CN106395913B - 一种具有铁缺陷的铁磁性纳米α‑Fe2O3及其制备方法 - Google Patents
一种具有铁缺陷的铁磁性纳米α‑Fe2O3及其制备方法 Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 230000005294 ferromagnetic effect Effects 0.000 title claims abstract description 18
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 125000004429 atom Chemical group 0.000 claims abstract description 4
- 125000004430 oxygen atom Chemical group O* 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- 230000007547 defect Effects 0.000 claims description 25
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 24
- 229910000859 α-Fe Inorganic materials 0.000 claims description 21
- 235000011187 glycerol Nutrition 0.000 claims description 12
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 230000005415 magnetization Effects 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 8
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 4
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 4
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- VEPSWGHMGZQCIN-UHFFFAOYSA-H ferric oxalate Chemical compound [Fe+3].[Fe+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O VEPSWGHMGZQCIN-UHFFFAOYSA-H 0.000 claims description 3
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical group [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- HUTBITLDXCEAPZ-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;iron Chemical compound [Fe].OC(=O)CC(O)(C(O)=O)CC(O)=O HUTBITLDXCEAPZ-UHFFFAOYSA-N 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 13
- 235000019441 ethanol Nutrition 0.000 description 13
- 229910052760 oxygen Inorganic materials 0.000 description 13
- 239000001301 oxygen Substances 0.000 description 13
- 230000005307 ferromagnetism Effects 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- 239000002184 metal Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 238000000151 deposition Methods 0.000 description 6
- 230000008021 deposition Effects 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 238000010791 quenching Methods 0.000 description 6
- 230000000171 quenching effect Effects 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000005291 magnetic effect Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 241000238366 Cephalopoda Species 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001860 citric acid derivatives Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910003153 β-FeOOH Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
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Abstract
本发明公开了一种具有铁缺陷的铁磁性纳米α‑Fe2O3,Fe原子与O原子的摩尔比小于1:1.5;本发明还公开了所述具有铁缺陷的铁磁性纳米α‑Fe2O3的制备方法。
Description
技术领域
本发明属于催化剂技术领域,具体涉及一种具有铁缺陷的铁磁性纳米α-Fe2O3及其制备方法。
背景技术
缺陷对于金属氧化物在物理和化学方面的应用有着十分重要的作用。目前金属氧化物中缺陷的引入技术主要包括掺杂、溅射、焙烧等。对于制备有缺陷的金属氧化物α-Fe2O3,目前被广泛报道的主要是对其氧缺陷的引入和调控,金属缺陷因其制备困难,尚未被报道。
Chen等人将Fe片暴露在氧等离子体中氧化形成含有氧缺陷的α-Fe2O3。通过表征和计算得出α-Fe2O3中有两种氧缺陷,并且两种缺陷生长方向平行。这种缺陷的形成是由于在生成的α-Fe2O3的过程中其与Fe基质之间结合松弛造成的。 (Chen Z.,et al.Chem.Mater.,2008,20(9):3224-3228.)
Schrebler等人利用电沉积法在FTO玻璃上通过电压循环法镀上厚度约为1 微米的含有氧缺陷的α-Fe2O3。在pH=13的0.1M NaOH+0.05M KI混合物电解液中观察其光电化学性质,发现制备出的α-Fe2O3具有n型半导体性质,平带电位为-1.08V vs.SMSE电极。(Schrebler R.,et al.Electrochem.solid-state lett.,2006, 9(7):C110-C113.)
Forster等人先在较低的pH(pH=1.5)值下在FTO玻璃基底上降解FeCl3 (0.15M),经过95℃高温反应4h形成β-FeOOH前躯体。将此前躯体在氧气不足的条件(氮气+空气)550℃焙烧2h最终形成带有氧缺陷的α-Fe2O3。将其应用于光电催化产氧气时的过电势比无缺陷α-Fe2O3降低了0.2V。(Forster M.,et al. Chem.Sci.,2015,6(7):4009-4016.)
以上报道的研究内容均为氧缺陷α-Fe2O3的合成,且未发现其明显的铁磁性表现。目前的技术条件在α-Fe2O3中引入氧缺陷较为容易,但是引入金属缺陷很困难,尚无文献或专利报道。
发明内容
本发明旨在提供一种具有大量铁缺陷的铁磁性纳米α-Fe2O3、及其制备方法。
本发明第一方面提供一种具有铁缺陷的铁磁性纳米α-Fe2O3,Fe原子与O原子的摩尔比小于1:1.5。
优选地,Fe原子与O原子的摩尔比为1:1.58。
本发明第二方面提供所述的具有铁缺陷的铁磁性纳米α-Fe2O3的制备方法,包括以下步骤:
(1)将铁盐和甘油,加入到无水乙醇中,搅拌均匀,其中铁盐与甘油的质量比为1:8~1:20;
(2)将步骤(1)得到的混合物在密闭容器中在100~200℃和自生压力下反应0.5~24h;
(3)将步骤(2)得到的反应结束后的物质冷却至室温;
(4)将步骤(3)冷却至室温的沉淀用无水乙醇进行洗涤,然后固液分离,将得到的固体在60~100℃下干燥至少12h,得到粉末物质;
(5)将步骤(4)得到的粉末物质在300~800℃下焙烧2~12h,得到所述的具有铁缺陷的铁磁性纳米α-Fe2O3。
优选地,所述铁盐为乙酸铁、草酸铁、柠檬酸铁、氯化铁、硝酸铁或硫酸铁的一种。
优选地,所述具有铁缺陷的铁磁性纳米α-Fe2O3的饱和磁化强度为10~25 emu/g,矫顽力为1000~2500Oe。
本发明的有益效果:
1、目前的技术条件在α-Fe2O3中引入氧缺陷较为容易,但是引入金属缺陷很困难,尚无文献或专利报道。本发明金属缺陷的引入会改变晶体结构和局部电子自旋结构,对于金属氧化物产生较强的室温铁磁性是一个新的策略。
2、金属氧化物的物理化学性质与其本征缺陷密切相关,主要表现在缺陷调控对于优化氧化物的功能特性具有十分重要的作用。α-Fe2O3是最稳定的铁氧化物,其本征结构具有n型半导体特性,已经被广泛应用在催化剂,药物和传感器等领域。目前报道的多为氧缺陷存在的α-Fe2O3,其在室温下铁磁性很弱。本发明通过溶剂热结合固相焙烧法首次合成了具有大量Fe缺陷的纳米α-Fe2O3,表现出了室温强铁磁性,是一种新型铁磁性材料。
3、本发明的具有大量Fe缺陷的纳米α-Fe2O3合成成本低,磁性较强,未来可用于磁性存储材料和电磁器件上。
附图说明
图1为本发明的具有大量Fe缺陷α-Fe2O3的X射线衍射图(XRD)
图2为本发明的具有大量Fe缺陷α-Fe2O3的TEM图
图3为本发明的具有大量Fe缺陷α-Fe2O3的TEM图
图4本发明的具有大量Fe缺陷α-Fe2O3被磁铁吸引图
具体实施方式
附图为本方法合成含有大量金属缺陷的α-Fe2O3的物性表征结果。
1,称取适量铁盐(乙酸铁、草酸铁、柠檬酸铁、氯化铁、硝酸铁和硫酸铁) 和甘油,先后加入到50~500mL无水乙醇中,其中铁盐与甘油的质量比为 1:8~1:20;
2,将上述混合好的溶液转移至具有聚四氟内胆的高压釜中加热搅拌均匀,密封之后放入烘箱中在100~200℃在自生压力下反应0.5~24h;
3,反应结束后对高压釜采取急冷措施,冷却至室温;
4,对生成的沉淀洗涤和离心,并于60~100℃烘箱中干燥至少12h,得到白色或浅棕色粉末;
5,将粉末置于马弗炉中300~800℃焙烧2~12h,最终的到含有金属缺陷的α-Fe2O3。
磁性测试:采用SQUID磁性测试系统对样品进行磁滞回线测试。测试结果:制备的样品均具有铁磁性,饱和磁化强度为10~25emu/g,矫顽力为1000~2500 Oe。
实例1:将1g乙酸铁、20.0g甘油和100mL乙醇混合,搅拌均匀获得的均相溶液转移至高压釜聚四氟内胆中。将聚四氟内胆放入高压釜中,密封后置于恒温烘箱中,于120℃烘箱中反应6.0h。反应结束后,对高压釜进行急冷处理。待高压釜冷却至室温,将水热沉淀取出,经离心和乙醇洗涤后,进行干燥。将干燥的粉末置于马弗炉中700℃焙烧2h,然后自然冷却降温。所制备样品表现出了较强铁磁性,饱和磁化强度为13emu/g,矫顽力为1200Oe。
实例2:将3g草酸铁、24.0g甘油和200mL乙醇混合,搅拌均匀获得的均相溶液转移至高压釜聚四氟内胆中。将聚四氟内胆放入高压釜中,密封后置于恒温烘箱中,于100℃烘箱中反应15.0h。反应结束后,对高压釜进行急冷处理。待高压釜冷却至室温,将水热沉淀取出,经离心和乙醇洗涤后,进行干燥。将干燥的粉末置于马弗炉中600℃焙烧4h,然后自然冷却降温。所制备样品表现出了较强铁磁性,饱和磁化强度为20emu/g,矫顽力为1600Oe。
实例3:将0.5g柠檬酸铁、10.0g甘油和50mL乙醇混合,搅拌均匀获得的均相溶液转移至高压釜聚四氟内胆中。将聚四氟内胆放入高压釜中,密封后置于恒温烘箱中,于180℃烘箱中反应2.0h。反应结束后,对高压釜进行急冷处理。待高压釜冷却至室温,将水热沉淀取出,经离心和乙醇洗涤后,进行干燥。将干燥的粉末置于马弗炉中400℃焙烧8h,然后自然冷却降温。所制备样品表现出了较强铁磁性,饱和磁化强度为15emu/g,矫顽力为1300Oe。
实例4:将4g氯化铁、40.0g甘油和500mL乙醇混合,搅拌均匀获得的均相溶液转移至高压釜聚四氟内胆中。将聚四氟内胆放入高压釜中,密封后置于恒温烘箱中,于150℃烘箱中反应3.0h。反应结束后,对高压釜进行急冷处理。待高压釜冷却至室温,将水热沉淀取出,经离心和乙醇洗涤后,进行干燥。将干燥的粉末置于马弗炉中500℃焙烧5h,然后自然冷却降温。所制备样品表现出了较强铁磁性,饱和磁化强度为25emu/g,矫顽力为2500Oe。
实例5:将8g硝酸铁、60.0g甘油和500mL乙醇混合,搅拌均匀获得的均相溶液转移至高压釜聚四氟内胆中。将聚四氟内胆放入高压釜中,密封后置于恒温烘箱中,于130℃烘箱中反应9.0h。反应结束后,对高压釜进行急冷处理。待高压釜冷却至室温,将水热沉淀取出,经离心和乙醇洗涤后,进行干燥。将干燥的粉末置于马弗炉中450℃焙烧10h,然后自然冷却降温。所制备样品表现出了较强铁磁性,饱和磁化强度为21emu/g,矫顽力为2050Oe。
实例6:将6g硫酸铁、35.0g甘油和100mL乙醇混合,搅拌均匀获得的均相溶液转移至高压釜聚四氟内胆中。将聚四氟内胆放入高压釜中,密封后置于恒温烘箱中,于130℃烘箱中反应24.0h。反应结束后,对高压釜进行急冷处理。待高压釜冷却至室温,将水热沉淀取出,经离心和乙醇洗涤后,进行干燥。将干燥的粉末置于马弗炉中700℃焙烧5h,然后自然冷却降温。所制备样品表现出了较强铁磁性,饱和磁化强度为18emu/g,矫顽力为1430Oe。
表征结果:制备样品的XRD曲线见图1,制备的缺陷氧化铁晶型为α-Fe2O3。所制备α-Fe2O3的TEM图见图2和图3。元素分析见表1,制备样品Fe/O比低于化学计量比Fe2O3,说明了Fe缺陷的存在。α-Fe2O3有较强的室温铁磁性,且在室温下可以被磁铁吸引,见图4。
表1制备样品的铁氧摩尔比
Claims (4)
1.一种具有铁缺陷的铁磁性纳米α-Fe2O3,其特征在于,Fe原子与O原子的摩尔比为1:1.58。
2.根据权利要求1所述的具有铁缺陷的铁磁性纳米α-Fe2O3,其特征在于,所述具有铁缺陷的铁磁性纳米α-Fe2O3的饱和磁化强度为10~25emu/g,矫顽力为1000~2500Oe。
3.根据权利要求1所述的具有铁缺陷的铁磁性纳米α-Fe2O3的制备方法,其特征在于,包括以下步骤:
(1)将铁盐和甘油,加入到无水乙醇中,搅拌均匀,其中铁盐与甘油的质量比为1:8~1:20;
(2)将步骤(1)得到的混合物在密闭容器中在100~200℃和自生压力下反应0.5~24h;
(3)将步骤(2)得到的反应结束后的物质冷却至室温;
(4)将步骤(3)冷却至室温的沉淀用无水乙醇进行洗涤,然后固液分离,将得到的固体在60~100℃下干燥至少12h,得到粉末物质;
(5)将步骤(4)得到的粉末物质在300~800℃下焙烧2~12h,得到所述的具有铁缺陷的铁磁性纳米α-Fe2O3。
4.根据权利要求3所述的制备方法,其特征在于,所述铁盐为乙酸铁、草酸铁、柠檬酸铁、氯化铁、硝酸铁或硫酸铁的一种。
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