CN104445443B - A kind of method preparing nanometer sheet structure cobalt oxide electrode - Google Patents
A kind of method preparing nanometer sheet structure cobalt oxide electrode Download PDFInfo
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- 229910000428 cobalt oxide Inorganic materials 0.000 title claims abstract description 43
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 23
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000007789 gas Substances 0.000 claims abstract description 28
- 229910052786 argon Inorganic materials 0.000 claims abstract description 17
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims abstract description 17
- 239000000758 substrate Substances 0.000 claims abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000001301 oxygen Substances 0.000 claims abstract description 13
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 13
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 238000000576 coating method Methods 0.000 claims abstract description 12
- 238000000151 deposition Methods 0.000 claims abstract description 10
- 230000008021 deposition Effects 0.000 claims abstract description 10
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 239000012300 argon atmosphere Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims 7
- 238000004062 sedimentation Methods 0.000 claims 2
- 239000012298 atmosphere Substances 0.000 claims 1
- 239000002135 nanosheet Substances 0.000 abstract description 26
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 abstract 1
- 229910001882 dioxygen Inorganic materials 0.000 abstract 1
- 239000007772 electrode material Substances 0.000 description 14
- 238000002484 cyclic voltammetry Methods 0.000 description 8
- 239000003990 capacitor Substances 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical group 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000011232 storage material Substances 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 238000006276 transfer reaction Methods 0.000 description 1
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Abstract
一种制备纳米片结构氧化钴电极的方法，本发明涉及制备电极的方法。本发明要解决现有氧化钴赝电容存在比电容较低的问题。本发明的方法：在Si基底上制备Co镀层，然后将其置于等离子体增强化学气相沉积真空装置中，通入氩气，调节气体流量、压强，升温到一定温度后，再通入氧气，调节氩气及氧气气体流量，调节温度、射频功率、压强，进行沉积，沉积结束后，即得到纳米片结构氧化钴电极。本发明用于制备纳米片结构氧化钴电极。
A method for preparing a cobalt oxide electrode with a nanosheet structure, and the invention relates to a method for preparing the electrode. The invention solves the problem of low specific capacitance in the existing cobalt oxide pseudocapacitor. The method of the present invention: prepare the Co coating on the Si substrate, then place it in a plasma-enhanced chemical vapor deposition vacuum device, feed argon gas, adjust the gas flow rate and pressure, heat up to a certain temperature, and then feed oxygen, Adjust the flow rate of argon and oxygen gas, adjust the temperature, radio frequency power, and pressure, and deposit. After the deposition is completed, a cobalt oxide electrode with a nanosheet structure is obtained. The invention is used for preparing cobalt oxide electrodes with nano sheet structure.
Description
技术领域technical field
本发明涉及制备电极的方法。The present invention relates to methods of preparing electrodes.
背景技术Background technique
超级电容器是一种介于传统电容器和电池之间的新型储能元件，它比传统电容器具有更高的比电容和能量密度，比电池具有更高的功率密度，因而具有广阔的应用前景。为了能够满足未来的各种应用，制备出高能量密度和功率密度、长循环寿命、低成本超级电容器电极材料成为其广泛使用的关键。Supercapacitor is a new type of energy storage element between traditional capacitors and batteries. It has higher specific capacitance and energy density than traditional capacitors, and higher power density than batteries, so it has broad application prospects. In order to meet various applications in the future, the preparation of high energy density and power density, long cycle life, and low-cost supercapacitor electrode materials has become the key to its widespread use.
根据储能机理的不同,目前电化学电容器分为双电层电容器和赝电容器。其中双电层电容器广泛使用的是各种碳材料,其特点是导电率高、比表面积大、循环性好，但是其比电容较低；另一类则是用作赝电容的是金属氧化物材料，比电容一般较高，但存在稳定性较差的问题。According to different energy storage mechanisms, electrochemical capacitors are currently divided into electric double layer capacitors and pseudocapacitors. Among them, various carbon materials are widely used in electric double layer capacitors, which are characterized by high conductivity, large specific surface area, and good circulation, but their specific capacitance is low; the other type is metal oxides used as pseudocapacitors. materials, the specific capacitance is generally higher, but there is a problem of poor stability.
通常认为，过渡金属氧化物是最好的赝电容候选电极材料，因其有各种氧化态可用于氧化还原电荷转移。其中，研究最多的金属氧化物是水合的氧化钌，但由于其价格昂贵，需要积极寻找用廉价的过渡金属氧化物及其他化合物材料来替代。氧化钴以其极高的理论电容、高的循环特性、低成本预示着其良好的应用前景，但是较低的电导率使得氧化钴基电极材料的电容性能未充分显现，与理论值相差很大，所以如何提高其导电性是近来研究的热点。随着纳米技术科学与技术的不断进步，各种纳米材料开始用于超级电容器。从而带来了一些优势：电极材料尺寸的降低能显著地增大单位质量电极/电解质接触面积，为电荷转移反应提供更多的离子吸附位点；可减少离子和电子通过多孔电极时扭曲的扩散距离，得到更短的扩散时间，提高充放电速率，进而得到高性能的电极材料。It is generally considered that transition metal oxides are the best candidate pseudocapacitive electrode materials because of their various oxidation states for redox charge transfer. Among them, the most studied metal oxide is hydrated ruthenium oxide, but due to its high price, it is necessary to actively seek alternatives to cheap transition metal oxides and other compound materials. Cobalt oxide has a good application prospect due to its extremely high theoretical capacitance, high cycle characteristics, and low cost, but the low electrical conductivity makes the capacitance performance of cobalt oxide-based electrode materials not fully manifested, which is very different from the theoretical value. , so how to improve its conductivity is the hot spot of recent research. With the continuous advancement of nanotechnology science and technology, various nanomaterials have begun to be used in supercapacitors. This brings some advantages: the reduction in the size of the electrode material can significantly increase the electrode/electrolyte contact area per unit mass, providing more ion adsorption sites for the charge transfer reaction; it can reduce the distorted diffusion of ions and electrons through the porous electrode The distance is shorter, the diffusion time is shorter, the charge and discharge rate is increased, and high-performance electrode materials are obtained.
发明内容Contents of the invention
本发明要解决现有氧化钴赝电容存在比电容较低的问题，而提供一种制备纳米片结构氧化钴电极的方法。The invention aims to solve the problem of low specific capacitance in the existing cobalt oxide pseudocapacitor, and provides a method for preparing a cobalt oxide electrode with a nanosheet structure.
一种制备纳米片结构氧化钴电极的方法，具体是按照以下步骤进行的：A method for preparing a nanosheet structure cobalt oxide electrode, specifically carried out according to the following steps:
一、将Si基底置于丙酮溶液中超声清洗10min～20min，然后利用磁控溅射设备在Si基底上制备Co镀层，得到Co镀层硅片；1. Put the Si substrate in an acetone solution and ultrasonically clean it for 10-20 minutes, and then use magnetron sputtering equipment to prepare a Co coating on the Si substrate to obtain a Co-coated silicon wafer;
二、将Co镀层硅片置于等离子体增强化学气相沉积真空装置中，抽真空至压强为5Pa以下，通入氩气，调节氩气气体流量为10sccm～50sccm，调节等离子体增强化学气相沉积真空装置中压强为100Pa～1000Pa，并在压强为100Pa～1000Pa和氩气气氛下，在25min内将温度升温至为500℃～800℃；2. Place the Co-coated silicon wafer in the plasma-enhanced chemical vapor deposition vacuum device, evacuate to a pressure below 5Pa, pass in argon gas, adjust the flow rate of the argon gas to 10sccm-50sccm, and adjust the plasma-enhanced chemical vapor deposition vacuum The pressure in the device is 100Pa～1000Pa, and under the pressure of 100Pa～1000Pa and argon atmosphere, the temperature is raised to 500℃～800℃ within 25min;
三、通入氧气，调节氧气的气体流量为10sccm，调节氩气的气体流量为50sccm～90sccm，调节等离子体增强化学气相沉积真空装置中压强为200Pa～500Pa，然后在射频功率为75W～225W、压强为200Pa～500Pa和温度为500℃～800℃条件下进行沉积，沉积时间为30min～90min，沉积结束后，关闭射频电源和加热电源，停止通入氧气，在氩气气氛下从温度为500℃～800℃冷却至室温，即得到纳米片结构的氧化钴电极。3. Introduce oxygen, adjust the gas flow rate of oxygen to 10sccm, adjust the gas flow rate of argon to 50sccm～90sccm, adjust the pressure in the plasma enhanced chemical vapor deposition vacuum device to 200Pa～500Pa, and then the radio frequency power is 75W～225W, The deposition is carried out under the condition of pressure of 200Pa～500Pa and temperature of 500℃～800℃. The deposition time is 30min～90min. °C to 800 °C and cooled to room temperature to obtain a cobalt oxide electrode with a nanosheet structure.
本发明的有益效果是：The beneficial effects of the present invention are:
1、采用简单的磁控溅射和等离子体增强化学气相沉积方法后，得到了在Si基底上垂直生长的氧化钴纳米片阵列结构，制备过程简单，成本低。其可直接用作集电极使用，而且提高了赝电容的整体性能。1. After adopting simple magnetron sputtering and plasma enhanced chemical vapor deposition methods, the cobalt oxide nanosheet array structure vertically grown on the Si substrate is obtained, the preparation process is simple and the cost is low. It can be used directly as a collector, and improves the overall performance of the pseudocapacitor.
2、本发明所制备的氧化钴纳米片阵列结构具有较大的比较面积和独特的片层结构，非常有利于电极材料和电解液充分润湿，有利于电子的扩散，提高充放电速率，进而得到高性能的电极材料，其比容量最高可达到450μF/cm2。2. The cobalt oxide nanosheet array structure prepared by the present invention has a relatively large relative area and a unique sheet structure, which is very conducive to the full wetting of the electrode material and the electrolyte, is conducive to the diffusion of electrons, and improves the charge and discharge rate. A high-performance electrode material is obtained, and its specific capacity can reach up to 450 μF/cm 2 .
3、本发明的方法简单，高效，便于工业化生产，制备得到的纳米片结构的氧化钴电极材料在储能材料、气体吸附材料等领域有广阔的应用前景。3. The method of the present invention is simple, efficient, and convenient for industrial production, and the prepared cobalt oxide electrode material with a nanosheet structure has broad application prospects in the fields of energy storage materials, gas adsorption materials, and the like.
本发明用于一种制备纳米片结构氧化钴电极的方法。The invention is used for a method for preparing a cobalt oxide electrode with a nanosheet structure.
附图说明Description of drawings
图1为实施例制备的纳米片结构的氧化钴电极材料的扫描电镜图；Fig. 1 is the scanning electron micrograph of the cobalt oxide electrode material of the nanosheet structure that embodiment prepares;
图2为循环伏安曲线图，1为扫速为50mV/s时实施例制备的纳米片结构的氧化钴电极的循环伏安曲线图，2为扫速为20mV/s时实施例制备的纳米片结构的氧化钴电极的循环伏安曲线图，3为扫速为10mV/s时实施例制备的纳米片结构的氧化钴电极的循环伏安曲线图。Fig. 2 is a cyclic voltammetry curve, 1 is the cyclic voltammetry curve of the cobalt oxide electrode of the nanosheet structure prepared by the embodiment when the scan rate is 50mV/s, and 2 is the nanometer electrode prepared by the embodiment when the scan rate is 20mV/s. 3 is the cyclic voltammetry curve of the cobalt oxide electrode with the sheet structure, and 3 is the cyclic voltammetry curve of the cobalt oxide electrode with the nanosheet structure prepared in the embodiment when the scan rate is 10 mV/s.
具体实施方式detailed description
本发明技术方案不局限于以下所列举的具体实施方式，还包括各具体实施方式之间的任意组合。The technical solution of the present invention is not limited to the specific embodiments listed below, but also includes any combination of the specific embodiments.
具体实施方式一：本实施方式所述的一种制备纳米片结构氧化钴电极的方法，具体是按照以下步骤进行的：Embodiment 1: A method for preparing a nanosheet structure cobalt oxide electrode described in this embodiment is specifically carried out according to the following steps:
一、将Si基底置于丙酮溶液中超声清洗10min～20min，然后利用磁控溅射设备在Si基底上制备Co镀层，得到Co镀层硅片；1. Put the Si substrate in an acetone solution and ultrasonically clean it for 10-20 minutes, and then use magnetron sputtering equipment to prepare a Co coating on the Si substrate to obtain a Co-coated silicon wafer;
二、将Co镀层硅片置于等离子体增强化学气相沉积真空装置中，抽真空至压强为5Pa以下，通入氩气，调节氩气气体流量为10sccm～50sccm，调节等离子体增强化学气相沉积真空装置中压强为100Pa～1000Pa，并在压强为100Pa～1000Pa和氩气气氛下，在25min内将温度升温至为500℃～800℃；2. Place the Co-coated silicon wafer in the plasma-enhanced chemical vapor deposition vacuum device, evacuate to a pressure below 5Pa, pass in argon gas, adjust the flow rate of the argon gas to 10sccm-50sccm, and adjust the plasma-enhanced chemical vapor deposition vacuum The pressure in the device is 100Pa～1000Pa, and under the pressure of 100Pa～1000Pa and argon atmosphere, the temperature is raised to 500℃～800℃ within 25min;
三、通入氧气，调节氧气的气体流量为10sccm，调节氩气的气体流量为50sccm～90sccm，调节等离子体增强化学气相沉积真空装置中压强为200Pa～500Pa，然后在射频功率为75W～225W、压强为200Pa～500Pa和温度为500℃～800℃条件下进行沉积，沉积时间为30min～90min，沉积结束后，关闭射频电源和加热电源，停止通入氧气，在氩气气氛下从温度为500℃～800℃冷却至室温，即得到纳米片结构的氧化钴电极。3. Introduce oxygen, adjust the gas flow rate of oxygen to 10sccm, adjust the gas flow rate of argon to 50sccm～90sccm, adjust the pressure in the plasma enhanced chemical vapor deposition vacuum device to 200Pa～500Pa, and then the radio frequency power is 75W～225W, The deposition is carried out under the condition of pressure of 200Pa～500Pa and temperature of 500℃～800℃. The deposition time is 30min～90min. °C to 800 °C and cooled to room temperature to obtain a cobalt oxide electrode with a nanosheet structure.
本实施方式通过对镀层厚度、反应参数等控制，可以控制氧化钴纳米片的生长状态，进而得到了性能优异的氧化钴纳米结构电极材料，测试结果表明其电化学性能优良。In this embodiment, the growth state of cobalt oxide nanosheets can be controlled by controlling the coating thickness and reaction parameters, and then a cobalt oxide nanostructure electrode material with excellent performance is obtained. The test results show that it has excellent electrochemical performance.
本实施方式的有益效果是：The beneficial effects of this embodiment are:
1、采用简单的磁控溅射和等离子体增强化学气相沉积方法后，得到了在Si基底上垂直生长的氧化钴纳米片阵列结构，制备过程简单，成本低。其可直接用作集电极使用，而且提高了赝电容的整体性能。1. After adopting simple magnetron sputtering and plasma enhanced chemical vapor deposition methods, the cobalt oxide nanosheet array structure vertically grown on the Si substrate is obtained, the preparation process is simple and the cost is low. It can be used directly as a collector, and improves the overall performance of the pseudocapacitor.
2、本实施方式所制备的氧化钴纳米片阵列结构具有较大的比较面积和独特的片层结构，非常有利于电极材料和电解液充分润湿，有利于电子的扩散，提高充放电速率，进而得到高性能的电极材料，其比容量最高可达到450μF/cm2。2. The cobalt oxide nanosheet array structure prepared in this embodiment has a large comparative area and a unique sheet structure, which is very conducive to the full wetting of the electrode material and the electrolyte, is conducive to the diffusion of electrons, and improves the charge and discharge rate. Furthermore, a high-performance electrode material can be obtained, and its specific capacity can reach up to 450 μF/cm 2 .
3、本实施方式的方法简单，高效，便于工业化生产，制备得到的纳米片结构的氧化钴电极材料在储能材料、气体吸附材料等领域有广阔的应用前景。3. The method of this embodiment is simple, efficient, and convenient for industrial production. The prepared cobalt oxide electrode material with a nanosheet structure has broad application prospects in the fields of energy storage materials, gas adsorption materials, and the like.
具体实施方式二：本实施方式与具体实施方式一不同的是：步骤一中利用磁控溅射设备在Si基底上制备厚度为10nm～1000nm的Co镀层。其它与具体实施方式一相同。Embodiment 2: This embodiment differs from Embodiment 1 in that: in Step 1, a Co coating with a thickness of 10 nm˜1000 nm is prepared on the Si substrate by using a magnetron sputtering device. Others are the same as in the first embodiment.
具体实施方式三：本实施方式与具体实施方式一或二之一不同的是：步骤一中利用磁控溅射设备在Si基底上制备厚度为100nm的Co镀层。其它与具体实施方式一或二相同。Embodiment 3: This embodiment differs from Embodiment 1 or Embodiment 2 in that in step 1, a Co coating with a thickness of 100 nm is prepared on the Si substrate by using a magnetron sputtering device. Others are the same as in the first or second embodiment.
具体实施方式四：本实施方式与具体实施方式一至三之一不同的是：步骤三中调节氧气的气体流量为10sccm，调节氩气的气体流量为50sccm。其它与具体实施方式一至三相同。Embodiment 4: The difference between this embodiment and one of Embodiments 1 to 3 is that in step 3, the gas flow rate of oxygen is adjusted to 10 sccm, and the gas flow rate of argon gas is adjusted to 50 sccm. Others are the same as those in Embodiments 1 to 3.
具体实施方式五：本实施方式与具体实施方式一至四之一不同的是：步骤二中在25min内将温度升温至为600℃～650℃。其它与具体实施方式一至四相同。Embodiment 5: This embodiment is different from Embodiment 1 to Embodiment 4 in that: in step 2, the temperature is raised to 600° C. to 650° C. within 25 minutes. Others are the same as the specific embodiments 1 to 4.
具体实施方式六：本实施方式与具体实施方式一至五之一不同的是：步骤二中在25min内将温度升温至为700℃。其它与具体实施方式一至五相同。Embodiment 6: This embodiment differs from Embodiment 1 to Embodiment 5 in that: in step 2, the temperature is raised to 700° C. within 25 minutes. Others are the same as those in Embodiments 1 to 5.
具体实施方式七：本实施方式与具体实施方式一至六之一不同的是：步骤三中调节等离子体增强化学气相沉积真空装置中压强为500Pa。其它与具体实施方式一至六相同。Embodiment 7: This embodiment differs from Embodiment 1 to Embodiment 6 in that: in step 3, the pressure in the plasma-enhanced chemical vapor deposition vacuum device is adjusted to 500 Pa. Others are the same as those in Embodiments 1 to 6.
具体实施方式八：本实施方式与具体实施方式一至七之一不同的是：步骤三中沉积时间为45min。其它与具体实施方式一至七相同。Embodiment 8: The difference between this embodiment and one of Embodiments 1 to 7 is that the deposition time in step 3 is 45 minutes. Others are the same as those in Embodiments 1 to 7.
采用以下实施例验证本发明的有益效果：Adopt the following examples to verify the beneficial effects of the present invention:
实施例：Example:
本实施例所述的一种制备纳米片结构氧化钴电极的方法，具体是按照以下步骤进行的：A method for preparing a nanosheet structure cobalt oxide electrode described in this embodiment is specifically carried out according to the following steps:
一、将Si基底置于丙酮溶液中超声清洗15min，然后利用磁控溅射设备在Si基底上制备厚度为75nm的Co镀层，得到Co镀层硅片；1. Place the Si substrate in an acetone solution for ultrasonic cleaning for 15 minutes, and then use a magnetron sputtering device to prepare a Co coating with a thickness of 75 nm on the Si substrate to obtain a Co-coated silicon wafer;
二、将Co镀层硅片置于等离子体增强化学气相沉积真空装置中，抽真空至压强为5Pa以下，通入氩气，调节氩气气体流量为30sccm，调节等离子体增强化学气相沉积真空装置中压强为200Pa，并在压强为200Pa和氩气气氛下，在25min内将温度升温至为700℃；2. Place the Co-coated silicon wafer in a plasma-enhanced chemical vapor deposition vacuum device, evacuate to a pressure below 5Pa, pass in argon gas, adjust the argon gas flow rate to 30 sccm, and adjust the plasma-enhanced chemical vapor deposition vacuum device The pressure is 200Pa, and under the pressure of 200Pa and argon atmosphere, the temperature is raised to 700°C within 25min;
三、通入氧气，调节氧气的气体流量为10sccm，调节氩气的气体流量为50sccm，调节等离子体增强化学气相沉积真空装置中压强为400Pa，然后在射频功率为200W、压强为400Pa和温度为700℃条件下进行沉积，沉积时间为45min，沉积结束后，关闭射频电源和加热电源，停止通入氧气，在氩气气氛下从温度为700℃冷却至室温，即得到纳米片结构的氧化钴电极。Three, feed oxygen, adjust the gas flow of oxygen to be 10sccm, adjust the gas flow of argon to be 50sccm, adjust the pressure in the plasma-enhanced chemical vapor deposition vacuum device to be 400Pa, then be 200W at the radio frequency power, the pressure is 400Pa and the temperature is Deposition was carried out at 700°C, and the deposition time was 45 minutes. After the deposition, turn off the radio frequency power supply and heating power supply, stop feeding oxygen, and cool down from 700°C to room temperature under an argon atmosphere to obtain cobalt oxide with a nanosheet structure. electrode.
图1为实施例制备的纳米片结构的氧化钴电极材料的扫描电镜图；从图中可以看出纳米片结构的氧化钴在Si基底表面分布均匀、密度适中，其垂直于Si基底生长，呈独特的片层结构。Fig. 1 is the scanning electron micrograph of the cobalt oxide electrode material of the nanosheet structure prepared by the embodiment; As can be seen from the figure, the cobalt oxide of the nanosheet structure is uniformly distributed on the surface of the Si substrate, and the density is moderate, and it grows perpendicular to the Si substrate, showing a Unique lamellar structure.
图2为循环伏安曲线图，1为扫速为50mV/s时实施例制备的纳米片结构的氧化钴电极的循环伏安曲线图，2为扫速为20mV/s时实施例制备的纳米片结构的氧化钴电极的循环伏安曲线图，3为扫速为10mV/s时实施例制备的纳米片结构的氧化钴电极的循环伏安曲线图。从图中可知，纳米片结构的氧化钴具有优异的电化学性能，其比电容在10mV/s扫速条件下高达450μF/cm2。Fig. 2 is a cyclic voltammetry curve, 1 is the cyclic voltammetry curve of the cobalt oxide electrode of the nanosheet structure prepared by the embodiment when the scan rate is 50mV/s, and 2 is the nanometer electrode prepared by the embodiment when the scan rate is 20mV/s. 3 is the cyclic voltammetry curve of the cobalt oxide electrode with the sheet structure, and 3 is the cyclic voltammetry curve of the cobalt oxide electrode with the nanosheet structure prepared in the embodiment when the scan rate is 10 mV/s. It can be seen from the figure that cobalt oxide with nanosheet structure has excellent electrochemical properties, and its specific capacitance is as high as 450 μF/cm 2 under the condition of 10 mV/s scan rate.
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