CN113193206A - 一种乙醇燃料电池阳极催化剂的制备方法 - Google Patents
一种乙醇燃料电池阳极催化剂的制备方法 Download PDFInfo
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000003054 catalyst Substances 0.000 title claims abstract description 48
- 239000000446 fuel Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 65
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 37
- 239000004744 fabric Substances 0.000 claims abstract description 37
- 238000004070 electrodeposition Methods 0.000 claims abstract description 28
- 239000003792 electrolyte Substances 0.000 claims abstract description 26
- 239000007810 chemical reaction solvent Substances 0.000 claims abstract description 19
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 19
- 229910001451 bismuth ion Inorganic materials 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- -1 palladium ions Chemical class 0.000 claims abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- 229910001152 Bi alloy Inorganic materials 0.000 claims abstract description 10
- 239000002105 nanoparticle Substances 0.000 claims abstract description 10
- 238000005520 cutting process Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 150000001621 bismuth Chemical class 0.000 claims abstract description 7
- 150000002940 palladium Chemical class 0.000 claims abstract description 7
- 230000003647 oxidation Effects 0.000 claims abstract description 6
- 238000000970 chrono-amperometry Methods 0.000 claims abstract description 5
- 238000006056 electrooxidation reaction Methods 0.000 claims abstract description 4
- 238000006722 reduction reaction Methods 0.000 claims abstract description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical group OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- LXXVRAOHTIEOQW-UHFFFAOYSA-K [Bi+3].CC(C)(C)CCCCCCCC([O-])=O.CC(C)(C)CCCCCCCC([O-])=O.CC(C)(C)CCCCCCCC([O-])=O Chemical compound [Bi+3].CC(C)(C)CCCCCCCC([O-])=O.CC(C)(C)CCCCCCCC([O-])=O.CC(C)(C)CCCCCCCC([O-])=O LXXVRAOHTIEOQW-UHFFFAOYSA-K 0.000 claims description 5
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 3
- 239000002082 metal nanoparticle Substances 0.000 abstract description 3
- 230000006911 nucleation Effects 0.000 abstract description 3
- 238000010899 nucleation Methods 0.000 abstract description 3
- 239000002659 electrodeposit Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 12
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000009210 therapy by ultrasound Methods 0.000 description 8
- 229960001484 edetic acid Drugs 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 5
- 238000000151 deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 239000010411 electrocatalyst Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000033116 oxidation-reduction process Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 101100116420 Aedes aegypti DEFC gene Proteins 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
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- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
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- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8853—Electrodeposition
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- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
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- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
- H01M4/905—Metals or alloys specially used in fuel cell operating at high temperature, e.g. SOFC
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- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
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Abstract
本发明提供了一种乙醇燃料电池阳极催化剂的制备方法,包括如下步骤:S10将一定量的表面活性剂溶于去离子水中获得反应溶剂;S20将前驱体钯盐和前驱体铋盐按照预设摩尔比溶于反应溶剂中,得到电解液;S30裁取一定面积的导电碳布;S40在一定电位,一定时间下,利用计时电流法,将电解液中的钯离子和铋离子电沉积氧化还原到导电碳布上,得到负载PdnBi合金纳米颗粒的导电碳布PdnBi/CC,PdnBi/CC为乙醇燃料电池阳极催化剂。本发明的一种乙醇燃料电池阳极催化剂的制备方法,使用电沉积方法将钯离子和铋离子电沉积氧化还原到导电碳布上,得到乙醇燃料电池阳极催化剂,整体制备方法简单,且易于控制不同尺寸、形状和分布的金属纳米粒子的形核和生长。
Description
技术领域
本发明涉及新能源技术领域,具体涉及一种乙醇燃料电池阳极催化剂的制备方法。
背景技术
直接乙醇燃料电池(Direct ethanol fuel cells,DEFCs)是将乙醇液体燃料的化学能直接转变成电能的电化学反应装置。为了得到理想的电池性能,目前多采用Pt基电催化剂。但是,Pt的自然储量有限,而且由于工业上的广泛应用,其价格越来越昂贵。降低Pt用量的最好办法是寻找替代材料,这不仅能减少燃料电池对Pt的依赖性,而且能降低成本从而促进DEFC的商业化进程。钯不仅价格比铂低廉,储量相对丰富,而且在低温燃料电池、电解和传感器等电化学领域显示了独特的性能,使得其有望成为铂的替用材料。
然而从燃料电池的角度考虑,价格并不是Pd能替代Pt的主要原因。其真正的吸引力在于Pd在碱性环境中,具有优于Pt基电催化剂的性能,但是,在碱性环境中,阳极和阴极均能使用非Pt催化剂,如果对Pd进行掺杂或修饰使之活性增加,且能稳定地催化醇类氧化,将极大地推动该类催化剂在直接乙醇醇燃料电池中应用。
发明内容
为了解决上述问题,本发明提供一种乙醇燃料电池阳极催化剂的制备方法,使用电沉积方法将钯离子和铋离子电沉积氧化还原到导电碳布上,得到负载PdnBi合金纳米颗粒的导电碳布PdnBi/CC,PdnBi/CC即乙醇燃料电池阳极催化剂,整体制备方法简单,且易于控制不同尺寸、形状和分布的金属纳米粒子的形核和生长。
为了实现以上目的,本发明采取的一种技术方案是:
一种乙醇燃料电池阳极催化剂的制备方法,包括如下步骤:S10将一定量的表面活性剂溶于去离子水中获得反应溶剂;S20将前驱体钯盐和前驱体铋盐按照预设摩尔比溶于反应溶剂中,得到电解液;S30裁取一定面积的导电碳布;S40在一定电位,一定时间下,利用计时电流法,将电解液中的钯离子和铋离子电沉积氧化还原到导电碳布上,得到负载PdnBi合金纳米颗粒的导电碳布即PdnBi/carbon cloth(PdnBi/CC),PdnBi/CC为乙醇燃料电池阳极催化剂,其中n为[0.5,10]。
进一步地,表面活性剂为乙二胺四乙酸(EDTA),反应溶剂中EDTA的浓度不小于0.5mol/L。
进一步地,电解液中钯离子的浓度为0.02-0.08mol/L,铋离子的浓度为0.02-0.08mol/L。
进一步地,电解液中钯离子与铋离子的摩尔比为(0.5-10):1。
进一步地,前驱体钯盐为氯钯酸或氯亚钯酸钾中的至少一种。
进一步地,前驱体铋盐为新十二酸铋或五水硝酸铋中的至少一种。
进一步地,步骤S40中电沉积所需固定电位为-0.297V,电沉积所需时间为100-5000s。
本发明的上述技术方案相比现有技术具有以下优点:
(1)本发明的一种乙醇燃料电池阳极催化剂的制备方法,使用电沉积方法将钯离子和铋离子电沉积氧化还原到导电碳布上,得到负载PdnBi合金纳米颗粒的导电碳布PdnBi/CC,PdnBi/CC即乙醇燃料电池阳极催化剂,整体制备方法简单,且易于控制不同尺寸、形状和分布的金属纳米粒子的形核和生长。
(2)本发明的一种乙醇燃料电池阳极催化剂的制备方法,通过电沉积发获得的阳极催化剂能通过两种金属的协同作用,提高CO的抗毒性,最终提高阳极催化剂在催化乙醇氧化上的活性和稳定性。
附图说明
下面结合附图,通过对本发明的具体实施方式详细描述,将使本发明的技术方案及其有益效果显而易见。
图1所示为本发明一实施例的乙醇燃料电池阳极催化剂的制备方法流程图;
图2所示为本发明一实施例的乙醇燃料电池阳极催化剂的扫描电子显微镜图;
图3所示为本发明一实施例的乙醇燃料电池阳极催化剂的X射线衍射图;
图4所示为本发明一实施例的乙醇燃料电池阳极催化剂的X射线光电子能谱图;
图5所示为本发明实施例1与实施例4获得的乙醇燃料电池阳极催化剂的乙醇氧化反应催化活性循环伏安曲线;
图6所示为本发明实施例1与实施例4获得的乙醇燃料电池阳极催化剂乙醇氧化反应催化活性计时电流曲线。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
本实施例提供了一种乙醇燃料电池阳极催化剂的制备方法,如图1~4所示,包括如下步骤:S10将一定量的表面活性剂溶于去离子水中获得反应溶剂。S20将前驱体钯盐和前驱体铋盐按照预设摩尔比溶于反应溶剂中,得到电解液;S30裁取一定面积的导电碳布;S40在一定电位,一定时间下,利用计时电流法,将电解液中的钯离子和铋离子电沉积氧化还原到导电碳布上,得到负载PdnBi合金纳米颗粒的导电碳布即PdnBi/carbon cloth(PdnBi/CC),PdnBi/CC为乙醇燃料电池阳极催化剂,其中n为[0.5,10]。
步骤S10中,表面活性剂为乙二胺四乙酸(EDTA),反应溶剂中EDTA的浓度不小于0.5mol/L。
步骤S20中,电解液中钯离子的浓度为0.02-0.08mol/L,铋离子的浓度为0.02-0.08mol/L,电解液中钯离子与铋离子的摩尔比为(0.5-10):1。前驱体钯盐为氯钯酸或氯亚钯酸钾中的至少一种,前驱体铋盐为新十二酸铋或五水硝酸铋中的至少一种。
步骤S40中电沉积所需固定电位为-0.297V,电沉积所需时间为100-5000s。
实施例1
乙醇燃料电池阳极催化剂的制备方法,包括如下步骤
S10将1.46g的表面活性剂溶于100mL的去离子水中超声30min,获得反应溶剂;
S20将摩尔比为5:1的氯钯酸与五水合硝酸铋溶于50mL反应溶剂中,超声30min,得到电解液,其中,电解液中,钯离子和铋离子的浓度均为0.02mol/L;
S30裁取2cm×2cm的导电碳布;
S40搭建三电极体系,将导电碳布固定在工作电极上,并浸没于电解液中,通过计时电流法进行电沉积。电沉积所需固定电位为-0.297V(相对于饱和甘汞电极,SCE),沉积时间为2000s,清洗电沉积后的导电碳布并晾干,获得具有Pd5Bi合金纳米颗粒的导电碳布,即Pd5Bi/CC。
通过扫描电子显微镜(SEM)对实施例1获得的乙醇燃料电池阳极催化剂进行观察,如图2所示,乙醇燃料电池阳极催化剂形貌为颗粒状结构,***有棱边。
将乙醇燃料电池阳极催化剂利用X射线衍射仪进行扫描,结果如图3所示,可以看出,所有XRD光谱峰均对应Pd的面心立方相(JCPDF,46-1043),其中,衍射峰2θ=43.4°,52.9°和78.9°可以被索引为纯Pd的(111)、(200)和(311)面。
进一步采用X射线光电子能谱检测乙醇燃料电池阳极催化剂中Bi的组分价态,如图4所示,对于Bi元素来说,在159.6eV和164.7eV处出现一对峰图谱,这可以归因于Bi(OH)3的存在,因此,可以证明上述制备出Bi(OH)3修饰的Pd纳米颗粒,即为Pd5Bi/CC催化剂。
乙醇氧化反应(EOR)催化活性测试:
(1)EOR测试
在Ar饱和的1mol/L NaOH+1mol/L C2H5OH中以50mV/s的扫描速率进行EOR测试。在含1mol/L C2H5OH的1mol/L NaOH溶液中,在-0.2V(相对于饱和甘汞电极,SCE),用计时安培法测定制备样品的长期稳定性。为了进行比较,此处将Pd/CC催化剂采用同样制备步骤和测试方法。
实施例1所得的Pd5Bi/CC催化剂的EOR性能通过采用晨华CHI660e工作站,在三极电池体系中进行测试。在三电极体系中,以饱和甘汞电极和Pt网分别作为参比电极和对电极。
图5为实施例1的Pd5Bi/CC催化剂催化剂在含1mol/L C2H5OH的1mol/LNaOH溶液中,电位范围-0.8V~0.2V(相对于饱和甘汞电极,SCE),扫速为50mV/s的循环伏安曲线。从图5可得出,Pd5Bi/CC催化剂的EOR活性为23.54mA cm-2,而相比之下,Pd/CC催化剂的活性仅有8.07mA cm-2。
图6为实施例1的Pd5Bi/CC催化剂在含1mol/L C2H5OH的1mol/L NaOH溶液中,电位-0.2V(相对于饱和甘汞电极,SCE)条件下,3600s后电位变化情况。从图6可以得出,3600s稳定性测试后,Pd5Bi/CC催化剂活性下降了70%。相比之下,Pd/CC,3600s稳定性测试后,活性下降了90%,活性几乎趋近于0,即失去活性。
实施例2
乙醇燃料电池阳极催化剂的制备方法,包括如下步骤
S10将1.46g的表面活性剂溶于100mL的去离子水中超声30min,获得反应溶剂;
S20将摩尔比为10:1的氯亚钯酸钾与五水合硝酸铋溶于50mL反应溶剂中,超声30min,得到电解液;
S30裁取2cm×2cm的导电碳布;
S40搭建三电极体系,将导电碳布固定在工作电极上,并浸没于电解液中,通过计时电流法进行电沉积。电沉积所需固定电位为-0.297V(相对于饱和甘汞电极,SCE),沉积时间为2000s,清洗电沉积后的导电碳布并晾干,获得具有Pd10Bi合金纳米颗粒的导电碳布,即Pd10Bi/CC。
实施例3
乙醇燃料电池阳极催化剂的制备方法,包括如下步骤
S10将1.46g的表面活性剂溶于100mL的去离子水中超声30min,获得反应溶剂;
S20将摩尔比5:1的氯亚钯酸钾与新十二酸铋溶于50mL反应溶剂中,超声30min,得到电解液,其中,电解液中,钯离子和铋离子的浓度均为0.08mol/L;
S30裁取2cm×2cm的导电碳布;
S40搭建三电极体系,将导电碳布固定在工作电极上,并浸没于电解液中,通过计时电流法进行电沉积。电沉积所需固定电位为-0.297V(相对于饱和甘汞电极,SCE),沉积时间为100s,清洗电沉积后的导电碳布并晾干,获得具有Pd5Bi合金纳米颗粒的导电碳布,即Pd5Bi/CC。
实施例4
乙醇燃料电池阳极催化剂的制备方法,包括如下步骤
S10将1.46g的表面活性剂溶于100mL的去离子水中超声30min,获得反应溶剂;
S20将摩尔比0.5:1的氯钯酸与新十二酸铋溶于50mL反应溶剂中,超声30min,得到电解液,其中,电解液中,钯离子和铋离子的浓度均为0.08mol/L;
S30裁取2cm×2cm的导电碳布;
S40搭建三电极体系,将导电碳布固定在工作电极上,并浸没于电解液中,通过计时电流法进行电沉积。电沉积所需固定电位为-0.297V(相对于饱和甘汞电极,SCE),沉积时间为5000s,清洗电沉积后的导电碳布并晾干,获得具有Pd0.5Bi合金纳米颗粒的导电碳布,即Pd0.5Bi/CC。
以上所述仅为本发明的示例性实施例,并非因此限制本发明专利保护范围,凡是利用本发明说明书及附图内容所作的等效结构或等效流程变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的专利保护范围内。
Claims (7)
1.一种乙醇燃料电池阳极催化剂的制备方法,其特征在于,包括如下步骤
S10将一定量的表面活性剂溶于去离子水中获得反应溶剂;
S20将前驱体钯盐和前驱体铋盐按照预设摩尔比溶于反应溶剂中,得到电解液;
S30裁取一定面积的导电碳布;
S40在一定电位,一定时间下,利用计时电流法,将电解液中的钯离子和铋离子电沉积氧化还原到导电碳布上,得到负载PdnBi合金纳米颗粒的导电碳布即PdnBi/carbon cloth(PdnBi/CC),PdnBi/CC为乙醇燃料电池阳极催化剂,其中n为[0.5,10]。
2.根据权利要求1所述的乙醇燃料电池阳极催化剂的制备方法,其特征在于,表面活性剂为乙二胺四乙酸(EDTA),反应溶剂中EDTA的浓度不小于0.5mol/L。
3.根据权利要求1所述的乙醇燃料电池阳极催化剂的制备方法,其特征在于,电解液中钯离子的浓度为0.02-0.08mol/L,铋离子的浓度为0.02-0.08mol/L。
4.根据权利要求1所述的乙醇燃料电池阳极催化剂的制备方法,其特征在于,电解液中钯离子与铋离子的摩尔比为(0.5-10):1。
5.根据权利要求1所述的乙醇燃料电池阳极催化剂的制备方法,其特征在于,前驱体钯盐为氯钯酸或氯亚钯酸钾中的至少一种。
6.根据权利要求1所述的乙醇燃料电池阳极催化剂的制备方法,其特征在于,前驱体铋盐为新十二酸铋或五水硝酸铋中的至少一种。
7.根据权利要求1所述的乙醇燃料电池阳极催化剂的制备方法,其特征在于,步骤S40中电沉积所需固定电位为-0.297V,电沉积所需时间为100-5000s。
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