CN102719812B - Method for preparing one-dimensional spinel type ferrite AxB1-xFe2O4 through chemical plating - Google Patents

Method for preparing one-dimensional spinel type ferrite AxB1-xFe2O4 through chemical plating Download PDF

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CN102719812B
CN102719812B CN201210169412.9A CN201210169412A CN102719812B CN 102719812 B CN102719812 B CN 102719812B CN 201210169412 A CN201210169412 A CN 201210169412A CN 102719812 B CN102719812 B CN 102719812B
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plating
dimension
spinel type
chemical
ferriferous oxide
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CN102719812A (en
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孙杰
孟锦宏
王文举
曹晓辉
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Shenzhen Kainafang Technology Co.,Ltd.
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Shenyang Ligong University
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Abstract

The invention discloses a method for preparing one-dimensional spinel type ferrite AxB1-xFe2O4 through chemical plating. The method is characterized by comprising the following steps of: coating a layer of metal or alloy on the surface of one-dimensional iron oxide through chemical plating, and thus obtaining the spinel type ferrite AxB1-xFe2O4 by a high-temperature roasting process, wherein A and B are Ni, Co, Cu or Zn, and x is more than or equal to 0 and less than or equal to 1; and the one-dimensional iron oxide is alpha-FeOOH, gamma-FeOOH, alpha-Fe2O3 or gamma-Fe2O3 which has a needle-shaped or stick-shaped system, and the length-diameter ratio of particles of the one-dimensional iron oxide is more than or equal to 5. The method is short in reaction time, low in cost and high in quality.

Description

A kind of through chemically plating for one dimension spinel type ferrite A xb 1-xfe 2o 4method
Technical field
The present invention relates to a kind of ferriferous oxide and prepare the method for one dimension spinel type ferrite through chemical plating method, specifically, is exactly at alpha-feooh, γ-FeOOH, α-Fe 2o 3or γ-Fe 2o 3carry out electroless plating on ferriferous oxide surface, by obtaining one dimension spinel type ferrite after high-temperature roasting.
Background technology
Spinel type ferrite crystalline structure belongs to isometric system.Its chemical formula is MFe 2o 4, wherein M is Ni 2+, Co 2+, Cu 2+, Zn 2+deng divalent-metal ion.The structure of spinel structure ferrite and Characteristics of Chemical Constituents make it both have ferromagnetism, certain dielectricity, good mechanical property, higher intensity and erosion resistance, and chemical stability is better, can be applicable to various fields, mainly comprise absorbing material aspect, medical aspect, catalysis aspect etc.
At present, the ferritic preparation method of one dimension pattern has many, common are chemical coprecipitation, hydrothermal method, sol-gel method etc.
Chemical coprecipitation divides two classes, and the one, use precipitation agent by coprecipitated to divalent metal salt and trivalent iron salt, and high-temperature roasting obtain product.Its advantage is that technique is simple, but precipitation is colloidal state more, is therefore difficult for filtering and washing.The 2nd, mineral alkali is added in the solution of divalent metal salt and divalent iron salt, pass into air and make it oxidation, after the reaction some time, can obtain product.Liu Hui etc. [Liu Hui, Wei Yu. the progress functional materials that Methods of Nanosized Ferrite Particals is synthetic, 2000,31(2): 124～125] utilize chemical precipitation method can make the CuFe that particle diameter is 50nm 2o 4, this method is easy to operate, equipment simple, pure phase and the granularity easy to control etc. of being easy to get advantage, but the proportioning of reaction mass, temperature of reaction and oxidization time have considerable influence to the quality of result.
Sol-gel method is made part by M by organic acid 2+salts solution and Fe 3+salts solution slow evaporation makes gel precursor, more at high temperature calcination can obtain required product.Li Qiaoling etc. [Li Qiaoling, Wang Yongfei, Ye Yun. acicular nanometer Sr Fe 12o 19sol-gel method preparation and magnetic research [J]. Chinese Journal of Inorganic Chemistry, 2008,24(6): 907] the associating Complexing Sol-Gel Method of employing citrate-EDTA, having made particle diameter is the acicular nanometer iron strontium oxide magnetic particulate of six side's Magnetoplumbate-type structures of 30 n m, the method has shortened preparation cycle, and the particle diameter of material reduces, HCJ has also had significant raising.
Hydrothermal method is by M 2+salts solution and Fe 3+solution is put into autoclave under alkaline condition, under agitation condition, heats up, and reaches to react the some time after preset temperature and obtain product.Wei Yu etc. [Wei Yu, Zheng Xuezhong, Shao Suxia etc. applied science journal, 1997,15 (2): 242-247.] with Fe (NO 3) 39 H 2o solution and NaOH solution are raw material, adopt HEDP (1-Hydroxy Ethylidene-1,1-Diphosphonic Acid) as growth-regulating agent, have prepared aciculiform α-Fe by hydrothermal method 2o 3.Hydrothermal method has been avoided high-temperature roasting, so the particle size were making is little, size distribution is more even.But the deficiencies such as ubiquity productivity is low, length consuming time.
Summary of the invention
The object of this invention is to provide a kind of through chemically plating for one dimension spinel type ferrite A xb 1-xfe 2o 4method, the reaction times is short, cost is low, quality is high.
The technical scheme adopting is:
A kind of through chemically plating for one dimension spinel type ferrite A xb 1-xfe 2o 4method, it is characterized in that being coated layer of metal or alloy on one dimension ferriferous oxide surface by electroless plating, then obtain spinel type ferrite A through high-temperature roasting technique xb 1-xfe 2o 4, wherein A, B are Ni, Co, Cu or Zn, 0≤x≤1; One dimension ferriferous oxide, refers to the alpha-feooh, γ-FeOOH, the α-Fe that are needle-like or bar-shaped shape system 2o 3, or γ-Fe 2o 3, its particle length-to-diameter ratio>=5.
Described one dimension ferriferous oxide surface is coated layer of metal or alloy prior by electroless plating, comprises following processing step:
(1) sensitization: ferriferous oxide powder is joined in sensitizing solution, under room temperature, stir, leave standstill, suction filtration, washed with de-ionized water is to neutral;
Ferriferous oxide loading capacity: 5 ~ 15g/L,
Sensitizing solution composition: SnCl 20.05 ~ 0.2mol/L,
HCI 30~50mL/L，
Churning time: 0.5 ~ 2.5h;
(2) activation: by the ferriferous oxide powder after sensitization, join in the silver ammino solution preparing, stir, then leave standstill successively, suction filtration, washed with de-ionized water be to neutral, dry, obtains having the ferriferous oxide powder in active centre;
Ferriferous oxide loading capacity: 15 ~ 25g/L,
The composition of silver ammino solution: AgNO 35 ~ 15g/L,
Ammoniacal liquor: 5-15mL/L,
Churning time: 1.5 ~ 3h;
(3) prepare precursor powder: activated and dry powder is added in chemical plating fluid, stir, after powder standing sedimentation, suction filtration, washed with de-ionized water, to neutral, obtains presoma after being dried at 80 DEG C, and presoma is one dimension pattern.
Described roasting is: by precursor roasting 2-4h at 600-1200 DEG C, obtain ferrite A xb 1-xfe 2o 4.
Chemical plating fluid is chemical nickel-plating solution or chemical nickel plating cobalt liquor, chemical nickel plating copper solutions and chemical nickel plating zinc solution:
1, chemical nickel-plating solution composition and preparation technology are:
NiSO 4·6H 2O 0~30g/L，
NaH 2PO 2·H 2O 10~30g／L，
Na 3C 6H 5O 7·2H 2O 10~30g／L，
(NH 4) 2SO 4 10~30g／L，
pH： 8.0-10.0，
Temperature of reaction: 70 DEG C～95 DEG C,
Churning time: 15min ~ 1h;
2, chemical nickel plating cobalt liquor composition and preparation technology are:
CoSO 4·7H 2O 0~30g/L，
NaH 2PO 2·H 2O 10~30g／L，
Na 3C 6H 5O 7·2H 2O 10~30g／L，
(NH 4) 2SO 4 10~30g／L，
pH： 8.0-10.0，
Temperature of reaction: 70 DEG C～95 DEG C,
Churning time: 15min ~ 1h;
3, electroless nickel-copper solution composition and preparation technology are:
NiSO 4·6H 2O 1~3g/L，
CuSO 4·5H 2O 5~15g/L，
Na 3C 6H 5O 7·2H 2O 10~30g／L，
NaH 2PO 2·H 2O 20~50g／L，
H 3BO 3 20~50g／L，
pH： 8.0-11.0，
Temperature of reaction: 70 DEG C～95 DEG C,
Churning time: 0.5h ~ 1.5h;
4, chemically plating nickel-zinc solution composition and preparation technology are:
NiSO 4·6H 2O 5~15g/L，
NaH 2PO 2·H 2O 20~50g／L，
ZnSO 4 10~30g／L，
Na 3C 6H 5O 7·2H 2O 10~30g／L，
（NH 4） 3C 6H 5O 7 50~70g/L，
CH 3COONH 4 10~30g/L，
NaOH 50~100g／L，
pH： 8.0-11.0，
Temperature of reaction: 70 DEG C～95 DEG C,
Churning time: 1h ~ 2h.
Advantage of the present invention and feature:
The present invention is by preparing spinel type ferrite A by the technology of electroless plating xb 1-xfe 2o 4(A, B are Ni, Co, Cu or Zn, 0≤x≤1), compared with additive method, electroless plating method has the following advantages:
(1) in the inorganic materials such as powder, carry out Electroless Plating Ni, Co, the technique that Cu plasma is comparative maturity, is easily covered with required particle at stock chart bread.
(2) reaction conditions is simple, and the reaction times is short.
(3) conversion unit is simple, and required cost is lower.
Embodiment
Embodiment 1
A kind of through chemically plating for one dimension spinel type ferrite A xb 1-xfe 2o 4method, comprise the steps:
(1) by 1g γ-Fe 2o 3powder joins in the sensitizing solution by 2.3g tin protochloride, 5ml hydrochloric acid and the configuration of 95ml deionized water, under room temperature, stirs 30min, leaves standstill suction filtration, washed with de-ionized water.
(2) by cleaned γ-Fe 2o 3powder joins in the fresh silver ammino solution being prepared by 0.5g Silver Nitrate, a small amount of ammoniacal liquor and 50ml deionized water, stirs 2 hours, then leaves standstill successively, suction filtration, washed with de-ionized water, at 70 DEG C, is dried 3 hours.
(3) get dried γ-Fe 2o 3powder is put in the chemical plating fluid being made up of 2g single nickel salt, 2g inferior sodium phosphate, 2g Trisodium Citrate, 2g ammonium sulfate and 100ml deionized water, regulating the pH of plating solution is 9, be chemical nickel plating 0.5h at 90 DEG C in temperature, after plating finishes, by washed with de-ionized water, at 70 DEG C, be dried 3 hours again, obtain precursor.
(4) by precursor in 1000 DEG C of roasting 180min, obtain product.
γ-Fe 2o 3after chemical nickel plating, γ-Fe 2o 3be Rod-like shape, particle length is 0.4-1.2 μ m, and particle diameter is 100-150nm, and length-to-diameter ratio is 5-12; Nickel γ-Fe after electroless plating 2o 3precursor is Rod-like shape, and its particle length is 0.4-1.2 μ m, and particle diameter is 100-200nm, and length-to-diameter ratio is 5-12; After chemical nickel plating, γ-Fe 2o 3the length-to-diameter ratio of particle has no considerable change, but its particle diameter slightly increases.After precursor roasting, in sample, principal product is the NiFe that crystallization order degree is higher 2o 4, but wherein there is a small amount of α-Fe 2o 3dephasign.The Ni ferrite preparing is Rod-like shape, and its particle length is 0.5-1 μ m, and particle diameter is 200-250nm, and length-to-diameter ratio is 4-8.The saturation magnetization (Ms) of Ni ferrite is 37.69emu/g, and residual magnetization (Mr) is 13.87 emu/g, and coercive force (Hc) is 160Oe.With Yuan Jin etc. [Yuan enters, Lv Yongkang. nano-Ni/Fe 2o 4the Preparation and characterization of magnetic-particle. Northcentral University's journal, 2010,31(2): 141-144] NiFe for preparing by hydrothermal method 2o 4compare, Ms has improved 23.3 emu/g.
The present embodiment explanation, with bar-shaped γ-Fe 2o 3can prepare and there is obvious one-dimensional rod-like shape characteristic and the good Ni ferrite of magnetic property for raw material.
Embodiment 2
A kind of through chemically plating for one dimension spinel type ferrite A xb 1-xfe 2o 4method, comprise the steps:
Step is prepared Ni ferrite as described in Example 1, and different condition is by raw material γ-Fe 2o 3change alpha-feooh into.
The microscopic appearance of the standby Ni ferrite of alpha-feooh chemically plating is bar-shaped.Particle length is 0.6-1 μ m, and particle diameter is 100-200nm, length-to-diameter ratio 5-15; And its Ms is 36.46emu/g, Mr is 12.05 emu/g, and Hc is 134Oe.
Compared with embodiment 1, the present embodiment explanation, by feed change kind, can prepare the obvious spinel type Ni ferrite of one dimension pattern equally; In addition, can also regulate particle length-to-diameter ratio and the magnetic property of prepared Ni ferrite.
Embodiment 3
A kind of through chemically plating for one dimension spinel type ferrite A xb 1-xfe 2o 4method, comprise the steps:
The preparation step before electroless plating is carried out in step (1)-(2) as described in Example 1.
(3) by γ-Fe 2o 3powder is put in the chemical plating fluid being made up of 2g single nickel salt, 2g inferior sodium phosphate, 2g Trisodium Citrate, 2g ammonium sulfate and 100ml deionized water, regulating the pH of plating solution is 9, be at 90 DEG C, to carry out chemical nickel plating 15min in temperature, after plating finishes, by washed with de-ionized water, be to be dried 3 hours at 70 DEG C.
(4) get dried γ-Fe 2o 3powder is put in the chemical plating fluid being made up of 3g rose vitriol, 2g inferior sodium phosphate, 3g Trisodium Citrate, 5g ammonium sulfate and 100ml deionized water, regulating the pH of plating solution is 9, be at 90 DEG C, to carry out electroless cobalt plating 1h in temperature, after plating finishes, by washed with de-ionized water, and be dried 3 hours at 70 DEG C, obtain precursor.
(5) by precursor at 900 DEG C of roasting 180min, obtain product.
γ-Fe 2o 3the microscopic appearance of the standby nickel vectolite of chemically plating is corynebacterium, and particle length is 0.6-1 μ m, and particle diameter is 100-200nm, length-to-diameter ratio 4-10.Its Ms is 53.84emu/g, and Hc is 936Oe.Compared with embodiment 1, its Ms has increased by 16.15 emu/g, and Hc has increased 776Oe.The Ni preparing by sol-gel method with Wei Yanyan 0.5co 0.5fe 2o 4the Ms41.91 emu/g of nano microcrystalline compares, and its Ms has improved 11.93 emu/g.
The present embodiment explanation, by twice electroless plating, can prepare spinel type nickel vectolite.Compare with embodiment 1, the present embodiment explanation, by changing composition and the reaction conditions thereof of chemical plating fluid, can be to the chemical constitution of prepared spinel type ferrite, the major diameter of particle when magnetic property regulates.

Claims (2)

  1. One kind through chemically plating for one dimension spinel type ferrite A xb 1-xfe 2o 4method, it is characterized in that being coated layer of metal or alloy on one dimension ferriferous oxide surface by electroless plating, then obtain spinel type ferrite A through high-temperature roasting technique xb 1-xfe 2o 4, wherein A, B are Ni, Co, Cu or Zn, 0≤x≤1; One dimension ferriferous oxide, refers to the alpha-feooh, γ-FeOOH, the α-Fe that are needle-like or Rod-like shape 2o 3or γ-Fe 2o 3, its particle length-to-diameter ratio>=5; Described one dimension ferriferous oxide surface is coated layer of metal or alloy prior by electroless plating, comprises following processing step:
    (1) ferriferous oxide powder is joined in sensitizing solution, under room temperature, stir, leave standstill, suction filtration, washed with de-ionized water is to neutral;
    (2) activation: by the ferriferous oxide powder after sensitization, join in the silver ammino solution preparing, stir, then leave standstill successively, suction filtration, washed with de-ionized water be to neutral, dry, obtains having the ferriferous oxide powder in active centre;
    (3) prepare precursor powder: activated and dry powder is added in chemical plating fluid, stir, after powder standing sedimentation, suction filtration, washed with de-ionized water, to neutral, obtains presoma after being dried at 80 DEG C, and presoma is one dimension pattern.
  2. One according to claim 1 through chemically plating for one dimension spinel type ferrite A xb 1-xfe 2o 4method, it is characterized in that: chemical plating fluid is wherein a kind of in chemical nickel-plating solution, electroless cobalt plating solution, chemical nickel plating copper solutions or chemical nickel plating zinc solution:
    (1), chemical nickel-plating solution composition and preparation technology are:
    (2), electroless cobalt plating solution composition and preparation technology are:
    (3), electroless nickel-copper solution composition and preparation technology are:
    (4), chemically plating nickel-zinc solution composition and preparation technology are:
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CN114835169B (en) * 2022-05-24 2023-05-23 沈阳理工大学 Spinel type ferrite, preparation method thereof and wave absorbing material

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