بررسی قابلیت جذب هیدروژن در ماده مرکب نانو‌ساختار SBA-16-Pd

نویسندگان

1 1- دانشکده مهندسی مواد و متالورژی، دانشگاه سمنان

2 2- دانشکده مهندسی شیمی، دانشگاه سمنان

چکیده

در این پژوهش قابلیت جذب هیدروژن در مواد متخلخل پایه سیلیکاتی SBA-16 اصلاح­شده با فلز واسطه پالادیوم با دما مورد بررسی قرار گرفت. مواد متخلخل پایه سیلیکا به‌دلیل داشتن سطح ویژه مناسب و قابل کنترل بودن پراکندگی و اندازه تخلخل­ها در محدوده 2 تا
10 نانومتر، قابلیت جذب و ذخیره­سازی گاز هیدروژن را دارند. ماده متخلخل SBA-16 به‌دلیل داشتن ساختار بلوری به شکل مکعب همراه با کانال‌های رو­باز برای این منظور می­تواند به‌کار رود. برای تهیه ماده مرکب نانو­ساختار و اضافه­کردن نمک کلرید پالادیوم به ماده متخلخل سیلیکا، از روشِ سل - ژلِ تک­مرحله­ای استفاده شد. پیرسازی در دمای C˚80 به‌مدت 12 ساعت انجام شد. در نهایت برای ایجاد حفرات و حذف ماده فعال­کننده، ماده در دمای C˚550 به‌مدت 6 ساعت کلسینه شد. مشخصه­یابی مواد به­وسیله پراش­سنجی اشعه ایکس زاویه بزرگ و زاویه کوچک، تحلیل جذب گاز هیدروژن تا فشار  kPa200 و در سه دمای C˚ 196- ( K77)،C ˚ 123- ( K150) و C˚ 30 ( K303) و هم‌چنین جذب- واجذب گاز نیتروژن انجام گرفت. ریخت شناسی توسط میکروسکوپ الکترونی روبشی نشر میدانی صورت پذیرفت. مقدار پالادیوم، سیلیکون و اکسیژن بر حسب درصد­وزنی، به­وسیله طیف­سنجی تفکیک انرژی اندازه­گیری شد. پیوندها وگروه‌های آلی ماده متخلخل سیلیکای خالص با دستگاه تبدیل فوریه فرا­سرخ مورد ارزیابی قرار گرفت. نتایج حاصل از پراش­سنجی پرتو ایکس و طیف­سنجی تفکیک انرژی، حضور ذرات فلزی و اکسید پالادیوم در حفرات ماده متخلخل سیلیکای غیر­بلوری را تأیید کرد. ریخت­ شناسی و نتایج حاصل از تحلیل جذب- واجذب گاز نیتروژن مشخص کرد با افزودن پالادیوم، سطح ویژه نسبت به ماده متخلخل خالص کاهش می­یابد. سطح ویژه برای ماده متخلخل سیلیکای خالص و برای ماده مرکب نانوساختار حاوی پالادیوم، به­ترتیب برابر با m2/g 791 و m2/g 538 به­دست آمد. مشاهده شد که جذب گاز هیدروژن در ماده مرکب نانو­ساختار حاوی پالادیوم در مقایسه با ماده متخلخل سیلیکای خالص رو به افزایش بوده، در حالی­که با افزایش دما رو کاهشی داشت. می­توان نتیجه گرفت که در ماده مرکب نانوساختار حاوی پالادیوم، بیشترین مقدار جذب گاز هیدروژن در دمای °C 196- روی داده است.

کلیدواژه‌ها

عنوان مقاله [English]

Evaluation of Ability of Hydrogen Absorption in SAB-16/Pd Nanostructure Composite

نویسندگان [English]

  • M.A. Yousefpour 1
  • F. Safari Kooshali 1
  • B. Khoshandam 2
1 1- Department of Materials and Metallurgical Engineering, Semnan University, Semnan, Iran
2 2- Department of Chemical Engineering, Semnan University, Semnan, Iran
چکیده [English]

The purpose of this work was to study the hydrogen adsorption on the surface of mesoporous materials based on silica (SBA-16) modified with palladium via temperature. Since mesoporous silica materials have a high specific surface area, and the ordered mesoporous size of 2-10nm, they are suitable for adsorption and storage of hydrogen. SBA-16 is suitable for this purpose due to its cubic crystalstructure and open pores. Single-stage sol-gel method was used to produce nanostructure composite from salt of palladium (PdCl3) and mesoporous silica precursor. The aging time was selected as 12 hr at 80˚C. Furthermore, the obtained materials were heated at 550˚C for 6 hr to remove surfactant and to form pores. Then the materials were characterized by large angle and small angle x-ray diffraction analysis, and hydrogen absorption analysis at upto 200kPa pressure at three different temperatures of -196˚C (77 K), -123˚C (150 K) and 30˚C (303 K). Furthermore, adsorption-desorption of nitrogen gas was studied. The surface morphology was observed by field emission scanning electron microscope (FESEM). In addition, the amount of palladium, oxygen, and silicon were measured by using energy dispersive spectroscopy) EDS ). Finally, the functional groups on the surface of mesoporous silica materials were evaluated using Fourier transform infrared spectroscopy (FTIR). The results of XRD and EDS analyses confirmed the presence of palladium and palladium oxide in mesoporous amorphous silica. In addition, BET results showed that addition of palladium in SBA-16 decreased the surface area, and produced 791 and 538m2/g for SBA-16 and SBA-16/Pd, respectively. Hydrogen absorption in nano structure composite was decreasing with temperatur in comparison with SAB-16. On the other hand, the maximum hydrogen absorption in the nano structure composite containing palladium was obtained at -196˚C (77 K).

کلیدواژه‌ها [English]

  • Mesoporous SBA-16
  • Hydrogen adsorption
  • Sol – Gelroute
  • Plladium

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مواد پیشرفته در مهندسی
دوره 34، شماره 3
آذر 1394
صفحه 13-27

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