CN108314095A - A kind of preparation method of nickel ferrite based magnetic loaded nano material - Google Patents
A kind of preparation method of nickel ferrite based magnetic loaded nano material Download PDFInfo
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- CN108314095A CN108314095A CN201810440019.6A CN201810440019A CN108314095A CN 108314095 A CN108314095 A CN 108314095A CN 201810440019 A CN201810440019 A CN 201810440019A CN 108314095 A CN108314095 A CN 108314095A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
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- 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
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- 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
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
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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
- C01P2002/30—Three-dimensional structures
- C01P2002/32—Three-dimensional structures spinel-type (AB2O4)
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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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/30—Particle morphology extending in three dimensions
Abstract
The invention discloses a kind of preparation methods of nickel ferrite based magnetic loaded nano material, belong to technical field of nanometer material preparation.NiFe provided by the present invention2O4Nano material is to prepare metal organic precursor material using solvent-thermal method, prepares using high-temperature calcination, is prepared by following steps：Nickelous nitrate hexahydrate, Fe(NO3)39H2O, fumaric acid and polyvinylpyrrolidone are dissolved in N, the mixed solution of N dimethylformamides and ethyl alcohol；It stirs at room temperature, obtained solution is transferred in reaction kettle and is heated under the conditions of certain temperature, centrifuge, vacuum drying obtains presoma Ni Fe MOF nano materials.Again through high-temperature calcination under certain temperature, NiFe is obtained2O4Nano material.Preparation method provided by the invention is simple, green non-pollution, and degree of being practical is high, and obtained NiFe2O4Nano material can be used directly as gas sensitive.
Description
Technical field
The present invention relates to a kind of preparation methods of nickel ferrite based magnetic loaded nano material, belong to technical field of nanometer material preparation.
Background technology
In recent years, with the aggravation of environmental pollution, various toxic and harmful gas also gradually increase, on the other hand, people couple
The attention degree of own health is increasing, and therefore, the demand to toxic and harmful gas detection also increasingly attracts attention.Metal
Oxide gas sensor because of it with simple in structure, fast response time, cheap, service life it is long and to flammable gas
Body and volatile organic compounds have many advantages, such as higher sensitivity and are used widely.Traditional metal oxide, such as
Fe2O3、ZnO、SnO2Deng though as certain effect that gas sensitive has taken, there are various disadvantages, such as γ-Fe2O3No
Stablize, is easy to happen phase transformation, the operating temperature requirements of ZnO are higher (400~450 DEG C), SnO2Selectivity it is poor etc..In order to change
The performance of kind gas sensor, may be used doped metallic oxide, Composite Oxide Gassensing Materials, precious metal catalyst (such as Ag,
Pd, Pt) etc..Composite Oxide Gassensing Materials, since the advantages that type is more, selectivity is good and high sensitivity is by vast scientific research people
The concern of member.
In composite oxides, nickel ferrite based magnetic loaded (NiFe2O4) it is a kind of novel gas sensitive, it is widely used in photocatalysis and super
Capacitor electrode material etc., in recent years, nickel ferrite based magnetic loaded (NiFe2O4) it is found to have good air-sensitive performance, work as nickel ferrite based magnetic loaded
(NiFe2O4) size of material is when reaching nanoscale, due to energy level, lattice structure and interface can etc. the variations of physical quantitys make
It is greatly improved in catalytic performance, magnetic property and air-sensitive performance etc., therefore, nano nickel ferrite (NiFe2O4) material
It prepares and studies by common concern.
Metal-organic framework material (Metal Organic Frameworks, abbreviation MOFs) is by metal ion or metal
Ion cluster is bonded with organic ligand in a manner of coordinate bond, periodically one-dimensional, two-dimentional or three by having of being self-assembly of
The metal organic framework crystalline material of the network structure of dimension；Due to its structure have crystallinity, adjustability, can modification and easy work(
The features such as capable of changing, makes it in main-guest chemistry, gas-selectively absorption, separation of small molecuies, energy storage, drug carrying, multiphase
The numerous areas such as catalysis and photoelectricity magnetics all show unique property and are used widely.In recent years, with to metal
Deepening continuously for organic framework materials research, utilizes it as presoma and prepares metal oxide nano-material in electrochemical energy
Storage and gas detection etc. show unique advantage.Therefore, the present invention prepares ferrous acid using metal-organic framework material
Nickel (NiFe2O4) nano material, for its green, efficiently preparation has great importance, while using it for gas detection, right
It is also had a wide range of applications in terms of environmental protection.
Invention content
The object of the present invention is to provide a kind of preparation methods of nickel ferrite based magnetic loaded nano material.
Technical scheme of the present invention：
A kind of preparation method of nickel ferrite based magnetic loaded nano material, with the Ni-Fe-MOF nanometers prepared under being controlled in surfactant
Material is presoma, prepares nickel ferrite based magnetic loaded nano material using high-temperature calcination method, steps are as follows：
By Nickelous nitrate hexahydrate, Fe(NO3)39H2O, fumaric acid and polyvinylpyrrolidone according to mass ratio 4-5:8-9:
30-40:20-25 be dissolved in N,N-dimethylformamide mixed with the mixed solution of ethyl alcohol or DMAC N,N' dimethyl acetamide with ethyl alcohol it is molten
In liquid, wherein the mass concentration of Nickelous nitrate hexahydrate is 5.3mg/mL, n,N-Dimethylformamide or n,N-dimethylacetamide
Volume ratio with ethyl alcohol is 2:1；Said mixture is stirred at room temperature, then obtained solution is transferred in reaction kettle
It heats under the conditions of certain temperature, after obtained product is centrifuged, is washed successively with DMF and ethyl alcohol respectively, Muffle is put in after dry
It in stove, is calcined at a certain temperature, nickel ferrite based magnetic loaded nano material is obtained after cooling.
The solvent heat temperature is 80-150 DEG C, heating time 6-24h.
The drying temperature is 60-120 DEG C, drying time 6-24h, preferably 6-12h.
The calcination temperature is 350-750 DEG C, and preferably 450-600 DEG C, time 2-6h, preferably time are 3~4h.
Beneficial effects of the present invention：Nickel ferrite based magnetic loaded (NiFe provided by the invention2O4) nano material have suitable biconial knot
Structure, higher specific surface area show good sensitivity and selection at lower operating temperatures as gas sensitive
Property.And the preparation method is simple, environmentally protective, and actual application value is high, and the design preparation of gas sensitive and environment are examined
Survey has great importance.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of Ni-Fe-MOF nano materials prepared by embodiment 1.
Fig. 2 is NiFe prepared by embodiment 32O4The X-ray diffractogram (XRD) of nano material.
Fig. 3 is NiFe prepared by embodiment 32O4The scanning electron microscope (SEM) photograph (SEM) of nano material.
Fig. 4 is that embodiment 5 prepares dynamic response recovery curve of the gas sensitive device for normal propyl alcohol.
Specific implementation mode
Below in conjunction with attached drawing and technical solution, the specific implementation mode that further illustrates the present invention.
Embodiment 1
Prepare Ni-Fe-MOF nano materials
By Nickelous nitrate hexahydrate (14.4mg), Fe(NO3)39H2O (29.2mg), fumaric acid (123.7mg), polyethylene pyrrole
Pyrrolidone (75mg) is dissolved in mixed solution (10mL, the V/V=2 of N,N-dimethylformamide and ethyl alcohol:1).By said mixture
10min is stirred at room temperature, and then obtained solution is transferred in 20mL reaction kettles and heats 12h at 120 DEG C, by what is obtained
After product centrifugation, DMF and ethyl alcohol 60 DEG C of dry 8h in vacuum drying chamber are successively used, Ni-Fe-MOF nanometers of materials of presoma are obtained
Material.
Embodiment 2
Prepare Ni-Fe-MOF nano materials
By Nickelous nitrate hexahydrate (19.2mg), Fe(NO3)39H2O (36.4mg), terephthalic acid (TPA) (182.6mg), poly- second
Alkene pyrrolidone (100mg) is dissolved in mixed solution (15mL, the V/V=2 of DMAC N,N' dimethyl acetamide and ethyl alcohol:1).It will be above-mentioned mixed
It closes object and stirs 10min at room temperature, then obtained solution is transferred in 20mL reaction kettles and heats 8h at 140 DEG C, will
Arrive product centrifugation after, successively use DMF and ethyl alcohol centrifugation after in vacuum drying chamber 80 DEG C of dry 6h, obtain presoma Ni-Fe-
MOF nano materials.
With the pattern for the Ni-Fe-MOF nano materials that scanning electron microscope characterizes.As shown in Figure 1, the Ni- of gained
Fe-MOF nano materials are in biconial structure, and grain size is at 1.5 μm or so.
Embodiment 3
Prepare NiFe2O4Nano material
Ni-Fe-MOF nano materials (20mg) in embodiment 1 or embodiment 2 are put into crucible, are placed in Muffle furnace,
High-temperature calcination is carried out in air atmosphere.Calcination temperature is 500 DEG C, heating rate 1 DEG C/min, calcination time 4h.
Its structure is analyzed with x-ray diffractometer, as shown in figure 3, nano material is the NiFe of spinel structure2O4Nanometer material
Material.
The NiFe characterized with scanning electron microscope2O4The pattern of nano material.As shown in figure 4, gained
NiFe2O4Nano material is in biconial structure, calcines front and back comparison it is found that a degree of contraction has occurred in material after firing,
Length-width ratio increases.
Embodiment 4
Prepare NiFe2O4Nano material
Ni-Fe-MOF nano materials (20mg) in embodiment 1 and 2 are weighed into crucible, are placed in Muffle furnace, in air
High-temperature calcination is carried out under atmosphere.Calcination temperature is 600 DEG C, heating rate 1 DEG C/min, calcination time 2h.
NiFe2O4The structure of nano material, morphology characterization are same as Example 3.
Embodiment 5
NiFe2O4Nano material air-sensitive property is tested
By NiFe2O4Nano material (10mg) is mixed to form uniform muddy mixture with deionized water, then with small Mao
Muddy mixture is uniformly coated on long 4mm by brush, outer diameter 1.2mm, on the ceramic tube of internal diameter 0.8mm, includes on ceramic tube
Two gold electrodes and four platinum filaments.After sample is dried at room temperature, nichrome resistance wire is inserted into ceramic tube, by adjusting nickel
The current control operation temperature of chromium alloy resistive silk.It is coated with NiFe2O4The ceramic tube of nano material is installed on air-sensitive tester
Socket on, complete device prepare and installment work.A certain amount of solvent to be measured is injected in cavity using micro syringe, so
Volatilization is steam to be measured afterwards.Test the resistance value under air atmosphere and vapor atmosphere to be measured by air-sensitive tester, with ratio come
Indicate the sensitivity of gas detection.
NiFe2O4For nano material at a temperature of different operating, to gas with various air-sensitive property, the results are shown in Table 1.
Table 1.NiFe2O4Nano material air-sensitive performance test result
Claims (3)
1. a kind of preparation method of nickel ferrite based magnetic loaded nano material, with the Ni-Fe-MOF nanometer materials prepared under being controlled in surfactant
Material is presoma, prepares nickel ferrite based magnetic loaded nano material using high-temperature calcination method, which is characterized in that steps are as follows：
By Nickelous nitrate hexahydrate, Fe(NO3)39H2O, fumaric acid and polyvinylpyrrolidone according to mass ratio 4-5:8-9:30-
40:20-25 is dissolved in the mixed solution or DMAC N,N' dimethyl acetamide and alcohol mixed solution of N,N-dimethylformamide and ethyl alcohol
In, wherein the mass concentration of Nickelous nitrate hexahydrate is 5.3mg/mL, n,N-Dimethylformamide or n,N-dimethylacetamide with
The volume ratio of ethyl alcohol is 2:1；Said mixture is stirred at room temperature, then obtained solution is transferred in reaction kettle
6-24h is heated under 80-150 DEG C of temperature condition, after obtained product is centrifuged, is washed successively with DMF and ethyl alcohol respectively, after dry
It is put in Muffle furnace, is 350-750 DEG C in calcination temperature, calcines 2-6h, nickel ferrite based magnetic loaded nano material is obtained after cooling.
2. preparation method according to claim 1, which is characterized in that the drying temperature is 60-120 DEG C, when dry
Between be 6-24h.
3. preparation method according to claim 1 or 2, which is characterized in that the calcination temperature is 450-600 DEG C, when
Between be 3~4h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109585825A (en) * | 2018-11-28 | 2019-04-05 | 成都理工大学 | The Ni/NiFe of bimetallic MOF precursor synthesis2O4Lithium ion battery negative material and preparation method thereof |
| CN112730563A (en) * | 2021-01-21 | 2021-04-30 | 河南工业大学 | Preparation method of sulfaquinoxaline electrochemical aptamer sensor based on internal circulation amplification strategy |
| CN113237926A (en) * | 2021-03-30 | 2021-08-10 | 中国石油大学(华东) | NiCo2O4/WO3Nano composite material and preparation method and application thereof |
| CN113444259A (en) * | 2021-07-14 | 2021-09-28 | 郑州大学 | Method for preparing two-dimensional nanosheet nickel-based metal organic framework material |
| CN114397331A (en) * | 2021-12-28 | 2022-04-26 | 郑州美克盛世电子科技有限公司 | Preparation method of gas-sensitive material for high-response and high-selectivity acetone sensor |
| CN114813880A (en) * | 2022-04-28 | 2022-07-29 | 安徽大学 | Integrated electrochemical gas sensor and preparation process thereof |
| CN116041053A (en) * | 2022-11-30 | 2023-05-02 | 国网智能电网研究院有限公司 | Preparation method of honeycomb nickel-zinc ferrite material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120149560A1 (en) * | 2010-12-08 | 2012-06-14 | Electronics And Telecommunications Research Institute | Method of manufacturing porous metal oxide |
| CN105777791A (en) * | 2016-03-17 | 2016-07-20 | 李亚丰 | Preparation method of zirconium-based microporous coordination polymer |
| CN107364897A (en) * | 2017-08-17 | 2017-11-21 | 大连理工大学 | A kind of preparation method of ferrous acid zinc nano material |
-
2018
- 2018-05-07 CN CN201810440019.6A patent/CN108314095A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120149560A1 (en) * | 2010-12-08 | 2012-06-14 | Electronics And Telecommunications Research Institute | Method of manufacturing porous metal oxide |
| CN105777791A (en) * | 2016-03-17 | 2016-07-20 | 李亚丰 | Preparation method of zirconium-based microporous coordination polymer |
| CN107364897A (en) * | 2017-08-17 | 2017-11-21 | 大连理工大学 | A kind of preparation method of ferrous acid zinc nano material |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109585825A (en) * | 2018-11-28 | 2019-04-05 | 成都理工大学 | The Ni/NiFe of bimetallic MOF precursor synthesis2O4Lithium ion battery negative material and preparation method thereof |
| CN112730563A (en) * | 2021-01-21 | 2021-04-30 | 河南工业大学 | Preparation method of sulfaquinoxaline electrochemical aptamer sensor based on internal circulation amplification strategy |
| CN113237926A (en) * | 2021-03-30 | 2021-08-10 | 中国石油大学(华东) | NiCo2O4/WO3Nano composite material and preparation method and application thereof |
| CN113444259A (en) * | 2021-07-14 | 2021-09-28 | 郑州大学 | Method for preparing two-dimensional nanosheet nickel-based metal organic framework material |
| CN114397331A (en) * | 2021-12-28 | 2022-04-26 | 郑州美克盛世电子科技有限公司 | Preparation method of gas-sensitive material for high-response and high-selectivity acetone sensor |
| CN114813880A (en) * | 2022-04-28 | 2022-07-29 | 安徽大学 | Integrated electrochemical gas sensor and preparation process thereof |
| CN116041053A (en) * | 2022-11-30 | 2023-05-02 | 国网智能电网研究院有限公司 | Preparation method of honeycomb nickel-zinc ferrite material |
| CN116041053B (en) * | 2022-11-30 | 2024-03-26 | 国网智能电网研究院有限公司 | Preparation method of honeycomb nickel-zinc ferrite material |
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Application publication date: 20180724 |