Pulse chemical electrodeposition device for blocky nanostructure precious metal

Abstract

The utility model relates to the field of chemical electrodeposition, in particular to a pulse chemical electrodeposition device for blocky nanostructure precious metal, which comprises a pulse signal generator, a constant potential rectifier, an electrolytic bath with an upper opening and a heating component, the electrolytic bath is arranged in the heating component, and the pulse signal generator is connected with the constant potential rectifier. The constant potential rectifier is in conductive connection with the counter electrode, the working electrode and the reference electrode, the motor is arranged, an output shaft of the motor is vertically arranged, and the output shaft of the motor can drive the rotating disc part to rotate, so that the rotating disc part, the electro-deposition substrate part and the insulating connecting sleeve part rotate together in the horizontal direction, and electrolyte in the electrolytic bath is stirred. Due to the fact that the electro-deposition substrate part rotates in the electrolyte at a constant speed to conduct pulse chemical electro-deposition, the defects of bubbles, pinholes and the like of materials can be effectively reduced, the phenomena of internal stress, uneven components and the like are greatly eliminated, and the electro-deposition quality of the blocky nano-structure precious metal is remarkably improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to chemical electro deposition field especially relates to a kind of for blocky nanostructure noble metal's pulse chemical electro deposition device. BACKGROUND

[0002] Pulse chemical electro deposition is a kind of commonly used nanomaterial preparation method, this technique has the characteristics such as fast, low cost, good reliability and has extremely extensive application in material engineering.Pulse chemical electro deposition can be adjusted pulse voltage, pulse frequency, electro deposition temperature etc. Parameter to control the microstructure of material, this method is simple and easy to implement and cost is lower, so this technique is in nanomaterial field by researchers's favor.

[0003] Blocky nanostructure noble metal has higher mechanical strength compared to traditional noble metal material, so blocky nanostructure noble metal can be applied to high-precision electronic components and key components manufacturing in extreme environment, but blocky nanostructure noble metal in pulse chemical electro deposition process, with the increase of nanostructure noble metal deposition thickness, bubble, pinhole and other defects will obviously increase, internal stress will also increase accordingly, nanostructure noble metal composition uniformity is poor, seriously affect blocky nanostructure noble metal electro deposition quality. SUMMARY

[0004] The utility model solves the technical problem to provide a kind of blocky nanostructure noble metal electro deposition quality better pulse chemical electro deposition device.

[0005] The utility model solves the technical problem and adopts the technical scheme that: for blocky nanostructure noble metal's pulse chemical electro deposition device, including pulse signal generator, constant potential instrument, upper open electrolytic cell and heating assembly, electrolytic cell is set in heating assembly, pulse signal generator is connected with constant potential instrument, constant potential instrument is respectively and with counter electrode, working electrode and reference electrode electrically connected, counter electrode, working electrode and reference electrode are suspended in electrolytic cell, still include connecting seat, motor, connecting seat is connected and set in the upper side of heating assembly, motor is vertically set on connecting seat;

[0006] Working electrode includes electrode stem part, rotating disc part, electro deposition base part and insulating connecting sleeve part, the lower end of electrode stem part is perpendicular and electrically connected with rotating disc part, the middle of insulating connecting sleeve part is provided with installation slot, the middle of the bottom of installation slot is provided with the shaped through-hole that passes through up and down, electro deposition base part, rotating disc part are matched and set in installation slot, and electro deposition base part is set on the bottom of installation slot, rotating disc part is set on electro deposition base part, and rotating disc part is electrically connected with electro deposition base part;

[0007] The outer surface of the side wall of the electrode rod part and the upper surface of the rotating disc part are respectively provided with an insulating layer, the output shaft of the motor is vertically arranged, and the upper end of the electrode rod part is vertically connected with the output shaft of the motor.

[0008] Further, the motor protection cover is arranged on the connecting seat, and the motor is arranged in the motor protection cover.

[0009] Further, the working electrode is arranged at the center of the electrolytic cell, the lower end of the electrode rod part is perpendicularly and conductively connected with the center of the rotating disc part, the center of the insulating connecting sleeve part is provided with a mounting groove, and the center of the bottom of the mounting groove is provided with a shaped through hole penetrating upward and downward.

[0010] Further, the outer surface of the side wall of the rotating disc part is provided with an insulating layer.

[0011] Further, the upper surface of the rotating disc part is flush with the top surface of the insulating connecting sleeve part.

[0012] Further, the rotating disc part, the electrodeposition base part and the insulating connecting sleeve part are provided with an anti-rotation structure.

[0013] Further, the anti-rotation structure comprises an anti-rotation protrusion arranged on the inner wall surface of the insulating connecting sleeve part and an anti-rotation groove arranged on the outer wall surface of the rotating disc part and the outer wall surface of the electrodeposition base part, and the anti-rotation protrusion is detachably matched and arranged in the anti-rotation groove.

[0014] Further, the heating assembly is a water bath heating assembly.

[0015] Further, the controller is further arranged, the motor is a servo motor, the pulse signal generator, the constant potential instrument and the heating assembly are electrically connected with the controller.

[0016] The utility model discloses an advantageous effect is: through being provided with motor, motor's output shaft is vertically arranged, and motor output shaft can drive rotating disc part rotation, makes rotating disc part, electrodeposition base part, insulating connecting sleeve part together in horizontal direction rotation, carries out the stirring to electrolyte in electrolytic cell. When the pulse chemical electrodeposition device is used to carry out the electrodeposition of block nanostructure noble metal, first, the electrolyte of corresponding noble metal material is added to the electrolytic cell, and the counter electrode, the working electrode and the reference electrode are suspended in the electrolyte. Then, the heating assembly is controlled to open to heat the electrolyte, and the electrolyte is heated to a specified temperature. Then, the motor is controlled to open, and the output shaft of the motor rotates to drive the rotating disc part, the electrodeposition base part and the insulating connecting sleeve part to rotate in the horizontal direction, and the rotation speed is in the specified range. Finally, the pulse signal generator sets the pulse signal parameters, and after completion, the potentiostat transmits the pulse voltage to the working electrode for pulse chemical electrodeposition. The nanostructure noble metal material is gradually adsorbed and deposited on the lower surface of the electrodeposition base part. Since the electrodeposition base part rotates uniformly in the electrolyte for pulse chemical electrodeposition, the defects such as bubbles and pinholes of the material can be effectively reduced, and the internal stress and composition unevenness are also greatly eliminated, so that the quality of the electrodeposition of block nanostructure noble metal is significantly improved. Moreover, the working electrode is composed of the electrode stem part, the rotating disc part, the electrodeposition base part and the insulating connecting sleeve part. The nanostructure noble metal material is adsorbed and deposited on the lower surface of the electrodeposition base part. Only by replacing different electrodeposition base parts, the chemical electrodeposition of different noble metal materials can be completed, which is convenient to use. BRIEF DESCRIPTION OF DRAWINGS

[0017] Figure 1 is the structure schematic diagram of the utility model;

[0018] Figure 2 is the structure schematic diagram of the working electrode;

[0019] Figure 3 is the structure schematic diagram of the insulating connecting sleeve part;

[0020] Components, parts and numbers in the figure: pulse signal generator 1, potentiostat 2, electrolytic cell 3, counter electrode 4, working electrode 5, electrode stem part 51, rotating disc part 52, electrodeposition base part 53, insulating connecting sleeve part 54, installation groove 541, shaped through hole 542, anti-rotation convex 543, connecting seat 6, motor protection cover 7, controller 8, heating assembly 9, reference electrode 10. DETAILED DESCRIPTION

[0021] The utility model is further illustrated below in connection with the drawings and specific embodiments.

[0022] As Figure 1 , Figure 2 and Figure 3The utility model is shown, pulse chemical electrodeposition device for blocky nanostructure noble metal, including pulse signal generator 1, constant potential instrument 2, the upper opening electrolytic cell 3 and heating assembly 9, electrolytic cell 3 sets up in heating assembly 9, pulse signal generator 1 is connected with constant potential instrument 2, and constant potential instrument 2 is respectively connected with counter electrode 4, working electrode 5 and reference electrode 10 electrically, and counter electrode 4, working electrode 5 and reference electrode 10 are suspended in electrolytic cell 3, still include connecting seat 6, motor, and connecting seat 6 is connected to set up in the upper side of heating assembly 9, and the motor is vertically arranged on connecting seat 6,

[0023] Working electrode 5 includes electrode stem part 51, rotating disc part 52, electrodeposition base part 53 and insulation connecting sleeve part 54, and the lower end of electrode stem part 51 is vertically connected with rotating disc part 52, and the middle of insulation connecting sleeve part 54 is provided with installation groove 541, and the middle of the bottom of installation groove 541 is provided with up-down through forming through-hole 542, and electrodeposition base part 53 and rotating disc part 52 are matched and arranged in installation groove 541, and electrodeposition base part 53 is arranged on the bottom of installation groove 541, and rotating disc part 52 is arranged on electrodeposition base part 53 (contact), and rotating disc part 52 is connected with electrodeposition base part 53 electrically.

[0024] The outer surface of the sidewall of electrode stem part 51 and the upper surface of rotating disc part 52 are respectively provided with insulation layer, and the output shaft of the motor is vertically arranged, and the upper end of electrode stem part 51 is vertically connected with the output shaft of the motor.

[0025] Insulation connecting sleeve part 54 connects rotating disc part 52 and electrodeposition base part 53 as a whole, and when the output shaft of the motor rotates to drive rotating disc part 52 to rotate, rotating disc part 52, electrodeposition base part 53 and insulation connecting sleeve part 54 rotate together in the horizontal direction to stir the electrolyte in electrolytic cell 3. By arranging insulation layer on the outer surface of the sidewall of electrode stem part 51 and the upper surface of rotating disc part 52 respectively, and by making insulation connecting sleeve part 54 from insulation material, the insulation connecting sleeve part 54 has insulation itself, so that when the pulse chemical electrodeposition device is used to electrodeposition blocky nanostructure noble metal, the nanostructure noble metal material is only gradually adsorbed and deposited on the lower surface of electrodeposition base part 53, and the nanostructure noble metal material forms a block shape which is the same as the shape of forming through-hole 542, and the shape of forming through-hole 542 can be rectangular or circular according to actual conditions.

[0026] When the pulse chemical electrodeposition device is used to carry out electrodeposition of block nano-structured noble metal, first, electrolyte corresponding to the noble metal material is added into the electrolytic tank 3, and the counter electrode 4, the working electrode 5 and the reference electrode 10 are suspended in the electrolyte; then the heating assembly 9 is controlled to be turned on to heat the electrolyte, so that the electrolyte is heated to a specified temperature; then the motor is controlled to be turned on, and the output shaft of the motor rotates to drive the rotating disc part 52, the electrodeposition base part 53 and the insulating connecting sleeve part 54 to rotate in the horizontal direction, and the rotating speed is controlled to be in a specified range; finally, the pulse signal generator 1 sets pulse signal parameters, and after completion, the potentiostat 2 is turned on to transmit pulse voltage to the working electrode 5 to carry out pulse chemical electrodeposition, and the nano-structured noble metal material is gradually adsorbed and deposited on the lower surface of the electrodeposition base part 53. Since the electrodeposition base part 53 rotates uniformly in the electrolyte to carry out pulse chemical electrodeposition, the defects such as bubbles and pinholes of the material can be effectively reduced, and the internal stress and composition unevenness are also greatly eliminated, so that the quality of the block nano-structured noble metal electrodeposition is significantly improved.

[0027] In order to further improve the quality of the block nano-structured noble metal electrodeposition, specifically: As shown in Figure 1 , the working electrode 5 is arranged at the middle of the electrolytic tank 3, the lower end of the electrode rod part 51 is perpendicularly and conductively connected with the middle of the rotating disc part 52, the middle of the insulating connecting sleeve part 54 is provided with a mounting groove 541, and the middle of the bottom of the mounting groove 541 is provided with a shaped through hole 542.

[0028] In order to protect the motor and improve the service life thereof, as shown in Figure 1 , the utility model also is provided with motor protection cover 7, motor protection cover 7 sets up on connecting seat 6, and motor sets up in motor protection cover 7.

[0029] The electrodeposition base part 53 and the rotating disc part 52 are matched and arranged in the mounting groove 541, in order to ensure the insulation and make the electrodeposition material only on the lower surface of the electrodeposition base part 53, the upper surface of the rotating disc part 52 is flush with the top surface of the insulating connecting sleeve part 54, and further, the side wall outer surface of the rotating disc part 52 is provided with an insulating layer.

[0030] In order to reduce the possibility of relative rotation of the rotating disc part 52, the electrodeposition base part 53 and the insulating connecting sleeve part 54, so as to affect the quality of the block nano-structured noble metal electrodeposition, as shown in Figure 1 , Figure 2 and Figure 3As shown, the rotating disc part 52, the electrodeposition base part 53 and the insulating connecting sleeve part 54 are provided with an anti-rotation structure. The anti-rotation structure limits the relative rotation between the rotating disc part 52, the electrodeposition base part 53 and the insulating connecting sleeve part 54. In order to improve the use effect of the anti-rotation structure, preferably, the anti-rotation structure comprises anti-rotation protrusions 543 arranged on the inner wall surface of the insulating connecting sleeve part 54 and anti-rotation grooves arranged on the outer wall surface of the rotating disc part 52 and the outer wall surface of the electrodeposition base part 53, and the anti-rotation protrusions 543 are detachably matched in the anti-rotation grooves. The number of the anti-rotation protrusions 543 and the anti-rotation grooves is preferably 4-6, the anti-rotation protrusions 543 are evenly distributed on the inner wall surface of the insulating connecting sleeve part 54, and the anti-rotation grooves are evenly distributed on the outer wall surface of the rotating disc part 52 and the outer wall surface of the electrodeposition base part 53. The anti-rotation structure not only can prevent the relative rotation between the rotating disc part 52, the electrodeposition base part 53 and the insulating connecting sleeve part 54, but also can improve the connection firmness between the rotating disc part 52, the electrodeposition base part 53 and the insulating connecting sleeve part 54.

[0031] In order to ensure and improve the heating effect of the heating assembly 9, the heating assembly 9 is preferably a water bath heating assembly.

[0032] In order to improve the automation level of the whole pulse chemical electrodeposition device and further improve the quality of the block-shaped nano-structured noble metal electrodeposition, again Figure 1 As shown, the utility model also is provided with controller 8, motor is servo motor, pulse signal generator 1, constant potential instrument 2, heating assembly 9, motor all with controller 8 electric connection. Controller 8 automatically control pulse signal generator 1, constant potential instrument 2, heating assembly 9, the opening and closure of motor, also can real-time adjustment motor output shaft's rotational speed and electrolyte's temperature.

Claims

1. A pulse chemical electrodeposition device for bulk nanostructured noble metal, comprising a pulse signal generator (1), a constant potential instrument (2), an upper open electrolytic cell (3) and a heating assembly (9), the electrolytic cell (3) is arranged in the heating assembly (9), the pulse signal generator (1) is connected with the constant potential instrument (2), the constant potential instrument (2) is respectively conductively connected with a counter electrode (4), a working electrode (5) and a reference electrode (10), the counter electrode (4), the working electrode (5) and the reference electrode (10) are suspendedly arranged in the electrolytic cell (3), characterized in that: The connecting seat (6) is connected to the upper side of the heating assembly (9), and the motor is vertically arranged on the connecting seat (6). ​ The working electrode (5) comprises an electrode stem part (51), a rotating disc part (52), an electrodeposition base part (53) and an insulating connecting sleeve part (54). The lower end of the electrode stem part (51) is perpendicularly and electrically connected to the rotating disc part (52). The middle of the insulating connecting sleeve part (54) is provided with a mounting groove (541). The middle of the bottom of the mounting groove (541) is provided with a shaped through hole (542) penetrating up and down. The electrodeposition base part (53) and the rotating disc part (52) are matched and arranged in the mounting groove (541). The electrodeposition base part (53) is arranged on the bottom of the mounting groove (541). The rotating disc part (52) is arranged on the electrodeposition base part (53). The rotating disc part (52) is electrically connected to the electrodeposition base part (53). The outer surface of the side wall of the electrode stem part (51) and the upper surface of the rotating disc part (52) are respectively provided with an insulating layer. The output shaft of the motor is vertically arranged. The upper end of the electrode stem part (51) is vertically connected to the output shaft of the motor.

2. The apparatus for pulse electrochemical deposition of bulk nanostructured noble metal according to claim 1, wherein: The motor protection cover (7) is arranged on the connecting seat (6), and the motor is arranged in the motor protection cover (7).

3. The apparatus for pulse electrochemical deposition of bulk nanostructured noble metal according to claim 1, wherein: The working electrode (5) is arranged at the middle of the electrolytic cell (3). The lower end of the electrode stem part (51) is perpendicularly and electrically connected to the middle of the rotating disc part (52). The middle of the insulating connecting sleeve part (54) is provided with a mounting groove (541). The middle of the bottom of the mounting groove (541) is provided with a shaped through hole (542) penetrating up and down.

4. The apparatus for pulse electrochemical deposition of bulk nanostructured noble metal according to claim 1, wherein: The outer surface of the side wall of the rotating disc part (52) is provided with an insulating layer.

5. The apparatus for pulse electrochemical deposition of bulk nanostructured noble metal according to claim 1, wherein: The upper surface of the rotating disc part (52) is flush with the top surface of the insulating connecting sleeve part (54).

6. The apparatus for pulse electrochemical deposition of bulk nanostructured noble metal of claim 1, wherein: Anti-rotation structures are arranged between the rotating disc part (52), the electrodeposition base part (53) and the insulating connecting sleeve part (54).

7. The apparatus for pulse electrochemical deposition of bulk nanostructured noble metal according to claim 6, wherein: The anti-rotation structures comprise anti-rotation protrusions (543) arranged on the inner wall surface of the insulating connecting sleeve part (54) and anti-rotation grooves arranged on the outer wall surface of the rotating disc part (52) and the outer wall surface of the electrodeposition base part (53). The anti-rotation protrusions (543) are detachably and matchingly arranged in the anti-rotation grooves.

8. The apparatus for pulse electrochemical deposition of bulk nanostructured noble metal according to claim 1, wherein: The heating assembly (9) is a water bath heating assembly.

9. The apparatus for pulse electrochemical deposition of bulk nanostructured noble metal according to any one of claims 1 to 8, characterized in that: The controller (8) is arranged. The motor is a servo motor. The pulse signal generator (1), the potentiostat (2), the heating assembly (9) and the motor are electrically connected to the controller (8).

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