CN101880156A - Method for synthesizing NiZnCu ferrite nano particles by sol-gel method taking water soluble polymers as ligands - Google Patents
Method for synthesizing NiZnCu ferrite nano particles by sol-gel method taking water soluble polymers as ligands Download PDFInfo
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- CN101880156A CN101880156A CN 201010227867 CN201010227867A CN101880156A CN 101880156 A CN101880156 A CN 101880156A CN 201010227867 CN201010227867 CN 201010227867 CN 201010227867 A CN201010227867 A CN 201010227867A CN 101880156 A CN101880156 A CN 101880156A
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Abstract
The invention discloses a method for synthesizing Ni<x>Zn<y>Cu<z>Fe<2>O<4> (wherein x + y + z = 1) ferrite nano powder which has the particle size of 5 to 100 nm. Water soluble polymers such as polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone, polyacrylic acid, alkyl ethylisobutyrate polymethacrylate, benzyl dimethylaminoethyl polymethacrylate, polyallylmethacrylate, alkyl imidazolone hydroxyl acetate polymethacrylate, cellulose derivative, chitosan and sodium alginate are taken as ligands, and cheap and water soluble metallic inorganic salts are taken as ferrite precursors to synthesize the Ni<x>Zn<y>Cu<z>Fe<2>O<4> (wherein x + y + z = 1) ferrite nano particles. The ferrite nano powder synthesized by a sol-gel method taking the water soluble polymers as the ligands is a nano material with narrow particle size distribution prepared at low temperature in short time. In the method, the inorganic salts are used as raw materials, so that the problem that the sol-gel method is generally difficult for industrial application is solved. The method has the characteristics of simple and convenient process and low cost, and can be applied to industrialized production.
Description
Technical field
The invention belongs to technical field of polymer materials, being specifically related to the water-soluble polymer is the NiZnCu ferrite nano particles of the synthetic different-grain diameter of sol-gel method of part.
Background technology
Spinel type ferrite is important commercial material because its good magnetic property and electrical property form.Multilayer chip inductor (MLCI) is greatly developed as indispensable element in the surface installation technique in recent years, it is to burn the monolithic structure that forms altogether by Ferrite Material and electrode materials alternative stacked, burn requirement altogether for satisfying with silver electrode, low temperature sintered ferrite material becomes key problem in technology.The NiZnCu ferrite is best, the most widely used a kind of high-frequency soft magnetic material of present performance, thereby becomes the best dielectric material of MLCI.But the ferritic sintering temperature of NiZnCu is generally higher, can not satisfy the needs that burn altogether with silver electrode among the MLCI.Usually reduce firing temperature by the method for adding low-melting-point glass phase or sintering agent, but magnetic property is reduced.
Studies show that adopting the ultrafine high activity nanometer powder is the effective way that realizes low-temperature sintering and high performance, has synthesized the ferrite particle of particle diameter in the 5-100nm scope by coprecipitation method, ball milled, hydrothermal synthesis method and sol-gel method.In these methods, sol-gel method has special advantages: the narrower nano material of size distribution is controlled and obtained to strict stoichiometry under short period of time and cold condition.But it is raw material that sol-gel method generally adopts metal organic salt, thereby cost is higher, is difficult to widespread use in industry.The present invention uses water-soluble polymer to be part, is the ferrite presoma with inexpensive water-soluble metal inorganic salt, successfully synthesizes the Ni of different-grain diameter by sol-gel method
xZn
yCu
zFe
2O
4(x+y+z=1) ferrite nano particles.
Summary of the invention
The objective of the invention is to obtain under short period of time and the cold condition the narrower nano material of size distribution.This technology has the advantage that cost is low, technology simple, be convenient to suitability for industrialized production.
Technical scheme of the present invention is as follows:
A kind of ferrite nano particles is characterized in that its component is NiZnCu, and the particle diameter of magnetic particle is 5-100nm.Adopting water-soluble polymer polyvinyl alcohol, polyoxyethylene glycol, polyvinylpyrrolidone, polyacrylic acid, polymethyl acrylic acid isobutyl alkyl ethyl ester, polymethyl acrylic acid dimethylamine benzyl ethyl ester, polymethyl acid propylene ester, polymethyl acrylic acid imidazolidyl ketone hydroxyl ethyl ester, derivatived cellulose, chitosan, sodium alginate is part, with water-soluble metal inorganic salt is the ferrite presoma, can obtain single-phase spinel type NiZnCu ferrite nano particles through thermal treatment, its normal temperature magnetic of the sample that obtains is adjustable between ferrimagnetism by superparamagnetism.
A kind of water-soluble polymer is the method for the synthetic NiZnCu ferrite nano particles of sol-gel method of part, it is characterized in that the concrete steps of this method are as follows:
A. with Ni
xZn
yCu
zFe
2O
4The water-soluble inorganic salt of the nickel that molar ratio weighing (x+y+z=1) is good, zinc, copper and iron, be dissolved in the deionized water, add water-soluble polymer, hydroxyl, carboxyl, amino or carbonyl in the control water-soluble polymer or the mol ratio that contains unsaturated double-bond group and water-soluble inorganic salt are (1-10): (1-10);
B. be stirred to water-soluble polymer and dissolve fully, slowly evaporation is up to forming colloidal sol down at 20-80 ℃ for solution, and colloidal sol gets xerogel at 50-120 ℃ of dry 1-48h then;
C. xerogel is got the ferrite nano particles of black after with the mortar porphyrize through 150-1200 ℃ of thermal treatment 0.5-48h in air atmosphere.
The ferriferous oxide nano-powder of the present invention's preparation, particle diameter is far smaller than conventional particle at 5-100nm.Adopting water-soluble polymer polyvinyl alcohol, polyoxyethylene glycol, polyvinylpyrrolidone, polyacrylic acid, polymethyl acrylic acid isobutyl alkyl ethyl ester, polymethyl acrylic acid dimethylamine benzyl ethyl ester, polymethyl acid propylene ester, polymethyl acrylic acid imidazolidyl ketone hydroxyl ethyl ester, derivatived cellulose, chitosan, sodium alginate is part, with inexpensive water-soluble metal nitrate is the ferrite presoma, has synthesized the Ni of different-grain diameter
xZn
yCu
zFe
2O
4(x+y+z=1) ferrite nano particles.Through the sample that 150-1200 ℃ of thermal treatment obtains, along with the raising of thermal treatment temp, its normal temperature magnetic of sample is adjustable between ferrimagnetism by superparamagnetism.Ni
xZn
yCu
zFe
2O
4(x+y+z=1) saturation magnetization of ferrite nano particles and coercive force are respectively 5.00-100.00emu/g and 6.00-80.00Oe.
Water-soluble polymer of the present invention is that the sol-gel method synthetic iron oxygen nano-powder of part is to obtain the narrower nano material of size distribution under short period of time and cold condition.The present invention uses inorganic salt to be raw material, solved sol-gel method and generally be difficult to the problem used in industry.It is easy that the present invention has technology, and the characteristics that cost is low can be used in suitability for industrialized production.
Embodiment
Describe the present invention below in conjunction with embodiment.
Embodiment 1
With the 1.19g nickelous nitrate, 0.47g zinc nitrate, 0.19g cupric nitrate, 4.84g iron nitrate is dissolved in the deionized water, adds the 10g polyvinyl alcohol, is stirred to polyvinyl alcohol and dissolves fully, solution is 50 ℃ of slowly evaporations down, get xerogel at 70 ℃ of dry 24h, xerogel is got the ferrite nano particles of black after with the mortar porphyrize through 150 ℃ of thermal treatment 2h in air atmosphere, its particle diameter is about 10nm.The saturation magnetization of ferrite nano particles and coercive force are respectively 5.21emu/g and 6.51Oe.
Embodiment 2
With the 14.64g nickelous nitrate, 3.76g cupric nitrate, 42.57 the gram iron nitrate is dissolved in the deionized water, add the 15g polyacrylic acid, be stirred to polyacrylic acid and dissolve fully, solution gets xerogel 40 ℃ of slowly evaporations down at 75 ℃ of dry 12h, xerogel is got the ferrite nano particles of black after with the mortar porphyrize through 250 ℃ of thermal treatment 2h in air atmosphere, its particle diameter is about 15nm.The saturation magnetization of ferrite nano particles and coercive force are respectively 31.52emu/g and 28.42Oe.
Embodiment 3
With the 9.45g zinc nitrate, 9.4g cupric nitrate, 53.89 the gram iron nitrate is dissolved in the deionized water, add the 20g polyoxyethylene glycol, be stirred to polyoxyethylene glycol and dissolve fully, solution gets xerogel 50 ℃ of slowly evaporations down at 70 ℃ of dry 30h, xerogel is got the ferrite nano particles of black after with the mortar porphyrize through 450 ℃ of thermal treatment 5h in air atmosphere, its particle diameter is about 15nm.The saturation magnetization of ferrite nano particles and coercive force are respectively 43.21emu/g and 38.51Oe.
Embodiment 4
With the 48.4g iron nitrate, 11.9g nickelous nitrate, 6.61g zinc nitrate, 48.4g iron nitrate is dissolved in the deionized water, adds polymethyl acrylic acid isobutyl alkyl ethyl ester 20g, is stirred to polymethyl acrylic acid isobutyl alkyl ethyl ester and dissolves fully, solution is 80 ℃ of slowly evaporations down, get xerogel at 110 ℃ of dry 15h, xerogel is got the ferrite nano particles of black after with the mortar porphyrize through 550 ℃ of thermal treatment 2.5h in air atmosphere, its particle diameter is about 17nm.The saturation magnetization of ferrite nano particles and coercive force are respectively 55.61emu/g and 79.31Oe.
Embodiment 5
With the 2.38g nickelous nitrate, 0.95g zinc nitrate, 0.38g cupric nitrate, 48.4g iron nitrate is dissolved in the deionized water, adds the 15g carboxymethyl cellulose, is stirred to carboxymethyl cellulose and dissolves fully, solution is 70 ℃ of slowly evaporations down, get xerogel at 120 ℃ of dry 40h, xerogel is got the ferrite nano particles of black after with the mortar porphyrize through 800 ℃ of thermal treatment 2h in air atmosphere, its particle diameter is about 20nm.The saturation magnetization of ferrite nano particles and coercive force are respectively 68.52emu/g and 43.41Oe.
Embodiment 6
With the 118.95g nickelous nitrate, 47.25g zinc nitrate, 18.8g cupric nitrate, the 484g iron nitrate is dissolved in the deionized water, adds the 20g chitosan, is stirred to chitosan and dissolves fully, solution is 80 ℃ of slowly evaporations down, get xerogel at 120 ℃ of dry 50h, xerogel is got the ferrite nano particles of black after with the mortar porphyrize through 1050 ℃ of thermal treatment 5h in air atmosphere, its particle diameter is about 20nm.The saturation magnetization of ferrite nano particles and coercive force are respectively 70.61emu/g and 31.23Oe.
Claims (2)
1. the method for a water-soluble polymer synthetic NiZnCu ferrite nano particles of sol-gel method that is part is characterized in that the concrete steps of this method are as follows:
A. press chemical formula Ni
xZn
yCu
zFe
2O
4The water-soluble inorganic salt of good nickel, zinc, copper and the iron of molar ratio weighing, x+y+z=1 wherein, be dissolved in the deionized water, add water-soluble polymer, hydroxyl in the control water-soluble polymer or carboxyl or amino or carbonyl or contained other unsaturated double-bond groups and the mol ratio of water-soluble inorganic salt are 1-10: 1-10;
B. be stirred to water-soluble polymer and dissolve fully, slowly evaporation is up to forming colloidal sol down at 20-80 ℃ for solution, and colloidal sol gets xerogel at 50-120 ℃ of dry 1-48h then;
C. xerogel is got the ferrite nano particles of black after with the mortar porphyrize through 150-1200 ℃ of thermal treatment 0.5-10h in air atmosphere.
2. one kind by the described method of claim 1, it is characterized in that described water-soluble polymer is a kind of in polyvinyl alcohol, polyoxyethylene glycol, polyvinylpyrrolidone, polyacrylic acid, polymethyl acrylic acid isobutyl alkyl ethyl ester, polymethyl acrylic acid dimethylamine benzyl ethyl ester, polymethyl acid propylene ester, polymethyl acrylic acid imidazolidyl ketone hydroxyl ethyl ester, derivatived cellulose, chitosan, the sodium alginate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110075886A (en) * | 2019-05-31 | 2019-08-02 | 中南林业科技大学 | Ni-based-carbon composite electrocatalyst and preparation method thereof |
| CN116040695A (en) * | 2022-12-29 | 2023-05-02 | 国网智能电网研究院有限公司 | Lamellar nickel-copper-zinc ferrite nano material and preparation method 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 (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1107128A (en) * | 1994-12-03 | 1995-08-23 | 西安交通大学 | High quality low-temp. agglutination negative temp. coefficient dielectric ceramic |
| CN1858021A (en) * | 2005-08-11 | 2006-11-08 | 横店集团东磁有限公司 | Mn-Zn ferrite material |
-
2010
- 2010-07-15 CN CN 201010227867 patent/CN101880156A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1107128A (en) * | 1994-12-03 | 1995-08-23 | 西安交通大学 | High quality low-temp. agglutination negative temp. coefficient dielectric ceramic |
| CN1858021A (en) * | 2005-08-11 | 2006-11-08 | 横店集团东磁有限公司 | Mn-Zn ferrite material |
Non-Patent Citations (1)
| Title |
|---|
| 《Journal of Alloys and Compounds》 20061206 Shifeng Yan et al. Study on the synthesis of NiZnCu ferrite nanoparticles by PVA sol-gel method and their magnetic properties 参见第2节第1段 1、2 第450卷, * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110075886A (en) * | 2019-05-31 | 2019-08-02 | 中南林业科技大学 | Ni-based-carbon composite electrocatalyst and preparation method 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 |
| CN116040695A (en) * | 2022-12-29 | 2023-05-02 | 国网智能电网研究院有限公司 | Lamellar nickel-copper-zinc ferrite nano material and preparation method thereof |
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Application publication date: 20101110 |