CN106083024A - A kind of cerium zinc is co-doped with NiFe2o4nano-powder and preparation method thereof - Google Patents

A kind of cerium zinc is co-doped with NiFe2o4nano-powder and preparation method thereof Download PDF

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CN106083024A
CN106083024A CN201610435603.3A CN201610435603A CN106083024A CN 106083024 A CN106083024 A CN 106083024A CN 201610435603 A CN201610435603 A CN 201610435603A CN 106083024 A CN106083024 A CN 106083024A
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cerium zinc
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罗驹华
颜柱
王旭
翟雪松
姜翠凤
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Yancheng Institute of Technology
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/624—Sol-gel processing
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3229—Cerium oxides or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof

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Abstract

The invention discloses a kind of cerium zinc and be co-doped with NiFe2O4Nano-powder, belongs to absorbing material technical field, and its formula is: Ni1‑ xCexFe2‑xZnxO4, wherein, 0≤x≤0.2.The invention also discloses a kind of cerium zinc and be co-doped with NiFe2O4The preparation method of nano-powder.A kind of cerium zinc of the present invention is co-doped with NiFe2O4Nano-powder, not only productivity is high, and purity is high, and particle diameter is little and uniform；It is a further object of the present invention to provide cerium zinc and be co-doped with NiFe2O4The preparation method of nano-powder, the method is simple to operate and is easily achieved large-scale production, utilizes Sol-Gel-Self-Propagating Process to prepare Ce, Zn and is co-doped with NiFe2O4Nanometer, is co-doped with NiFe for large-scale production Ce, Zn2O4Nano-powder provides a practicable approach, by prepared novel nano powder application in inhaling ripple field, has good prospect.

Description

A kind of cerium zinc is co-doped with NiFe2O4Nano-powder and preparation method thereof
Technical field
The invention belongs to absorbing material technical field, be specifically related to a kind of cerium zinc and be co-doped with NiFe2O4Nano-powder and preparation thereof Method.
Background technology
Along with companion's scientific and technological progress and social development, the electronic product such as mobile phone, computer has come into huge numbers of families, to people's Life brings many facilities, but the electromagnetic pollution thus brought occurs the most therewith, and absorbing material is increasingly becoming of concern Focus.Electromagnetism is hidden, draws attention the military equipment of radar protection or isolation in numerous countries.With this, high performance Electromagnetic-wave absorbent becomes the direction that scientific research is made great efforts.
Inverse spinel structure NiFe2O4Nanocrystalline have higher resistance coefficient as a kind of anisotropic soft magnetic material, Relatively low eddy current losses and high saturation and magnetic intensity.These characteristics come from the structure of its uniqueness, NiFe2O4Crystal structure is used Formula can be expressed as (Fe3+)[Ni2+Fe3+]O4, Fe3+Occupy tetrahedron and octahedral position, Ni respectively2+Occupy octahedron Position, the two non-parallel rotation creates stronger magnetic torque.Therefore high frequency magnetic recording, magnetic resonance dress it are widely used in Put, the field such as sensor.Further, since the imaginary part of compound pcrmeability is very big, be constantly subjected to the biggest attention, be widely used in Electro-magnetic wave absorption field.
Research finds, at NiFe2O4The introducing of rare earth elements can improve the magnetic property of Ferrite Material further, improves The stability of material, and lay the foundation for studying the Ferrite Material of novel extraordinary characteristic.Rare earth element ion has underfill 4f electron shell, there is abundant energy level, 4f electronics is shielded, when in rare earth element ion doped matrix lattice, 4f Electronics is affected by the surrounding environment the most weak, thus increases the electromagnetic consumable of material.Great majority research at present is just for single dilute The impact of earth elements doping, is co-doped with NiFe about rare earth element and transition metal2O4Report actually rare.
Summary of the invention
Goal of the invention: it is an object of the invention to provide a kind of cerium zinc and be co-doped with NiFe2O4Nano-powder, not only productivity is high, and And purity is high, particle diameter is little；It is a further object of the present invention to provide cerium zinc and be co-doped with NiFe2O4The preparation method of nano-powder.
Technical scheme: for achieving the above object, the present invention adopts the following technical scheme that
A kind of cerium zinc is co-doped with NiFe2O4Nano-powder, its formula is:
Ni1-xCexFe2-xZnxO4, wherein, 0≤x≤0.2.
A kind of cerium zinc of preparation is co-doped with NiFe2O4The method of nano-powder, comprises the following steps:
1) weigh the slaine of Ni, Ce, Fe and Zn in proportion, be dissolved in distilled water, magnetic agitation, it is thus achieved that light green is molten Liquid A；
2) weigh chelating agent to be dissolved in distilled water, magnetic agitation, it is thus achieved that colourless solution B；
3) in stirring, colourless solution B is slowly dropped in light green solution A, continues stirring after dripping, obtain molten Liquid C；Dropping citric acid process must be slow, and to be stirred continuously；
4) adding pH adjusting agent in solution C, regulation pH is 6～7, and stirring obtains blackish green colloidal sol D；
5) transferring in water-bath by blackish green colloidal sol D, stirring in water bath obtains wet gel E；
6) put into wet gel E baking oven is dried and obtain xerogel F；
7) xerogel F is lighted in atmosphere, obtain fluffy presoma, after grinding, obtain precursor powder G；
8) obtain target product cerium zinc after precursor powder G calcining and be co-doped with NiFe2O4Nano-powder.
Step 1) in, the slaine of described Ni, Ce, Fe and Zn is respectively analytically pure six water nickel nitrates, nitric acid Cerium, nine water ferric nitrate and zinc nitrates.
Step 2) in, described chelating agent be the mol ratio of citric acid, slaine and citric acid be 1: 1～1: 2.
Step 4) in, described pH adjusting agent is ammonia.
Step 5) in, the temperature of described stirring in water bath is 70～90 DEG C, and the time is 3～5h.
Step 6) in, described baking temperature is 100～120 DEG C, and drying time is 20～30h.
Step 8) in, the temperature of described calcining is 800～1000 DEG C, and the time is 2～5h.
Beneficial effect: compared with prior art, a kind of cerium zinc of the present invention is co-doped with NiFe2O4Nano-powder, not only productivity Height, and purity is high, and particle diameter is little and uniform；It is a further object of the present invention to provide cerium zinc and be co-doped with NiFe2O4The preparation of nano-powder Method, the method is simple to operate and is easily achieved large-scale production, utilizes collosol and gel-self-propagating method to prepare Ce, Zn and is co-doped with NiFe2O4Nanometer, is co-doped with NiFe for large-scale production Ce, Zn2O4Nano-powder provides a practicable approach, by institute The novel nano powder application of preparation, in inhaling ripple field, has good prospect.
Accompanying drawing explanation
Fig. 1 is the XRD figure of nano-powder prepared by embodiment 1-5；
Fig. 2 is the Ni of embodiment 3 preparation0.9Ce01Fe1.9Zn0.1O4The TEM figure of nano-powder；
Fig. 3 is the hysteresis curve figure of nano-powder prepared by embodiment 1-5；
Fig. 4 is the graph of a relation of the complex permeability of nano-powder prepared by embodiment 1-5, complex dielectric permittivity and frequency；
Fig. 5 is that nano-powder prepared by embodiment 1-5 inhales wave profile.
Detailed description of the invention
Below in conjunction with the accompanying drawings and detailed description of the invention, it is further elucidated with the present invention.
A kind of cerium zinc is co-doped with NiFe2O4Nano-powder, its formula is Ni1-xCexFe2-xZnxO4(0≤x≤0.2)。
A kind of cerium zinc is co-doped with NiFe2O4The preparation method of nano-powder, comprises the following steps:
1) according to chemical composition Ni1-xCexFe2-xZnxO4In (0≤x≤0.2), each metal ion chemistry metering ratio weighs one Quantitative slaine, is dissolved in distilled water, magnetic agitation, it is thus achieved that light green solution A；
2) according to metal ion: it is molten as chelating agent that citric acid is that 1: 1～1: 2 (mol ratio) weighs a certain amount of citric acid Solution in distilled water, magnetic agitation, it is thus achieved that colourless solution B；
3) in stirring, colourless solution B is slowly dropped in light green solution A, continues stirring after dripping, obtain molten Liquid C；
4) dripping ammonia in solution C, regulation pH is 6～about 7, continues stirring, obtains blackish green colloidal sol D；
5) blackish green colloidal sol D is transferred in water-bath, 70～90 DEG C of stirring in water bath 3～5h, it is thus achieved that wet gel E；
6) putting in baking oven by wet gel E, baking temperature is 100～120 DEG C, and drying time is 20～30h, it is thus achieved that dry solidifying Glue F；
7) xerogel F is lighted in atmosphere, obtain fluffy presoma, after grinding, obtain precursor powder G；
8) precursor powder G calcines 2～5h at 800～1000 DEG C, it is thus achieved that target product.
Embodiment 1
A kind of cerium zinc is co-doped with NiFe2O4The preparation method of nano-powder, comprises the following steps:
1) by 2.9081g six water nickel nitrate, 8.08g nine liquid glauber salt acid dissolved ferric iron in 100ml distilled water, magnetic agitation 30min, it is thus achieved that light green solution A；
2) 6.3g citric acid is dissolved in the stirring of 50ml distilled water, magnetic agitation 30min, it is thus achieved that colourless solution B；
3) in stirring, colourless solution B is slowly dropped in light green solution A, continues stirring 1h after dripping, obtain Solution C；
4) dripping ammonia in solution C, regulation pH is about 7, continues stirring 30min, obtains blackish green colloidal sol D；
5) blackish green colloidal sol D is transferred in water-bath, 80 DEG C of stirring in water bath 4h, it is thus achieved that wet gel E；
6) wet gel E is put in baking oven, 110 DEG C of dry 24h, it is thus achieved that xerogel F；
7) xerogel F is lighted in atmosphere, obtain fluffy presoma, after grinding, obtain precursor powder G；
8) precursor powder G calcines 3h at 900 DEG C, it is thus achieved that target product NiFe2O4。
Embodiment 2
A kind of cerium zinc is co-doped with NiFe2O4The preparation method of nano-powder, comprises the following steps:
1) by molten to 2.7626g six water nickel nitrate, 7.878g nine water ferric nitrate, 0.2170g cerous nitrate and 0.1487g zinc nitrate Solution is in 100ml distilled water, magnetic agitation 30min, it is thus achieved that light green solution A；
2) 6.3g citric acid is dissolved in the stirring of 50ml distilled water, magnetic agitation 30min, it is thus achieved that colourless solution B；
3) in stirring, colourless solution B is slowly dropped in light green solution A, continues stirring 1h after dripping, obtain Solution C；
4) dripping ammonia in solution C, regulation pH is about 7, continues stirring 30min, obtains blackish green colloidal sol D；
5) blackish green colloidal sol D is transferred in water-bath, 70 DEG C of stirring in water bath 5h, it is thus achieved that wet gel E；
6) wet gel E is put in baking oven, 100 DEG C of dry 30h, it is thus achieved that xerogel F；
7) xerogel F is lighted in atmosphere, obtain fluffy presoma, after grinding, obtain precursor powder G；
8) precursor powder G calcines 5h at 800 DEG C, it is thus achieved that target product Ni0.95Ce0.05Fe1.95Zn0.05O4。
Embodiment 3
A kind of cerium zinc is co-doped with NiFe2O4The preparation method of nano-powder, comprises the following steps:
1) by molten to 2.6173g six water nickel nitrate, 7.676g nine water ferric nitrate, 0.4341g cerous nitrate and 0.2975g zinc nitrate Solution is in 100ml distilled water, magnetic agitation 30min, it is thus achieved that light green solution A；
2) 6.3g citric acid is dissolved in the stirring of 50ml distilled water, magnetic agitation 30min, it is thus achieved that colourless solution B；
3) in stirring, colourless solution B is slowly dropped in light green solution A, continues stirring 1h after dripping, obtain Solution C；
4) dripping ammonia in solution C, regulation pH is about 7, continues stirring 30min, obtains blackish green colloidal sol D；
5) blackish green colloidal sol D is transferred in water-bath, 90 DEG C of stirring in water bath 3h, it is thus achieved that wet gel E；
6) wet gel E is put in baking oven, 120 DEG C of dry 20h, it is thus achieved that xerogel F；
7) xerogel F is lighted in atmosphere, obtain fluffy presoma, after grinding, obtain precursor powder G；
8) precursor powder G calcines 2h at 1000 DEG C, it is thus achieved that target product Ni0.9Ce0.1Fe1.9Zn0.1O4。
Embodiment 4
A kind of cerium zinc is co-doped with NiFe2O4The preparation method of nano-powder, comprises the following steps:
1) by molten to 2.4719g six water nickel nitrate, 7.474g nine water ferric nitrate, 0.6511g cerous nitrate and 0.4462g zinc nitrate Solution is in 100ml distilled water, magnetic agitation 30min, it is thus achieved that light green solution A；
2) 6.3g citric acid is dissolved in the stirring of 50ml distilled water, magnetic agitation 30min, it is thus achieved that colourless solution B；
3) in stirring, colourless solution B is slowly dropped in light green solution A, continues stirring 1h after dripping, obtain Solution C；
4) dripping ammonia in solution C, regulation pH is about 7, continues stirring 30min, obtains blackish green colloidal sol D；
5) blackish green colloidal sol D is transferred in water-bath, 80 DEG C of stirring in water bath 4h, it is thus achieved that wet gel E；
6) wet gel E is put in baking oven, 110 DEG C of dry 24h, it is thus achieved that xerogel F；
7) xerogel F is lighted in atmosphere, obtain fluffy presoma, after grinding, obtain precursor powder G；
8) precursor powder G calcines 3h at 900 DEG C, it is thus achieved that target product Ni0.85Ce0.15Fe1.85Zn0.15O4。
Embodiment 5
A kind of cerium zinc is co-doped with NiFe2O4The preparation method of nano-powder, comprises the following steps:
1) by molten to 2.3264g six water nickel nitrate, 7.272g nine water ferric nitrate, 0.8682g cerous nitrate and 0.5949g zinc nitrate Solution is in 100ml distilled water, magnetic agitation 30min, it is thus achieved that light green solution A；
2) 6.3g citric acid is dissolved in the stirring of 50ml distilled water, magnetic agitation 30min, it is thus achieved that colourless solution B；
3) in stirring, colourless solution B is slowly dropped in light green solution A, continues stirring 1h after dripping, obtain Solution C；
4) dripping ammonia in solution C, regulation pH is about 7, continues stirring 30min, obtains blackish green colloidal sol D；
5) blackish green colloidal sol D is transferred in water-bath, 80 DEG C of stirring in water bath 4h, it is thus achieved that wet gel E；
6) wet gel E is put in baking oven, 110 DEG C of dry 24h, it is thus achieved that xerogel F；
7) xerogel F is lighted in atmosphere, obtain fluffy presoma, after grinding, obtain precursor powder G；
8) precursor powder G calcines 3h at 900 DEG C, it is thus achieved that target product Ni0.8Ce0.2Fe1.8Zn0.2O4。
Product structure and service check
Utilize X-ray diffractometer that gained sample is carried out phase structure analysis；Utilize transmission electron microscope to sample Appearance structure is analyzed；Utilize vibrating specimen magnetometer that the magnetic property of sample is determined；Utilize vector network analysis pair The electromagnetic parameter of sample is analyzed.Utilize measured electromagnetic parameter and the reflection of following electromagnetic transmission theoretical formula method Rate loss (RL):
R L = 20 log | 1 - μ r ϵ r tan ( j 2 πf 0 d / c ϵ r μ r ) 1 + μ r ϵ r tan ( j 2 πf 0 d / c ϵ r μ r ) |
F in formula0For wave frequency, d is the thickness inhaling ripple layer, and c is electromagnetic transmission speed, ε in vacuumr、μrGeneration respectively Complex dielectric permittivity (the ε of ripple layer inhaled by tabler=ε '-j ε ") and complex permeability (μr=μ '-j μ ").
The XRD figure of the nano-powder that Fig. 1 provides for embodiment of the present invention 1-5.From figure 1 it appears that when Ce, Zn content During less than 0.1, sample is single cubic spinel Ni ferrite, each characteristic peak and standard PDF of Ni ferrite (No.0711232) card is the most identical, does not has other impurity peaks to occur, it means that when doping is less than 0.1, Ce3+With Zn2+Can enter well in the lattice of Ni ferrite.But, when doping is more than 0.15, occur in that a little impurity peaks, pass through Comparison, this impurity is CeO2。
The Ni that Fig. 2 provides for the embodiment of the present invention 30.9Ce01Fe1.9Zn0.1O4The TEM figure of nano wave-absorption powder body.From Fig. 2 Can be seen that the nano-particle of the sample substantially almost spherical of preparation, particle diameter is distributed between 30-50nm, this result and XRD Analyze basically identical.It addition, from Fig. 2 it has also been found that due to the particle of nanoscale has high surface can so that made There is slight reunion in standby sample.
The hysteresis curve of the nano-powder that Fig. 3 provides for embodiment of the present invention 1-5.From figure 3, it can be seen that all of sample All there is the high intensity of magnetization and low coercivity, meet soft magnetic bodies feature.When doping x≤0.1, the saturated magnetization of sample Intensity MsIncrease along with doping x and improve, and when x >=0.15, saturation magnetization M of samplesReduce therewith.
The relation of the complex permeability of the nano-powder that Fig. 4 provides for embodiment of the present invention 1-5, complex dielectric permittivity and frequency. Sample complex dielectric permittivity real part from Fig. 4 (a)-Fig. 4 (b) it can be seen that during x=0.15 is maximum, sample during x=0.1 Complex dielectric permittivity imaginary part reaches maximum at about 14GHz, it is meant that volume is that the dielectric loss of the sample of 0.1 is maximum；From Fig. 4 It can be seen that the complex permeability real part of the sample of x=0.1 and imaginary part are all higher than other samples in (c)-Fig. 4 (d), therefore have Bigger magnetic loss.
The nano-powder that Fig. 5 provides for embodiment of the present invention 1-5 inhales wave profile.From figure 5 it can be seen that volume is 0.1 Time, sample has the absorbing property of optimum, and its thickness is 2.5mm, minimal reflection 14.4GHz at be lost reach- 19.63dB.It addition, its effective Absorber Bandwidth (RL≤-10dB) reaches 6.12GHz.

Claims (8)

1. a cerium zinc is co-doped with NiFe2O4Nano-powder, it is characterised in that: its formula is:
Ni1-xCexFe2-xZnxO4, wherein, 0≤x≤0.2.
2. the preparation a kind of cerium zinc described in claim 1 is co-doped with NiFe2O4The method of nano-powder, it is characterised in that: include following Step:
1) weigh the slaine of Ni, Ce, Fe and Zn in proportion, be dissolved in distilled water, magnetic agitation, it is thus achieved that light green solution A；
2) weigh chelating agent to be dissolved in distilled water, magnetic agitation, it is thus achieved that colourless solution B；
3) in stirring, colourless solution B is slowly dropped in light green solution A, continues stirring after dripping, obtain solution C；
4) adding pH adjusting agent in solution C, regulation pH is 6～7, and stirring obtains blackish green colloidal sol D；
5) transferring in water-bath by blackish green colloidal sol D, stirring in water bath obtains wet gel E；
6) put into wet gel E baking oven is dried and obtain xerogel F；
7) xerogel F is lighted in atmosphere, obtain fluffy presoma, after grinding, obtain precursor powder G；
8) obtain target product cerium zinc after precursor powder G calcining and be co-doped with NiFe2O4Nano-powder.
Cerium zinc of preparing the most according to claim 2 is co-doped with NiFe2O4The method of nano-powder, it is characterised in that: step 1) In, the slaine of described Ni, Ce, Fe and Zn be respectively analytically pure six water nickel nitrates, cerous nitrate, nine water ferric nitrates and Zinc nitrate.
Cerium zinc of preparing the most according to claim 2 is co-doped with NiFe2O4The method of nano-powder, it is characterised in that: step 2) In, described chelating agent be the mol ratio of citric acid, slaine and citric acid be 1: 1～1: 2.
Cerium zinc of preparing the most according to claim 2 is co-doped with NiFe2O4The method of nano-powder, it is characterised in that: step 4) In, described pH adjusting agent is ammonia.
Cerium zinc of preparing the most according to claim 2 is co-doped with NiFe2O4The method of nano-powder, it is characterised in that: step 5) In, the temperature of described stirring in water bath is 70～90 DEG C, and the time is 3～5h.
Cerium zinc of preparing the most according to claim 2 is co-doped with NiFe2O4The method of nano-powder, it is characterised in that: step 6) In, described baking temperature is 100～120 DEG C, and drying time is 20～30h.
Cerium zinc of preparing the most according to claim 2 is co-doped with NiFe2O4The method of nano-powder, it is characterised in that: step 8) In, the temperature of described calcining is 800～1000 DEG C, and the time is 2～5h.
CN201610435603.3A 2016-06-17 2016-06-17 A kind of cerium zinc is co-doped with NiFe2o4nano-powder and preparation method thereof Pending CN106083024A (en)

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CN108373327A (en) * 2018-04-18 2018-08-07 成都信息工程大学 A kind of nickel zinc cerium soft magnetic ferrites and preparation method thereof
CN116371414A (en) * 2023-04-04 2023-07-04 华中科技大学 High-temperature stable reduction-resistant cerium oxide-nickel ferrite composite catalyst and preparation method and application thereof
US11827529B1 (en) 2023-07-07 2023-11-28 King Faisal University Ce and Zn-doped NiFe2O4 catalysts for urea fuel cells

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