CN109115952A - 一种mof诱导氧化铁纺锤体复合金纳米颗粒气敏材料的制备方法 - Google Patents
一种mof诱导氧化铁纺锤体复合金纳米颗粒气敏材料的制备方法 Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 19
- 230000003647 oxidation Effects 0.000 title claims abstract description 19
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 19
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 239000010931 gold Substances 0.000 title claims abstract description 18
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 18
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 16
- 239000002131 composite material Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 52
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 48
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000000956 alloy Substances 0.000 claims abstract description 17
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 17
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 17
- 239000004472 Lysine Substances 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 12
- 239000001509 sodium citrate Substances 0.000 claims abstract description 12
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims abstract description 12
- 229940038773 trisodium citrate Drugs 0.000 claims abstract description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000019766 L-Lysine Nutrition 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000005054 agglomeration Methods 0.000 claims description 10
- 230000002776 aggregation Effects 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 10
- 239000002086 nanomaterial Substances 0.000 claims description 8
- ZSDJVGXBJDDOCD-UHFFFAOYSA-N benzene dioctyl benzene-1,2-dicarboxylate Chemical compound C(C=1C(C(=O)OCCCCCCCC)=CC=CC1)(=O)OCCCCCCCC.C1=CC=CC=C1 ZSDJVGXBJDDOCD-UHFFFAOYSA-N 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 230000001376 precipitating effect Effects 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 235000018977 lysine Nutrition 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 26
- 239000000523 sample Substances 0.000 description 9
- 235000013339 cereals Nutrition 0.000 description 7
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 7
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 238000010276 construction Methods 0.000 description 5
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 229910003145 α-Fe2O3 Inorganic materials 0.000 description 2
- 206010037423 Pulmonary oedema Diseases 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 238000001523 electrospinning Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 208000005333 pulmonary edema Diseases 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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Abstract
本发明提供一种MOF诱导氧化铁纺锤体复合金纳米颗粒气敏材料的制备方法。该制备方法具体包括:以六水合三氯化铁为原料,以N‑N二甲基甲酰胺(DMF)为溶剂,对苯二甲酸为有机连接剂,采用传统的溶剂热法,得到均匀纺锤体结构的MIL‑88‑Fe,在500°C下煅烧20分钟后得到多孔氧化铁纺锤体;进而以四氯合金酸和L‑赖氨酸为原料,柠檬酸三钠为还原剂,在其表面附着金纳米颗粒,最终得到MOF诱导氧化铁纺锤体复合金纳米颗粒气敏材料。本方法生产工艺简单,所得的氧化铁复合金纳米颗粒的气敏材料具有多孔兼吸附点结构,大幅度增加了材料的比表面积和吸附性,获得高灵敏度的新型气敏材料。
Description
技术领域
本发明涉及涉及一种MOF诱导氧化铁纺锤体复合金纳米颗粒气敏材料的制备方法,属于先进纳米功能材料制备工艺技术领域。
背景技术
进入21世纪后,全球工业迅速发展,为人类的发展带来巨大的益处,但是与此同时,环境污染问题也越来越严重,其中尤其是气体污染,不仅对社会财产产生巨大损失,同时也会给人类的身体健康产生巨大的挑战。因此,人们越来越重视对有毒气体的检测。例如,三乙胺作为一种易燃且有毒的气体,会对人体皮肤和黏膜有刺激性,浓度较高时会产生肺水肿甚至死亡。对于气体的检测方法有多种,其中由金属氧化物制备的半导体气敏传感器由于其灵敏度高,使用寿命长,成本低等优点而被广泛应用。主要的金属氧化物有SnO2、ZnO、Fe2O3等传统气敏材料,也有In2O3、NiO、CuO等新型气敏材料。本实验主要讨论的是Fe2O3的气敏性能。Fe2O3是一种典型的N型半导体,禁带宽度为2.2 eV,Fe2O3具有对气体检测可逆、吸脱附时间短、气敏稳定性好、原料易于获取、成本低等优点, 但其仍然存在工作温度偏高,灵敏不不高等缺陷,因此长久以来是气敏研究领域的重点。为了进一步提高Fe2O3气敏性能,可以通过与其他贵金属复合形成活性吸附点,加快金属氧化物与气体之间的吸脱附,从而提高材料整体的气敏性能。
对于纳米材料来说,其形态结构的变化会对材料的气敏性能产生较大的影响,不仅能够进一步改善Fe2O3气敏材料的选择性,还能使其灵敏度得到进一步提升。目前已经有多种形态的纳米结构Fe2O3被成功制备,如Guo 等人(L. Guo, N. Xie, C. Wang, Enhancedhydrogen sulfide sensing properties of Pt-functionalized α-Fe2O3 nanowiresprepared by one-step electrospinning, Sens. Actuators B 255 (2018) 1015-1023.)对α-Fe2O3纳米管的成功制备并且该材料对H2S具有较好的气敏性。此外,利用MOF诱导的办法来制备金属半导体的方法越来越受研究界的关注。该方法利用有机物的形态具有多样性且易于控制的特点,通过煅烧去除有机物,得到的氧化物仍能保持原来的形态且形成多孔结构,这有利于提高材料的比表面积,从而改善其其气敏性。例如,Lü 等人(Y. Lü,W. Zhan, Y. He, MOF-templated synthesis of porous Co3O4 concave nanocubes withhigh specific surface area and their gas sensing properties, ACS Appl. Mater.Interfaces 6 (2014) 4186-4195.)发现MOF诱导的Co3O4纳米立方体具有较大的比表面积及优异的气敏性能。由于单一的气敏材料始终存在一定的限制,所以人们越来越关注对于贵金属复合气敏材料的制备。与其他贵金属复合后,一方面使氧化物半导体表面形成较多的活性位点,使得气敏材料能够吸附更多的测试气体;另一方面,在接触气体时,贵金属与不同金属氧化物之间的相互作用有利于加快电子传输,从而缩短气敏响应恢复时间,如Li等人(W. Li, H. Xu, T. Zhai, Enhanced triethylamine sensing properties bydesigning Au@ SnO2/MoS2 nanostructure directly on alumina tubes, Sens.Actuators B, 253 (2017) 97-107.)研究了复合金纳米颗粒后对气敏性的影响。Fe2O3虽然是一种传统的气敏材料,但是关于利用MOF诱导的方法制备气敏材料的研究较少,因此在这一领域还需要进一步探究。
发明内容
本发明的目的在于,提供一种MOF诱导氧化铁纺锤体复合金纳米颗粒的制备方法,该方法具有成本低、操作简单、产率高且不产生有毒物质,因此能够实现工业化的大规模生产。所得到的氧化铁纺锤体复合金纳米颗粒与纯氧化铁相比气敏性有了明显的提升,可以应用于气敏传感器领域。实现本发明目的的技术方案是:一种MOF诱导氧化铁纺锤体复合金纳米颗粒的制备方法,其特征在于:以六水合三氯化铁为原料,以N-N二甲基甲酰胺(DMF)为溶剂,对苯二甲酸为有机连接剂,采用传统的溶剂热法,得到均匀纺锤体结构的MIL-88-Fe,在500 °C下煅烧20分钟后得到多孔氧化铁纺锤体;进而以四氯合金酸和L-赖氨酸为原料,柠檬酸三钠为还原剂,在其表面附着金纳米颗粒,最终得到MOF诱导氧化铁纺锤体复合金纳米颗粒气敏材料。具体步骤如下:
(1)先量取15 ml N-N二甲基甲酰胺于烧杯中,再加入一定量的六水合三氯化铁和对苯二甲酸,其中六水合三氯化铁的浓度为0.005~0.015 mol/L,对苯二甲酸的浓度为0.005~0.015 mol/L, 控制六水合三氯化铁和对苯二甲酸的摩尔比为1:1;
(2)搅拌数分钟后,将所得溶液倒入40 ml反应釜中,在100~200 °C下保温2~4 h;获得的沉淀分别用N-N二甲基甲酰胺洗涤三次,无水乙醇洗涤两次(该过程中适当使用超声清洗器进行分散,减少颗粒的团聚现象);
(3)秤取0.005~0.015 g 氧化铁粉末于烧杯中,加入15 ml的去离子水,氧化铁纺锤体的浓度为0.002~0.006 mol/L;之后量取1 ml的四氯合金酸(浓度为0.01 mol/L)和1 ml L-赖氨酸(浓度为0.01 mol/L)于烧杯中;其中,氧化铁与四氯合金酸的摩尔比为(0.2~0.6):1,氧化铁与L-赖氨酸的摩尔比为(0.2~0.6):1;超声数分钟后,用移液枪逐滴加入0.1 ml的柠檬酸三钠(浓度为0.1 mol/L),且氧化铁与柠檬酸三钠的摩尔比为(0.02~0.06):1,之后在室温下搅拌半小时;
(4)将步骤(3)所得的溶液用去离子水洗涤三次,无水乙醇洗涤两次(该过程中适当使用超声清洗器进行分散,减少颗粒的团聚现象);
(5)将步骤(4)得到的离心产物倒入表面皿,在烘箱内60 °C保温6 h;之后将样品烘干;将烘干后的样品放到马弗炉中在300 °C下煅烧30 min, 即可获得MOF诱导氧化铁纺锤体复合金纳米颗粒的纳米结构。
附图说明
图1为MOF诱导氧化铁纺锤体与金纳米颗粒复合结构的XRD图谱。
图2为MOF诱导氧化铁纺锤体与金纳米颗粒复合结构的FESEM图。
图3为MOF诱导氧化铁纺锤体与金纳米颗粒复合结构的TEM图。
图4为最佳工作电压下MOF诱导氧化铁纺锤体与金纳米颗粒复合结构与纯氧化铁气敏元件对10-1000 ppm的乙醇气体的灵敏度曲线对比图。
图5为最佳工作电压下MOF诱导氧化铁纺锤体与金纳米颗粒复合结构与纯氧化铁气敏元件的响应恢复曲线对比。
具体实施方式
下面对本发明的实施例做详细说明,本实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。
实施例1
(1)先量取15 ml N-N二甲基甲酰胺于烧杯中,再加入一定量的六水合三氯化铁和对苯二甲酸,其中六水合三氯化铁的浓度为0.005 mol/L,对苯二甲酸的浓度为0.005 mol/L,控制六水合三氯化铁和对苯二甲酸的摩尔比为1:1;
(2)搅拌数分钟后,将所得溶液倒入40 ml反应釜中,在100 °C下保温2 h;获得的沉淀分别用N-N二甲基甲酰胺洗涤三次,无水乙醇洗涤两次(该过程中适当使用超声清洗器进行分散,减少颗粒的团聚现象);
(3)秤取0.005 g 氧化铁粉末于烧杯中,加入15 ml的去离子水,氧化铁纺锤体的浓度为0.002 mol/L;之后量取1 ml的四氯合金酸(浓度为0.01 mol/L)和1 ml L-赖氨酸(浓度为0.01 mol/L)于烧杯中;其中,氧化铁与四氯合金酸的摩尔比为0.2:1,氧化铁与L-赖氨酸的摩尔比为0.2:1;超声数分钟后,用移液枪逐滴加入0.1 ml 的柠檬酸三钠(浓度为0.1mol/L),且氧化铁与柠檬酸三钠的摩尔比为0.02:1,之后在室温下搅拌半小时;
(4)将步骤(3)所得的溶液用去离子水洗涤三次,无水乙醇洗涤两次(该过程中适当使用超声清洗器进行分散,减少颗粒的团聚现象);
(5)将步骤(4)得到的离心产物倒入表面皿,在烘箱内60 °C保温6 h;之后将样品烘干;将烘干后的样品放到马弗炉中在300 °C下煅烧30 min, 即可获得MOF诱导氧化铁纺锤体复合金纳米颗粒的纳米结构。
实施例2
(1)先量取15 ml N-N二甲基甲酰胺于烧杯中,再加入一定量的六水合三氯化铁和对苯二甲酸,其中六水合三氯化铁的浓度为0.01 mol/L,对苯二甲酸的浓度为0.01 mol/L, 控制六水合三氯化铁和对苯二甲酸的摩尔比为1:1;
(2)搅拌数分钟后,将所得溶液倒入40 ml反应釜中,在150 °C下保温3 h;获得的沉淀分别用N-N二甲基甲酰胺洗涤三次,无水乙醇洗涤两次(该过程中适当使用超声清洗器进行分散,减少颗粒的团聚现象);
(3)秤取0.01 g 氧化铁粉末于烧杯中,加入15 ml的去离子水,氧化铁纺锤体的浓度为0.004 mol/L;之后量取1 ml的四氯合金酸(浓度为0.01 mol/L)和1 ml L-赖氨酸(浓度为0.01 mol/L)于烧杯中;其中,氧化铁与四氯合金酸的摩尔比为0.4:1,氧化铁与L-赖氨酸的摩尔比为0.4:1;超声数分钟后,用移液枪逐滴加入0.1 ml 的柠檬酸三钠(浓度为0.1 mol/L),且氧化铁与柠檬酸三钠的摩尔比为0.04:1,之后在室温下搅拌半小时;
(4)将步骤(3)所得的溶液用去离子水洗涤三次,无水乙醇洗涤两次(该过程中适当使用超声清洗器进行分散,减少颗粒的团聚现象);
(5)将步骤(4)得到的离心产物倒入表面皿,在烘箱内60 °C保温6 h;之后将样品烘干;将烘干后的样品放到马弗炉中在300 °C下煅烧30 min, 即可获得MOF诱导氧化铁纺锤体复合金纳米颗粒的纳米结构。
实施例3
(1)先量取15 ml N-N二甲基甲酰胺于烧杯中,再加入一定量的六水合三氯化铁和对苯二甲酸,其中六水合三氯化铁的浓度为0.015 mol/L,对苯二甲酸的浓度为0.015 mol/L,控制六水合三氯化铁和对苯二甲酸的摩尔比为1:1;
(2)搅拌数分钟后,将所得溶液倒入40 ml反应釜中,在200 °C下保温4 h;获得的沉淀分别用N-N二甲基甲酰胺洗涤三次,无水乙醇洗涤两次(该过程中适当使用超声清洗器进行分散,减少颗粒的团聚现象);
(3)秤取0.015 g 氧化铁粉末于烧杯中,加入15 ml的去离子水,氧化铁纺锤体的浓度为0.006 mol/L;之后量取1 ml的四氯合金酸(浓度为0.01 mol/L)和1 ml L-赖氨酸(浓度为0.01 mol/L)于烧杯中;其中,氧化铁与四氯合金酸的摩尔比为0.6:1,氧化铁与L-赖氨酸的摩尔比为0.6:1;超声数分钟后,用移液枪逐滴加入0.1 ml 的柠檬酸三钠(浓度为0.1mol/L),且氧化铁与柠檬酸三钠的摩尔比为0.06:1,之后在室温下搅拌半小时;
(4)将步骤(3)所得的溶液用去离子水洗涤三次,无水乙醇洗涤两次(该过程中适当使用超声清洗器进行分散,减少颗粒的团聚现象);
(5)将步骤(4)得到的离心产物倒入表面皿,在烘箱内60 °C保温6 h;之后将样品烘干;将烘干后的样品放到马弗炉中在300 °C下煅烧30 min, 即可获得MOF诱导氧化铁纺锤体复合金纳米颗粒的纳米结构。
Claims (1)
1.一种MOF诱导氧化铁纺锤体复合金纳米颗粒气敏材料的制备方法,具体合成步骤如下:
(1)先量取15 ml N-N二甲基甲酰胺于烧杯中,再加入一定量的六水合三氯化铁和对苯二甲酸,其中六水合三氯化铁的浓度为0.005~0.015 mol/L,对苯二甲酸的浓度为0.005~0.015 mol/L, 控制六水合三氯化铁和对苯二甲酸的摩尔比为1:1;
(2)搅拌数分钟后,将所得溶液倒入40 ml反应釜中,在100~200 °C下保温2~4h;获得的沉淀分别用N-N二甲基甲酰胺洗涤三次,无水乙醇洗涤两次(该过程中适当使用超声清洗器进行分散,减少颗粒的团聚现象);
(3)秤取0.005~0.015 g 氧化铁粉末于烧杯中,加入15 ml的去离子水,氧化铁纺锤体的浓度为0.002~0.006 mol/L;之后量取1 ml的四氯合金酸(浓度为0.01 mol/L)和1 ml L-赖氨酸(浓度为0.01 mol/L)于烧杯中;其中,氧化铁与四氯合金酸的摩尔比为(0.2~0.6):1,氧化铁与L-赖氨酸的摩尔比为(0.2~0.6):1;超声数分钟后,用移液枪逐滴加入0.1 ml的柠檬酸三钠(浓度为0.1 mol/L),且氧化铁与柠檬酸三钠的摩尔比为(0.02~0.06):1,之后在室温下搅拌半小时;
(4)将步骤(3)所得的溶液用去离子水洗涤三次,无水乙醇洗涤两次(该过程中适当使用超声清洗器进行分散,减少颗粒的团聚现象);
(5)将步骤(4)得到的离心产物倒入表面皿,在烘箱内60 °C保温6 h;之后将样品烘干;将烘干后的样品放到马弗炉中在300 °C下煅烧30 min, 即可获得MOF诱导氧化铁纺锤体复合金纳米颗粒的纳米结构。
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