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1、四氧化三铁和碳纤维复合方案1. Ni/CF :碳纤维粉碎 用丙酮洗掉表面残余物 蒸馏水洗净 120度下烘4小时；为了增强碳纤维与包覆物间的界面结合力，将碳纤维用硝酸浸泡4小时，最后用蒸馏水彻底洗干净；碳纤维的活化：室温下超声震动：150 mL, 20 g/L SnCl22H2O and 40 mL/L HCl for 75 min and then activated by an activation solution (150 mL, 0.25 g/L PdCl2 and 2.5 mL/L HCl) for 75 min。然后在碱性溶液中沉积镍2.2.1. Pretreatment of C
2、F and FG The CF was comminuted and the surface residual sizing materials were removed by acetone. Then the CF was rinsed with distilled water and dried at 120 C for 4 h. To enhance the interfacial adhesion between the CF (FG) and the coating, 0.3 gCF (FG)was immersed in nitric acid for 4 h andwashed
3、 thoroughly with distilled water. Sequentially, a two-step treatment was used to facilitate uniform activation throughout the entire surface of the CF (FG) with ultrasonic vibration at room temperature: the CF (FG) was sensitized by a sensitization solution (150 mL, 20 g/L SnCl22H2O and 40 mL/L HCl)
4、 for 75 min and then activated by an activation solution (150 mL, 0.25 g/L PdCl2 and 2.5 mL/L HCl) for 75 min.2.2.2. Preparation of NCF and NFGThe pretreated CF (FG) was dipped in an alkaline bath to deposit nickel. The bath solution (150 mL, 40 g/L NiSO46H2O, 20 g/L NaH2PO2H2O, 100 g/L NaC6H5O72H2O
5、 and 50 g/L NH4Cl) with pH adjusted by NH4OH to 9.0 was kept at a constant temperature of 70 C. The plating time was 20 min. Stirring was used to homogenize the bath solution a eliminate the gas bubbles from the CF (FG) surfaces during plating. Finally, as-prepared products were washed with distille
6、d water and then dried in an oven at 120 C for 2 h.2.Fe3O4/CF: 碳纤维浸入丙酮 2小时，蒸馏水洗；浸入硝酸5小时，蒸馏水洗；30 g/l SnCl22H2O 和3m mol HCL，蒸馏水洗；510 g/l silver nitrate AgNO3 and 2.1mM ammonia monohydrate NH3H2OC + Sn2+ = CSn2+ (1) CSn2+ +2Ag+ = CAg2 + Sn4+ (2)Fe(NO3)3 Fe3+ +3NO3 (3)(CH3)2NHBH3 +2H2O BO2 +(CH3)2NH + 7
7、H+ +6e (4)Fe3+ +e Fe2+ (5)NO3 +H2O + 2e NO2 +2OH (6)Fe2+ +2Fe3+ +8OH (Fe2+, 2Fe3+)(OH)8 (7)(Fe2+, 2Fe3+)3(OH)8 Fe3O4 +4H2O4.Fe3O4/CNT: CNT表面处理，在60度硝酸溶液中浸泡12小时；CNT在110度下烘干；Fe3O4/CNT溶解在200mL CTS solution (0.1 wt.%) instead of water, the obtained precipitate was CNT/Fe3O4/CTS composite.，20mg CNT/Fe3O4/
8、CTS was dispersed in 2mL of 5 mg/ml GOx solution by1 min sonication and the mixture was kept in a 4C refrigerator for 2 h. And then, the supernatant was removed from the precipitate by decanting with the aid of a magnet. The precipitate was dispersed in 2mL of 5 mg/mL of glutaraldehyde for 15 min to
9、 cross-link the primary amino groups of chitosan and GOx. The magnetic enzyme material was washed with water and immersed in 50mMphosphate buffer (pH 7.4) at 4C overnight to remove the reagents and the excess nonimmobilized GOx from the composite. The obtained magnetic biosensing composite, CNT/Fe3O
10、4/CTS/GOx, was dispersed in 10mL of 50mM phosphate buffer (pH 7.4) and was kept in a 4 C refrigerator for future use. (Fe3O4/CF)5. Iron nitrate Fe(NO3)39H2O, used as a starting material,was dissolved in aquous solution to form 54 ml of 0.6 M solution. Then 0.2 g acid-treated MWNTs was added into the
11、 solution and then the suspension was ultrasonicated for 5 min 2.5Mammonia solution was dropwised into the above mixed solution with vigorous stirring until the final pH of the suspension reached above 9. The precipitate was filtered, rinsed with anhydrous ethanol, and then dried at 80C for 24 h. Th
12、e sample was subsequently calcinated at 300C for2 h. The obtained powders were loaded into a quartz boat and heated in flowing NH3 (1 L min1) at 400 and 500C for 4 h in a tube furnace to obtain Fe3O4/CNTs and Fe2N/CNTs composites, respectively. The same method was applied to fabricate pure Fe3O4 and Fe2N powders without CNTs. (Fe3O4/CF)四氧化三铁在氮气气氛下烧结工艺研究：不同烧结温度对四氧化三铁性能的影响（XRD、VSM）
