镍-磷-钛硅分子筛复合材料的制备与催化性能

张萍萍; 聂鹏飞; 王桂雪; 王兆波; 张宝泉

doi:10.13801/j.cnki.fhclxb.20210320.002

镍-磷-钛硅分子筛复合材料的制备与催化性能

doi: 10.13801/j.cnki.fhclxb.20210320.002

张萍萍^1, ,,
聂鹏飞^1,,
王桂雪^1,,
王兆波^1,,
张宝泉^{1, 2,}

1.
青岛科技大学　材料科学与工程学院，青岛， 266042
2.
天津大学　化工学院，天津， 300350

基金项目: 国家自然科学基金联合基金项目 (U20A20152)；山东省自然科学基金项目(ZR201910220411)

详细信息

通讯作者:
张萍萍，博士，讲师，研究方向为功能复合材料的制备及催化性能研究　E-mail：ppzhang@qust.edu.cn

中图分类号: TB333
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- 被引次数: 0
出版历程
- 收稿日期: 2021-01-13
- 修回日期: 2021-03-11
- 录用日期: 2021-03-15
- 网络出版日期: 2021-03-22
- 刊出日期: 2022-01-15

Preparation and catalytic performance of nickel-phosphorus-titanium silicalite zeolite composite

ZHANG Pingping^{1
, ,},
NIE Pengfei^1
,,
WANG Guixue^1
,,
WANG Zhaobo^1
,,
ZHANG Baoquan^{1, 2
,}

1.
College of Materials Science and Engineering, Qingdao University of Science and Technology, Qingdao 266042, China
2.
School of Chemical Engineering and Technology, Tianjin University, Tianjin 300350, China.

摘要

摘要: 以多级孔钛硅分子筛(HTS-1)为复合相、泡沫镍(NF)为基体，采用化学复合镀和原位处理工艺制备了镍-磷-钛硅分子筛(Ni-P-HTS-1/NF-T)复合材料，并对其电催化析氧反应(OER)性能进行研究。结果表明，Ni-P-HTS-1/NF-T复合材料在1 mol/L的KOH电解液中具有较快的OER动力学及电子转移速率，优异的OER性能及长期运行稳定性。HTS-1分子筛的掺杂及原位处理工艺降低了Ni-P-HTS-1/NF-T复合材料的电子转移电阻，增大其电催化活性表面积，此外还改变了复合材料的化学组成，生成了能为电催化析氧反应提供催化活性中心的镍的磷化物和氢氧化物，从而有效提升了Ni-P-HTS-1/NF-T复合材料的OER性能。
- 钛硅分子筛 /
- 化学复合镀 /
- 镍-磷-钛硅分子筛复合材料 /
- 非晶态 /
- 电催化析氧反应(OER)
Abstract: Nickel-phosphorus-titanium silicalite zeolite (Ni-P-HTS-1/NF-T) composite was prepared by electroless composite plating and in-situ treatment process with hierarchical titanium silicalite (HTS-1) zeolite as composite phase and nickel foam (NF) as matrix materials, and its electrocatalytic oxygen evolution reaction (OER) performance was studied. The results show that Ni-P-HTS-1/NF-T composite has faster OER kinetics and electron transfer rate, excellent OER performance and long-term stability in 1.0 mol/L KOH electrolyte. The doping of HTS-1 zeolite and in-situ treatment process reduce the electron transfer resistance of Ni-P-HTS-1/NF-T composite, increase its electrocatalytic active surface area, and change the chemical composition of the composite to form nickel phosphide and hydroxide which can provide catalytic active centers for electrocatalytic oxygen evolution reaction, thus effectively improving the OER performance of Ni-P-HTS-1/NF-T composite.
- titanium silicalite zeolite /
- electroless composite plating /
- nickel-phosphorus-titanium silicalite zeolite composite /
- amorphous state /
- electrocatalytic oxygen evolution reaction (OER)

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图 1 多级孔钛硅分子筛(HTS-1)分子筛的XRD图谱(a)、氮气吸附脱附等温线图(内置DFT模型孔径分布图) (b)、TEM图像(c)和SEM图像(d)

Figure 1. XRD pattern (a), N₂ adsorption and desorption isotherm (inserted with DFT model pore size distribution) (b), TEM image (c) and SEM image (d) of hierarchical titanium silicalite (HTS-1) zeolite

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图 2 (a)不同样品的XRD图谱；(b) Ni-P-HTS-1/泡沫镍(NF)复合材料的EDS图谱和元素分布图

Figure 2. (a) XRD patterns of different samples; (b) EDS spectrum and element mapping of Ni-P-HTS-1/nickel foam (NF) composite

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图 3 Ni-P-HTS-1/NF复合材料XPS全图谱(a)和Ni2p (b)、P2p (c)和O1s (d)的分图谱

Figure 3. XPS survey (a), Ni2p (b), P2p (c) and O1s (d) spectra of the Ni-P-HTS-1/NF composite

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图 4 Ni-P-HTS-1/NF (a)和Ni-P-HTS-1/NF-T (b)的SEM图像

Figure 4. SEM images of Ni-P-HTS-1/NF (a) and Ni-P-HTS-1/NF-T (b)

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图 5 Ni-P-HTS-1/NF-T复合材料XPS全图谱(a)及Ni2p (b)、P2p (c)和O1s (d)的分图谱

Figure 5. XPS survey (a), Ni2p (b), P2p (c) and O1s (d) spectra of the Ni-P-HTS-1/NF-T composite

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图 6 Ni-P-HTS-1/NF-T复合材料的极化曲线(a)、Tafel斜率(b)、奈奎斯特曲线(c)和双层电容曲线(d)

Figure 6. Polarization curves (a), Tafel plots (b), Nyquist plots (c) and Electrochemical double-layer capacitance (d) of Ni-P-HTS-1/NF-T composite

j —Current density; Z′—Real impedance; Z′′—Imaginary impedance; C_dl—Electrochemical double-layer capacitance; j_anodic, j_cathodic—Difference of current density between anode and cathode corresponding to fixed potential in cyclic voltammetry curve at a certain scanning speed

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图 7 Ni-P-HTS-1/NF-T复合材料的计时电位曲线

Figure 7. Chronopotentiometry curve of Ni-P-HTS-1/NF-T composite

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表 1 化学复合镀的配方及工艺参数

Table 1. Bath components and operating conditions of electroless composite plating

Bath component and operating condition	Effect of component	Amount
Nickel sulfate(NiSO₄·6H₂O)	Mental salts	25 g·L⁻¹
Sodium hypophosphite(NaH₂PO₂·H₂O)	Reducing agent	30 g·L⁻¹
Lactic acid(C₃H₆O₃)	Complexing agent	20 mL·L⁻¹
Sodium citrate(Na₃C₆H₅O₇·2H₂O)	Complexing agent	12.5 g·L⁻¹
Sodium acetate(CH₃COONa·3H₂O)	Buffer	25 g·L⁻¹
Titanium silicalite zeolite(TS-1)	Composite phase	0.2 g·L⁻¹
Sodium dodecyl sulfate(SDS)	Surfactant	0.1 g·L⁻¹
Potassium iodate(KIO₃)	Stabilizer	0.002 g·L⁻¹
pH value	−	5
Temperature	−	80℃

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表 2 钛硅分子筛的结构性质

Table 2. Texture properties of titanium silicalite zeolites

Materials	S_T/(m²·g⁻¹)	S_M/(m²·g⁻¹)	S_E/(m²·g⁻¹)	V_T/(cm⁻³·g⁻¹)	V_M/(cm⁻³·g⁻¹)
TS-1 (cal)	363.30	113.49	249.81	0.45	0.064
HTS-1 (cal)	462.28	177.63	284.65	0.57	0.096
Notes: S_T—Surface area of micropores; S_M—Surface area of mesopores by t−plot method; S_E—Surface area by Brunnauer-Emmet-Teller method; V_M—Micropore volume by t−plot method; V_T—Total pore volume.

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