CN107381515A - 一种氮化钒电催化剂的制备方法及产品 - Google Patents
一种氮化钒电催化剂的制备方法及产品 Download PDFInfo
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- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000003054 catalyst Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004202 carbamide Substances 0.000 claims abstract description 11
- 239000012535 impurity Substances 0.000 claims abstract description 11
- OQUOOEBLAKQCOP-UHFFFAOYSA-N nitric acid;hexahydrate Chemical compound O.O.O.O.O.O.O[N+]([O-])=O OQUOOEBLAKQCOP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000013049 sediment Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000000376 reactant Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 4
- 230000035484 reaction time Effects 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract 3
- 235000021110 pickles Nutrition 0.000 claims abstract 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000004570 mortar (masonry) Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 238000000643 oven drying Methods 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims 1
- 238000007654 immersion Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 229910000428 cobalt oxide Inorganic materials 0.000 description 7
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 7
- 229910052573 porcelain Inorganic materials 0.000 description 7
- 238000002791 soaking Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000011858 nanopowder Substances 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
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- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000001507 sample dispersion Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/0617—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with vanadium, niobium or tantalum
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B01J35/33—
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
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Abstract
本发明公开了一种氮化钒电催化剂的制备方法及产品,包括以下步骤:1)将尿素、偏钒酸铵、六水合硝酸钴按照配方比例充分混合,充分研磨,得到反应物原料;2)将步骤一制备的反应物原料于气氛保护下高温反应,反应温度700‑900℃,反应时间2‑5h,冷却后得到的粉体用稀酸液去除杂质,洗涤下层沉淀,干燥沉淀,充分研磨,得到氮化钒电催化剂。本发明制备的氮化钒电催化剂,具有工艺过程简单、反应周期短、材料化学组成均一、形貌尺寸均匀和电催化活性、稳定性高等特点。
Description
技术领域
本发明涉及氮化钒纳米粉体制备技术领域,具体涉及一种氮化钒电催化剂的制备方法及产品。
背景技术
随着全球经济的快速增长,能源问题和环境污染问题深深困扰着人类生活,人们急需寻找清洁可持续能源来解决这两大问题,而氢能作为新一代的绿色可持续能源,人们对其寄予厚望。水裂解技术是实现可持续制备氢气的有效途径之一,该技术的核心问题是开发高效、廉价的水裂解催化剂。目前,贵金属基催化剂(比如Pt,Ru或Ir的氧化物)是催化性能最好的水裂解催化剂,但是,价格昂贵、储量低的缺点极大地限制了该类催化剂的广泛应用,因此,开发由地壳含量丰富的廉价元素构成的高效水裂解催化剂是目前的研究热点。氮化钒(VN)具有较高的机械强度,电子传导率,耐腐蚀,稳定性高,在物理、化学、材料领域具有广泛的应用,是很有潜力的电催化材料,而氮化钒在电催化领域的应用国内还未见报导,因此制备纳米氮化钒粉体应用于电催化领域具有重要的意义。
申请号为CN101717076A的中国专利“一种氮化钒的制备方法”将含钒化合物与有机氮化物混合,在含氮气体中煅烧,得到氮化钒。该方法原料准备的工序较复杂,制备过程需要控制的参数多,应用于超级电容器材料制备领域。
申请号为CN104016314A的中国专利“一种氮化钒的制备方法”采用液相溶剂热法制备氮化钒,液相采用水溶液或醇类溶剂,钒源是钒的二价、三价或者四价氯化物、硫酸盐、硝酸盐以及醋酸盐,氮源是氨气、尿素、腈、氯化铵、碳酸铵、醋酸铵、硫酸铵。这种方法得到的氮化钒纳米粉体,制备工艺较复杂,应用于金属材料技术领域中的钢铁材料添加剂。
发明内容
本发明的目的在于提供一种氮化钒电催化剂的制备方法及产品,以克服现有技术存在的工艺复杂、氮化钒粉体尺寸大、电催化领域应用很少的缺陷。本发明通过一步法烧结得到工艺过程简单、反应周期短、材料化学组成均一、形貌尺寸均匀和电催化活性、稳定性高的氮化钒电催化剂。
为了达到上述目的,本发明采用如下技术方案:
一种氮化钒电催化剂的制备方法,包括以下步骤:
步骤一:将尿素、偏钒酸铵、六水合硝酸钴按照一定比例充分混合,三者质量比为10:(1-2):2,于研钵中研磨20~50min,得到反应物原料;
步骤二:将步骤一制备的反应物原料转移到瓷舟中,一定气氛下在管式炉中反应,温度范围为700-900℃,保温时间为2-5h,升温速率为5-10℃/min,冷却后得到的粉体用0.5M的H2SO4溶液浸泡10-20h(除去氧化钴等杂质),下层沉淀经过水洗醇洗交替共六次,于60℃烘箱干燥6-10 h后,研钵中研磨20~50min,得到氮化钒电催化剂。
上述步骤二中的一定气氛是指氩气、氮气、真空中的任意一种。
以及一种通过上述方法制备的氮化钒电催化剂,本发明制备的氮化钒电催化剂尺寸小于25nm,形貌均匀,分散性好。
与现有技术相比,本发明具有以下有益的技术效果:
1)本发明所使用的一步烧结法,工艺简单,耗时短,克服了被大量使用的前驱体法繁琐的缺陷;
2)六水合硝酸钴的引入促进了纯相氮化钒的低温合成;
3)各原料的反应活性高,提高了反应效率;
4)反应得到的纳米氮化钒粉体尺寸20nm左右,远小于所报道的文献上碳化钒粉体尺寸,并且其形貌均匀,分散性好;
5)该方法制备的纳米氮化钒粉体可被应用于电催化领域中的水裂解产氢电催化剂。
附图说明
图1为实施例1中制备的纳米氮化钒的XRD图;
图2为实施例4中制备的纳米氮化钒SEM图;
图3为实施例5中制备的纳米氮化钒LSV曲线图。
具体实施方式
下面结合附图及实施实例对本发明作进一步详细说明,应理解,这些实施例仅用于说明而不用于限制本发明的范围。此处应理解,在阅读了本发明授权的内容之后本领域技术人员可以对本发明做任何改动或修改,这些等价同样落于本申请所附权利要求书所限定的范围。
实施例1
步骤一:称取1.5g尿素,0.3g偏钒酸铵,0.3g六水合硝酸钴,充分混合研磨20min;
步骤二:将步骤一所得的原料放入瓷舟,在以氩气为气氛的管式炉中反应,升温速率为5℃/min,保温温度为700℃,保温时间为2h,冷却后得到的粉体用0.5M的H2SO4溶液浸泡10h(除去氧化钴等杂质),下层沉淀经过水洗醇洗交替共六次,于60℃烘箱干燥6h后,研钵中研磨20min,得到氮化钒电催化剂。
图1是本实施例所制备的纳米氮化钒的XRD图谱,从图中可以看出样品对应的标准PDF卡片号为78-1315 ,衍射峰尖锐,且强度高,说明该实施例得到的氮化钒纳米粉体结晶性很好。
实施例2
步骤一:称取1.5g尿素,0.3g偏钒酸铵,0.3g六水合硝酸钴,充分混合研磨40min;
步骤二:将步骤一所得的原料放入瓷舟,在以氮气为气氛的管式炉中反应,升温速率为8℃/min,保温温度为800℃,保温时间为5h,冷却后得到的粉体用0.5M的H2SO4溶液浸泡15h(除去氧化钴等杂质),下层沉淀经过水洗异丙醇洗交替共六次,于60℃烘箱干燥8h后,研钵中研磨30min,得到氮化钒电催化剂。
实施例3
步骤一:称取1.5g尿素,0.2g偏钒酸铵,0.3g六水合硝酸钴,充分混合研磨20min;
步骤二:将步骤一所得的原料放入瓷舟,在以氩气为气氛的管式炉中反应,升温速率为10℃/min,保温温度为900℃,保温时间为5h,冷却后得到的粉体用0.5M的H2SO4溶液浸泡20h(除去氧化钴等杂质),下层沉淀经过水洗甲醇洗交替共六次,于60℃烘箱干燥6 h后,研钵中研磨40min,得到氮化钒电催化剂。
实施例4
步骤一:称取1.5g尿素,0.2g偏钒酸铵,0.3g六水合硝酸钴,充分混合研磨20min;
步骤二:将步骤一所得的原料放入瓷舟,在以真空为气氛的管式炉中反应,升温速率为8℃/min,保温温度为900℃,保温时间为4h,冷却后得到的粉体用0.5M的H2SO4溶液浸泡15h(除去氧化钴等杂质),下层沉淀经过水洗醇洗交替共六次,于60℃烘箱干燥10 h后,研钵中研磨20min,得到氮化钒电催化剂。
图2是本实施例所制备的纳米氮化钒的SEM图,从图中可以看出样品形貌为小颗粒,颗粒粒径分布在20nm左右,颗粒间存在疏松的孔隙,样品分散性良好,孔隙由反应过程中反应物产生的气体造成。
实施例5
步骤一:称取1.5g尿素,0.15g偏钒酸铵,0.3g六水合硝酸钴,充分混合研磨20min;
步骤二:将步骤一所得的原料放入瓷舟,在以氩气为气氛的管式炉中反应,升温速率为5℃/min,保温温度为800℃,保温时间为2h,冷却后得到的粉体用0.5M的H2SO4溶液浸泡10h(除去氧化钴等杂质),下层沉淀经过水洗醇洗交替共六次,于60℃烘箱干燥6 h后,研钵中研磨40min,得到氮化钒电催化剂。
图3是本实施例所制备的纳米氮化钒的LSV图,表示pH 0测试条件下,当电流密度为10mA/cm2,扫描速率为3 mV/s时,该样品过电势为240mV,说明具有优异的催化活性。
实施例6
步骤一:称取1.5g尿素,0.15g偏钒酸铵,0.3g六水合硝酸钴,充分混合研磨50min;
步骤二:将步骤一所得的原料放入瓷舟,在以氮气为气氛的管式炉中反应,升温速率为10℃/min,保温温度为700℃,保温时间为2h,冷却后得到的粉体用0.5M的H2SO4溶液浸泡20h(除去氧化钴等杂质),下层沉淀经过水洗乙醇洗交替共六次,于60℃烘箱干燥10 h后,研钵中研磨50min,得到氮化钒电催化剂。
Claims (10)
1.一种氮化钒电催化剂的制备方法,其特征在于,包括以下步骤:
步骤一:将尿素、偏钒酸铵、六水合硝酸钴按照配方比例充分混合,充分研磨,得到反应物原料;
步骤二:将步骤一制备的反应物原料于气氛保护下高温反应,反应温度700-900℃,反应时间2-5h,冷却后得到的粉体用稀酸液去除杂质,洗涤下层沉淀,干燥沉淀,充分研磨,得到氮化钒电催化剂。
2.根据权利要求1所述的一种氮化钒电催化剂的制备方法,其特征在于,所述尿素、偏钒酸铵、六水合硝酸钴的质量比为10:(1-2):2。
3.根据权利要求1所述的一种氮化钒电催化剂的制备方法,其特征在于,所述步骤一、步骤二中的研磨,采用研钵对所得粉体充分研磨20~50min。
4.根据权利要求1所述的一种氮化钒电催化剂的制备方法,其特征在于,所述步骤二的气氛为氩气、氮气或者真空中的任意一种。
5.根据权利要求1所述的一种氮化钒电催化剂的制备方法,其特征在于,所述步骤二中的高温反应,以陶瓷作为样品载体。
6.根据权利要求1所述的一种氮化钒电催化剂的制备方法,其特征在于,所述步骤二中的高温反应,采用管式炉进行加热,升温速率5-10℃/min,反应温度700-900℃,反应时间2-5h。
7.根据权利要求1所述的一种氮化钒电催化剂的制备方法,其特征在于,所述步骤二中的用稀酸液去除杂质,以0.5M的H2SO4溶液浸泡10-20h去除杂质。
8.根据权利要求1所述的一种氮化钒电催化剂的制备方法,其特征在于,所述步骤二洗涤下层溶液,采用水洗与醇洗交替洗涤。
9.根据权利要求1所述的一种氮化钒电催化剂的制备方法,其特征在于,所述步骤二中对下层沉淀的干燥,于60℃烘箱干燥6-10 h。
10.一种通过权利要求1所述方法制备的氮化钒电催化剂,其特征在于,通过权利要求1所述方法制备,形貌均匀。
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