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CN107188242A - Co0.4Fe0.6LaO3The preparation method of nano particle - Google Patents

Co0.4Fe0.6LaO3The preparation method of nano particle Download PDF

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CN107188242A
CN107188242A CN201710404477.XA CN201710404477A CN107188242A CN 107188242 A CN107188242 A CN 107188242A CN 201710404477 A CN201710404477 A CN 201710404477A CN 107188242 A CN107188242 A CN 107188242A
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范佳晨
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/80—Compounds containing cobalt, with or without oxygen or hydrogen, and containing one or more other elements
    • C01G51/82—Compounds containing cobalt, with or without oxygen or hydrogen, and containing two or more other elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28—Electrolytic cell components
    • G01N27/30—Electrodes, e.g. test electrodes; Half-cells
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

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  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
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Abstract

This application discloses a kind of Co0.4Fe0.6LaO3The preparation method of nano particle, including step：(1), by La (NO3)3·6H2O、Fe(NO3)3·9H2O、Co(NO3)2·6H2O and citric acid are well mixed；(2) pH value of mixed solution, is adjusted to 8~9 by alkaline solution；(3), mixed solution is reacted 8~10 hours under the conditions of 90~100 DEG C；(4) after, drying, calcined 1.5~3 hours under the conditions of 800~900 DEG C, obtain Co0.4Fe0.6LaO3Nano particle.The present invention passes through Co0.4Fe0.6LaO3Nano particle is modified electrode, can reduce its impedance, and the modified electrode can be used for hydrogen peroxide sensor.

Description

Co0.4Fe0.6LaO3纳米颗粒的制备方法Preparation method of Co0.4Fe0.6LaO3 nanoparticles

技术领域technical field

本申请属于材料技术领域，特别是涉及一种Co0.4Fe0.6LaO3纳米颗粒的制备方法。The application belongs to the field of material technology, and in particular relates to a preparation method of Co 0.4 Fe 0.6 LaO 3 nanoparticles.

背景技术Background technique

由于过氧化氢极易发生化学反应，目前工业上过氧化氢的测定普遍采用实验室化学分析或仪器分析法，这些方法由于存在过程复杂、分析时间长。而且人工取样常会导致错误的结果。因此现有的过氧化氢检测方法难以迅速监测到装置即时运行情况和安全状况。Because hydrogen peroxide is very prone to chemical reactions, laboratory chemical analysis or instrumental analysis is generally used for the determination of hydrogen peroxide in industry. These methods are complicated in process and long in analysis time. Moreover, manual sampling often leads to erroneous results. Therefore, the existing hydrogen peroxide detection method is difficult to quickly monitor the immediate operation and safety status of the device.

发明内容Contents of the invention

本发明的目的在于提供一种Co0.4Fe0.6LaO3纳米颗粒的制备方法，以克服现有技术中的不足。The object of the present invention is to provide a method for preparing Co 0.4 Fe 0.6 LaO 3 nanoparticles to overcome the deficiencies in the prior art.

为实现上述目的，本发明提供如下技术方案：To achieve the above object, the present invention provides the following technical solutions:

本申请实施例公开一种Co0.4Fe0.6LaO3纳米颗粒的制备方法，包括步骤：The embodiment of the present application discloses a preparation method of Co 0.4 Fe 0.6 LaO 3 nanoparticles, including steps:

(1)、将La(NO3)3·6H2O、Fe(NO3)3·9H2O、Co(NO3)2·6H2O和柠檬酸混合均匀；(1) Mix La(NO 3 ) 3 6H 2 O, Fe(NO 3 ) 3 9H 2 O, Co(NO 3 ) 2 6H 2 O and citric acid evenly;

(2)、通过碱性溶液调节混合溶液的pH值至8～9；(2), adjust the pH value of the mixed solution to 8-9 by alkaline solution;

(3)、将混合溶液在90～100℃条件下反应8～10小时；(3), reacting the mixed solution at 90-100°C for 8-10 hours;

(4)、干燥后，在800～900℃条件下煅烧1.5～3小时，得到Co0.4Fe0.6LaO3纳米颗粒。(4) After drying, calcining at 800-900° C. for 1.5-3 hours to obtain Co 0.4 Fe 0.6 LaO 3 nanoparticles.

优选的，在上述的Co0.4Fe0.6LaO3纳米颗粒的制备方法中，所述步骤(1)中，La(NO3)3·6H2O、Ni(NO3)2·6H2O和Co(NO3)2·6H2O的体积比为(5～7)：(3～4)：(3～4)。Preferably, in the above method for preparing Co 0.4 Fe 0.6 LaO 3 nanoparticles, in the step (1), La(NO 3 ) 3 ·6H 2 O, Ni(NO 3 ) 2 ·6H 2 O and Co The volume ratio of (NO 3 ) 2 ·6H 2 O is (5-7):(3-4):(3-4).

优选的，在上述的Co0.4Fe0.6LaO3纳米颗粒的制备方法中，所述碱性溶液为0.05mol/L以上易挥发性弱碱离子的液体。Preferably, in the above method for preparing Co 0.4 Fe 0.6 LaO 3 nanoparticles, the alkaline solution is a liquid containing more than 0.05 mol/L volatile weak base ions.

优选的，在上述的Co0.4Fe0.6LaO3纳米颗粒的制备方法中，所述易挥发性弱碱离子包括：氨根NH4 +、胺根R4N+中的一种或多种。Preferably, in the above method for preparing Co 0.4 Fe 0.6 LaO 3 nanoparticles, the volatile weak base ions include: one or more of NH 4 + amide and R 4 N + amine.

与现有技术相比，本发明的优点在于：本发明通过Co0.4Fe0.6LaO3纳米颗粒对电极进行修饰，可以降低其阻抗，该修饰电极可用于过氧化氢传感器。Compared with the prior art, the present invention has the advantages that: the electrode is modified by Co 0.4 Fe 0.6 LaO 3 nanoparticles in the present invention, which can reduce its impedance, and the modified electrode can be used as a hydrogen peroxide sensor.

具体实施方式detailed description

本发明通过下列实施例作进一步说明：根据下述实施例，可以更好地理解本发明。然而，本领域的技术人员容易理解，实施例所描述的具体的物料比、工艺条件及其结果仅用于说明本发明，而不应当也不会限制权利要求书中所详细描述的本发明。The present invention is further illustrated by the following examples: According to the following examples, the present invention can be better understood. However, those skilled in the art can readily understand that the specific material ratios, process conditions and results described in the examples are only used to illustrate the present invention, and should not and will not limit the present invention described in the claims.

实施例1Example 1

Co0.4Fe0.6LaO3纳米颗粒的制备方法Preparation method of Co 0.4 Fe 0.6 LaO 3 nanoparticles

1、将La(NO3)3·6H2O、Fe(NO3)3·9H2O、Co(NO3)2·6H2O和柠檬酸混合均匀，其中La(NO3)3·6H2O、Ni(NO3)2·6H2O和Co(NO3)2·6H2O的体积比为7：4：3；1. Mix La(NO 3 ) 3 ·6H 2 O, Fe(NO 3 ) 3 ·9H 2 O, Co(NO 3 ) 2 ·6H 2 O and citric acid evenly, wherein La(NO 3 ) 3 ·6H The volume ratio of 2 O, Ni(NO 3 ) 2 ·6H 2 O and Co(NO 3 ) 2 ·6H 2 O is 7:4:3;

2、通过碱性溶液调节混合溶液的pH值至8，碱性溶液为氨水；2. Adjust the pH value of the mixed solution to 8 through an alkaline solution, and the alkaline solution is ammonia water;

3、将混合溶液在90℃条件下反应10小时；3. React the mixed solution at 90°C for 10 hours;

4、干燥后，在850℃条件下煅烧2小时，得到Co0.4Fe0.6LaO3纳米颗粒。4. After drying, calcining at 850° C. for 2 hours to obtain Co 0.4 Fe 0.6 LaO 3 nanoparticles.

对获得的样品进行XRD表征，颗粒呈片状结构、大小均匀、表面光滑，粒径在50nm左右。通过Co0.4Fe0.6LaO3纳米颗粒对电极进行修饰，可以降低其阻抗，该修饰电极可用于过氧化氢传感器。The obtained samples were characterized by XRD, and the particles showed a flake structure, uniform size, smooth surface, and a particle size of about 50nm. Modification of the electrode by Co 0.4 Fe 0.6 LaO 3 nanoparticles can reduce its impedance, and the modified electrode can be used as a hydrogen peroxide sensor.

实施例2Example 2

Co0.4Fe0.6LaO3纳米颗粒的制备方法Preparation method of Co 0.4 Fe 0.6 LaO 3 nanoparticles

1、将La(NO3)3·6H2O、Fe(NO3)3·9H2O、Co(NO3)2·6H2O和柠檬酸混合均匀，其中La(NO3)3·6H2O、Ni(NO3)2·6H2O和Co(NO3)2·6H2O的体积比为5：3：3；1. Mix La(NO 3 ) 3 ·6H 2 O, Fe(NO 3 ) 3 ·9H 2 O, Co(NO 3 ) 2 ·6H 2 O and citric acid evenly, wherein La(NO 3 ) 3 ·6H The volume ratio of 2 O, Ni(NO 3 ) 2 ·6H 2 O and Co(NO 3 ) 2 ·6H 2 O is 5:3:3;

2、通过碱性溶液调节混合溶液的pH值至9，碱性溶液为氨水；2. Adjust the pH value of the mixed solution to 9 through an alkaline solution, and the alkaline solution is ammonia water;

3、将混合溶液在95℃条件下反应9小时；3. React the mixed solution at 95°C for 9 hours;

4、干燥后，在800℃条件下煅烧1.5小时，得到Co0.4Fe0.6LaO3纳米颗粒。4. After drying, calcining at 800° C. for 1.5 hours to obtain Co 0.4 Fe 0.6 LaO 3 nanoparticles.

对获得的样品进行XRD表征，颗粒呈片状结构、大小均匀、表面光滑，粒径在55nm左右。通过Co0.4Fe0.6LaO3纳米颗粒对电极进行修饰，可以降低其阻抗，该修饰电极可用于过氧化氢传感器。The obtained samples were characterized by XRD, and the particles showed a flake structure, uniform size, smooth surface, and a particle size of about 55nm. Modification of the electrode by Co 0.4 Fe 0.6 LaO 3 nanoparticles can reduce its impedance, and the modified electrode can be used as a hydrogen peroxide sensor.

最后，还需要说明的是，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者设备所固有的要素。Finally, it should also be noted that the term "comprises", "comprises" or any other variation thereof is intended to cover a non-exclusive inclusion such that a process, method, article or apparatus comprising a set of elements includes not only those elements, but also Other elements not expressly listed, or inherent to the process, method, article, or apparatus are also included.

Claims (4)

1. a kind of Co0.4Fe0.6LaO3The preparation method of nano particle, it is characterised in that including step：
(1), by La (NO3)3·6H2O、Fe(NO3)3·9H2O、Co(NO3)2·6H2O and citric acid are well mixed；
(2) pH value of mixed solution, is adjusted to 8~9 by alkaline solution；
(3), mixed solution is reacted 8~10 hours under the conditions of 90~100 DEG C；
(4) after, drying, calcined 1.5~3 hours under the conditions of 800~900 DEG C, obtain Co0.4Fe0.6LaO3Nano particle.
2. Co according to claim 10.4Fe0.6LaO3The preparation method of nano particle, it is characterised in that：The step (1) In, La (NO3)3·6H2O、Ni(NO3)2·6H2O and Co (NO3)2·6H2O volume ratio is (5~7)：(3~4)：(3~4).
3. Co according to claim 10.4Fe0.6LaO3The preparation method of nano particle, it is characterised in that：The alkalescence is molten Liquid is the liquid of more than 0.05mol/L effumability weak base ions.
4. Co according to claim 30.4Fe0.6LaO3The preparation method of nano particle, it is characterised in that：It is described volatile Property weak base ion includes：Ammonia root NH4 +, amine root R4N+In one or more.
CN201710404477.XA 2017-06-01 2017-06-01 Co0.4Fe0.6LaO3The preparation method of nano particle Pending CN107188242A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111272843A (en) * 2020-02-25 2020-06-12 衡阳师范学院 Nano material with FeCo network structure constructed by nano wires and preparation method and application thereof

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CN1631771A (en) * 2003-12-24 2005-06-29 中国科学院大连化学物理研究所 A kind of preparation method of metal composite oxide
CN101092297A (en) * 2006-06-21 2007-12-26 中国科学院大连化学物理研究所 Composite oxygen penetrating ceramics membrane, preparation method, and application
CN103771530A (en) * 2014-01-16 2014-05-07 南开大学 Spinel structural infrared radiation material doped with rare-earth element and preparation method

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111272843A (en) * 2020-02-25 2020-06-12 衡阳师范学院 Nano material with FeCo network structure constructed by nano wires and preparation method and application thereof
CN111272843B (en) * 2020-02-25 2023-01-06 衡阳师范学院 FeCo network structure nanomaterial constructed by nanowires and its preparation method and application

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