heating magnetic stirring apparatus on, heat magnetic stirring apparatus temp probe access plating or Passivation Treatment pond cooling sandwith layer C2 it is cold
But in water, set temperature shows and controls 25 DEG C of window D4 equilibrium temperature.Then, power supply unit anode is connect by conducting wire male and female
Head connects positive wire, and power supply unit cathode connects cathode wire by conducting wire pin and box sub.It controls window D5 and sets magnetic agitation
Rotor speed 200rpm adjusts solution uniformity, opens High Purity Nitrogen bottle into valve, exhaust outlet immerses in exhaust bottle water, with current potential EBvsA
=-0.64V is criterion, DO 100ppb.At this point, constant speed stablizes the logical general 2h of High Purity Nitrogen, air-breather is closed.
(2) when electroplating experiments: intrusion cathode and anode sample are placed in Solutions Center, the parallel face 3mm of reaction surface.This process
Notice that sealing screw rod stablizes the insulating air for keeping solution.Then, open power supply unit, electrogram and control section H2 and
Electric current record and control section H3 adjust current density, JkFor 5A/dm2, control electroplating time t is 20min.
(3) Inactivation experiment prepares: closing and the devices such as removes exhaust, heat preservation, is powered, opens plating or Passivation Treatment pond upper cover
C1 takes out cathode anode, and anode cleaning saves, and cathode carries out 5s in the nitric acid that concentration is 1.0wt% after being cleaned and dried and goes out light
Processing.Clean up that dry cathode sample is fixed to be placed in and sample electroplating experiments handle same shape 500mL plating or passivation
In processing pond, sealing plating or Passivation Treatment pond after heating, cooling attachment are connected.
(4) when Inactivation experiment: 300mL trivalent blue-white chromating liquid, 25 DEG C of passivation time 20s of equilibrium temperature are added.
(5) passivation post-processing: after deionized water cleaning, 100 DEG C of placement 30min of drying box solidify steady oxide, next
Step preparation is to sample surfaces layer performance evaluation.
According to Q235 carbon steel skin covering of the surface SEM sectional view after plating Passivation Treatment, internal layer is the uniform Zn plating of 14~15 μ m-thicks
Layer, outer layer are 2~4 μm of uniform Cr (III) layers.Zn layers substantially after uniform fold matrix in the modification, Cr passivation layer is not anticipated
Outer property zinc layers are protected.Double-layer structure is all without there is crackle that general coating structure is easy to appear or especially coarse
Crystal grain, it is anticipated that the highly resistance corrosion of the modified layer.System run all right in whole experiment process, the apparatus structure is simple, ginseng
It is accurate to count control, working service is all more convenient, is not in that the leakage of device inclination liquid, unlimited gaseous volatilization poisoning etc. are asked
Topic.
Embodiment the result shows that, the utility model utilizes plating or modification technology, the flexibly accurate plating of control or passivation
The experiment conditions such as environment temperature, uniformity, atmosphere, ingredient, current density, metallic conductor surface deposit monometallic film layer or
Person's alloy film.The utility model is easy to operate, easy to maintain, and the good adhesive force of coating uniformity is strong, can be applied to machinery, electronics,
Precision instrument etc..
Claims (4)
1. a kind of coating or passivation layer preparation facilities of flexibly control environmental parameter, which is characterized in that the device being capable of control ring
It is metal material surface depositing homogeneous cover film under the accurate parameter in border, the parameter is temperature, the uniformity, gas of experimental solutions
Atmosphere, dissolved gas, concentration, ion concentration, current density and anode and cathode type, experiment leakproofness, the device include plating or
Passivation Treatment system, conducting wire, power supply provider, plating or Passivation Treatment system include anode, cathode, heating magnetic stirring apparatus with
And plating or Passivation Treatment pond, anode, cathode bestow fixed current density by cathode and an anode conducting wire external power supply power supply unit
Or current potential；Wherein:
Plating or Passivation Treatment pond (C) periphery setting cooling sandwith layer (C2), the beneath side of cooling sandwith layer (C2) opens up a cooling
Water inlet (C3) opens on cooling sandwith layer (C2) and sets a cooling water outlet (C4), seals with plating or Passivation Treatment pond (C)
Plating or Passivation Treatment pond upper cover (C1) be equipped with anode port, cathode port, air inlet (C5), exhaust outlet (C6) and filling opening
(C7)；
Heating magnetic stirring apparatus (D) tool, there are three control window: heating time display window (D3), temperature display and control window
(D4), magnetic agitation rotor speed control window (D5), magnetic stir bar (D2) are located at plating or the bottom of Passivation Treatment pond (C),
The revolving speed output end of magnetic stir bar (D2) is connect with magnetic agitation rotor speed control window (D5), temperature display and control window
(D4) show and control target temperature and temp probe (D6) ambient temperature；One end insertion plating or passivation of temp probe (D6)
In the cooling water of processing pond cooling sandwith layer (C2), the other end of temp probe (D6) passes through conducting wire and temperature display and control window
(D4) it connects, experimental temperature is in temperature display and control window (D4) real-time display；Heating magnetic stirring apparatus (D) passes through platform
(D8) loading fixed frame (D1) is stablized fixed frame (D1) in the platform for heating magnetic stirring apparatus (D) by fastening nut cooperation
(D8) on, the movable iron clamp position (D7) in adjustment fixed frame (D1) consolidates temp probe (D6) and plating or Passivation Treatment pond
(C)。
2. the coating or passivation layer preparation facilities of flexible control environmental parameter described in accordance with the claim 1, which is characterized in that electricity
Source power supply unit (H) by positive and negative anodes nut respectively with the U-shaped fork (F2) of the positive connecting wire of the one end positive connecting wire (F) and bear
The U-shaped fork (G2) of the cathode connecting wire of the one end pole connecting wire (G) is fixed, the anode connection of positive connecting wire (F) other end
Conducting wire electric wire butt joint (F1) and the cathode connecting wire electric wire butt joint (G1) of cathode connecting wire (G) other end are transferred respectively
To plating or the anode (A) and cathode (B) of Passivation Treatment system.
3. the coating or passivation layer preparation facilities of flexible control environmental parameter described in accordance with the claim 1, which is characterized in that sun
The anode sample (A1) that pole (A) uses exposes reaction surface in electrolyte or passivating solution, and the other faces of anode sample (A1) are by exhausted
Edge potting resin (A2) insulation-encapsulated, by insulation-encapsulated resin (A2) medial surface conducting wire connection welding (A3) by anode sample
(A1) it is connect with positive wire (A4)；The cathode sample (B1) that cathode (B) uses exposes reaction surface in electrolyte or passivating solution,
The other faces of cathode sample (B1) pass through insulation-encapsulated resin (B2) medial surface conducting wire by insulation-encapsulated resin (B2) insulation-encapsulated
Cathode sample (B1) is connect by connection welding (B3) with cathode wire (B4).
4. the coating or passivation layer preparation facilities of flexible control environmental parameter described in accordance with the claim 1, which is characterized in that electricity
The programmable controller PLC unit of source power supply unit (H) designs three parts: time record and control section (H1), electrogram
And control section (H2) and electric current record and control section (H3).
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|---|---|---|---|
| CN201820836388.2U CN208266299U (en) | 2018-05-31 | 2018-05-31 | The flexibly coating or passivation layer preparation facilities of control environmental parameter |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108385156A (en) * | 2018-05-31 | 2018-08-10 | 东北大学 | The flexibly coating or passivation layer preparation facilities and application method of control environmental parameter |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108385156A (en) * | 2018-05-31 | 2018-08-10 | 东北大学 | The flexibly coating or passivation layer preparation facilities and application method of control environmental parameter |
| CN108385156B (en) * | 2018-05-31 | 2023-12-15 | 东北大学 | Plating layer or passivation layer preparation device capable of flexibly controlling environmental parameters and application method |
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