CN109663930B - Spontaneous combustion micro-nano metal material and preparation method thereof - Google Patents

Spontaneous combustion micro-nano metal material and preparation method thereof Download PDF

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CN109663930B
CN109663930B CN201910111643.6A CN201910111643A CN109663930B CN 109663930 B CN109663930 B CN 109663930B CN 201910111643 A CN201910111643 A CN 201910111643A CN 109663930 B CN109663930 B CN 109663930B
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pyrophoric
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CN109663930A (en
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林媛
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Minjiang Teachers College
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/32—Radiation-absorbing paints

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Abstract

The invention discloses a spontaneous combustion micro-nano metal material and a preparation method thereof. The preparation method has the advantages of low cost, single product, simple argon calcining device with a tubular furnace, strong operability, no pollution, good reproducibility and wide synthesis application prospect.

Description

Spontaneous combustion micro-nano metal material and preparation method thereof
Technical Field
The invention relates to a spontaneous combustion micro-nano metal material and a preparation method thereof, belonging to the technical field of nano metal materials.
Background
The pyrophoric micro-nano metal material has wide application, micro-nano effect, large specific surface area and high surface activity. Different pyrophoric micro-nano metal materials are obtained by using different metal salts as reactants, and have greatly different chemical properties. The pyrophoric micro-nano cobalt metal material can be used as a lithium ion battery cathode material, the pyrophoric micro-nano nickel metal is often used as a catalyst, and the pyrophoric micro-nano cobalt, nickel, iron metal and alloy material have magnetism and can be used as an electromagnetic wave absorption material.
The autoignition material refers to a material which can ignite within five minutes after contacting with air, and is divided into an autoignition liquid material and an autoignition solid material. The spontaneous combustion solid material can protect the shell of the inflating equipment of the air bag of the vehicle and improve the personal safety of the vehicle owner (J.B.candelilla, K.J.Patel, L.Lange. spontaneous combustion material for the gas generator [ P ]. Chinese patent No. CN1535256, 2004-10-06.). The disposable heating sheet is sold for more than 1.81 hundred million years in China, and the principle is that chemical energy is converted into heat energy by utilizing the primary battery reaction of spontaneous combustion metal iron powder. Based on the analysis, the method for preparing the spontaneous combustion micro-nano metal material is very meaningful.
Disclosure of Invention
The invention aims to provide a novel and effective method for synthesizing a large amount of spontaneous combustion micro-nano metal materials, which has the advantages of simple raw materials, no need of adding a stabilizer or a surfactant, single product, strong operability, good reproducibility and larger synthesis application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an pyrophoric micro-nano metal material comprises the following steps:
1) dissolving metal salt and triethanolamine in distilled water to obtain metal salt solution;
2) placing the metal salt solution prepared in the step 1) in a hydrothermal kettle, and uniformly stirring by using a magnetic stirrer;
3) putting the metal salt solution prepared in the step 2) into an oven for reaction to obtain turbid liquid, and then washing precipitates obtained by centrifugation with distilled water to obtain a micro-nano metal precursor;
4) heating and drying the micro-nano metal precursor obtained in the step 3), and calcining to obtain a spontaneous combustion micro-nano metal product.
Further, the mass of the metal salt in the step 1) is 1.3 g-53.4 g.
Further, the weight of the triethanolamine in the step 1) is 1.1g to 56.0 g.
Further, in the step 1), the metal salt is soluble salt, and the concentration of the metal salt in the metal salt solution is 0.1-3.8M.
Further, the stirring speed in the step 2) is 30-40 rpm, and the stirring time is 30 min.
Further, the reaction temperature in the step 3) is 120-180 DEGoAnd C, the reaction time is 4-48 h.
Further, the drying temperature in the step 4) is 60-100 DEGoAnd C, heating and drying for 4-6 h.
Further, the calcining condition in the step 4) is that the obtained dry micro-nano metal precursor is placed into a tube furnace, argon is introduced for calcining, and the calcining temperature is 350-500 DEG CoAnd C, calcining for 2-8 h.
The invention has the outstanding advantages that: 1) the hydrothermal-calcination method is adopted to prepare the pyrophoric micro-nano metal material in a large scale, the material has pyrophoric property and nano material property, and has potential application prospect in the fields of lithium ion batteries, disposable warmer sheets, vehicle air bag inflation equipment parts, wave-absorbing materials and the like; 2) the low-temperature hydrothermal-calcining method is beneficial to the formation of micro-nano metal materials, and the method is simple and pollution-free; 3) the synthesis method has the advantages of simple raw materials, no need of adding a stabilizer or a surfactant, single product, strong operability, good reproducibility and larger synthesis application prospect; 4) the prepared pyrophoric micro-nano metal material has electromagnetic wave absorption performance and can be used as electromagnetic wave absorption coating.
Drawings
FIG. 1 is a scanning electron microscope image of the micro-nano metal precursor prepared in example 1;
FIG. 2 is a thermogravimetric analysis diagram of the micro-nano metal precursor prepared in example 1;
FIG. 3 is a scanning electron microscope image of the pyrophoric micro-nano metal material prepared in example 1;
fig. 4 is an electromagnetic wave absorption performance diagram of the pyrophoric micro-nano iron metal material prepared in example 6.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings.
Example 1
1) Preparing a cobalt nitrate solution: 1.3g of cobalt nitrate hexahydrate and 1.1g of triethanolamine were weighed and dissolved in 50mL of distilled water to obtain a cobalt nitrate solution (0.1 mM);
2) placing the aqueous solution of cobalt nitrate prepared in the step 1) into a hydrothermal kettle, and stirring for 30 minutes by using a magnetic stirrer;
3) putting the hydrothermal kettle into an oven, and keeping the temperature at 120 DEGoC, reacting for 4 hours to ensure the reaction to be complete. Finally obtaining pink turbid liquid, centrifuging, and washing the obtained precipitate with distilled water for 3 times to obtain a micro-nano cobalt metal precursor;
4) heating and drying the precipitate obtained in the step 3), and controlling the temperature to be 60 DEGoC；
5) Putting the dried sample obtained in the step 4) into a tube furnace, and introducing argon 350OAnd C, calcining for 2 hours to obtain the pyrophoric micro-nano cobalt metal material.
As can be seen from FIG. 1, the product obtained in this example has a large amount and relatively uniform morphology, and the thermogravimetric analysis chart of FIG. 2 can obtain the calcination temperature of argon gas at 350 deg.COAnd C is higher than the above, so that a stable product can be obtained. Fig. 3 can further determine that the morphology of the pyrophoric micro-nano cobalt metal material is basically maintained after calcination, and the pyrophoric micro-nano cobalt metal material is a micro-nano flower-shaped product.
Example 2
1) Preparing a cobalt nitrate solution: 20g of cobalt nitrate hexahydrate and 1.1g of triethanolamine were weighed and dissolved in 50mL of distilled water to obtain a cobalt nitrate solution (1.49 mM);
2) placing the aqueous solution of cobalt nitrate prepared in the step 1) into a hydrothermal kettle, and stirring for 30 minutes by using a magnetic stirrer;
3) putting the hydrothermal kettle into an oven, and keeping the temperature for 150 DEGoC, reacting for 12 hours to ensure the reaction to be complete. Finally obtaining pink turbid liquid, centrifuging, and washing the obtained precipitate with distilled water for 3 times to obtain a micro-nano cobalt metal precursor;
4) heating and drying the precipitate obtained in the step 3), and controlling the temperature to be 80 DEGoC；
5) Putting the dried sample obtained in the step 4) into a tube furnace, and introducing argon gas 400OAnd C, calcining for 2 hours to obtain the pyrophoric micro-nano cobalt metal material.
Example 3
1) Preparing a cobalt nitrate solution: 53.4g of cobalt nitrate hexahydrate and 1.1g of triethanolamine were weighed and dissolved in 50mL of distilled water to obtain a cobalt nitrate solution (3.8 mM);
2) placing the aqueous solution of cobalt nitrate prepared in the step 1) into a hydrothermal kettle, and stirring for 30 minutes by using a magnetic stirrer;
3) putting the hydrothermal kettle into an oven, and keeping the temperature for 180 DEGoC, reacting for 48 hours to ensure the reaction to be complete. Finally obtaining pink turbid liquid, centrifuging, and washing the obtained precipitate with distilled water for 3 times to obtain a micro-nano cobalt metal precursor;
4) heating and drying the precipitate obtained in the step 3), and controlling the temperature to be 100 DEGoC；
5) Putting the dried sample obtained in the step 4) into a tube furnace, and introducing argon 500OAnd C, calcining for 4 hours to obtain the pyrophoric micro-nano cobalt metal material.
Example 4
1) Preparing a nickel nitrate solution: 53.4g of nickel nitrate hexahydrate and 56g of triethanolamine were weighed and dissolved in 50mL of distilled water to obtain a nickel nitrate solution (1.8 mM);
2) putting the aqueous solution of the nickel nitrate prepared in the step 1) into a hydrothermal kettle, and stirring for 30 minutes by using a magnetic stirrer;
3) putting the hydrothermal kettle into an oven, and keeping the temperature for 180 DEGoC, reacting for 48 hours to ensure the reaction to be complete. Finally, obtaining green turbid liquid, centrifuging, and washing the obtained precipitate with distilled water for 3 times to obtain the micro-nano nickel metal precursor;
4) heating and drying the precipitate obtained in the step 3), and controlling the temperature to be 100 DEGoC；
5) Putting the dried sample obtained in the step 4) into a tube furnace, and introducing argon 500OAnd C, calcining for 4 hours to obtain the spontaneous combustion micro-nano nickel metal material.
Example 5
1) Preparing a nickel nitrate solution: 53.4g of nickel nitrate hexahydrate and 20g of triethanolamine were weighed and dissolved in 50mL of distilled water to obtain a nickel nitrate solution (2.8 mM);
2) putting the aqueous solution of the nickel nitrate prepared in the step 1) into a hydrothermal kettle, and stirring for 30 minutes by using a magnetic stirrer;
3) putting the hydrothermal kettle into an oven, and keeping the temperature for 160 DEGoC, reacting for 48 hours to ensure the reaction to be complete. Finally, obtaining green turbid liquid, centrifuging, and washing the obtained precipitate with distilled water for 3 times to obtain the micro-nano nickel metal precursor;
4) heating and drying the precipitate obtained in the step 3), and controlling the temperature to be 80 DEGoC；
5) Putting the dried sample obtained in the step 4) into a tube furnace, and introducing argon 450OAnd C, calcining for 4 hours to obtain the spontaneous combustion micro-nano nickel metal material.
Example 6
1) Preparing a ferric chloride solution: 35g of ferric chloride hexahydrate and 35g of triethanolamine were weighed and dissolved in 50mL of distilled water to obtain a ferric chloride solution (1.5 mM);
2) placing the aqueous solution of ferric nitrate prepared in the step 1) into a hydrothermal kettle, and stirring for 30 minutes by using a magnetic stirrer;
3) putting the hydrothermal kettle into an oven, and keeping the temperature for 180 DEGoC, reacting for 24 hours to ensure the reaction to be complete. Finally, obtaining yellow turbid liquid, centrifuging, and washing the obtained precipitate for 3 times by using distilled water to obtain a micro-nano iron metal precursor;
4) subjecting the product of step 3)Heating and drying the precipitate at 80 deg.CoC；
5) Putting the dried sample obtained in the step 4) into a tube furnace, and introducing argon gas 400OAnd C, calcining for 4 hours to obtain the spontaneous combustion micro-nano iron metal material.
6) And (3) carrying out an electromagnetic wave absorption performance test on the pyrophoric micro-nano iron metal material obtained in the step 5), wherein the test result is shown in fig. 4, when the thickness of the sample is 2mm, the reflection losses of the electromagnetic waves in the frequency range from 10.32GHz to 17.68GHz are all less than-10 dB, and the wave absorption effect of the material is higher than 90%, and the material has good electromagnetic wave absorption performance.
Example 7
1) Preparing a nickel cobalt nitrate solution: 26.7g of nickel nitrate hexahydrate, 26.7g of cobalt nitrate hexahydrate and 56g of triethanolamine were weighed and dissolved in 50mL of distilled water to obtain a nickel-cobalt nitrate solution (1.8 mM);
2) putting the aqueous solution of nickel cobalt nitrate prepared in the step 1) into a hydrothermal kettle, and stirring for 30 minutes by using a magnetic stirrer;
3) putting the hydrothermal kettle into an oven, and keeping the temperature for 180 DEGoC, reacting for 48 hours to ensure the reaction to be complete. Finally, obtaining green turbid liquid, centrifuging, and washing the obtained precipitate with distilled water for 3 times to obtain a micro-nano nickel-cobalt metal precursor;
4) heating and drying the precipitate obtained in the step 3), and controlling the temperature to be 100 DEGoC；
5) Putting the dried sample obtained in the step 4) into a tube furnace, and introducing argon 500OAnd C, calcining for 4 hours to obtain the spontaneous combustion micro-nano nickel cobalt metal material.
Example 8
1) Preparing a nickel cobalt nitrate solution: weighing 26.7g of nickel nitrate hexahydrate, 26.7g of cobalt nitrate hexahydrate and 26g of triethanolamine, and dissolving the materials in 50mL of distilled water to obtain a nickel-cobalt nitrate solution (2.62 mM);
2) putting the aqueous solution of nickel cobalt nitrate prepared in the step 1) into a hydrothermal kettle, and stirring for 30 minutes by using a magnetic stirrer;
3) putting the hydrothermal kettle into an oven, and keeping the temperature for 180 DEGoC, reacting for 48 hours to ensure the reaction to be complete. Finally obtaining green turbid liquid, centrifuging, thus obtainingWashing the obtained precipitate with distilled water for 3 times to obtain a micro-nano nickel-cobalt metal precursor;
4) heating and drying the precipitate obtained in the step 3), and controlling the temperature to be 80 DEGoC；
5) Putting the dried sample obtained in the step 4) into a tube furnace, and introducing argon gas 400OAnd C, calcining for 2h to obtain the pyrophoric micro-nano nickel metal material.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.

Claims (6)

1. The utility model provides a micro-nano metal material of spontaneous combustion nature which characterized in that: the preparation method of the spontaneous combustion micro-nano metal material comprises the following steps:
1) dissolving metal salt and triethanolamine in distilled water to obtain metal salt solution;
2) placing the metal salt solution prepared in the step 1) in a hydrothermal kettle, and uniformly stirring by using a magnetic stirrer;
3) putting the metal salt solution prepared in the step 2) into an oven for reaction to obtain turbid liquid, and then washing precipitates obtained by centrifugation with distilled water to obtain a micro-nano metal precursor;
4) heating and drying the micro-nano metal precursor obtained in the step 3), and calcining to obtain a spontaneous combustion micro-nano metal product with electromagnetic wave absorption performance;
the reaction temperature in the step 3) is 120-180 ℃, the reaction time is 4-48 hours, and the calcining condition in the step 4) is that the obtained dry micro-nano metal precursor is placed into a tube furnace, argon is introduced for calcining, the calcining temperature is 350-500 ℃, and the calcining time is 2-8 hours.
2. The pyrophoric micro-nano metallic material of claim 1, wherein: the mass of the metal salt in the step 1) is 1.3 g-53.4 g.
3. The pyrophoric micro-nano metallic material of claim 1, wherein: the weight of the triethanolamine in the step 1) is 1.1 g-56.0 g.
4. The pyrophoric micro-nano metallic material of claim 1, wherein: in the step 1), the metal salt is soluble salt, and the concentration of the metal salt in the metal salt solution is 0.1-3.8M.
5. The pyrophoric micro-nano metallic material of claim 1, wherein: in the step 2), the stirring speed is 30-40 rpm, and the stirring time is 30 min.
6. The pyrophoric micro-nano metallic material of claim 1, wherein: in the step 4), the drying temperature is 60-100 ℃, and the heating and drying time is 4-6 h.
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KR100541093B1 (en) * 2003-11-10 2006-01-11 삼성전기주식회사 A Method for Producing Nickel Metal Powder With High Purity
CN100556586C (en) * 2004-11-01 2009-11-04 中国科学院福建物质结构研究所 A kind of preparation method of yttrium borate doped nano powder
CN101284958B (en) * 2008-06-05 2010-04-21 上海交通大学 Preparation method of solar energy heat absorbing coating using nickel or nickel alloy hollow ball as absorbent
CN101728045B (en) * 2009-11-10 2012-04-18 厦门大学 Cobalt oxide/carbon composite nano wave-absorbing material and preparation method thereof
US8721763B2 (en) * 2012-08-01 2014-05-13 Chung Shan Institute Of Science And Technology Method for separating metal nanoparticles from colloidal metal solution
CN104014815B (en) * 2014-06-19 2016-12-28 厦门大学 A kind of cobalt base amorphous nano wave-absorbing material and synthetic method thereof
CN105328202A (en) * 2014-08-13 2016-02-17 南京理工大学 Preparation method of cobalt nano material
CN104263317B (en) * 2014-09-26 2016-03-09 厦门大学 The synthetic method of a kind of cobalt oxide/Graphene composite wave-suction material
US10850330B2 (en) * 2015-10-19 2020-12-01 Sumitomo Metal Mining Co., Ltd. Process for producing nickel powder
CN105382252B (en) * 2015-11-18 2017-12-01 山东大学 A kind of monodispersed nickel microballoon powder electromagnetic wave absorbent material and preparation method thereof
GB2555608A (en) * 2016-11-04 2018-05-09 Rolls Royce Plc A magnetic material and a method of sythesising the same

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