CN104894626A - Rotatable electroplating experimental device for loading spherical micrometer particles - Google Patents
Rotatable electroplating experimental device for loading spherical micrometer particles Download PDFInfo
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- CN104894626A CN104894626A CN201510347255.XA CN201510347255A CN104894626A CN 104894626 A CN104894626 A CN 104894626A CN 201510347255 A CN201510347255 A CN 201510347255A CN 104894626 A CN104894626 A CN 104894626A
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Abstract
The invention relates to an electroplating experimental device, and aims to provide a rotatable electroplating experimental device for loading spherical micrometer particles. The rotatable electroplating experimental device comprises a conical flask, a support, a direct-current motor and a driven gear. The conical flask is used as an electroplating container. The support is provided with a support plate, and a 50-degree included angle is formed between the support plate and the horizontal direction. A driving gear is fixedly arranged at the tail end of the rotary shaft of the direct-current motor. The driven gear and the driving gear are positioned on the same side of the rotatable electroplating experimental device and are meshed with each other. A clamp is arranged on the driven gear to fixedly clamp the conical flask, and included angles formed between the bottom of the flask and the generation line of a conical surface are symmetrical to each other relative to the vertical direction. A negative electrode and a positive electrode penetrate the bearing of the driven gear and are inserted into the conical flask. The rotatable electroplating experimental device has the advantages that the rotatable electroplating experimental device can be used for loading the spherical micrometer particles, functional properties of the spherical micrometer particles can be improved, and the application range of the spherical micrometer particles can be expanded; small electrode particles can be uniformly loaded on the spherical micrometer particles in composite materials, the sizes of the electrode particles can be controlled, the electrode particles are high in dispersion degree, and materials can be saved; the rotatable electroplating experimental device can be applied to the field of electric contact material manufacturing.
Description
Technical field
The present invention relates to a kind of electroplating experiments device, particularly a kind of for powdered object uniformly-coating in a liquid, and can the device of evenly temperature adjustment simultaneously.
Background technology
Ag-SnO
2contact material is as a kind of novel Ag metal oxide materials, part commercialization in the world, it has good electric property, higher resistance fusion welding energy and arc resistance energy, be specially adapted to powerful contactor and low-tension switch, become the ideal candidate replacing Ag-CdO contact material.SnO
2there is the thermostability (fusing point be 1625 DEG C) more much higher than CdO, molten mass viscosity in molten bath, electric arc root place is increased, reduce splash loss during arc burning.Use Ag-SnO
2contact material replaces Ag-CdO contact material, material volume can be made to reduce about 25%, and still can keep the same life-span.But, Ag-SnO
2contact material also exposes obvious deficiency in utilization process, urgently researchs and solves further:
1) under electric arc repeatedly acts on, SnO
2composition is enriched in contact surface and causes contact resistance to increase, and temperature rise is very high, has had a strong impact on electric use properties;
2) SnO
2high rigidity make Ag-SnO
2plasticity and the ductility of material are poor, cause Ag-SnO
2the extruding of material, rolling, the extruding of silk material, drawing, the pier system of rivet becomes abnormal difficult;
3) Ag base and SnO
2bonding force not enough, cause the two easily to depart from, this problem seems particularly outstanding after sintering process, seriously reduces the performance of contact material, makes it be subject to arc erosion, and electric life reduces.
Ag-SnO
2a difficult problem maximum in Material Manufacturing Process is that material hardness is high, and not yielding, annealing effect is not obvious, easy fracture of wire.For addressing these problems, have studied many production technique both at home and abroad, wherein powder metallurgic method is one of comparatively successful method.The feature of powder metallurgic method is the composition that can adjust alloy in a big way, can prepare homogeneous microstructure, contact that volume is larger, but due to the restriction of alloy density, electrical contact endurance is poor.
For above-mentioned deficiency, contriver is by a large amount of contrast experiments and summary, and optimization experiment parameter reduce experimental procedure repeatedly, improves the technique in early stage of prior powder metallurgy method, successfully prepared based on micron SnO
2the spherical hum silicon dioxide tin supported micron of solid sphere powder, nano-Ag particles novel material.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes deficiency of the prior art, provides the preparation method of a kind of spherical hum silicon dioxide tin supported micron, nano-Ag particles material.The present invention adopts electroplating technology at micron SnO
2supported micron, nano-Ag particles on solid sphere powder, improve the functional property of spherical hum silicon dioxide tin and expand its range of application.
For technical solution problem, solution of the present invention is:
A kind of rotatable electroplating experiments device for carrying out load to spherical micron particle is provided, comprises the Erlenmeyer flask as electroplating container, and:
Support, having with one and horizontal direction is the support plate of 50 ° of angles;
Direct-current machine, its turning axle is through support plate, and turning axle end is fixedly equipped with driving toothed gear; Direct-current machine is fixed in support plate, and lays respectively at the both sides of support plate with driving toothed gear;
Follower gear, is positioned at homonymy with driving toothed gear and engages each other, and its central position is set on shaft insulation by angular contact ball bearing, and shaft insulation is arranged in support plate;
Described follower gear is provided with fixture, Erlenmeyer flask can be gripped and the angle formed with cone element at the bottom of making bottle is symmetrical in vertical; Negative electrode and the anode of silver material pass the bearing of follower gear and are inserted in Erlenmeyer flask.
In the present invention, the end of described negative electrode and anode has the silver-colored material top electrode that can dismantle.
In the present invention, the shaft insulation of described follower gear central position is made up of insulating material, is provided with the hole of two axis for passing negative electrode and anode.
In the present invention, described fixture comprises permanent seat and screw base, screw base is equipped with the trip bolt of a band plastics jacking block.
In the present invention, described follower gear is 10: 1 with the ratio of the radius of driving toothed gear.
In the present invention, this device also comprises water-bath, and Erlenmeyer flask part is immersed in water-bath.
Rotatable electroplating experiments device of the present invention is for the preparation of the example of spherical hum silicon dioxide tin supported micron, nano-Ag particles material:
(1) by mass concentration be the SnCl that the NaOH solution of 111.1g/L is added to 0.3mol/L
45H
2in O solution, and mixed solution ph is adjusted to 13, stirs 0.5h subsequently;
(2) consoluet mixing solutions after stirring is transferred in tetrafluoroethylene reactor, hydro-thermal reaction 20h at 180 DEG C;
(3) by the centrifugation of hydro-thermal reaction product, and with deionized water and washing with alcohol, centrifugal rotational speed 2000r/min; Dry at 90 DEG C, namely obtain spherical hum silicon dioxide tin;
(4) spherical hum silicon dioxide tin is added to the AgNO of 0.001 ~ 1mol/L
3in the aqueous solution, be inserted in mixture with the negative electrode of silver-colored material and anode and electroplate; During plating, inclination electroplating container also makes its centrally axle rotation, allows mixture keep agitated conditions; The rotating speed controlling electroplating container is 6 ~ 300r/min, and in electroplating container, the temperature of mixture is 15 ~ 100 DEG C, and electroplating voltage is 1 ~ 30V, and electroplating time is 60 ~ 3600s;
(5) abandon filtrate to the mixture suction filtration after plating, suction filtration product dries 2h at 90 DEG C, namely obtains spherical hum silicon dioxide tin supported micron, nano-Ag particles material.
In the present invention, put into spherical micron particle (spherical hum silicon dioxide tin) and corresponding solution when Erlenmeyer flask and be held on after on device, the angle almost symmetry that the bottle end and cone element are formed is in vertical, and electrode and direct-current machine all switch on power and get final product work.In Erlenmeyer flask Sloped rotating process, in bottle, powder both slided with bottle bottom surface and the conical surface, stirs again, namely reach plating object along sense of rotation.Compared with using the mode of agitator, the application of this device can make spherical hum silicon dioxide glass putty body by gravity and electrode continuous contact, and can not accumulate and make powder gap be difficult to be plated.
Compared with prior art, the invention has the beneficial effects as follows:
Electroplating technology of the present invention can be used in the load of spherical micron particle (as the micron SnO prepared in hydrothermal method
2supported micron, nano-Ag particles on solid sphere powder), improve the functional property of spherical micron particle and expand its range of application; In the matrix material obtained, less electrode particle (as micron, nano-Ag particles) can be carried on spherical micron particle (as spherical hum silicon dioxide tin) equably, the size tunable (diameter is 50nm ~ 1 μm) of electrode particle (as Argent grain), dispersity is high, and can save material; This device can be applicable to the preparation field of contact material.
Accompanying drawing explanation
Fig. 1 be embodiment 1 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Fig. 2 be embodiment 2 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Fig. 3 be embodiment 3 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Fig. 4 be embodiment 4 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Fig. 5 be embodiment 5 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Fig. 6 be embodiment 6 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Fig. 7 be embodiment 7 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Fig. 8 be embodiment 8 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Fig. 9 be embodiment 9 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 10 be embodiment 10 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 11 be embodiment 11 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 12 be embodiment 12 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 13 be embodiment 13 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 14 be embodiment 14 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 15 be embodiment 15 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 16 be embodiment 16 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 17 be embodiment 17 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 18 be embodiment 18 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 19 be embodiment 19 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 20 be embodiment 20 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 21 be embodiment 21 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 22 be embodiment 22 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 23 be embodiment 23 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 24 be embodiment 24 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 25 be embodiment 25 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 26 be embodiment 26 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 27 be embodiment 27 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 28 be embodiment 28 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 29 be embodiment 29 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 30 be embodiment 30 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 31 be embodiment 31 obtain spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material field emission scanning electron microscope photo;
Figure 32 is non-implementation step 4) and 5) the field emission scanning electron microscope photo of spherical hum silicon dioxide glass putty body that obtains;
Figure 33 be the present invention prepare spherical hum silicon dioxide tin supported micron, nano-Ag particles novel material X ray diffracting spectrum;
Figure 34 is the signal of rotatable electroplating experiments device one-piece construction;
Figure 35 is follower gear and the signal of axle section;
Figure 36 is the signal of Erlenmeyer flask clamping section;
Figure 37 is electrode and the signal of changeable electrodes head;
In Figure 34-37, Reference numeral is: 1 support plate; 2 follower gears; 3 permanent seats; 4 electrodes; 5 Erlenmeyer flasks; 6 top electrodes; 7 water-baths; 8 jacking blocks; 9 screw bases; 10 trip bolts; 11 driving toothed gears; 12 supports; 13 direct-current machine; 14 electric wires; 15 angular contact ball bearings; 16 shaft insulations.
Embodiment
Provide the preparation method of spherical hum silicon dioxide tin supported micron exemplarily, nano-Ag particles material in the present invention, its step is as follows:
(1) by mass concentration be the SnCl that the NaOH solution of 111.1g/L is added to 0.3mol/L
45H
2in O solution, and mixed solution ph is adjusted to 13, stirs 0.5h subsequently;
(2) consoluet mixing solutions after stirring is transferred in tetrafluoroethylene reactor, hydro-thermal reaction 20h at 180 DEG C;
(3) by the centrifugation of hydro-thermal reaction product, and with deionized water and washing with alcohol, centrifugal rotational speed 2000r/min; Dry at 90 DEG C, namely obtain spherical hum silicon dioxide tin;
(4) spherical hum silicon dioxide tin is added to the AgNO of 0.001 ~ 1mol/L
3in the aqueous solution, be inserted in mixture with the negative electrode of silver-colored material and anode and electroplate; In this process, rotary container makes mixture keep agitated conditions, and the rotating speed of container is 6 ~ 300r/min; In electroplating process, control temperature is 15 ~ 100 DEG C, and voltage is 1 ~ 30V, and the time is 60 ~ 3600s;
(5) abandon filtrate to the mixture suction filtration after plating, suction filtration product dries 2h at 90 DEG C, namely obtains spherical hum silicon dioxide tin supported micron, nano-Ag particles material.
In aforesaid step (4), use rotatable electroplating experiments device of the present invention.
This device comprises the Erlenmeyer flask 5 as electroplating container.It is the support plate 1 of 50 ° of angles that support 12 has with one and horizontal direction.The turning axle of direct-current machine 13 is through support plate 1, and turning axle end is fixedly equipped with driving toothed gear 11; Direct-current machine 13 is fixed in support plate 1, and direct-current machine 13 and driving toothed gear 11 lay respectively at the both sides of support plate 1.Follower gear 2 and driving toothed gear 11 are positioned at homonymy and engage each other, and its central position is set on shaft insulation 16 by angular contact ball bearing 15, and shaft insulation 16 is arranged in support plate 1; Follower gear 2 is 10: 1 with the ratio of the radius of driving toothed gear 10.Shaft insulation 16 is made up of insulating material, is provided with the hole of two axis for passing electrode 4 (negative electrode and anode).Described follower gear 2 is provided with fixture, Erlenmeyer flask 5 can be gripped and the angle formed with cone element at the bottom of making bottle is symmetrical in vertical; Erlenmeyer flask 5 is partially submerged in water-bath 7, the control of realization response temperature.Fixture comprises permanent seat 3 and screw base 9, screw base 9 is equipped with the trip bolt 10 of a band plastics jacking block 8.Negative electrode and the anode of silver material pass the shaft insulation 16 at follower gear 2 center and are inserted in Erlenmeyer flask 5, and the end of negative electrode and anode has the silver-colored material top electrode 6 that can dismantle.
Below in conjunction with drawings and Examples, invention is further described;
Embodiment 1
The SnCl of preparation 0.3mol/L
45H
2mass concentration, in beaker, is that the NaOH solution of 111.1g/L is added in beaker, and mixed solution ph is adjusted to 13, stir 0.5h subsequently by O solution; Mixing solutions after dissolving completely and stir imports in the polytetrafluoroethylene bushing of reactor, and hand power screw is firm, puts into loft drier subsequently and is incubated, and setting hydro-thermal reaction steady temperature is 180 DEG C, reacts the 20h that holds time; Hydro-thermal reaction product is taken out to import in centrifuge tube and carries out centrifugal treating, deionized water and alcohol is successively adopted to clean reaction product, centrifugal rotational speed is 2000r/min, product after cleaning is placed in glassware, in loft drier, carry out drying and processing namely obtain spherical hum silicon dioxide tin, bake out temperature is 90 DEG C; Start the experimental installation of rotatable plating, 100mL solute is consisted of the AgNO of 0.001mol/L
3the aqueous solution imports in Erlenmeyer flask 5, getting spherical hum silicon dioxide tin prepared by some previous steps pours in Erlenmeyer flask 5, Erlenmeyer flask 5 is held in device, negative electrode, anode choice of material are silver and negative electrode are contacted naturally with the spherical hum silicon dioxide tin at the bottom of bottle, setting Erlenmeyer flask rotating speed is 120r/min, bath temperature is 60 DEG C, and electroplating voltage is 10V, and electroplating time is 600s; Taken out by device by Erlenmeyer flask 5, carry out suction filtration to liquid in bottle, the product of filter paper and acquisition being put in the lump glass dish, to be placed in baking oven drier, and temperature is set as 90 DEG C, and time of drying is 2h.
Embodiment 2
With reference to embodiment 1, AgNO wherein
3aqueous solution solute consists of 0.005mol/L, and other conditions are constant.
Embodiment 3
With reference to embodiment 1, AgNO wherein
3aqueous solution solute consists of 0.01mol/L, and other conditions are constant.
Embodiment 4
With reference to embodiment 1, AgNO wherein
3aqueous solution solute consists of 0.05mol/L, and other conditions are constant.
Embodiment 5
With reference to embodiment 1, AgNO wherein
3aqueous solution solute consists of 0.1mol/L, and other conditions are constant.
Embodiment 6
With reference to embodiment 1, AgNO wherein
3aqueous solution solute consists of 0.5mol/L, and other conditions are constant.
Embodiment 7
With reference to embodiment 1, AgNO wherein
3aqueous solution solute consists of 1mol/L, and other conditions are constant.
Embodiment 8
The SnCl of preparation 0.3mol/L
45H
2mass concentration, in beaker, is that the NaOH solution of 111.1g/L is added in beaker, and mixed solution ph is adjusted to 13, stir 0.5h subsequently by O solution; Mixing solutions after dissolving completely and stir imports in the polytetrafluoroethylene bushing of reactor, and hand power screw is firm, puts into loft drier subsequently and is incubated, and setting reaction steady temperature is 180 DEG C, reacts the 20h that holds time; Hydro-thermal reaction product is taken out to import in centrifuge tube and carries out centrifugal treating, deionized water and alcohol is successively adopted to clean reaction product, centrifugal rotational speed is 2000r/min, product after cleaning is placed in glassware, in loft drier, carry out drying and processing namely obtain spherical hum silicon dioxide tin, bake out temperature is 90 DEG C; Enable the experimental installation of rotatable plating, 100mL solute is consisted of the AgNO of 0.01mol/L
3the aqueous solution imports in Erlenmeyer flask 5, getting spherical hum silicon dioxide tin prepared by some previous steps pours in Erlenmeyer flask 5, Erlenmeyer flask 5 is held in device, negative electrode, anode choice of material are silver and negative electrode are contacted naturally with the spherical hum silicon dioxide tin at the bottom of bottle, setting Erlenmeyer flask rotating speed is 120r/min, bath temperature is 60 DEG C, and electroplating voltage is 10V, and electroplating time is 60s; Taken out by device by Erlenmeyer flask 5, carry out suction filtration to liquid in bottle, the product of filter paper and acquisition being put in the lump glass dish, to be placed in baking oven drier, and temperature is set as 90 DEG C, and time of drying is 2h.
Embodiment 9
With reference to embodiment 8, electroplating time is wherein 120s, and other conditions are constant.
Embodiment 10
With reference to embodiment 8, electroplating time is wherein 300s, and other conditions are constant.
Embodiment 11
With reference to embodiment 8, electroplating time is wherein 1200s, and other conditions are constant.
Embodiment 12
With reference to embodiment 8, electroplating time is wherein 2400s, and other conditions are constant.
Embodiment 13
With reference to embodiment 8, electroplating time is wherein 3600s, and other conditions are constant.
Embodiment 14
The SnCl of preparation 0.3mol/L
45H
2mass concentration, in beaker, is that the NaOH solution of 111.1g/L is added in beaker, and mixed solution ph is adjusted to 13, stir 0.5h subsequently by O solution; Mixing solutions after dissolving completely and stir imports in the polytetrafluoroethylene bushing of reactor, and hand power screw is firm, puts into loft drier subsequently and is incubated, and setting reaction steady temperature is 180 DEG C, reacts the 20h that holds time; Hydro-thermal reaction product is taken out to import in centrifuge tube and carries out centrifugal treating, deionized water and alcohol is successively adopted to clean reaction product, centrifugal rotational speed is 2000r/min, product after cleaning is placed in glassware, in loft drier, carry out drying and processing namely obtain spherical hum silicon dioxide tin, bake out temperature is 90 DEG C; Enable the experimental installation of rotatable plating, 100mL solute is consisted of the AgNO of 0.01mol/L
3the aqueous solution imports in Erlenmeyer flask 5, getting spherical hum silicon dioxide tin prepared by some previous steps pours in Erlenmeyer flask 5, Erlenmeyer flask 5 is held in device, negative electrode, anode choice of material are silver and negative electrode are contacted naturally with the spherical hum silicon dioxide tin at the bottom of bottle, setting Erlenmeyer flask 5 rotating speed is 6r/min, bath temperature is 60 DEG C, and electroplating voltage is 10V, and electroplating time is 600s; Taken out by device by Erlenmeyer flask 5, carry out suction filtration to liquid in bottle, the product of filter paper and acquisition being put in the lump glass dish, to be placed in baking oven drier, and temperature is set as 90 DEG C, and time of drying is 2h.
Embodiment 15
With reference to embodiment 14, Erlenmeyer flask rotating speed is wherein 30r/min, and other conditions are constant.
Embodiment 16
With reference to embodiment 14, Erlenmeyer flask rotating speed is wherein 60r/min, and other conditions are constant.
Embodiment 17
With reference to embodiment 14, Erlenmeyer flask rotating speed is wherein 180r/min, and other conditions are constant.
Embodiment 18
With reference to embodiment 14, Erlenmeyer flask rotating speed is wherein 240r/min, and other conditions are constant.
Embodiment 19
With reference to embodiment 14, Erlenmeyer flask rotating speed is wherein 300r/min, and other conditions are constant.
Embodiment 20
The SnCl of preparation 0.3mol/L
45H
2mass concentration, in beaker, is that the NaOH solution of 111.1g/L is added in beaker, and mixed solution ph is adjusted to 13, stir 0.5h subsequently by O solution; Mixing solutions after dissolving completely and stir imports in the polytetrafluoroethylene bushing of reactor, and hand power screw is firm, puts into loft drier subsequently and is incubated, and setting reaction steady temperature is 180 DEG C, reacts the 20h that holds time; Hydro-thermal reaction product is taken out to import in centrifuge tube and carries out centrifugal treating, deionized water and alcohol is successively adopted to clean reaction product, centrifugal rotational speed is 2000r/min, product after cleaning is placed in glassware, in loft drier, carry out drying and processing namely obtain spherical hum silicon dioxide tin, bake out temperature is 90 DEG C; Enable the experimental installation of rotatable plating, 100mL solute is consisted of the AgNO of 0.01mol/L
3the aqueous solution imports in Erlenmeyer flask 5, getting spherical hum silicon dioxide tin prepared by some previous steps pours in Erlenmeyer flask 5, Erlenmeyer flask is held in device, negative electrode, anode choice of material are silver and negative electrode are contacted naturally with the spherical hum silicon dioxide tin at the bottom of bottle, setting Erlenmeyer flask 5 rotating speed is 120r/min, bath temperature is 15 DEG C, and electroplating voltage is 10V, and electroplating time is 600s; Taken out by device by Erlenmeyer flask 5, carry out suction filtration to liquid in bottle, the product of filter paper and acquisition being put in the lump glass dish, to be placed in baking oven drier, and temperature is set as 90 DEG C, and time of drying is 2h.
Embodiment 21
With reference to embodiment 20, bath temperature is wherein 30 DEG C, and other conditions are constant.
Embodiment 22
With reference to embodiment 20, bath temperature is wherein 45 DEG C, and other conditions are constant.
Embodiment 23
With reference to embodiment 20, bath temperature is wherein 75 DEG C, and other conditions are constant.
Embodiment 24
With reference to embodiment 20, bath temperature is wherein 90 DEG C, and other conditions are constant.
Embodiment 25
With reference to embodiment 20, bath temperature is wherein 100 DEG C, and other conditions are constant.
Embodiment 26
The SnCl of preparation 0.3mol/L
45H
2mass concentration, in beaker, is that the NaOH solution of 111.1g/L is added in beaker, and mixed solution ph is adjusted to 13, stir 0.5h subsequently by O solution; Mixing solutions after dissolving completely and stir imports in the polytetrafluoroethylene bushing of reactor, and hand power screw is firm, puts into loft drier subsequently and is incubated, and setting reaction steady temperature is 180 DEG C, reacts the 20h that holds time; Hydro-thermal reaction product is taken out to import in centrifuge tube and carries out centrifugal treating, deionized water and alcohol is successively adopted to clean reaction product, centrifugal rotational speed is 2000r/min, product after cleaning is placed in glassware, in loft drier, carry out drying and processing namely obtain spherical hum silicon dioxide tin, bake out temperature is 90 DEG C; Enable the experimental installation of rotatable plating, 100mL solute is consisted of the AgNO of 0.01mol/L
3the aqueous solution imports in Erlenmeyer flask 5, getting spherical hum silicon dioxide tin prepared by some previous steps pours in Erlenmeyer flask 5, Erlenmeyer flask 5 is held in device, negative electrode, anode choice of material are silver and negative electrode are contacted naturally with the spherical hum silicon dioxide tin at the bottom of bottle, setting Erlenmeyer flask rotating speed is 120r/min, bath temperature is 60 DEG C, and electroplating voltage is 1V, and electroplating time is 600s; Taken out by device by Erlenmeyer flask 5, carry out suction filtration to liquid in bottle, the product of filter paper and acquisition being put in the lump glass dish, to be placed in baking oven drier, and temperature is set as 90 DEG C, and time of drying is 2h.
Embodiment 27
With reference to embodiment 26, electroplating voltage is wherein 5V, and other conditions are constant.
Embodiment 28
With reference to embodiment 26, electroplating voltage is wherein 15V, and other conditions are constant.
Embodiment 29
With reference to embodiment 26, electroplating voltage is wherein 20V, and other conditions are constant.
Embodiment 30
With reference to embodiment 26, electroplating voltage is wherein 25V, and other conditions are constant.
Embodiment 31
With reference to embodiment 26, electroplating voltage is wherein 30V, and other conditions are constant.
Figure 33 is the spherical hum silicon dioxide tin supported micron of embodiment 3 preparation, the X ray diffracting spectrum of nano-Ag particles novel material, in figure, 2 θ equal 38.35 °, 44.52 °, 64.66 °, occur the characteristic diffraction peak of silver when 77.59 °, what load was described is Argent grain.
Table 1 is the different experiments parameter (embodiment 1-31) of the spherical hum silicon dioxide tin supported micron of preparation, nano-Ag particles novel material.
Table 1 experiment parameter designs
As can be seen from Fig. 1-31, when other Parameter Conditions is identical, by changing AgNO respectively
3aqueous solution solute composition, electroplating time, Erlenmeyer flask rotating speed, bath temperature, electroplating voltage, the Argent grain size of institute's load on gained spherical hum silicon dioxide tin supported micron, nano-Ag particles matrix material can be changed, when illustrating that employing present method prepares spherical hum silicon dioxide tin supported micron, nano-Ag particles matrix material, Argent grain size is controlled.
In addition, Figure 32 is the field emission scanning electron microscope photo of the spherical hum silicon dioxide glass putty body of non-load Argent grain.Field emission scanning electron microscope is utilized to observe not adopting the spherical hum silicon dioxide glass putty body of the inventive method with the spherical hum silicon dioxide tin supported micron adopting the inventive method to prepare, nano-Ag particles novel material; carry out microscopic dimensions measurement simultaneously; in Fig. 1-31, the white particle that brightness is larger or floss are micron, the nano-Ag particles of load.By contrasting with Figure 32, obviously can find out the spherical hum silicon dioxide tin supported micron, the nano-Ag particles novel material that adopt the inventive method to prepare, surface uniform is distributed with micron, nano-Ag particles or floss, and dispersity is higher.
What finally illustrate is, above embodiment is only unrestricted for illustration of technical scheme of the present invention, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (6)
1., for carrying out a rotatable electroplating experiments device for load to spherical micron particle, comprise the Erlenmeyer flask as electroplating container, it is characterized in that, also comprise:
Support, having with one and horizontal direction is the support plate of 50 ° of angles;
Direct-current machine, its turning axle is through support plate, and turning axle end is fixedly equipped with driving toothed gear; Direct-current machine is fixed in support plate, and lays respectively at the both sides of support plate with driving toothed gear;
Follower gear, is positioned at homonymy with driving toothed gear and engages each other, and its central position is set on shaft insulation by angular contact ball bearing, and shaft insulation is arranged in support plate;
Described follower gear is provided with fixture, Erlenmeyer flask can be gripped and the angle formed with cone element at the bottom of making bottle is symmetrical in vertical; Negative electrode and the anode of silver material pass the bearing of follower gear and are inserted in Erlenmeyer flask.
2. device according to claim 1, is characterized in that, the end of described negative electrode and anode has the silver-colored material top electrode that can dismantle.
3. device according to claim 1, is characterized in that, the shaft insulation of described follower gear central position is made up of insulating material, is provided with the hole of two axis for passing negative electrode and anode.
4. device according to claim 1, is characterized in that, described fixture comprises permanent seat and screw base, screw base is equipped with the trip bolt of a band plastics jacking block.
5. device according to claim 1, is characterized in that, described follower gear is 10: 1 with the ratio of the radius of driving toothed gear.
6. device according to claim 1, is characterized in that, this device also comprises water-bath, and Erlenmeyer flask part is immersed in water-bath.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510347255.XA CN104894626B (en) | 2015-06-20 | 2015-06-20 | A kind of rotatable electroplating experiments device for being loaded to spherical micron particles |
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| RU2006535C1 (en) * | 1991-04-16 | 1994-01-30 | Арендное объединение "Краматорский машиностроительный завод" | Electroplating bell |
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| CN204125556U (en) * | 2014-07-21 | 2015-01-28 | 宁波韩华磁电有限公司 | A kind of mini turbine type electro-plating roller device |
| CN204738035U (en) * | 2015-06-20 | 2015-11-04 | 浙江大学 | A rotatable electroplating experimental apparatus for being directed at globular micron granule carries out load |
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| RU2006535C1 (en) * | 1991-04-16 | 1994-01-30 | Арендное объединение "Краматорский машиностроительный завод" | Electroplating bell |
| JPH08283996A (en) * | 1995-04-10 | 1996-10-29 | Yamamoto Mekki Shikenki:Kk | Barrel plating device |
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| JP2008223109A (en) * | 2007-03-15 | 2008-09-25 | Hitachi Metals Ltd | Plating equipment and plating method |
| CN101956225A (en) * | 2010-09-17 | 2011-01-26 | 河南科技大学 | Method for preparing nano composite plating layer |
| CN204125556U (en) * | 2014-07-21 | 2015-01-28 | 宁波韩华磁电有限公司 | A kind of mini turbine type electro-plating roller device |
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