CN105195755A - Method for preparing iron-nickel bimetallic alloy nano material - Google Patents
Method for preparing iron-nickel bimetallic alloy nano material Download PDFInfo
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- CN105195755A CN105195755A CN201410259045.0A CN201410259045A CN105195755A CN 105195755 A CN105195755 A CN 105195755A CN 201410259045 A CN201410259045 A CN 201410259045A CN 105195755 A CN105195755 A CN 105195755A
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Abstract
The invention discloses a method for preparing an iron-nickel bimetallic alloy nano material through the sol-gel process. The method comprises the following steps that 1, a mixed solution of ferric nitrate and nickel nitrate is prepared, a chelating agent is added while stirring, the molar ratio of nitrate to the chelating agent is 1:0.5-1:5, the chelating agent is any one of lactic acid, malic acid, saccharose and citric acid, and finally a certain quantity of dispersing agents is added; 2, the solution is dried for 8-12 hours at the temperature of 90 DEG C to 150 DEG C till porous dry gel is obtained; 3, in an argon atmosphere, high-heat treatment is carried out on the dry gel at the temperature of 400 DEG C to 700 DEG C, and therefore the iron-nickel bimetallic alloy nano material is obtained. The preparation process is simple, energy is saved, the method is suitable for industrial production, and the obtained iron-nickel bimetallic alloy nano material is uniform in grain size, good in dispersity and high in stability.
Description
Technical field
The present invention relates to a kind of bimetallic alloy nano material, especially relate to a kind of preparation method of iron nickel bimetal alloy nano-material.
Background technology
Iron nickel bimetal alloy material, as the widely used material of one, plays unrivaled effect in present industrial technology.Iron nickel bimetal material is in the application aspect of magnetic material, and compared with silicon steel sheet, its maximum feature is exactly in low-intensity magnetic field, have good magnetic property.Because it has favorable comprehensive mechanical property, in structural absorbing mater ials and coat absorbing material, iron-nickel alloy material also plays huge effect; Iron-nickel alloy material has good magnetic in low-intensity magnetic field, there is higher saturation magnetization, coercivity and signal to noise ratio, thus also can be widely used in the field such as control system, precision instrumentation, bimetallic element and glass, size constancy part as expansion alloy and soft magnetic materials; Fe-Ni Alloy Powder as bimetallic catalyst, active, selective, stability and resistance to poisoning etc. in be all better than the catalyst that traditional monometallic iron and nickel makes.In addition, Fe-Ni Alloy Powder also has other purposes widely: plate iron-nickel alloy at fabric face, makes the composite of iron-nickel alloy and fabric, fabric not only can be made to have flexible nature, also make it have electromagnetic shielding and sound damping.
Based on the extensive use of iron-nickel alloy in actual production, researchers conduct in-depth research and exploration its preparation method, have impelled the preparation method of iron-nickel alloy to be constantly tending towards development with ripe.At present, the method preparing iron-nickel alloy material mainly contains liquid phase reduction, machine-alloying, microwave plasma method, introduction by magnetic field pyrolysis of carbonyl method and template etc.These methods respectively have pluses and minuses, and liquid phase reduction has that equipment is simple, cost-saving, particle size distribution is narrow and the advantage such as chemical uniformity is good, but the powder particle prepared is easier to assemble, the NaBH used in experimentation
4toxicity is comparatively large, hinders production to a certain extent.Machine-alloying production equipment is fairly simple, and efficiency comparison is high, but the powder produced depends on that stress applies mode, breaking method, disintegrating process condition, pulverizes the factors such as environment, be difficult to control in actual production process, the powder otherness produced is also larger, is unfavorable for producing.Microwave plasma legal system is continuous for nano-powder material process, and chemical reaction velocity is fast, and reaction temperature low (300-900 DEG C) good stability, carries out at ambient pressure, and the nanometer powder purity of synthesis is high.The price of this method to be shortcoming be equipment needed thereby is higher, and production efficiency is low.Powder morphology prepared by template is more homogeneous, is a kind of preparation method that effectively can control powder size and pattern, but is difficult to the continuity and the scale that realize production.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of controlled iron nickel bimetal alloy nano-material, existing complicated synthetic technology energy consumption be large to overcome, the deficiency of contaminated environment, flow process complexity.
The technical solution realizing the object of the invention is: a kind of preparation method of iron nickel bimetal alloy nano-material, comprises the following steps:
1. the preparation of mixed liquor
Select water or absolute ethyl alcohol as solvent, ferric nitrate and nickel nitrate are as solute, chelating agent selects the one in lactic acid, malic acid, sucrose or citric acid, nitrate, chelating agent, dispersant, as dispersant, join in water or absolute ethyl alcohol by lauryl sodium sulfate (SDS) or oleic acid (OA) successively;
2. dry
Above-mentioned mixed solution is placed in 90-140 DEG C of drying box dry, until the complete evaporate to dryness of moisture becomes xerogel;
3. heat treatment
Xerogel is placed in the tube furnace being connected with protection gas and calcines.
The mol ratio of the ferric nitrate described in step 1 and nickel nitrate is 1:3; The molar concentration of iron nitrate solution is 0.01-0.03mol/L.
The mol ratio of the iron described in step 1, nickel ion sum and chelating agent is 1:0.5-1:5; The mol ratio of iron, nickel ion sum and dispersant is 1:1-1:3.
Drying time described in step 2 is 8-12 hour.
Protection gas described in step 3 is argon gas, and described shielding gas flow amount is 10-20ml/min; Calcining temperature required is 400-700 DEG C; Calcination time is 2-6 hour; Heating rate is 5-15 DEG C/min.
Compared with prior art, the invention has the advantages that;
1) instant invention overcomes large, high to equipment requirement, the heavy-polluted shortcoming of existing synthetic technology energy consumption, there is technique simple, raw material is easy to get, what slaine was selected is nitrate, what chelating agent was selected is the carbohydrate of some non-toxic inexpensives, initial reaction mild condition, does not occur in experimentation the influential toxic gas of environment.
2) the iron nickel bimetal alloy nano-material favorable dispersibility prepared by the present invention, epigranular, stability are high.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of iron-nickel alloy nano material in the embodiment of the present invention 1.
Fig. 2 is the X-ray diffractogram of iron-nickel alloy nano material in the embodiment of the present invention 2.
Fig. 3 is transmission electron microscope (TEM) picture of iron-nickel alloy nano material in embodiment 2.
Fig. 4 is the X-ray energy spectrum analysis result of iron-nickel alloy nano material in the embodiment of the present invention 3.
Fig. 5 is the X-ray diffractogram of iron-nickel alloy nano material in the embodiment of the present invention 4.
Fig. 6 is superconductive quantum interference test (SQUID) result of iron-nickel alloy nano material in the embodiment of the present invention 4.
Detailed description of the invention
Below in conjunction with example and accompanying drawing, the present invention is described in detail.
Embodiment 1: at room temperature take 0.4102g ferric nitrate and 0.8903g nickel nitrate is dissolved in 100ml absolute ethyl alcohol, open and stir, make its abundant mixed dissolution, and then in solution, add 15ml dispersant oleic acid and 1.8200g chelating agent lactic acid, continue to stir 10min.Mixed solution is heated 2 hours under water bath condition, then solution to be put in drying box at 140 DEG C dry 8 hours, obtain xerogel, then xerogel is put in heat treatment in tube furnace, the heating rate controlling tube furnace is 5 DEG C/min, and heat treatment temperature is 400 DEG C, and the time is 6 hours.Continue in tube furnace during heat treatment to pass into argon gas as protection gas, the flow of gas is 10ml/min.After calcining terminates, close tube furnace, after the temperature of tube furnace reduces to room temperature, stop passing into protection gas, product is taken out.Fig. 1 is the X-ray diffractogram of obtained iron nickel bimetal alloy nano-material, be 44.28,51.53,75.90 ° in the angle of diffraction as can be seen from Figure 1 and occur three diffraction maximums clearly, homologue phase structure is (111), (200), (220) crystal face of face-centered cubic iron-nickel alloy respectively, and these diffraction maximums have very large halfwidth, show that the crystallite dimension of product is less.
Embodiment 2: the deionized water measuring 100ml is placed in glass beaker, then 0.8204g ferric nitrate and 1.7806g nickel nitrate is added, magnetic agitation is dissolved completely to nitrate, then 4.3125g malic acid is added in the solution as chelating agent, magnetic agitation adds 0.6g dispersant lauryl sodium sulfate again to solution clarification in solution, continue to stir until dispersant dissolves completely, mixed solution is heated 2 hours under water bath condition, again solution to be put in drying box at 120 DEG C dry 10 hours, obtain xerogel, then xerogel is put in heat treatment in tube furnace, the heating rate controlling tube furnace is 10 DEG C/min, heat treatment temperature is 500 DEG C, time is 5 hours.Continue in tube furnace during heat treatment to pass into argon gas as protection gas, the flow of gas is 15ml/min.After calcining terminates, close tube furnace, after the temperature of tube furnace reduces to room temperature, stop passing into protection gas, product is taken out.The characterization result of the transmission electron microscope (Fig. 3) of sample proves that the crystallite dimension of the iron nickel bimetal alloy nano-material of preparation is 5-20 nanometer.
Embodiment 3: at room temperature take 1.2306g ferric nitrate and 2.6709g nickel nitrate is dissolved in 100ml deionized water, open and stir, make its abundant mixed dissolution, and then in solution, add 0.3g dispersant lauryl sodium sulfate and 8.3102g chelating agent sucrose, continue to stir 10min.Mixed solution is heated 2 hours under water bath condition, then solution to be put in drying box at 100 DEG C dry 12 hours, obtain xerogel, then xerogel is put in heat treatment in tube furnace, the heating rate controlling tube furnace is 15 DEG C/min, and heat treatment temperature is 600 DEG C, and the time is 3 hours.Continue in tube furnace during heat treatment to pass into argon gas as protection gas, the flow of gas is 5ml/min.After calcining terminates, close tube furnace, after the temperature of tube furnace reduces to room temperature, stop passing into protection gas, product is taken out.Fig. 4 is the X-ray energy spectrum analysis result of the sample of obtained iron nickel bimetal alloy nano-material, and result shows that the surface of product only has Fe and Ni two kinds of elements, and the mass ratio of two kinds of elements is 79.53:20.47.
Embodiment 4: at room temperature take 1.2306g ferric nitrate and 2.6709g nickel nitrate is dissolved in 100ml deionized water, open and stir, make its abundant mixed dissolution, and then in solution, add 0.3g dispersant lauryl sodium sulfate and 1.2672g chelator acid citrate, continue to stir 10min.Mixed solution is heated 2 hours under water bath condition, then solution to be put in drying box at 90 DEG C dry 12 hours, obtain xerogel, then xerogel is put in heat treatment in tube furnace, the heating rate controlling tube furnace is 10 DEG C/min, and heat treatment temperature is 700 DEG C, and the time is 2 hours.Continue in tube furnace during heat treatment to pass into argon gas as protection gas, the flow of gas is 15ml/min.After calcining terminates, close tube furnace, after the temperature of tube furnace reduces to room temperature, stop passing into protection gas, product is taken out.Clearly can find out that diffraction maximum has very large halfwidth from the X-ray diffraction analysis (Fig. 5) of sample.Superconductive quantum interference test (SQUID) result (Fig. 6) proves that the iron nickel bimetal alloy nano-material prepared has superparamagnetism.
Claims (8)
1. a preparation method for iron nickel bimetal alloy nano-material, is characterized in that, comprises the following steps:
(1) preparation of mixed liquor
Select water or absolute ethyl alcohol as solvent, ferric nitrate and nickel nitrate are as solute, chelating agent selects the one in lactic acid, malic acid, sucrose or citric acid, and nitrate, chelating agent, dispersant, as dispersant, join in water or absolute ethyl alcohol by lauryl sodium sulfate or oleic acid successively;
(2) dry
Above-mentioned mixed solution is placed in 90-140 DEG C of drying box dry, until the complete evaporate to dryness of moisture becomes xerogel;
(3) heat treatment
Xerogel is placed in the tube furnace being connected with protection gas and calcines.
2. the preparation method of iron nickel bimetal alloy nano-material according to claim 1, is characterized in that, the mol ratio of the ferric nitrate described in step 1 and nickel nitrate is 1:3.
3. the preparation method of iron nickel bimetal alloy nano-material according to claim 1, is characterized in that, the molar concentration of the iron nitrate solution described in step 1 is 0.01-0.03mol/L.
4. the preparation method of iron nickel bimetal alloy nano-material according to claim 1, is characterized in that, the mol ratio of the iron described in step 1, nickel ion sum and chelating agent is 1:0.5-1:5.
5. the preparation method of iron nickel bimetal alloy nano-material according to claim 1, is characterized in that, the mol ratio of the iron described in step 1, nickel ion sum and dispersant is 1:1-1:3.
6. the preparation method of iron nickel bimetal alloy nano-material according to claim 1, is characterized in that, the drying time described in step 2 is 8-12 hour.
7. the preparation method of iron nickel bimetal alloy nano-material according to claim 1, is characterized in that, the protection gas described in step 3 is argon gas, and described shielding gas flow amount is 10-20ml/min.
8. the preparation method of iron nickel bimetal alloy nano-material according to claim 1, is characterized in that, the calcining described in step 3 is temperature required is 400-700 DEG C; Calcination time is 2-6 hour; Heating rate is 5-15 DEG C/min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107737948A (en) * | 2017-10-20 | 2018-02-27 | 成都理工大学 | The preparation method of the Fe@Ni nanocrystals of cube structure |
| CN111644177A (en) * | 2020-05-21 | 2020-09-11 | 安徽师范大学 | Iron-nickel bimetallic catalyst, preparation method and application |
| CN112206805A (en) * | 2020-10-14 | 2021-01-12 | 扬州大学 | Hollow iron-nickel nitride catalyst, preparation method and all-water electrolysis application thereof |
| CN113840528A (en) * | 2021-09-01 | 2021-12-24 | 浙江工业大学 | MOF-derived composite wave-absorbing material and preparation method and application thereof |
| CN115254118A (en) * | 2022-08-31 | 2022-11-01 | 中国科学院上海硅酸盐研究所 | For photocatalytic reduction of CO 2 Organic xerogel nano material and preparation method and application thereof |
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| JP4860386B2 (en) * | 2006-07-18 | 2012-01-25 | 住友大阪セメント株式会社 | Method for producing nickel-iron alloy nanoparticles |
| CN102373343A (en) * | 2011-11-02 | 2012-03-14 | 南京大学 | Small-size magnetic binary alloy nanometer material and preparation method thereof |
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| JP4860386B2 (en) * | 2006-07-18 | 2012-01-25 | 住友大阪セメント株式会社 | Method for producing nickel-iron alloy nanoparticles |
| CN101299914A (en) * | 2008-06-20 | 2008-11-05 | 广东工业大学 | Nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent and preparation method thereof |
| CN101332515A (en) * | 2008-08-05 | 2008-12-31 | 中南大学 | Preparation method of fibrous iron-nickel alloy powder |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107737948A (en) * | 2017-10-20 | 2018-02-27 | 成都理工大学 | The preparation method of the Fe@Ni nanocrystals of cube structure |
| CN107737948B (en) * | 2017-10-20 | 2019-05-10 | 成都理工大学 | The preparation method of the Fe@Ni nanocrystal of cube structure |
| CN111644177A (en) * | 2020-05-21 | 2020-09-11 | 安徽师范大学 | Iron-nickel bimetallic catalyst, preparation method and application |
| CN111644177B (en) * | 2020-05-21 | 2022-08-02 | 安徽师范大学 | Iron-nickel bimetallic catalyst, preparation method and application |
| CN112206805A (en) * | 2020-10-14 | 2021-01-12 | 扬州大学 | Hollow iron-nickel nitride catalyst, preparation method and all-water electrolysis application thereof |
| CN112206805B (en) * | 2020-10-14 | 2023-05-19 | 扬州大学 | Hollow iron-nickel nitride catalyst, preparation method and full-water electrolysis application thereof |
| CN113840528A (en) * | 2021-09-01 | 2021-12-24 | 浙江工业大学 | MOF-derived composite wave-absorbing material and preparation method and application thereof |
| CN115254118A (en) * | 2022-08-31 | 2022-11-01 | 中国科学院上海硅酸盐研究所 | For photocatalytic reduction of CO 2 Organic xerogel nano material and preparation method and application thereof |
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