CN102719812A - 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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CN102719812A
CN102719812A CN2012101694129A CN201210169412A CN102719812A CN 102719812 A CN102719812 A CN 102719812A CN 2012101694129 A CN2012101694129 A CN 2012101694129A CN 201210169412 A CN201210169412 A CN 201210169412A CN 102719812 A CN102719812 A CN 102719812A
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plating
dimension
ferriferous oxide
spinel type
type ferrite
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CN102719812B (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 ofly prepare one dimension spinel type ferrite A through electroless plating 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 the ferriferous oxide surface, through obtaining the one dimension spinel type ferrite after the high-temperature roasting.
Background technology
The 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 chemical constitution characteristics make it both have ferromagnetism, certain dielectricity, good mechanical property; Higher intensity and erosion resistance, and chemicalstability is better, can be applicable to various fields; Mainly comprise the absorbing material aspect, medical aspect, catalysis aspect etc.
At present, the ferritic preparation method of one dimension pattern has many, and common have chemical coprecipitation, hydrothermal method, a sol-gel method etc.
Chemical coprecipitation divides two types, and one is to use precipitation agent that divalent metal salt and trivalent iron salt is heavy altogether, and high-temperature roasting obtains product.Its advantage is that technology is simple, but deposition is colloidal state more, therefore is difficult for filtering and washing.The 2nd, mineral alkali is added in the solution of divalent metal salt and divalent iron salt, bubbling air makes it oxidation, can get product after the reaction some time.Liu Hui etc. [Liu Hui, Wei Yu. nano-size ferrates powder body material synthetic progress functional materials, 2000,31 (2): 124～125] utilize chemical precipitation method can make the CuFe of particle diameter for 50nm 2O 4, this method is easy to operate, equipment is simple, the advantages such as pure phase and granularity easy to control that are easy to get, but the proportioning of reaction mass, temperature of reaction and oxidization time have considerable influence to result's quality.
Sol-gel method is made part with M through organic acid 2+Salts solution and Fe 3+Salts solution slowly evaporation makes the gel precursor, and calcination at high temperature can get required product again.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 Hydrocerol A-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, this method has shortened preparation cycle; And the particle diameter of material reduces, and HCJ has also had significant raising.
Hydrothermal method is with M 2+Salts solution and Fe 3+Solution is put into autoclave under alkaline condition, under agitation condition, heat up, and reaches the preset temperature afterreaction some time promptly to 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 (HEDP) as growth-regulating agent, have gone out aciculiform α-Fe through Hydrothermal Preparation 2O 3Hydrothermal method has been avoided high-temperature roasting, so the product particle diameter that makes is little, size distribution is more even.But deficiencies such as ubiquity productivity is low, length consuming time.
Summary of the invention
The purpose of this invention is to provide and a kind ofly prepare one dimension spinel type ferrite A through electroless plating xB 1-xFe 2O 4Method, the reaction times is short, cost is low, quality is high.
The technical scheme that adopts is:
A kind ofly prepare one dimension spinel type ferrite A through electroless plating xB 1-xFe 2O 4Method, it is characterized in that coating layer of metal or alloy through electroless plating on one dimension ferriferous oxide surface, obtain spinel type ferrite A through high-temperature roasting technology again xB 1-xFe 2O 4, wherein A, B are Ni, Co, Cu or Zn, 0≤x≤1; The one dimension ferriferous oxide is meant 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.
Said one dimension ferriferous oxide surface coats layer of metal or alloy prior through electroless plating, comprises following process step:
(1) sensitization: the ferriferous oxide powder is joined in the sensitizing solution, stir under the room temperature, leave standstill, suction filtration, washed with de-ionized water is to neutral;
Ferriferous oxide tonburden: 5 ~ 15g/L,
Sensitizing solution is formed: SnCl 20.05 ~ 0.2mol/L,
HCI 30~50mL/L，
Churning time: 0.5 ~ 2.5h;
(2) activation: with the ferriferous oxide powder after the sensitization, join in the silver ammino solution for preparing, stir, leave standstill successively then, suction filtration, washed with de-ionized water be to neutral, dry, obtains having the ferriferous oxide powder in active site;
Ferriferous oxide tonburden: 15 ~ 25g/L,
The composition of silver ammino solution: AgNO 35 ~ 15g/L,
Ammoniacal liquor: 5-15mL/L,
Churning time: 1.5 ~ 3h;
(3) preparation precursor powder: add activated and exsiccant powder in the chemical plating fluid, stir, treat the powder standing sedimentation after, suction filtration, washed with de-ionized water obtains presoma to neutrality after 80 ℃ of following dryings, presoma is the one dimension pattern.
Said roasting is: precursor at 600-1200 ℃ of following roasting 2-4h, is obtained 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 2O10~30g／L，
Na 3C 6H 5O 7·2H 2O10~30g／L，
(NH 4) 2SO 4?10~30g／L，
pH： 8.0-10.0，
Temperature of reaction: 70 ℃～95 ℃,
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 410~30g／L，
pH： 8.0-10.0，
Temperature of reaction: 70 ℃～95 ℃,
Churning time: 15min ~ 1h;
3, chemical nickel plating copper solutions 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 320~50g／L，
pH： 8.0-11.0，
Temperature of reaction: 70 ℃～95 ℃,
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 ℃～95 ℃,
Churning time: 1h ~ 2h.
Advantage of the present invention and characteristics:
The present invention prepares spinel type ferrite A through the technology of using electroless plating xB 1-xFe 2O 4(A, B are Ni, Co, Cu or Zn, 0≤x≤1), with data by MoM and MEI, electroless plating method has the following advantages:
(1) on inorganic materials such as powder, carry out Electroless Plating Ni, Co, Cu plasma are the technology of comparative maturity, are covered with required particle at stock chart bread easily.
(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 ofly prepare one dimension spinel type ferrite A through electroless plating xB 1-xFe 2O 4Method, comprise the steps:
(1) with 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, stirs 30min under the room temperature, leaves standstill suction filtration, washed with de-ionized water.
(2) with cleaned γ-Fe 2O 3Powder joins in the fresh silver ammino solution that is prepared by 0.5g Silver Nitrate, less ammonia and 50ml deionized water, stirs 2 hours, leave standstill successively then, suction filtration, washed with de-ionized water, 70 ℃ dry 3 hours down.
(3) get dry good γ-Fe 2O 3Powder is put in the chemical plating fluid of being made up of 2g single nickel salt, 2g inferior sodium phosphate, 2g Trisodium Citrate, 2g ammonium sulfate and 100ml deionized water; The pH that regulates plating bath is 9; In temperature is 90 ℃ of following chemical nickel plating 0.5h, and plating is used washed with de-ionized water after finishing; In 70 ℃ times dry 3 hours, get precursor again.
(4) with precursor in 1000 ℃ of roasting 180min, promptly obtain product.
γ-Fe 2O 3Behind the chemical nickel plating, γ-Fe 2O 3Be bar-shaped pattern, 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 the electroless plating 2O 3Precursor is bar-shaped pattern, 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; Behind the chemical nickel plating, γ-Fe 2O 3The particulate length-to-diameter ratio is not seen considerable change, but its particle diameter slightly increases.After the precursor roasting, principal product is the higher NiFe of crystallization order degree in the sample 2O 4, but wherein have a small amount of α-Fe 2O 3Dephasign.The Ni ferrite for preparing is bar-shaped pattern, 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 of Ni ferrite (Ms) is 37.69emu/g, and residual magnetization (Mr) is 13.87 emu/g, and coercive force (Hc) is 160Oe.With Yuan Jin etc. [Yuan advances, Lv Yongkang. nano-Ni/Fe 2O 4The preparation of magnetic-particle and sign. Northcentral University's journal, 2010,31 (2): 141-144] NiFe through Hydrothermal Preparation 2O 4Compare, Ms has improved 23.3 emu/g.
The present embodiment explanation is with bar-shaped γ-Fe 2O 3Can prepare for raw material and to have obvious one-dimensional rod-like shape characteristic and magnetic property Ni ferrite preferably.
Embodiment 2
A kind ofly prepare one dimension spinel type ferrite A through electroless plating xB 1-xFe 2O 4Method, comprise the steps:
Prepare Ni ferrite like embodiment 1 said step, different condition is with raw material γ-Fe 2O 3Change alpha-feooh into.
The microscopic appearance of the Ni ferrite of alpha-feooh electroless plating preparation 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, and Mr is 12.05 emu/g, and Hc is 134Oe.
Compare with embodiment 1, the present embodiment explanation can prepare the tangible spinel type Ni ferrite of one dimension pattern equally through changing raw material type; In addition, can also regulate the particle length-to-diameter ratio and the magnetic property of prepared Ni ferrite.
Embodiment 3
A kind ofly prepare one dimension spinel type ferrite A through electroless plating xB 1-xFe 2O 4Method, comprise the steps:
Carry out the preceding preparation step of electroless plating like embodiment 1 said step (1)-(2).
(3) with γ-Fe 2O 3Powder is put in the chemical plating fluid of being made up of 2g single nickel salt, 2g inferior sodium phosphate, 2g Trisodium Citrate, 2g ammonium sulfate and 100ml deionized water; The pH that regulates plating bath is 9; In temperature is to carry out chemical nickel plating 15min under 90 ℃; After treating that plating finishes, use washed with de-ionized water, be 70 ℃ of following dryings 3 hours.
(4) get dry good γ-Fe 2O 3Powder is put in the chemical plating fluid of being made up of 3g rose vitriol, 2g inferior sodium phosphate, 3g Trisodium Citrate, 5g ammonium sulfate and 100ml deionized water; The pH that regulates plating bath is 9; In temperature is to carry out electroless cobalt plating 1h under 90 ℃, treat that plating finishes after, use washed with de-ionized water; And, get precursor in 70 ℃ times dry 3 hours.
(5) with precursor at 900 ℃ of roasting 180min, obtain product.
γ-Fe 2O 3The microscopic appearance of the nickel vectolite of electroless plating preparation is a 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.Compare with embodiment 1, its Ms has increased by 16.15 emu/g, and Hc has increased 776Oe.With the Ni of Wei Yanyan through the sol-gel method preparation 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 through twice electroless plating, can prepare spinel type nickel vectolite.Compare with embodiment 1, the present embodiment explanation, through changing the composition and the reaction conditions thereof of chemical plating fluid, can be to the chemical constitution of prepared spinel type ferrite, particulate major diameter when magnetic property is regulated.

Claims (3)

1. one kind prepares one dimension spinel type ferrite A through electroless plating xB 1-xFe 2O 4Method, it is characterized in that coating layer of metal or alloy through electroless plating on one dimension ferriferous oxide surface, obtain spinel type ferrite A through high-temperature roasting technology again xB 1-xFe 2O 4, wherein A, B are Ni, Co, Cu or Zn, 0≤x≤1; The one dimension ferriferous oxide is meant 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.
2. according to claim 1ly a kind ofly prepare one dimension spinel type ferrite A through electroless plating xB 1-xFe 2O 4Method, it is characterized in that: said one dimension ferriferous oxide surface coats layer of metal or alloy prior through electroless plating, comprises following process step:
(1) sensitization: the ferriferous oxide powder is joined in the sensitizing solution, stir under the room temperature, leave standstill, suction filtration, washed with de-ionized water is to neutral;
Ferriferous oxide tonburden: 5 ~ 15g/L,
Sensitizing solution is formed: SnCl 20.05 ~ 0.2mol/L,
HCI 30~50mL/L，
Churning time: 0.5 ~ 2.5h;
(2) activation: with the ferriferous oxide powder after the sensitization, join in the silver ammino solution for preparing, stir, leave standstill successively then, suction filtration, washed with de-ionized water be to neutral, dry, obtains having the ferriferous oxide powder in active site;
Ferriferous oxide tonburden: 15 ~ 25g/L,
The composition of silver ammino solution: AgNO 35 ~ 15g/L,
Ammoniacal liquor: 5-15mL/L,
Churning time: 1.5 ~ 3h;
(3) preparation precursor powder: add activated and exsiccant powder in the chemical plating fluid, stir, treat the powder standing sedimentation after, suction filtration, washed with de-ionized water obtains presoma to neutrality after 80 ℃ of following dryings, presoma is the one dimension pattern.
3. according to claim 1ly a kind ofly prepare one dimension spinel type ferrite A through electroless plating xB 1-xFe 2O 4Method, it is characterized in that: 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 2O10~30g／L，
Na 3C 6H 5O 7·2H 2O10~30g／L，
(NH 4) 2SO 4?10~30g／L，
pH： 8.0-10.0，
Temperature of reaction: 70 ℃～95 ℃,
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 410~30g／L，
pH： 8.0-10.0，
Temperature of reaction: 70 ℃～95 ℃,
Churning time: 15min ~ 1h;
(3), chemical nickel plating copper solutions 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 320~50g／L，
pH： 8.0-11.0，
Temperature of reaction: 70 ℃～95 ℃,
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 ℃～95 ℃,
Churning time: 1h ~ 2h.
CN201210169412.9A 2012-05-29 2012-05-29 Method for preparing one-dimensional spinel type ferrite AxB1-xFe2O4 through chemical plating Active CN102719812B (en)

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CN114835169A (en) * 2022-05-24 2022-08-02 沈阳理工大学 Spinel type ferrite, preparation method thereof and wave-absorbing material

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