CN110560068A - 一种具有颗粒状镍、铁、钴三元金属氢氧化物高性能析氧催化剂的制备方法 - Google Patents
一种具有颗粒状镍、铁、钴三元金属氢氧化物高性能析氧催化剂的制备方法 Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 45
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 23
- 229910000000 metal hydroxide Inorganic materials 0.000 title claims abstract description 23
- 150000004692 metal hydroxides Chemical class 0.000 title claims abstract description 23
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 22
- 239000010941 cobalt Substances 0.000 title claims abstract description 22
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000001301 oxygen Substances 0.000 title claims abstract description 22
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 22
- 239000003054 catalyst Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 12
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims abstract description 6
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 239000011734 sodium Substances 0.000 claims abstract description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001308 synthesis method Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 238000000840 electrochemical analysis Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000010411 electrocatalyst Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- KGWWEXORQXHJJQ-UHFFFAOYSA-N [Fe].[Co].[Ni] Chemical compound [Fe].[Co].[Ni] KGWWEXORQXHJJQ-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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Abstract
本发明涉一种具有颗粒状镍、铁、钴三元金属氢氧化物高性能析氧催化剂的制备方法，具体涉及一种利用水热法法一步合成，其具体制备工艺为：称取5.463g硝酸镍(H12N2NiO12)和2.517g硝酸铁(H18FeN3O18)以及0.604g硝酸钴(CoH12N2O12)溶于30mL去离子水中，将2.304g氢氧化钠(NaOH)和2.544g碳酸钠(Na2CO3)溶于30mL去离子水中，后将两种溶液混合剧烈搅拌后，在70－90℃温度范围内，水热条件下反应48h，将得到的沉淀离心，在60℃下干燥24h。所得到的具有具有颗粒状镍、铁、钴三元金属氢氧化物析氧催化剂具有析氧活性高，导电性好，碱性条件下稳定性高等优点。本发明材料制备方法简易，设备简单；原材料价格低廉，重复性好。
Description
技术领域
本发明涉及一种具有颗粒状镍、铁、钴三元金属氢氧化物高性能析氧催化剂的制备方法，具体涉及一种利用水热法合成暴露更多活性位点的颗粒状镍、铁、钴三元金属氢氧化物高性能析氧催化剂的方法，所得到的颗粒状镍、铁、钴三元金属氢氧化物高性能析氧催化剂具有析氧催化活性高，导电性好，碱性条件下稳定性高等优点。
背景技术
具有比表面积大、暴露的活性位点多等特点的高效的催化剂是可以降低过电位的材料，其在燃料电池、太阳能电池、金属空气电池以及生产清洁氢燃料等方面有重要的应用。
近年来，基于非贵金属的过渡金属(Ni，Fe，Co，)化合物和合金由于其优异的理论催化性能，环境友好性和丰富的来源，成为水分解的有效催化剂，并且被认定为催化活性中心。过渡金属氢氧化物因其成本低廉和来源丰富而在电催化领域获得了很多研究兴趣，除此之外，在酸碱介质中还具有良好的稳定性。设计和合成可以暴露更多活性位点的高效催化剂显得尤为重要。
镍、铁、钴金属元素作为典型的电催化剂材料，由于成本低廉和来源丰富在电催化析氧领域方面被广泛研究。通过一步水热法制备镍、铁、钴三元金属氢氧化物，因其结构单元是由细小颗粒能够提供更多的活性位点使得电催化活性显著增强。因此，颗粒状镍、铁、钴三元金属氢氧化物电催化剂在析氧反应中具有很大优势。
对于颗粒堆状镍、铁、钴三元金属氢氧化物电催化剂而言，具有更丰富的活性中心，这在设计电化学析氧反应方面具有明显优势。到目前为止，通过水热法合成具有颗粒状镍、铁、钴三元金属氢氧化物高性能析氧催化剂的制备方法未见报道。
发明内容
本发明涉及一种具有颗粒状镍、铁、钴三元金属氢氧化物高性能析氧催化剂的制备方法，具体涉及一种利用水热法一步合成，所得到镍、铁、钴三元金属氢氧化物催化剂具有析氧活性高，导电性好，碱性条件下稳定性高等优点，且易于批量生产。
本发明先通过一步水热法制备具有颗粒状镍、铁、钴三元金属氢氧化物高性能析氧催化剂，其具体制备工艺为：
称取5.463g硝酸镍(H12N2NiO12)和2.517g硝酸铁(H18FeN3O18)以及0.604g硝酸钴(CoH12N2O12)溶于30mL去离子水中，将2.304g氢氧化钠(NaOH)和2.544g碳酸钠(Na2CO3)溶于30mL去离子水中，后将两种溶液混合剧烈搅拌后，在80℃水热条件下反应48h，将得到的沉淀离心，在60℃下干燥24h。
本发明所涉及产品工艺简单易实现，产品质量稳定且工艺重复性能好，反应参数容易控制、安全可靠、原材料廉价易得，以及易于放大和工业化生产等优点；所制备的细小颗粒堆积结构的镍铁钴三元金属氢氧化物电催化剂具有析氧活性高，导电性好，碱性条件下稳定性高等优点。
附图说明
图1为实施例1所示产物的扫描电铲(SEM)形貌照片；
具体实施方式
实施例1
称取5.463g硝酸镍(H12N2NiO12)和2.517g硝酸铁(H18FeN3O18)以及0.604g硝酸钴(CoH12N2O12)溶于30mL去离子水中，将2.304g氢氧化钠(NaOH)和2.544g碳酸钠(Na2CO3)溶于30mL去离子水中，后将两种溶液混合剧烈搅拌后，在80℃水热条件下反应48h，将得到的沉淀离心，在60℃下干燥24h。所得到的具颗粒状镍、铁、钴三元金属氢氧化物高性能析氧催化剂，暴露的活性位点较多，其电流密度达到10mA·cm-2时，过电位仅有230mV，Tafel斜率较小为72.7mV·dec-1。
实施例2
称取5.463g硝酸镍(H12N2NiO12)和2.517g硝酸铁(H18FeN3O18)以及0.604g硝酸钴(CoH12N2O12)溶于30mL去离子水中，将2.304g氢氧化钠(NaOH)和2.544g碳酸钠(Na2CO3)溶于30mL去离子水中，后将两种溶液混合剧烈搅拌，在70℃下反应48h，将得到的沉淀离心，在60℃下干燥24h。所得到的具颗粒状镍、铁、钴三元金属氢氧化物高性能析氧催化剂，暴露的活性位点较多，其电流密度达到10mA·cm-2时，过电位仅有230mV，Tafel斜率较小为72.7mV·dec-1。
实施例3
称取5.463g硝酸镍(H12N2NiO12)和2.517g硝酸铁(H18FeN3O18)以及0.604g硝酸钴(CoH12N2O12)溶于30mL去离子水中，将2.304g氢氧化钠(NaOH)和2.544g碳酸钠(Na2CO3)溶于30mL去离子水中，后将两种溶液混合剧烈搅拌，在90℃下反应48h，将得到的沉淀离心，在60℃下干燥24h。所得到的具颗粒状镍、铁、钴三元金属氢氧化物高性能析氧催化剂，暴露的活性位点较多，其电流密度达到10mA·cm-2时，过电位仅有230mV，Tafel斜率较小为72.7mV·dec-1。
从本发明制得的镍、铁、钴三元金属氢氧化物催化剂测试结果来看，本发明所得到的镍、铁、钴三元金属氢氧化物催化剂具有析氧活性高，导电性好，碱性条件下稳定性高等优点。
应当理解的是，对本领域普通技术人员来说，可以根据上述说明加以改进或变换，而所有这些改进和变换都应属于本发明所附权利要求的保护范围。
Claims (2)
1.本发明涉及一种具有颗粒状镍、铁、钴三元金属氢氧化物高性能析氧催化剂的制备方法，具体涉及一种利用一步水热法合成暴露活性位点更多的镍、铁、钴三元金属氢氧化物高性能析氧催化剂的方法，合成方法为：称取5.463g硝酸镍(H12N2NiO12)和2.517g硝酸铁(H18FeN3O18)以及0.604g硝酸钴(CoH12N2O12)溶于30mL去离子水中，将2.304g氢氧化钠(NaOH)和2.544g碳酸钠(Na2CO3)溶于30mL去离子水中，后将两种溶液混合剧烈搅拌后，在70－90℃温度范围内，水热条件下反应48h，将得到的沉淀离心，在60℃下干燥24h。
2.根据权利要求1所述的制备方法，所得到的具颗粒状镍、铁、钴三元金属氢氧化物高性能析氧催化剂，暴露的活性位点较多，电化学测试表明：其电流密度达到10mA·cm-2时，过电位仅有230mV，Tafel斜率较小为72.7mV·dec-1。
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| CN111437819A (zh) * | 2020-02-29 | 2020-07-24 | 北京工业大学 | 一种合成钴掺杂镍铁网状纳米片阵列高效双功能电催化剂的方法和应用 |
| CN115094457A (zh) * | 2022-08-04 | 2022-09-23 | 湖北大学 | 一种原位生长型复合过渡金属氧化物析氧催化电极材料及其制备方法和应用 |
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