CN108793054A - A kind of micro-nano electrode preparation facilities and preparation method based on bidirectional pulse power supply - Google Patents
A kind of micro-nano electrode preparation facilities and preparation method based on bidirectional pulse power supply Download PDFInfo
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Abstract
本发明提供了一种基于双向脉冲电源的微纳米电极制备装置及制备方法。制备装置包括:工作台板、电解液槽、凸形支架块、双向脉冲电源、连接轴、铂金属环、横向支架臂以及竖直支架臂。制备方法步骤包括:在电解液槽装载氢氧化钾溶液,且使氢氧化钾溶液的液面高于铂金属环的安装高度;将电极棒的上端装夹在夹头上,且电极棒的下端贯穿铂金属环的中心环孔,电极棒与铂金属环的中心环孔同轴心设置;利用双向脉冲电源周期交替向夹头发送脉宽为100ns‑150ns的正向脉冲以及向铂金属环发送脉宽为150ns‑160ns的反向脉冲,从而对电极棒进行刻蚀。该微纳米电极制备装置及制备方法在于不施加任何外界的运动情况下,仅仅采用双向脉冲电源即可实现减小制备出纳米电极的锥度。
The invention provides a micro-nano electrode preparation device and a preparation method based on a bidirectional pulse power supply. The preparation device includes: a working table, an electrolyte tank, a convex support block, a bidirectional pulse power supply, a connecting shaft, a platinum metal ring, a horizontal support arm and a vertical support arm. The preparation method steps include: loading potassium hydroxide solution in the electrolytic solution tank, and making the liquid level of the potassium hydroxide solution higher than the installation height of the platinum metal ring; clamping the upper end of the electrode rod on the clamp, and the lower end of the electrode rod Through the central ring hole of the platinum metal ring, the electrode rod is set concentrically with the central ring hole of the platinum metal ring; the positive pulse with a pulse width of 100ns‑150ns is alternately sent to the collet and sent to the platinum metal ring by using a bidirectional pulse power supply cycle A reverse pulse with a pulse width of 150ns-160ns to etch the electrode rod. The preparation device and method of the micro-nano electrode can reduce the taper of the prepared nano-electrode by only using a bidirectional pulse power supply without applying any external motion.
Description
技术领域technical field
本发明创造涉及一种微纳米电极制备装置及制备方法,尤其是一种基于双向脉冲电源的微纳米电极制备装置及制备方法。The invention relates to a micro-nano electrode preparation device and a preparation method, in particular to a micro-nano electrode preparation device and a preparation method based on a bidirectional pulse power supply.
背景技术Background technique
微纳米尺度的电极是进行微细加工的必要条件,目前制备微纳米电极的方法主要有机械剪切、聚焦离子铣削、电解加工等。机械剪切制备出的电极主要为尖锥状电极,成功率低且制备精度很难保证。聚焦离子铣削可以制备出各种形貌的电极,但是聚焦离子铣削设备昂贵,加工效率低,制备电极成本高。电解加工是目前制备微纳米电极最常用的方法,电极尺寸可控且较为简捷。Micro-nano-scale electrodes are a necessary condition for microfabrication. At present, the methods for preparing micro-nano electrodes mainly include mechanical shearing, focused ion milling, and electrolytic machining. Electrodes prepared by mechanical shearing are mainly tapered electrodes, which have a low success rate and are difficult to guarantee the preparation accuracy. Focused ion milling can prepare electrodes with various shapes, but focused ion milling equipment is expensive, processing efficiency is low, and electrode preparation costs are high. Electrolytic machining is currently the most commonly used method for preparing micro-nano electrodes, and the size of the electrodes is controllable and relatively simple.
采用电解加工方法,在加工过程中由于电解产物的积聚状态使得加工出的工具电极呈上大下小尖锥状,这种锥状电极在一定程度上限制了其用于加工的精度。若采用此种形状电极进行电解打孔,那么加工出的孔的侧壁则具有很大的锥度。为了减少制备出的电极的锥度,增加电极的长径比,也常将各种运动施加于加工过程中,使得电解产物分布趋于均匀。利用在电解加工过程中采用压电陶瓷对电解液膜进行频率为35HZ上下振动,减小扩散层对电极形貌的影响,从而减小纳米电极的锥度,但是这需要在电极制备装置中额外配备振动系统。Using the electrolytic machining method, due to the accumulation of electrolytic products during the machining process, the processed tool electrode is in the shape of a large and small pointed cone. This cone-shaped electrode limits its machining accuracy to a certain extent. If the electrodes of this shape are used for electrolytic drilling, the side walls of the processed holes will have a large taper. In order to reduce the taper of the prepared electrode and increase the aspect ratio of the electrode, various movements are often applied during the processing, so that the distribution of electrolytic products tends to be uniform. Use piezoelectric ceramics to vibrate the electrolyte film up and down at a frequency of 35HZ in the process of electrolytic processing to reduce the influence of the diffusion layer on the electrode shape, thereby reducing the taper of the nano-electrode, but this requires additional equipment in the electrode preparation device. Equipped with vibration system.
发明内容Contents of the invention
本发明要解决的技术问题是现有的制备装置及制备方法需要额外的辅助装置,增加的制备成本。The technical problem to be solved by the present invention is that the existing preparation device and preparation method require additional auxiliary devices and increase the preparation cost.
为了解决上述技术问题,本发明提供了一种基于双向脉冲电源的微纳米电极制备装置,包括工作台板、电解液槽、凸形支架块、双向脉冲电源、连接轴、铂金属环、横向支架臂以及竖直支架臂;电解液槽设置于工作台板上,竖直支架臂竖向固定安装在工作台板上;横向支架臂的一端通过第一安装螺栓固定安装竖直支架臂上;连接轴的一端通过第二安装螺栓固定安装在横向支架臂的另一端上;连接轴与竖直支架臂相平行;凸形支架块固定安装在电解液槽内,铂金属环通过悬臂水平安装在凸形支架块上,且铂金属环位于电解液槽内;连接轴的下端指向铂金属环的中心环孔;在连接轴的下端上设有用于夹持固定电极棒的夹头;双向脉冲电源的正极端通过防水导线与夹头电连接;双向脉冲电源的负极端通过防水导线与铂金属环电连接。In order to solve the above technical problems, the present invention provides a micro-nano electrode preparation device based on a bidirectional pulse power supply, including a worktable, an electrolyte tank, a convex support block, a bidirectional pulse power supply, a connecting shaft, a platinum metal ring, and a transverse support arm and vertical support arm; the electrolyte tank is arranged on the worktable, and the vertical support arm is vertically fixedly installed on the worktable; one end of the horizontal support arm is fixedly installed on the vertical support arm through the first mounting bolt; One end of the shaft is fixedly installed on the other end of the horizontal support arm through the second mounting bolt; the connecting shaft is parallel to the vertical support arm; the convex support block is fixedly installed in the electrolyte tank, and the platinum metal ring is installed horizontally on the convex support shaped bracket block, and the platinum metal ring is located in the electrolyte tank; the lower end of the connecting shaft points to the central ring hole of the platinum metal ring; the lower end of the connecting shaft is provided with a chuck for clamping and fixing the electrode rod; the bidirectional pulse power supply The positive end is electrically connected to the chuck through a waterproof wire; the negative end of the bidirectional pulse power supply is electrically connected to the platinum metal ring through a waterproof wire.
进一步地,铂金属环的环片厚度为2-3mm,中心环孔的直径为6-7mm。Further, the thickness of the ring piece of the platinum metal ring is 2-3 mm, and the diameter of the central ring hole is 6-7 mm.
进一步地,包括如下步骤:Further, the following steps are included:
步骤1,在电解液槽装载氢氧化钾溶液,且使氢氧化钾溶液的液面高于铂金属环的安装高度;Step 1, loading potassium hydroxide solution in the electrolytic solution tank, and making the liquid level of the potassium hydroxide solution higher than the installation height of the platinum metal ring;
步骤2,将电极棒的上端装夹在夹头上,且电极棒的下端贯穿铂金属环的中心环孔,电极棒与铂金属环的中心环孔同轴心设置;Step 2, the upper end of the electrode rod is clamped on the chuck, and the lower end of the electrode rod passes through the central ring hole of the platinum metal ring, and the electrode rod and the central ring hole of the platinum metal ring are arranged concentrically;
步骤3,利用双向脉冲电源周期交替向夹头发送脉宽为100ns-150ns的正向脉冲以及向铂金属环发送脉宽为150ns-160ns的反向脉冲,从而对电极棒进行刻蚀。Step 3, using a bidirectional pulse power supply to alternately send forward pulses with a pulse width of 100 ns-150 ns to the chuck and send reverse pulses with a pulse width of 150 ns-160 ns to the platinum metal ring, so as to etch the electrode rod.
进一步地,在电解液槽中装载的氢氧化钾溶液的溶度为1.5mol/L。Further, the solubility of the potassium hydroxide solution loaded in the electrolyte tank is 1.5 mol/L.
本发明的有益效果在于:为了得到较好的长径比,应采取措施使得电极棒周围电解产物分布趋于均匀,本发明在于不施加任何外界的运动,仅仅采用双向脉冲电源即可实现减小制备出纳米电极的锥度;在正向脉冲时,作为阳极的电极棒发生电化学溶解,产物在重力的作用下下移并积聚在电极棒周围,形成锥状的堆积;反向脉冲时,电极棒又作为阴极产生氢气,氢气泡的形成及逸出对正向脉冲时积聚在电极棒周围的电解产物形成扰动,使产物分布趋于均匀或者分散于电解液中,使得电极棒周围电导率趋于均匀,周而复始从而使得制备出的工具电极具有良好的长径比。The beneficial effect of the present invention is that: in order to obtain a better length-to-diameter ratio, measures should be taken to make the distribution of electrolytic products around the electrode rod tend to be uniform. The taper of the nano-electrode is prepared; during the forward pulse, the electrode rod as the anode is electrochemically dissolved, and the product moves down under the action of gravity and accumulates around the electrode rod, forming a cone-shaped accumulation; when the reverse pulse is applied, the electrode The rod acts as the cathode to generate hydrogen gas. The formation and escape of hydrogen bubbles disturb the electrolysis products accumulated around the electrode rod during the positive pulse, making the product distribution tend to be uniform or dispersed in the electrolyte, making the conductivity around the electrode rod tend to be It is uniform and repeated so that the prepared tool electrode has a good aspect ratio.
附图说明Description of drawings
图1为本发明的微纳米电极制备装置整体结构示意图;1 is a schematic diagram of the overall structure of the micro-nano electrode preparation device of the present invention;
图2为本发明在正向脉冲时钨棒周围电解产物的分布情况;Fig. 2 is the distribution situation of the electrolysis product around the tungsten rod when Fig. 2 is positive pulse;
图3为本发明在反向脉冲时钨棒周围电解产物的分布情况。Fig. 3 shows the distribution of electrolytic products around the tungsten rod during the reverse pulse of the present invention.
具体实施方式Detailed ways
如图1所示,本发明提供的基于双向脉冲电源的微纳米电极制备装置包括:工作台板1、电解液槽2、凸形支架块4、双向脉冲电源6、连接轴9、铂金属环12、横向支架臂13以及竖直支架臂15;电解液槽2设置于工作台板1上,竖直支架臂15竖向固定安装在工作台板1上;横向支架臂13的一端通过第一安装螺栓14固定安装竖直支架臂15上;连接轴9的一端通过第二安装螺栓8固定安装在横向支架臂13的另一端上;连接轴9与竖直支架臂15相平行;凸形支架块4通过螺钉3固定安装在电解液槽2内,铂金属环12通过悬臂水平安装在凸形支架块4上,悬臂的端部通过螺钉3安装在凸形支架块4上,且铂金属环12位于电解液槽2内;连接轴9的下端指向铂金属环12的中心环孔;在连接轴9的下端上设有用于夹持固定电极棒11的夹头10;双向脉冲电源6的正极端通过防水导线7与夹头10电连接;双向脉冲电源6的负极端通过防水导线7与铂金属环12电连接。铂金属环12的环片厚度为2-3mm,中心环孔的直径为6-7mm。As shown in Figure 1, the micro-nano electrode preparation device based on bidirectional pulse power supply provided by the present invention includes: worktable 1, electrolyte tank 2, convex support block 4, bidirectional pulse power supply 6, connecting shaft 9, platinum metal ring 12. The horizontal support arm 13 and the vertical support arm 15; the electrolyte tank 2 is arranged on the worktable 1, and the vertical support arm 15 is vertically fixedly installed on the worktable 1; one end of the horizontal support arm 13 passes through the first Mounting bolt 14 is fixedly installed on the vertical support arm 15; One end of connection shaft 9 is fixedly installed on the other end of transverse support arm 13 by second mounting bolt 8; Connection shaft 9 is parallel with vertical support arm 15; Convex support The block 4 is fixedly installed in the electrolyte tank 2 through the screw 3, the platinum metal ring 12 is horizontally installed on the convex support block 4 through the cantilever, and the end of the cantilever is installed on the convex support block 4 through the screw 3, and the platinum metal ring 12 is located in the electrolyte tank 2; the lower end of the connecting shaft 9 points to the central ring hole of the platinum metal ring 12; the lower end of the connecting shaft 9 is provided with a chuck 10 for clamping and fixing the electrode rod 11; the positive side of the bidirectional pulse power supply 6 The extreme end is electrically connected to the chuck 10 through the waterproof wire 7; the negative end of the bidirectional pulse power supply 6 is electrically connected to the platinum metal ring 12 through the waterproof wire 7. The ring piece thickness of the platinum metal ring 12 is 2-3mm, and the diameter of the central ring hole is 6-7mm.
本发明提供的基于双向脉冲电源的微纳米电极制备方法,包括如下步骤:The micro-nano electrode preparation method based on bidirectional pulse power supply provided by the present invention comprises the following steps:
步骤1,在电解液槽2装载氢氧化钾溶液,且使氢氧化钾溶液5的液面高于铂金属环12的安装高度,氢氧化钾溶液5的溶度为1.5mol/L;Step 1, loading potassium hydroxide solution in electrolyte tank 2, and make the liquid level of potassium hydroxide solution 5 higher than the installation height of platinum metal ring 12, the solubility of potassium hydroxide solution 5 is 1.5mol/L;
步骤2,将电极棒11的上端装夹在夹头10上,且电极棒11的下端贯穿铂金属环12的中心环孔,电极棒11与铂金属环12的中心环孔同轴心设置;Step 2, the upper end of the electrode rod 11 is clamped on the chuck 10, and the lower end of the electrode rod 11 passes through the central ring hole of the platinum metal ring 12, and the electrode rod 11 and the central ring hole of the platinum metal ring 12 are arranged concentrically;
步骤3,利用双向脉冲电源6周期交替向夹头10发送脉宽为100ns-150ns的正向脉冲以及向铂金属环12发送脉宽为150ns-160ns的反向脉冲,即向夹头10发送脉宽为100ns-150ns的正向脉冲后,再向铂金属环12发送脉宽为150ns-160ns的反向脉冲,如此交替循环,正向脉冲和反向脉冲的幅值为4V,从而对电极棒11进行刻蚀,当正向脉冲时,电极棒11在电解液槽2中由于电解反应的进行逐渐被刻蚀,电解产物是积聚在电极棒11的周围,由于重力的作用形成上小下大的分布状态,如图2所示;当反向脉冲时,此时电极棒11相当于接电源的负极,产生大量气泡,由于气泡的浮动及爆破对电极棒11周围的电解产物产生扰动,使得电极棒11周围电解产物分布趋于均布,如图3所示,周而复始,从而使制备出的微纳米电极锥度更小。Step 3, use the bidirectional pulse power supply 6 cycles to alternately send forward pulses with a pulse width of 100ns-150ns to the chuck 10 and send reverse pulses with a pulse width of 150ns-160ns to the platinum metal ring 12, that is, send pulses to the chuck 10 After the forward pulse with a width of 100ns-150ns, a reverse pulse with a pulse width of 150ns-160ns is sent to the platinum metal ring 12, so that the cycle alternates, the amplitude of the forward pulse and the reverse pulse is 4V, so that the electrode rod 11 for etching, when the positive pulse, the electrode rod 11 is gradually etched in the electrolyte tank 2 due to the electrolytic reaction, and the electrolytic products are accumulated around the electrode rod 11, forming a small upper part and a larger lower part due to the action of gravity. distribution state, as shown in Figure 2; when the reverse pulse is applied, the electrode rod 11 is equivalent to the negative pole connected to the power supply, and a large number of bubbles are generated. The floating and bursting of the bubbles disturb the electrolytic product around the electrode rod 11, making The distribution of electrolytic products around the electrode rod 11 tends to be uniform, as shown in FIG. 3 , and the cycle repeats itself, so that the taper of the prepared micro-nano electrode is smaller.
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