CN104746117A - Cathode-anode synchronous frequency-vibration strong-magnetic auxiliary electro-deposition processing device and method - Google Patents
Cathode-anode synchronous frequency-vibration strong-magnetic auxiliary electro-deposition processing device and method Download PDFInfo
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- CN104746117A CN104746117A CN201510191917.9A CN201510191917A CN104746117A CN 104746117 A CN104746117 A CN 104746117A CN 201510191917 A CN201510191917 A CN 201510191917A CN 104746117 A CN104746117 A CN 104746117A
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- 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
- C25D5/22—Electroplating combined with mechanical treatment during the deposition
Abstract
The invention provides a cathode-anode synchronous frequency-vibration strong-magnetic auxiliary electro-deposition processing device and method. The device comprises a reaction kettle, a vibration assembly, a magnetic control assembly, a mechanical stirrer, an anode basal body, a cathode basal body and a direct-current power supply; the vibration assembly comprises a vibration controller, a vibration rod, an anode hanger, a cathode hanger and a magnet hanger; the magnetic control assembly comprises a magnetic field controller, a first super-conductor magnet and a second super-conductor magnet; the mechanical stirrer, the anode basal body and the cathode basal body are arranged in a main body of the reaction kettle; the anode basal body, the cathode basal body and the two super-conductor magnets can vibrate synchronously at a same frequency. The processing comprises the steps of carrying out preliminary chemical plating treatment for the cathode basal body, installing the anode basal body and the cathode basal body, preparing an electroplating liquid system, and carrying out the electro-deposition and the after-treatment under the assisting condition. By utilizing the device and the method, an electric coating which is flat in surface, compact in tissue, small in particle size and excellent in mechanical property can be prepared.
Description
Technical field
The present invention relates to electrochemical deposition processing technique field, be specifically related to a kind of based on the synchronous frequency ventilating type of cathode and anode strong magnetic assist in electrodeposition processing unit (plant) and method.
Background technology
Electro-deposition techniques is the processing technology preparing a kind of effective practicality of high-performance coating based on the cathodic reduction of electrochemical principle, anodic oxidation.Conventional electrodeposition technology is in actual procedure, and deposition layer surface is uneven, have pin hole pit and internal stress is excessive etc., and defect often occurs.For meeting the demand of social production to quality product, solve the defect of conventional electrodeposition technology, ultrasonic wave added, temperature-negative pressure, magnetic field are assisted and the electro-deposition techniques of the multiple advanced person such as supercutical fluid galvanic deposit obtains research application, and present good economic worth; Especially supercutical fluid electrodip process, not only solves electrodeposition process intermediate ion mass transfer problem, can also the unnecessary hydrogen of effective miscible negative electrode, greatly improves the quality of deposition layer.Therefore, constantly research and develop and improve electro-deposition techniques supplementary means, can effectively improve deposition layer quality, preparing the galvanic deposit product of satisfied social industrial requirement.
Summary of the invention
The object of the invention is: be difficult to for existing electro-deposition method the problem of high-performance coating that successive sedimentation goes out surfacing, dense structure, provide a kind of and effectively can improve settled layer quality and the synchronous frequency ventilating type of anode and cathode strong magnetic assist in electrodeposition processing unit (plant) and the method for electro-deposition techniques Application Areas can be widened.
Technical scheme of the present invention is: the synchronous frequency ventilating type of anode and cathode of the present invention strong magnetic assist in electrodeposition device, and its constructional feature is: comprise reactor, vibration component, magnetic control assembly, mechanical stirrer, anode substrate, cathode base and direct supply;
Above-mentioned reactor comprises main body and top cover; Thermal insulation layer is provided with and for heater coil in main body; The middle of top cover is provided with the through through hole of upward and downward;
Vibration component involving vibrations controller, vibrating arm, anode hang tool, cathode hanging fixture and magnet hanger; Upper end and the vibrating controller of vibrating arm are in transmission connection; The lower end of vibrating arm is stretched out in the main body of reactor through the through hole of the top cover of reactor; Anode hang tool, cathode hanging fixture and magnet hanger are all arranged in the main body of reactor; Anode hang tool, cathode hanging fixture are fixedly connected with vibrating arm respectively with magnet hanger;
Magnetic control assembly comprises field controller, the first superconducting magnet and the second superconducting magnet; First superconducting magnet and the second superconducting magnet are all arranged in the main body of reactor; And the first superconducting magnet and the second superconducting magnet divide left and right to be oppositely arranged; First superconducting magnet is N pole, and the second superconducting magnet is S pole; First superconducting magnet and the second superconducting magnet are fixedly connected with the magnet hanger of vibration component respectively; Field controller is for controlling the first superconducting magnet and the second superconducting magnet makes magneticstrength continuously adjustabe in 0T to 16T scope;
Mechanical stirrer is arranged in the main body of reactor;
Anode substrate and cathode base divide left and right to be oppositely arranged in the main body of reactor; Spacing range between anode substrate and cathode base is 2cm to 4cm; Anode substrate is arranged on the right side of the first superconducting magnet; Cathode base is arranged on the left side of the second superconducting magnet; Anode substrate is fixedly connected with the anode hang tool of vibration component; Cathode base is fixedly connected with the cathode hanging fixture of vibration component; Thus make anode substrate and cathode base do with frequently moving in the same way respectively by anode hang tool and cathode hanging fixture and vibrating arm; Anode substrate and cathode base are respectively with the positive pole of direct supply with negative pole is corresponding is electrically connected.
Further scheme is: the gap between the top cover of above-mentioned reactor and vibrating arm is 0.8 ~ 1.5cm; Spacing between anode substrate and cathode base is 2cm; Spacing between the first superconducting magnet of magnetic control assembly and the second superconducting magnet is 10cm.
Further scheme is: the first superconducting magnet of above-mentioned magnetic control assembly and the second superconducting magnet are electro-magnet, and the first superconducting magnet and the second superconducting magnet are circular arc camber towards the one side of electrode, arc radius is 50cm, and angle is 6 degree to 12 degree.
A working method for the synchronous frequency ventilating type of above-mentioned anode and cathode strong magnetic assist in electrodeposition device, comprises the following steps:
1. cathode base electroless plating process in advance: the metal needing the plated surface last layer of the cathode base of galvanic deposit to be easy to carry out galvanic deposit;
2. anode substrate and cathode base are installed: by anode substrate and cathode base respectively corresponding be arranged on vibration component anode hang tool and cathode hanging fixture on; Time regulate the two poles of the earth relative position and distance;
3. electroplate liquid system is prepared: in the main body of reactor, add the electroplate liquid containing surface additive or composite plating solution that configure; Shake parameter and the magnitude of field intensity frequently of setting system temperature, mechanical stirring parameter, current density, vibration, make it to meet electrodeposition condition;
4. galvanic deposit processing: switch on power, carries out electrodeposition process at the outside surface of cathode base under mechanical stirring, magnetic force driving and vibrating controller drive anode substrate and the subsidiary conditions of cathode base with synchronous vibration frequently by vibrating arm;
5. galvanic deposit completion of processing aftertreatment: after galvanic deposit completion of processing, by aftertreatment, can obtain the electrocoat of desired properties and dense structure at the outside surface of cathode base.
Further scheme is: above-mentioned step 1. in, the surface chemistry of cathode base plates about 10 μm of thick uniform copper layers; Above-mentioned step 3. in, the electroplate liquid containing surface additive is nickel salt solution or copper salt solution; Surface additive is the additive be made up of dodecyl compounds and ether compound; Above-mentioned nickel salt or the concentration of copper salt solution are 300 ~ 500g/L; The concentration of surface additive is 0.1 ~ 2g/L; Concentration be the boric acid of 30g/L ~ 60g/L as galvanic deposit sustained release dosage.
Further scheme is: above-mentioned step 3. middle mechanical stirring is bottom level Keep agitation, and stir speed (S.S.) is 200 ~ 500rpm; System temperature controls at 20 ~ 50 DEG C; Cathode current density controls at 1A ~ 16A/dm
2.
Further scheme is: above-mentioned step 4. in vibrating controller by vibrating arm drive anode substrate and cathode base do before and after to or left and right to vibration, amplitude is no more than 0.5cm, and vibrational frequency is 0 ~ 50KHz.
Further scheme also have: above-mentioned step 3. in, the size of magneticstrength is controlled by field controller, makes magneticstrength continuously adjustabe within the scope of 0T to 16 T.
The present invention has positive effect: (1) the present invention can disperse the concentration of metal ions of cathode surface effectively during the synchronous frequency vibration galvanic deposit of cathode and anode by adopting, ensure each to homogeneity; Simultaneously can effectively shake the metal ion of cathode surface weakly stable, strong adsorbing metal ions energy fast restore deposited, suppresses grain growing simultaneously, make electrocoat dense structure, performance efficiency.(2) the present invention effectively can destroy the diffusion layer of cathode surface by electrode frequency vibration mode, forms mass transfer in liquid phase, diffusion mass transfer and the coefficient turbulent layer of electrophoresis mass transfer, accelerates the rate of mass transfer of metal ion.(3) the present invention due to amplitude less, direction of vibration and frequency can be adjusted as required, effectively can suppress edge's electrocoat skewness situation.(4) the present invention by the mode of magnetic field and motor in synchrony frequency vibration for electrodeposition process provides stable high-intensity magnetic field.
Accompanying drawing explanation
Fig. 1 is the structural representation of the synchronous frequency ventilating type of anode and cathode of the present invention strong magnetic assist in electrodeposition device.
Reference numeral in above-mentioned accompanying drawing is as follows:
Reactor 1, main body 11, thermal insulation layer 11-1, heater coil 11-2, top cover 12;
Vibration component 2, vibrating controller 21, vibrating arm 22, anode hang tool 23, cathode hanging fixture 24, magnet hanger 25;
Magnetic control assembly 3, field controller 31, the first superconducting magnet 32, second superconducting magnet 33;
Mechanical stirrer 4;
Anode substrate 5;
Cathode base 6;
Direct supply 7.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
(embodiment 1)
See Fig. 1, the synchronous frequency ventilating type of the anode and cathode strong magnetic assist in electrodeposition device of the present embodiment, forms primarily of reactor 1, vibration component 2, magnetic control assembly 3, mechanical stirrer 4, anode substrate 5, cathode base 6 and direct supply 7.
Reactor 1 forms primarily of main body 11 and top cover 12.Thermal insulation layer 11-1 and the heater coil 11-2 for heating is provided with in main body 11.The middle of top cover 12 is provided with the through through hole of upward and downward.
Vibration component 2 forms primarily of vibrating controller 21, vibrating arm 22, anode hang tool 23, cathode hanging fixture 24 and magnet hanger 25.Upper end and the vibrating controller 21 of vibrating arm 22 are in transmission connection; The lower end of vibrating arm 22 is stretched out in the main body 11 of reactor 1 through the through hole of the top cover 12 of reactor 1; Gap preferably 0.8 ~ 1.5cm between the top cover 12 of reactor 1 and vibrating arm 22.Vibrating arm 22 action under the control of the driving of vibrating controller 21.Anode hang tool 23, cathode hanging fixture 24 and magnet hanger 25 are all arranged in the main body 11 of reactor 1; Anode hang tool 23, cathode hanging fixture 24 are fixedly connected with vibrating arm 22 respectively with magnet hanger 25, thus anode hang tool 23, cathode hanging fixture 24 and magnet hanger 25 can be done with frequently moving in the same way with vibrating arm 22.
Magnetic control assembly 3 forms primarily of field controller 31, first superconducting magnet 32 and the second superconducting magnet 33.First superconducting magnet 32 and the second superconducting magnet 33 are all arranged in the main body 11 of reactor 1; And the first superconducting magnet 32 and the second superconducting magnet about 33 points are oppositely arranged, the first superconducting magnet 32 is N pole, and the second superconducting magnet 33 is S pole.First superconducting magnet 32 is fixedly connected with the magnet hanger 25 of vibration component 2 respectively with the second superconducting magnet 33.In the present embodiment, first superconducting magnet 32 and the second superconducting magnet 33 all preferentially adopt electro-magnet, and the first superconducting magnet 32 and the second superconducting magnet 33 are circular arc camber towards the one side of electrode, arc radius is 50cm, angle is 6 degree to 12 degree, the preferential 10cm of spacing between the first superconducting magnet 32 and the second superconducting magnet 33.Field controller 31, for controlling the first superconducting magnet 32 and the second superconducting magnet 33, makes magneticstrength continuously adjustabe in 0T to 16T scope.
Mechanical stirrer 4 is arranged in the main body 11 of reactor 1; Be used for during use carrying out auxiliary stirring to deposit fluid.
Anode substrate 5 and cathode base about 6 points are oppositely arranged in the main body 11 of reactor 1; Spacing between anode substrate 5 and cathode base 6 is 2cm to 4cm scope, preferred 2cm; Anode substrate 5 is arranged on the right side of the first superconducting magnet 32; Cathode base 6 is arranged on the left side of the second superconducting magnet 33; Anode substrate 5 is fixedly connected with the anode hang tool 23 of vibration component 2; Cathode base 6 is fixedly connected with the cathode hanging fixture 24 of vibration component 2, thus anode substrate 5 and cathode base 6 can be done with frequently moving in the same way with vibrating arm 22 respectively by anode hang tool 23 and cathode hanging fixture 24.
Cathode base 6 is processed component.
Anode substrate 5 and cathode base 6 are respectively with the positive pole of direct supply 7 with negative pole is corresponding is electrically connected.
The present embodiment based on the synchronous frequency ventilating type of anode and cathode strong magnetic assist in electrodeposition device, the method for its galvanic deposit process components and parts in use, be described for Ni-based electroplate liquid and stainless steel cathode, its working method mainly comprises the following steps:
1. cathode base 6 carries out electroless plating process in advance, is easy at the plated surface last layer of cathode base 6 metal carrying out galvanic deposit; This metal can select fine copper or pure nickel, in the present embodiment, preferably adopts 10 μm of thick uniform copper layers on the plated surface of cathode base 6; Then cathode base 6 is fixed on cathode hanging fixture 24; Anode substrate 5 is fixed on anode hang tool 23 simultaneously, and regulates two interpole gaps to be 2cm.
2. in reactor 1, add nickel salt solution, boric acid and additive, stir 60 minutes under ultrasound environments, make it fully mix; Boric acid, as galvanic deposit sustained release dosage, optionally adds, and the concentration of boric acid is 30g/L ~ 60g/L.
Nickel salt solution is the solution of sulfur acid nickel and nickelous chloride; Wherein single nickel salt consumption is 300 ~ 500g/L, and nickelous chloride consumption is 30 ~ 60g/L; Described additive is dodecyl compounds and ether compound composition, and wherein dodecyl compounds consumption is 0.1 ~ 2g/L, and ether compound consumption is 0.1 ~ 1g/L.
In the present embodiment, additive preferably adopts sodium lauryl sulphate and polyoxyethylene glycol trimethylammonium nonyl ethers; The concentration of each material is preferably: single nickel salt 300g/L, nickelous chloride 40g/L, boric acid 50g/L, sodium lauryl sulphate 0.2g/L, polyoxyethylene glycol trimethylammonium nonyl ethers 0.8g/L.
3. heated under the effect of electromagnetic induction by heater coil 11-2, utilize thermal insulation layer 11-1 control temperature at 30 ~ 55 DEG C, in the present embodiment preferably 40 DEG C; Undertaken stirring by mechanical stirrer 4 and form uniform and stable galvanic deposit system, stir speed (S.S.) is 200 ~ 500rpm, and in the present embodiment, preferred mechanical stir speed (S.S.) is 400rmp.
4. need according to processing the vibrational frequency and the direction that set vibrating arm 22 by vibrating controller 21; Set magnetic field size by field controller 31, magnetic field size setting range is 0T to 16T; The outward current density arranging direct supply 7 is 1 ~ 13A/dm
-2; In the present embodiment, the outward current density of direct supply 7 is preferably 7A/dm
2, magnetic field size is for being preferably 8T, and the vibrational frequency of vibrating arm 22 is preferably 15KHz, amplitude is preferably 0.3cm.
5. switch on power, vibrating arm 22 does simple harmonic motion under the parameter set, and cathode base 6 does with frequently moving in the same way with anode substrate 5 with vibrating arm 22; Cathode base 6 and anode substrate 5 discharge simultaneously, make to form metastable electric field between the two poles of the earth; Metastable magnetic field is formed between the first superconducting magnet 32 and the second superconducting magnet 33; Nickel ion in solution deposits to the surface of cathode base 6 under electric field action; Electrodeposition time is 2 ~ 5 hours.In the present embodiment, electrodeposition time is preferably 2.5 hours.
6. after galvanic deposit, cathode base 6 is taken out from reactor 1, air-dry clean by pickling again by washing, the dense structure namely obtaining combining closely with cathode base, crystal grain is tiny, surfacing, excellent performance coating.
Above embodiment is the explanation to the specific embodiment of the present invention; but not limitation of the present invention; person skilled in the relevant technique without departing from the spirit and scope of the present invention; can also make various conversion and change and obtain corresponding equivalent technical scheme, therefore all equivalent technical schemes all should be included into scope of patent protection of the present invention.
Claims (8)
1. the synchronous frequency ventilating type of an anode and cathode strong magnetic assist in electrodeposition device, is characterized in that: comprise reactor (1), vibration component (2), magnetic control assembly (3), mechanical stirrer (4), anode substrate (5), cathode base (6) and direct supply (7);
Described reactor (1) comprises main body (11) and top cover (12); Thermal insulation layer (11-1) is provided with and for heater coil (11-2) in main body (11); The middle of top cover (12) is provided with the through through hole of upward and downward;
Vibration component (2) involving vibrations controller (21), vibrating arm (22), anode hang tool (23), cathode hanging fixture (24) and magnet hanger (25); Upper end and the vibrating controller (21) of vibrating arm (22) are in transmission connection; The lower end of vibrating arm (22) is stretched out in the main body (11) of reactor (1) through the through hole of the top cover (12) of reactor (1); Anode hang tool (23), cathode hanging fixture (24) and magnet hanger (25) are all arranged in the main body (11) of reactor (1); Anode hang tool (23), cathode hanging fixture (24) are fixedly connected with vibrating arm (22) respectively with magnet hanger (25);
Magnetic control assembly (3) comprises field controller (31), the first superconducting magnet (32) and the second superconducting magnet (33); First superconducting magnet (32) and the second superconducting magnet (33) are all arranged in the main body (11) of reactor (1); And the first superconducting magnet (32) and the second superconducting magnet (33) point left and right are oppositely arranged; First superconducting magnet (32) is N pole, and the second superconducting magnet (33) is S pole; First superconducting magnet (32) and the second superconducting magnet (33) are fixedly connected with the magnet hanger (25) of vibration component (2) respectively; Field controller (31) is for controlling the first superconducting magnet (32) and the second superconducting magnet (33) makes magneticstrength continuously adjustabe in 0T to 16T scope;
Mechanical stirrer (4) is arranged in the main body (11) of reactor (1);
Anode substrate (5) and cathode base (6) point left and right are oppositely arranged in the main body (11) of reactor (1); Spacing range between anode substrate (5) and cathode base (6) is 2cm to 4cm; Anode substrate (5) is arranged on the right side of the first superconducting magnet (32); Cathode base (6) is arranged on the left side of the second superconducting magnet (33); Anode substrate (5) is fixedly connected with the anode hang tool (23) of vibration component (2); Cathode base (6) is fixedly connected with the cathode hanging fixture (24) of vibration component (2); Thus make anode substrate (5) and cathode base (6) do with frequently moving in the same way respectively by anode hang tool (23) and cathode hanging fixture (24) with vibrating arm (22); Anode substrate (5) and cathode base (6) are respectively with the positive pole of direct supply (7) with negative pole is corresponding is electrically connected.
2. the synchronous frequency ventilating type of anode and cathode according to claim 1 strong magnetic assist in electrodeposition device, is characterized in that: the gap between the top cover (12) of described reactor (1) and vibrating arm (22) is 0.8 ~ 1.5cm; Spacing between anode substrate (5) and cathode base (6) is 2cm; Spacing between first superconducting magnet (32) of magnetic control assembly (3) and the second superconducting magnet (33) is 10cm.
3. the synchronous frequency ventilating type of anode and cathode according to claim 1 strong magnetic assist in electrodeposition device, it is characterized in that: the first superconducting magnet (32) and second superconducting magnet (33) of described magnetic control assembly (3) are electro-magnet, and the first superconducting magnet (32) and the second superconducting magnet (33) are circular arc camber towards the one side of electrode, arc radius is 50cm, and angle is 6 degree to 12 degree.
4. a working method for the synchronous frequency ventilating type of anode and cathode according to claim 1 strong magnetic assist in electrodeposition device, is characterized in that: comprise the following steps:
1. cathode base (6) electroless plating process in advance: the metal needing the plated surface last layer of the cathode base of galvanic deposit (6) to be easy to carry out galvanic deposit;
Anode substrate (5) and cathode base (6) are 2. installed: by anode substrate (5) and cathode base (6) respectively the correspondence anode hang tool (23) that is arranged on vibration component (2) and cathode hanging fixture (24); Time regulate the two poles of the earth relative position and distance;
3. electroplate liquid system is prepared: in the main body (11) of reactor (1), add the electroplate liquid containing surface additive or composite plating solution that configure; Shake parameter and the magnitude of field intensity frequently of setting system temperature, mechanical stirring parameter, current density, vibration, make it to meet electrodeposition condition;
4. galvanic deposit processing: switch on power, carries out electrodeposition process at the outside surface of cathode base (6) under mechanical stirring, magnetic force driving and vibrating controller (21) drive anode substrate (5) and the subsidiary conditions of cathode base (6) with synchronous vibration frequently by vibrating arm (22);
5. galvanic deposit completion of processing aftertreatment: after galvanic deposit completion of processing, by aftertreatment, can obtain the electrocoat of desired properties and dense structure at the outside surface of cathode base (6).
5. the working method of the synchronous frequency ventilating type of anode and cathode according to claim 4 strong magnetic assist in electrodeposition device, is characterized in that: described step 1. in, the surface chemistry of cathode base (6) plates about 10 μm of thick uniform copper layers; Described step 3. in, the electroplate liquid containing surface additive is nickel salt solution or copper salt solution; Surface additive is the additive be made up of dodecyl compounds and ether compound; Described nickel salt or the concentration of copper salt solution are 300 ~ 500g/L; The concentration of surface additive is 0.1 ~ 2g/L; Concentration be the boric acid of 30g/L ~ 60g/L as galvanic deposit sustained release dosage.
6. the working method of the synchronous frequency ventilating type of anode and cathode according to claim 4 strong magnetic assist in electrodeposition device, is characterized in that: described step 3. middle mechanical stirring is bottom level Keep agitation, and stir speed (S.S.) is 200 ~ 500rpm; System temperature controls at 20 ~ 50 DEG C; Cathode current density controls at 1A ~ 16A/dm
2.
7. the working method of the synchronous frequency ventilating type of anode and cathode according to claim 4 strong magnetic assist in electrodeposition device, it is characterized in that: described step 4. in vibrating controller (21) by vibrating arm (22) drive anode substrate (5) and cathode base (6) do front and back to or left and right to vibration, amplitude is no more than 0.5cm, and vibrational frequency is 0 ~ 50KHz.
8. the working method of the synchronous frequency ventilating type of anode and cathode according to claim 4 strong magnetic assist in electrodeposition device, it is characterized in that: described step 3. in, the size of magneticstrength is controlled by field controller (31), makes magneticstrength continuously adjustabe within the scope of 0T to 16 T.
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| CN107858735A (en) * | 2017-12-26 | 2018-03-30 | 西北工业大学 | A kind of electrolytic cell for composite electrodeposition |
| CN111005055A (en) * | 2020-01-04 | 2020-04-14 | 焦作大学 | Multi-source synchronous frequency oscillation type electrodeposition processing device and processing method |
| CN111232439A (en) * | 2020-01-15 | 2020-06-05 | 付*** | Solid-liquid quick-mixing type cosmetic storage bottle |
| CN114086233A (en) * | 2022-01-10 | 2022-02-25 | 雷尼尔家具(南通)有限公司 | Cabinet door accessory electroplating equipment |
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| CN114086233A (en) * | 2022-01-10 | 2022-02-25 | 雷尼尔家具(南通)有限公司 | Cabinet door accessory electroplating equipment |
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