CN104810165A - 一种制备磷化镍/石墨烯复合薄膜材料的方法 - Google Patents
一种制备磷化镍/石墨烯复合薄膜材料的方法 Download PDFInfo
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 40
- FBMUYWXYWIZLNE-UHFFFAOYSA-N nickel phosphide Chemical compound [Ni]=P#[Ni] FBMUYWXYWIZLNE-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 79
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 35
- 239000006185 dispersion Substances 0.000 claims abstract description 26
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000006260 foam Substances 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 30
- 239000010409 thin film Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000007970 homogeneous dispersion Substances 0.000 claims description 7
- 239000011159 matrix material Substances 0.000 claims description 5
- 229910001453 nickel ion Inorganic materials 0.000 claims description 2
- -1 phosphonium ion Chemical class 0.000 claims 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000002791 soaking Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 6
- 238000009413 insulation Methods 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 239000007772 electrode material Substances 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229910000314 transition metal oxide Inorganic materials 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000002322 conducting polymer Substances 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910001463 metal phosphate Inorganic materials 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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Abstract
本发明公开了一种制备磷化镍/石墨烯复合薄膜材料的方法。首先在超声作用下，将氧化石墨烯和红磷分散在去离子水中制得分散液，然后将分散液转移到水热釜中，并将金属镍基体（泡沫镍、镍片或镍网）浸入分散液，水热反应后得到磷化镍/石墨烯复合薄膜材料。该制备方法简单易行，合成条件温和，材料成本低且易于大规模生产和利用。
Description
技术领域
本发明涉及一种制备磷化镍/石墨烯复合薄膜材料的方法，特别涉及一种储能（超级电容器、电池）电极材料的制备方法。
背景技术
近年来，能源危机和环境污染已经成为全球性的难题，为了实现社会的可持续发展，新能源（太阳能，风能，潮汐能等）的开发和利用得到了广泛的关注。伴随着新能源的发展，我们对储能设备的要求也越来越高。
作为一种新型储能设备，超级电容器具有功率密度高、循环寿命长、充放电快等优点，被广泛应用于计算机、消费电子、电动汽车、航空航天等领域。超级电容器的电极材料主要有碳基材料（活性炭、介孔碳、碳纳米管等），过渡金属氧化物或氢氧化物（RuO2、MnO2、NiO2、Ni(OH)2等），导电聚合物等。其中，碳基材料比表面积大、双电层间距小及循环寿命高，但放电容量较低。导电聚合物价格低廉，但材料的热稳定性、化学稳定性以及充放电的可循环性较差。过渡金属氧化物或氢氧化物为赝电容储存机理，比电容量大，但导电性差，循环稳定性不佳。因此，寻找一种兼具高容量和良好循环稳定性的复合电极材料成为超级电容器发展的关键。
目前，石墨烯与过渡金属氧化物的复合材料被广泛研究。近期研究发现过渡金属磷化物有类金属性质，更适合做超级电容器的电极材料。目前过渡金属磷化物的合成方法主要有溶剂热反应法、单一有机金属前驱体的热分解法、纳米级金属磷酸盐前体的高温热分解法、金属或金属氧化物纳米粒子被PH3/H2还原等。但是这些方法大都利用金属纳米粒子作为反应物，且反应温度高，反应条件苛刻；得到的产物主要为粉体材料。
发明内容
为了克服上述方法的不足，本发明采用一种简单的水热法，以金属镍基体（泡沫镍、镍片或镍网）作为镍源，红磷作为磷源，与石墨烯复合生成磷化镍/石墨烯复合薄膜材料。制备方法简单易行，合成条件温和，材料成本低且易于大规模生产和利用。
本发明的技术解决方案如下：
以泡沫镍、镍片或镍网为镍源，红磷为磷源，利用水热法制备磷化镍/石墨烯复合薄膜材料的方法，包括如下步骤：
(1) 称取一定量氧化石墨烯，加入到去离子水中，超声分散，形成氧化石墨烯均一分散液；
(2) 称取一定量的红磷加入步骤（1）制得的分散液中，超声分散0.5~2小时，形成红磷和氧化石墨烯的分散液；
(3) 将步骤（2）制得的分散液加入到水热釜中，并将金属镍基体（泡沫镍、镍片或镍网)浸入分散液中，在150-210℃条件下水热反应12~36小时；
(4) 将反应结束后的以镍基体为载体的磷化镍/石墨烯复合薄膜材料在去离子水中清洗，干燥，保存待用。
所述的制备磷化镍/石墨烯复合薄膜材料的方法，其特征在于氧化石墨烯和红磷的质量比为1:5~5:1。
所述的制备磷化镍/石墨烯复合薄膜材料的方法，其特征在于磷化镍包括磷化二镍、二磷化三镍、二磷化镍、三磷化镍等。
本发明利用金属镍基体（泡沫镍、镍片或镍网）作为制备磷化镍/石墨烯复合薄膜材料的载体和镍离子源，红磷作为磷源，成功合成出磷化镍/石墨烯复合薄膜材料。该实验方法简单易控，容易实现规模化生产。
附图说明
图1为实施例1中制备的磷化镍/石墨烯复合薄膜材料的扫描电子显微镜（SEM）图片。
图2为实施例3中制备的磷化镍/石墨烯复合薄膜材料的扫描电子显微镜（SEM）图片。
具体实施方式
下面结合实施例对本发明做进一步说明，但本发明的保护范围并不限于此。
实施例 1
称取31 mg氧化石墨烯，加入到30 mL的去离子水中，超声分散形成均一分散液，然后称取31 mg红磷溶于上述分散液中，超声2小时。将氧化石墨烯和红磷的分散液加入到水热釜的聚四氟乙烯内衬中，将1×2 cm2的泡沫镍浸入分散液中，拧紧不锈钢外套后置于180℃下保温12小时。对产物进行洗涤，干燥，保存待用。制备的磷化镍/石墨烯如附图1所示。
实施例 2
称取31 mg氧化石墨烯，加入到30 mL的去离子水中，超声分散形成均一分散液，然后称取15.5 mg红磷溶于上述分散液中，超声1小时。将氧化石墨烯和红磷的分散液加入到水热釜的聚四氟乙烯内衬中，将1×2 cm2的泡沫镍浸入分散液中，拧紧不锈钢外套后置于210℃下保温24小时。对产物进行洗涤，干燥，保存待用。
实施例 3
称取40 mg氧化石墨烯，加入到30 mL的去离子水中，超声分散形成均一分散液，然后称取8 mg红磷溶于上述分散液中，超声0.5小时。将氧化石墨烯和红磷的分散液加入到水热釜的聚四氟乙烯内衬中，将1×2 cm2的泡沫镍浸入分散液中，拧紧不锈钢外套后置于150℃下保温36小时。对产物进行洗涤，干燥，保存待用。制备的磷化镍/石墨烯如附图2所示。
实施例 4
称取8 mg氧化石墨烯，加入到30 mL的去离子水中，超声分散形成均一分散液，然后称取40 mg红磷溶于上述分散液中，超声1小时。将氧化石墨烯和红磷的分散液加入到水热釜的聚四氟乙烯内衬中，将1× 2 cm2的泡沫镍浸入分散液中，拧紧不锈钢外套后置于180℃下保温24小时。对产物进行洗涤，干燥，保存待用。
实施例 5
称取24 mg氧化石墨烯，加入到30 mL的去离子水中，超声分散形成均一分散液，然后称取40 mg红磷溶于上述分散液中，超声1小时。将氧化石墨烯和红磷的分散液加入到水热釜的聚四氟乙烯内衬中，将1× 2 cm2的泡沫镍浸入分散液中，拧紧不锈钢外套后置于210℃下保温12小时。对产物进行洗涤，干燥，保存待用。
Claims (4)
1.一种制备磷化镍/石墨烯复合薄膜材料的方法，其特征在于包括如下步骤：
称取一定量氧化石墨烯，加入到去离子水中，超声分散，形成氧化石墨烯均一分散液；
称取一定量红磷，加入到步骤（1）制得的分散液中，超声分散0.5~2小时，形成红磷和氧化石墨烯的分散液；
将步骤（2）制得的分散液加入到水热釜中，并将金属镍基体（泡沫镍、镍片或镍网)浸入分散液中，在150-210℃条件下水热反应12~36小时；
将反应结束后的以镍基体为载体的磷化镍/石墨烯复合薄膜材料在去离子水中清洗，干燥，保存待用。
2.根据权利要求1所述的方法，其特征在于，金属镍基体（泡沫镍、镍片或镍网）作为制备磷化镍/石墨烯复合薄膜材料的载体和镍离子源，红磷作为磷离子源。
3.根据权利要求1所述的方法，其特征在于，氧化石墨烯和红磷的质量比为1:5~5:1。
4.根据权利要求1和2所述的方法，其特征在于，磷化镍包括磷化二镍、二磷化三镍、二磷化镍、三磷化镍等。
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105926021A (zh) * | 2016-03-24 | 2016-09-07 | 西北师范大学 | 一种磷化镍纳米薄膜及其制备方法和应用 |
| CN106964381A (zh) * | 2017-03-02 | 2017-07-21 | 西北大学 | 一种高浓度纳米红磷光催化剂分散液的制备方法 |
| CN107715898A (zh) * | 2017-10-11 | 2018-02-23 | 肇庆市华师大光电产业研究院 | 一种氧化石墨烯/红磷复合材料及其制备方法与应用 |
| CN108671947A (zh) * | 2018-04-11 | 2018-10-19 | 西安石油大学 | 用于生物油加氢脱氧反应的Ni2P/还原氧化石墨烯催化剂及其制备方法 |
| CN108864636A (zh) * | 2018-08-08 | 2018-11-23 | 燕山大学 | 一种磷化镍/氟化石墨烯-聚四氟乙烯复合材料及其制备方法和应用 |
| CN109894129A (zh) * | 2019-04-15 | 2019-06-18 | 内蒙古大学 | 一种Ni2P负载石墨烯泡沫结构催化剂的制备方法及其应用 |
| CN110183589A (zh) * | 2019-05-24 | 2019-08-30 | 燕山大学 | 聚酯树脂/聚四氟乙烯-苄氯-二乙烯三胺-氧化石墨/磷化镍复合摩擦材料的制备方法 |
| CN110952112A (zh) * | 2019-12-24 | 2020-04-03 | 济南大学 | 一种石墨烯外层@磷化镍夹层@镍内层框架复合材料及其制备方法和应用 |
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