复合多相Pt基REOx载体膜电极的结构与析氢性能研究
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摘要
Pt基REOx载体膜电极是一类应用广泛的非均相析氢催化剂。目前,其在新能源、环境保护等高技术领域的应用开发,存在需要解决的关键科学技术问题有：核壳结构载体膜电极短流程制备新方法；载体膜电极材料与膜系类型、性价比以及使用能耗的综合调控；稀土(RE)助剂氧化程度以及电子转移途径对载体膜电极主相的助催化机制；载体膜电极制备因素对其结构及性能的综合调控等。
针对这些关键问题,选择Pt为载体膜电极主相,Cu为合金元素,稀土镧(La)、铈(Ce)的氧化物为助剂,石墨纤维布(GFC)、Si(111)单晶片、镍网为载体,稀H2S04溶液为析氢性能测试的化合物,采用含作者授权发明专利的离子束溅射沉积(IBSD)设备及后处理技术,制备长效高性价比低能耗的复合多相Pt基REOx载体膜电极。具体开展了四方面的研究工作：
(1)掺Cu与后处理对PtCu载体膜电极的影响研究；
(2)膜层体系对Pt基载体膜电极的影响研究；
(3) Pt-CeOx单层膜表面的Ce与Pt之间相互作用机制的研究：
(4) Pt-CeOx载体膜电极的IBSD制备工艺的影响研究。
通过上述工作,获得研究结论研究结论：
在PtCu载体膜电极含Cu量以及后处理工艺的影响研究方面,提出的"IBSD+真空热处理+酸蚀处理”短流程方法制备类核壳结构Pt基载体膜电极,该方法可调控载体膜电极表层的组分,避免中间产物的污染并降低能耗,易于在廉价制氢行业获得实际应用。研究结果包括：①IBSD制备的载体膜电极元素含量分布连续均匀,Cu含量增加促进表面晶粒细化,膜层组织均匀,增强Pt(111)择优生长。②载体膜电极经真空热处理(400℃、保温60min、真空度～10-5Pa)后,PtCu合金化程度最大(58.7%的Cu参与合金化),PtCu合金中Cu含量上升到54at.%,膜层晶粒仅发生微量长大。③载体膜电极经真空热处理与酸蚀处理(30min、50℃、0.50mol L-1的H2SO4溶液)后,均一组成的PtCu合金晶粒表层的Cu析出,晶粒表层富集Pt,且表层的Pt-Pt晶面间距下降6.33%,PtCu合金的平均晶粒粒径为6.67nm(降低了16%),平均比表面积增大250.2%。④经真空热处理的载体膜电极析氢活性增强11.6%,酸蚀处理可进一步提升13.4%,且析氢峰电位降低3%,综合析氢性能优异。
在膜层体系对Pt基载体膜电极的影响研究方面,在综合分析层状结构的膜层体系与真空热处理工艺的基础上,制备出具有实际使用价值的高性价比低能耗的复合Pt基载体膜电极。研究结果包括：①PtCuLa2O3系单层载体膜电极膜层晶粒细小均匀,增加La含量将增大Pt5La的平均原子体积收缩程度,增强载体膜电极的热稳定性及富氧能力。②PtCu/La2O3系双层载体膜电极中Pt(111)择优生长,La2O3/PtCu系双层载体膜电极中Pt晶粒明显细化。③PtCu/La2O3/PtCu系多层载体膜电极表面晶粒呈细小球状晶团且分布更均匀,经真空热处理后的含Pt量低于0.1mg·cm-2,电化学活性比表面积达到94.172m2·g-1,远高于单层及双层载体膜电极,在50℃析氢反应时,交换电流密度>200mA·cm-2,分解电压<0.63V,因此,复合层状结构的膜层体系以及真空热处理工艺是影响载体膜电极析氢性能和性价比的主要因素。
针对应用广泛且具有代表性的稀土Ce,本文通过测定表面原子结合能态的变化,直接表征界面上的电子转移途径,提出Pt-CeOx单层膜表面的Ce与Pt之间存在的相互作用机制为：Pt向Ce离子转移电子的过程中存在单电子转移与多电子激发；高价Ce离子通过Ce3+/Ce4+离子偶的氧化-还原循环形成流动的O空位,O空位向吸附的02分子提供电子使其还原为活性O2-及O-离子,促进了Pt之间的电子传递。
本研究还获得了IBSD制备工艺影响Pt-CeOx载体膜电极物相结构及析氢性能的研究结果：①载体膜电极存在CeO、Ce6O11和CeO2以及Pt2Ce和Pt5Ce物相,Pt(111)衍射峰位发生负移。②靶位移动距离以20mm为宜,过大或过小则明显减小载体膜电极的平均比表面积。③室温下制膜有利于Pt(111)择优生长,增强载体膜电极析氢活性且降低析氢能耗。④通入辅助沉积离子源的高纯02流量应以8sccm为宜；过高则强烈抑制P“111)择优生长,降低交换电流密度；过低则阻碍CeOx及Pt-Ce合金的生成,直接影响高价Ce离子的浓度。⑤综合调整溅射离子源的屏压与束流,才能有效控制载体膜电极中CeOx的组成及含量,3.0kV的屏压与60～70mA的束流可使Pt(111)获得最强的择优生长。⑥实际溅射沉积时间宜选择为300s,易制备高性价比的Pt基REOx载体膜电极。
Pt-REOx carrier membrane electrode is a applied widely heterogeneous hydrogen evolution catalyst. At present, the key problems of science and technology-Pt-REOx carrier membrane electrode used in high technology fields of new energy, environmental protection and etc.-work out:researching in the new method about short process manufacture of Core-Shell structure membrane electrode; researching in comprehensive control about membrane electrode material, membrane system type, cost performance and energy consumption; researching in Auxiliary catalytic mechanism about oxidation degree and electron transfer way in Rare-Earth (abbr. RE) additives; researching in the structure and performance of membrane electrode through comprehensive control manufacture factors.
Consideration of these problems, in this paper, Pt was used as main phase of membrane electrode, Cu was used as alloying element, the oxides of La and Ce were used as cocatalyst, the graphite fiber cloth (abbr. GFC), Si(111) slice and Ni mesh were used as carrier, and dilute H2SO4solution was used as compound in hydrogen evolution performance testing. The Compound multiphase Pt-REOx carrier membrane electrodes (abbr. Pt-REOx MEs)-provided with long-acting, high cost performance, and low-energy were all manufactured by Ion Beam Sputter Deposition (abbr. IBSD) equipment-including with authorized invention patents of author-and Post-processing techniques. The specific research works have:
(1) Study on different adulterated amount of Cu and Post-processing techniques influence on PtCu carrier MEs.
(2) Study on different membrane system type of La influence on PtCu-La2O3carrier MEs.
(3) Study on interaction mechanism between Ce and Pt on surface of Pt-CeOx carrier MEs.
(4) Study on manufactured technology influence on Pt-CeOx carrier MEs.
After complete these research work, we have acquired some significative experimental results and research conclusions.
1. These research results in studying on different adulterated amount of Cu and Post-processing techniques influence on PtCu carrier MEs showed that:
(1) The element content distribute equably in PtCu carrier MEs manufactured by IBSD. Along with increasing content of Cu doping, the crystal particle size in PtCu carrier MEs surface was decrease, and membrane organization became densification, and the preferred orientation degree of Pt(111) would be intensified.
(2) Through vacuum heat-treatment-at400℃,60min and～10-5Pa, the maximum alloying degree of Pt and Cu was happened in PtCu carrier MEs-about58.7at.%Cu in PtCu carrier MEs was alloyed, and Cu content in PtCu alloy was rised to54at.%, and the crystal particle size in PtCu carrier MEs only had tiny enlargement.
(3) After vacuum heat-treatment and acid etching processes-at0.50mol L-1H2SO4solution,30min and50℃, about73.7%Cu in surface of PtCu carrier MEs was separated out, and the dealloying degree in surface than it in inside of PtCu carrier MEs, so, the shell with high concentration Pt was produced and it wrapped outside PtCu alloy particle surface, that was similar core-shell type PtCu@Pt catalyst. The data of Pt-Pt interplanar spacing from HRTEM in fringe area had6.33%decrease than it in core area, and the average crystal particle size had been decreased about16%-from7.93nm fell to6.67nm, and the average specific surface area had been increased about250.2%.
(4) The testing data in hydrogen evolution performance of PtCu carrier MEs also indicated that its io had been enhanced respectively11.6%and13.4%after vacuum heat-treatment and acid etching processes, and Ed had been decreased about3%. Therefore, higher alloying degree of PtCu and similar core-shell structure were primary cause result in promoting compositive hydrogen evolution performance of PtCu carrier MEs.
(5) It had been accepted by SIPO that the patent for invention-IBSD+Vacuum heat-treatment+Acid etching treatment-relate to short process manufacture similar core-shell structure MEs, and it could control superficial component of PtCu carrier MEs, and it could avoid pollution of intermediate product and reduce energy consumption, and it would be apt to obtain actual application in cheap manufacture hydrogen industry.
2. These research results in studying on different membrane system type of La influence on Pt-REOx carrier MEs showed that:
(1) It was showed that PtCuLa2O3series monolayer carrier MEs (abbr. PL MEs) had fine homogeneous crystalline grain. Along with the increased doping amount of La, it would be enhanced in PL MEs that the average atomic volume shrinkage degree of Pt5La, thermostability and Oxygen enrichment ability.
(2) It would be intensified that the preferred orientation degree of Pt(111) in PtCu/La2O3series bilayer carrier MEs (abbr. P/L MEs), and would be decreased obviously that the average PtCu crystal particle size in La2O3/PtCu series bilayer carrier MEs (abbr. L/P MEs).
(3) Its research results indicated that PtCu crystal particle in surface of PtCu/La2O3/PtCu series trilayer carrier MEs (abbr. P/L/P MEs) existed more homogeneous and fine globularity. In addition, after vacuum heat-treatment process-at400℃,60min and～10-5Pa, the testing data in hydrogen evolution performance of P/L/P MEs-at0.50mol L-1H2SO4solution and50℃-indicated that i0>200mA·cm-2,Ed<0.63V, Pt content<0.1mg·cm-2and EAS≥94.172m2·g-1, and its hydrogen evolution performance and performance price ratio were superior to P/L and L/P MEs.
(4) Therefore, based on analysis by synthesis of different membrane system type and vacuum heat-treatment technology, it could be manufactured that composite PtCu-La2O3carrier MEs had higher cost performance, lower energy consumption and actual application value.
3. Through assaying change in binding energy state of surface atom, the e transfer way on interface could be reflected directly. In this paper, it also had been investigated that the interaction mechanism between Ce and Pt on surface of Pt-CeOx carrier MEs. It could be considered that Ce cation obtained e from Pt, the transfer way of e concurrently have single electron transfer and polyelectrons excitation process. Its innate character was high valence state Ce cation engendered O vacancy get through Oxidation-Reduction cycle of ion-pair-Ce3+/Ce4+, and occurred following e transfer processes: O2+e→O2-→O+O-and O2+2e→2O-
4. It was also showed that the research results in studying on manufactured technology influence on Pt-CeOX carrier MEs. There research results indicated that:
(1) CeO, Ce6O11, CeO2, Pt2Ce and Pt5Ce had been produced in Pt-CeOx carrier MEs-Ce doped-and Pt(111) peak position in XRD existed negative shift phenomenon.
(2) The optimal target position mobile distance (ST) value was20mm, and it would be decreased obviously that the average specific area of Pt-CeOx carrier MEs under overlarge or undersized ST value.
(3) After Pt-CeOx carrier MEs were manufactured in room temperature, they had preferential growth of Pt(111), optimal hydrogen evolution activity and lower energy consumption.
(4) The optimal flow of high purity O2that had been accessed Auxiliary Deposit Ion Source was8sccm. The preferential growth of Pt(111) would restrain mightily by excessive flow of O2, as well as, the lower flow of O2would impede producing CeOx and Pt-Ce alloy, and then dropped directly concentration of Ce4+.
(5) It was indicated that composition and content of CeOx in Pt-CeOx carrier MEs could be controlled effectively through adjusted synthetically energy and current of ion beam. Under3.0kV and60-70mA, the strongest preferential growth of Pt(111) would happen in Pt-CeOx carrier MEs.
(6) In the optimal time of actual sputtering deposition-300s, it could be manufactured easily that Pt-CeOx carrier MEs with higher performance price ratio.
针对这些关键问题,选择Pt为载体膜电极主相,Cu为合金元素,稀土镧(La)、铈(Ce)的氧化物为助剂,石墨纤维布(GFC)、Si(111)单晶片、镍网为载体,稀H2S04溶液为析氢性能测试的化合物,采用含作者授权发明专利的离子束溅射沉积(IBSD)设备及后处理技术,制备长效高性价比低能耗的复合多相Pt基REOx载体膜电极。具体开展了四方面的研究工作：
(1)掺Cu与后处理对PtCu载体膜电极的影响研究；
(2)膜层体系对Pt基载体膜电极的影响研究；
(3) Pt-CeOx单层膜表面的Ce与Pt之间相互作用机制的研究：
(4) Pt-CeOx载体膜电极的IBSD制备工艺的影响研究。
通过上述工作,获得研究结论研究结论：
在PtCu载体膜电极含Cu量以及后处理工艺的影响研究方面,提出的"IBSD+真空热处理+酸蚀处理”短流程方法制备类核壳结构Pt基载体膜电极,该方法可调控载体膜电极表层的组分,避免中间产物的污染并降低能耗,易于在廉价制氢行业获得实际应用。研究结果包括：①IBSD制备的载体膜电极元素含量分布连续均匀,Cu含量增加促进表面晶粒细化,膜层组织均匀,增强Pt(111)择优生长。②载体膜电极经真空热处理(400℃、保温60min、真空度～10-5Pa)后,PtCu合金化程度最大(58.7%的Cu参与合金化),PtCu合金中Cu含量上升到54at.%,膜层晶粒仅发生微量长大。③载体膜电极经真空热处理与酸蚀处理(30min、50℃、0.50mol L-1的H2SO4溶液)后,均一组成的PtCu合金晶粒表层的Cu析出,晶粒表层富集Pt,且表层的Pt-Pt晶面间距下降6.33%,PtCu合金的平均晶粒粒径为6.67nm(降低了16%),平均比表面积增大250.2%。④经真空热处理的载体膜电极析氢活性增强11.6%,酸蚀处理可进一步提升13.4%,且析氢峰电位降低3%,综合析氢性能优异。
在膜层体系对Pt基载体膜电极的影响研究方面,在综合分析层状结构的膜层体系与真空热处理工艺的基础上,制备出具有实际使用价值的高性价比低能耗的复合Pt基载体膜电极。研究结果包括：①PtCuLa2O3系单层载体膜电极膜层晶粒细小均匀,增加La含量将增大Pt5La的平均原子体积收缩程度,增强载体膜电极的热稳定性及富氧能力。②PtCu/La2O3系双层载体膜电极中Pt(111)择优生长,La2O3/PtCu系双层载体膜电极中Pt晶粒明显细化。③PtCu/La2O3/PtCu系多层载体膜电极表面晶粒呈细小球状晶团且分布更均匀,经真空热处理后的含Pt量低于0.1mg·cm-2,电化学活性比表面积达到94.172m2·g-1,远高于单层及双层载体膜电极,在50℃析氢反应时,交换电流密度>200mA·cm-2,分解电压<0.63V,因此,复合层状结构的膜层体系以及真空热处理工艺是影响载体膜电极析氢性能和性价比的主要因素。
针对应用广泛且具有代表性的稀土Ce,本文通过测定表面原子结合能态的变化,直接表征界面上的电子转移途径,提出Pt-CeOx单层膜表面的Ce与Pt之间存在的相互作用机制为：Pt向Ce离子转移电子的过程中存在单电子转移与多电子激发；高价Ce离子通过Ce3+/Ce4+离子偶的氧化-还原循环形成流动的O空位,O空位向吸附的02分子提供电子使其还原为活性O2-及O-离子,促进了Pt之间的电子传递。
本研究还获得了IBSD制备工艺影响Pt-CeOx载体膜电极物相结构及析氢性能的研究结果：①载体膜电极存在CeO、Ce6O11和CeO2以及Pt2Ce和Pt5Ce物相,Pt(111)衍射峰位发生负移。②靶位移动距离以20mm为宜,过大或过小则明显减小载体膜电极的平均比表面积。③室温下制膜有利于Pt(111)择优生长,增强载体膜电极析氢活性且降低析氢能耗。④通入辅助沉积离子源的高纯02流量应以8sccm为宜；过高则强烈抑制P“111)择优生长,降低交换电流密度；过低则阻碍CeOx及Pt-Ce合金的生成,直接影响高价Ce离子的浓度。⑤综合调整溅射离子源的屏压与束流,才能有效控制载体膜电极中CeOx的组成及含量,3.0kV的屏压与60～70mA的束流可使Pt(111)获得最强的择优生长。⑥实际溅射沉积时间宜选择为300s,易制备高性价比的Pt基REOx载体膜电极。
Pt-REOx carrier membrane electrode is a applied widely heterogeneous hydrogen evolution catalyst. At present, the key problems of science and technology-Pt-REOx carrier membrane electrode used in high technology fields of new energy, environmental protection and etc.-work out:researching in the new method about short process manufacture of Core-Shell structure membrane electrode; researching in comprehensive control about membrane electrode material, membrane system type, cost performance and energy consumption; researching in Auxiliary catalytic mechanism about oxidation degree and electron transfer way in Rare-Earth (abbr. RE) additives; researching in the structure and performance of membrane electrode through comprehensive control manufacture factors.
Consideration of these problems, in this paper, Pt was used as main phase of membrane electrode, Cu was used as alloying element, the oxides of La and Ce were used as cocatalyst, the graphite fiber cloth (abbr. GFC), Si(111) slice and Ni mesh were used as carrier, and dilute H2SO4solution was used as compound in hydrogen evolution performance testing. The Compound multiphase Pt-REOx carrier membrane electrodes (abbr. Pt-REOx MEs)-provided with long-acting, high cost performance, and low-energy were all manufactured by Ion Beam Sputter Deposition (abbr. IBSD) equipment-including with authorized invention patents of author-and Post-processing techniques. The specific research works have:
(1) Study on different adulterated amount of Cu and Post-processing techniques influence on PtCu carrier MEs.
(2) Study on different membrane system type of La influence on PtCu-La2O3carrier MEs.
(3) Study on interaction mechanism between Ce and Pt on surface of Pt-CeOx carrier MEs.
(4) Study on manufactured technology influence on Pt-CeOx carrier MEs.
After complete these research work, we have acquired some significative experimental results and research conclusions.
1. These research results in studying on different adulterated amount of Cu and Post-processing techniques influence on PtCu carrier MEs showed that:
(1) The element content distribute equably in PtCu carrier MEs manufactured by IBSD. Along with increasing content of Cu doping, the crystal particle size in PtCu carrier MEs surface was decrease, and membrane organization became densification, and the preferred orientation degree of Pt(111) would be intensified.
(2) Through vacuum heat-treatment-at400℃,60min and～10-5Pa, the maximum alloying degree of Pt and Cu was happened in PtCu carrier MEs-about58.7at.%Cu in PtCu carrier MEs was alloyed, and Cu content in PtCu alloy was rised to54at.%, and the crystal particle size in PtCu carrier MEs only had tiny enlargement.
(3) After vacuum heat-treatment and acid etching processes-at0.50mol L-1H2SO4solution,30min and50℃, about73.7%Cu in surface of PtCu carrier MEs was separated out, and the dealloying degree in surface than it in inside of PtCu carrier MEs, so, the shell with high concentration Pt was produced and it wrapped outside PtCu alloy particle surface, that was similar core-shell type PtCu@Pt catalyst. The data of Pt-Pt interplanar spacing from HRTEM in fringe area had6.33%decrease than it in core area, and the average crystal particle size had been decreased about16%-from7.93nm fell to6.67nm, and the average specific surface area had been increased about250.2%.
(4) The testing data in hydrogen evolution performance of PtCu carrier MEs also indicated that its io had been enhanced respectively11.6%and13.4%after vacuum heat-treatment and acid etching processes, and Ed had been decreased about3%. Therefore, higher alloying degree of PtCu and similar core-shell structure were primary cause result in promoting compositive hydrogen evolution performance of PtCu carrier MEs.
(5) It had been accepted by SIPO that the patent for invention-IBSD+Vacuum heat-treatment+Acid etching treatment-relate to short process manufacture similar core-shell structure MEs, and it could control superficial component of PtCu carrier MEs, and it could avoid pollution of intermediate product and reduce energy consumption, and it would be apt to obtain actual application in cheap manufacture hydrogen industry.
2. These research results in studying on different membrane system type of La influence on Pt-REOx carrier MEs showed that:
(1) It was showed that PtCuLa2O3series monolayer carrier MEs (abbr. PL MEs) had fine homogeneous crystalline grain. Along with the increased doping amount of La, it would be enhanced in PL MEs that the average atomic volume shrinkage degree of Pt5La, thermostability and Oxygen enrichment ability.
(2) It would be intensified that the preferred orientation degree of Pt(111) in PtCu/La2O3series bilayer carrier MEs (abbr. P/L MEs), and would be decreased obviously that the average PtCu crystal particle size in La2O3/PtCu series bilayer carrier MEs (abbr. L/P MEs).
(3) Its research results indicated that PtCu crystal particle in surface of PtCu/La2O3/PtCu series trilayer carrier MEs (abbr. P/L/P MEs) existed more homogeneous and fine globularity. In addition, after vacuum heat-treatment process-at400℃,60min and～10-5Pa, the testing data in hydrogen evolution performance of P/L/P MEs-at0.50mol L-1H2SO4solution and50℃-indicated that i0>200mA·cm-2,Ed<0.63V, Pt content<0.1mg·cm-2and EAS≥94.172m2·g-1, and its hydrogen evolution performance and performance price ratio were superior to P/L and L/P MEs.
(4) Therefore, based on analysis by synthesis of different membrane system type and vacuum heat-treatment technology, it could be manufactured that composite PtCu-La2O3carrier MEs had higher cost performance, lower energy consumption and actual application value.
3. Through assaying change in binding energy state of surface atom, the e transfer way on interface could be reflected directly. In this paper, it also had been investigated that the interaction mechanism between Ce and Pt on surface of Pt-CeOx carrier MEs. It could be considered that Ce cation obtained e from Pt, the transfer way of e concurrently have single electron transfer and polyelectrons excitation process. Its innate character was high valence state Ce cation engendered O vacancy get through Oxidation-Reduction cycle of ion-pair-Ce3+/Ce4+, and occurred following e transfer processes: O2+e→O2-→O+O-and O2+2e→2O-
4. It was also showed that the research results in studying on manufactured technology influence on Pt-CeOX carrier MEs. There research results indicated that:
(1) CeO, Ce6O11, CeO2, Pt2Ce and Pt5Ce had been produced in Pt-CeOx carrier MEs-Ce doped-and Pt(111) peak position in XRD existed negative shift phenomenon.
(2) The optimal target position mobile distance (ST) value was20mm, and it would be decreased obviously that the average specific area of Pt-CeOx carrier MEs under overlarge or undersized ST value.
(3) After Pt-CeOx carrier MEs were manufactured in room temperature, they had preferential growth of Pt(111), optimal hydrogen evolution activity and lower energy consumption.
(4) The optimal flow of high purity O2that had been accessed Auxiliary Deposit Ion Source was8sccm. The preferential growth of Pt(111) would restrain mightily by excessive flow of O2, as well as, the lower flow of O2would impede producing CeOx and Pt-Ce alloy, and then dropped directly concentration of Ce4+.
(5) It was indicated that composition and content of CeOx in Pt-CeOx carrier MEs could be controlled effectively through adjusted synthetically energy and current of ion beam. Under3.0kV and60-70mA, the strongest preferential growth of Pt(111) would happen in Pt-CeOx carrier MEs.
(6) In the optimal time of actual sputtering deposition-300s, it could be manufactured easily that Pt-CeOx carrier MEs with higher performance price ratio.
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