CN113620298B - Diatom-based silicon carbide material and preparation method and application thereof - Google Patents
Diatom-based silicon carbide material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a diatom-based silicon carbide material and a preparation method and application thereof, and relates to the technical field of silicon carbide. The preparation method comprises the following steps: placing the high-iron diatom in a closed heating device, heating to 500-1200 ℃ under an anaerobic condition, and carrying out heat treatment for 3-7 hours, wherein the mass percentage of iron in the high-iron diatom is 0.98% -2.4%. The preparation method reduces the iron-containing oxide which is uniformly distributed in the diatom shell into an iron simple substance which can be used as a catalyst during heat treatment, and other metals are not required to be added to be used as a reducing agent or a catalyst, so that impurities are not introduced, and the purity of the obtained silicon carbide is higher. The preparation method has the advantages of high efficiency, easy operation, low cost, easy popularization and the like. The prepared diatom-based silicon carbide material has the advantages of large specific surface area, large total pore volume, high purity and wide application.
Description
Technical Field
The invention relates to the technical field of silicon carbide, in particular to a diatom-based silicon carbide material and a preparation method and application thereof.
Background
Silicon carbide has high oxidation resistance, corrosion resistance and good chemical inertness, it also has high thermal stability and conductivity and a small coefficient of thermal expansion, and it can also exhibit semiconducting properties at high temperatures. Therefore, the material can be used in the fields of national defense and aviation, metallurgy, chemical engineering and the like, and can be used as a material for heat exchangers, electronics, sensing and the like.
Previous methods of preparing diatomaceous earth-based silicon carbide by using diatomaceous earth combined with carbon powder and then calcining at high temperature have produced porous silicon carbide having high porosity, but the methods have problems, for example, they require purification of diatomaceous earth and production of diatomaceous earth shells by using hot acid; and certain carbon powder is required to be added as a carbon source. This results in the problems of difficulty in obtaining high purity products, high cost, and a certain risk of environmental damage, etc. when diatomite is used to prepare silicon carbide, large-scale industrialization is difficult.
Diatoms is a unicellular algae widely distributed in the ocean and fresh water. The diatom is composed of organic film on the surface, siliceous shell and other organic components in the shell. Wherein, the silica shell has rich pore canal structure, takes macropores as main components and also contains a small amount of mesopores and micropores, and is a natural porous material. The outer surface of the siliceous shell is attached with a layer of organic film, and the organic film is not only a main platform for the photosynthesis of the diatom, but also effectively prevents toxic substances or bacteria and the like from entering the shell and damaging the life activity of the diatom.
Siliceous diatom shells (which are accumulated and enriched to form diatomaceous earth and diatomaceous earth deposits) are used as biogenic materials in many fields, such as diatomaceous earth, which is a siliceous shell that is aggregated in large quantities and then mineralized, filter aids, adsorbents, etc. However, as noted above, the formation of diatomaceous earth has a significant amount of contaminating minerals present, which can affect the purity of the minerals and require further purification. And so far, no high-purity diatom shell can be obtained. Therefore, the above problems can be effectively solved by using diatoms containing organic matter instead of diatomaceous earth.
On the other hand, researchers have used natural diatoms to prepare silicon carbide, which is based on the principle that organic matter contained in diatoms is reduced to carbon and then forms silicon carbide with the shell. However, the preparation process requires the addition of a metal reducing agent, and this step has two problems: 1) The reducing agent is a metal simple substance which is difficult to uniformly contact with the diatom, and part of positions cannot be catalyzed; 2) After the metal is added and the reaction is finished, metal or metal oxide impurities are introduced, so that high-purity silicon carbide (2-10 g of metal/100 g of diatom) is difficult to obtain; 3) Removal of these metals and their oxides requires higher concentrations of acid treatment, resulting in potential environmental hazards.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a diatom-based silicon carbide material and a preparation method thereof, wherein the specific surface area of the diatom-based silicon carbide material prepared by the diatom-based silicon carbide material is 140-220m 2 Per g, total pore volume of 0.12-0.25cm 3 Per gram, purity > 96%.
The invention aims to provide application of a diatom-based silicon carbide material as a functional material in national defense, aviation, metallurgy or chemical industry.
The invention is realized in the following way:
in a first aspect, the present invention provides a method for preparing a diatom-based silicon carbide material, comprising: placing the high-iron diatom in a closed heating device, heating to 500-1200 ℃ under an anaerobic condition, and carrying out heat treatment for 3-7 hours, wherein the mass percentage content of ferrous in the high-iron diatom is 0.98% -2.4%.
In an alternative embodiment, the ferric diatom is artificially cultured freshwater diatoms, and the concentration of ferrous ions in the culture broth is maintained between 50 and 500nmol/L during artificial cultivation.
In an alternative embodiment, before the high-iron diatom is placed in the closed heating device, the fresh water diatom of the living bodies after cultivation is scooped up from the culture solution and then drained.
In an alternative embodiment, the freshwater diatoms comprises at least one of Mei Ni micrococcus and granola rhombifolia.
In an alternative embodiment, the heat treatment at elevated temperature to 500-1200 ℃ for 3-7 hours in the absence of oxygen comprises: heating to 500-700 deg.C under oxygen-free condition, maintaining the temperature for 2-4 hr, and then continuously raising the temperature to 1100-1200 deg.C and maintaining the temperature for 1-3 hr.
In alternative embodiments, the oxygen-free conditions are inert gas conditions;
preferably, the inert gas in the inert gas condition includes at least one of nitrogen and argon.
In an alternative embodiment, the heat treatment under anaerobic conditions further comprises reducing the temperature to 350-450 ℃ and calcining under aerobic conditions for 1-3 hours.
In an alternative embodiment, calcining under aerobic conditions comprises calcining after the passage of at least one of air and oxygen.
In a second aspect, the present invention provides a diatom-based silicon carbide material prepared by the method according to any one of the previous embodiments.
In an alternative embodiment, the diatom-based silicon carbide material has a specific surface area of 140-220m 2 (ii)/g, total pore volume of 0.12-0.25cm 3 Per gram, purity > 96%.
In a third aspect, the present invention provides the use of the diatom-based silicon carbide material according to the previous embodiment as a functional material in defense, aviation, metallurgy or chemical engineering;
preferably, the functional material comprises a heat exchanger material, an electronic material or a sensing material.
The invention has the following beneficial effects:
according to the preparation method of the diatom-based silicon carbide material, the high-iron diatom with high iron content is used as a raw material to prepare the silicon carbide material, and the high-iron diatom is the iron content increased in the growth process, so that the increased iron can be uniformly distributed in diatom, then the Gao Tiegui diatom is subjected to anaerobic heat treatment, and organic matters in the shell of the high-iron diatom are subjected to reduction reaction and become carbon. Because diatoms are enriched with divalent and trivalent iron, carbon can promote iron oxides contained in diatoms to be reduced to elemental iron during anaerobic heat treatment. The iron simple substance can be used as a catalyst to promote the carbon to react with the diatom shell to generate silicon carbide. The iron-containing oxide which is uniformly distributed in the diatom shell is reduced into the iron simple substance which can be used as a catalyst during heat treatment, other metals are not required to be added to serve as a reducing agent or a catalyst, impurities cannot be introduced, and the purity of the obtained silicon carbide is higher. The preparation method has the advantages of high efficiency, easy operation, low cost, easy popularization and the like. Prepared by the above methodThe diatom-based silicon carbide material prepared by the method has the specific surface area of 140-220m 2 Per g, total pore volume of 0.12-0.25cm 3 The purity is more than 96 percent per gram. The diatom-based silicon carbide material can be widely used as a functional material in national defense, aviation, metallurgy or chemical engineering, and the functional material comprises a heat exchanger material, an electronic material or a sensing material.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is an X-ray diffraction pattern of silicon carbide obtained in example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The invention provides a preparation method of a diatom-based silicon carbide material, which comprises the following steps:
s1, artificially cultivating fresh water diatoms.
The method comprises the following steps of artificially culturing the freshwater diatom, wherein ferrous ions with a certain concentration are added in the culturing process to ensure the growth and proliferation of the diatom, and the concentration of the ferrous ions in a culture solution is kept to be 50-500nmol/L, so that the mass percentage content of iron in the cultured high-iron diatom is 0.98% -2.4%. The cultured living body of the high-iron diatom is taken out from the culture pond by a screen, and most of the contained water is drained.
In the application, the growing environment of the diatom is regulated and controlled in the growing process of the diatom, so that the iron content in the diatom is increased, and the increased iron can be uniformly distributed in the diatom to form the high-iron diatom.
S2, carrying out heat treatment under an anaerobic condition.
Placing the high-iron diatom in a closed heating device, and heating to 500-1200 ℃ under an anaerobic condition for heat treatment for 3-7 hours.
Specifically, the heat treatment at 500-1200 ℃ for 3-7 hours in the absence of oxygen comprises: heating to 500-700 deg.C under oxygen-free condition, maintaining the temperature for 2-4 hr, and then continuously raising the temperature to 1100-1200 deg.C and maintaining the temperature for 1-3 hr. In the present application, the oxygen-free condition is an inert gas condition; preferably, the inert gas in the inert gas condition includes at least one of nitrogen and argon.
In the application, anaerobic heat treatment is carried out at the temperature of 500-700 ℃, and organic matters in the diatom shells are subjected to reduction reaction and then are changed into carbon. Because the high-iron diatom is enriched with divalent and trivalent iron, carbon can promote iron oxide contained in the high-iron diatom to be reduced into iron simple substance during anaerobic heat treatment. Then raising the temperature to 1100-1200 ℃, wherein the generated iron can be used as a catalyst to promote the carbon to react with the diatom shell to generate silicon carbide.
And S3, carrying out heat treatment under an aerobic condition.
The temperature is lowered to 350-450 ℃, aerobic conditions are formed after at least one of air and oxygen is introduced, and then calcination is carried out for 1-3 hours.
In this application, through carrying out heat treatment under aerobic condition, can calcine the carbon that does not react completely in the diatom shell to promote the purity of carborundum.
The diatom-based silicon carbide material prepared by the preparation method has the specific surface area of 140-220m 2 (ii)/g, total pore volume of 0.12-0.25cm 3 Per gram, purity > 96%. The siliconThe algae-based silicon carbide material can be widely used as a functional material in national defense, aviation, metallurgy or chemical engineering, and the functional material comprises a heat exchanger material, an electronic material or a sensing material. Therefore, the preparation method has the advantages of high efficiency, easiness in implementation, low cost, easiness in popularization and the like.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a preparation method of a diatom-based silicon carbide material, which comprises the following steps:
s1, artificially culturing Mei Ni Cyclotella, wherein the culture medium is an f/2 culture medium, and adding ferrous sulfate in the culturing process until the concentration of ferrous ions in a culture solution is 100nmol/L to obtain the high-iron diatom with the iron content of 1.67%. The cultured living diatoms are taken out of the culture pond by a screen, and most of the water contained in the living diatoms is drained.
S2, directly placing the drained Mei Ni chlorella in a sealed heating device, firstly heating to 500 ℃ under the condition of nitrogen, keeping the temperature for 2 hours, and then continuously heating to 1100 ℃ and keeping the temperature for 1 hour.
And S3, reducing the temperature to 400 ℃, introducing air or oxygen, and calcining for 1 hour to obtain the diatom-based silicon carbide material.
As can be seen from the X-ray diffraction pattern of the silicon carbide shown in fig. 1, all diffraction peaks are SiC peaks, and no impurity peak appears, which fully proves that the diatom-based silicon carbide material obtained in this example has high purity.
Example 2
The embodiment provides a preparation method of a diatom-based silicon carbide material, which comprises the following steps:
s1, artificially culturing Mei Ni Cyclotella, wherein the culture medium is an f/2 culture medium, and adding ferrous sulfate in the culturing process until the concentration of ferrous ions in a culture solution is 500nmol/L to obtain the high-iron diatom with the iron content of 2.40%. After the cultured living diatoms are scooped out of the culture pond with a screen, most of the water contained therein is drained.
S2, directly placing the drained Mei Ni chlorella in a sealed heating device, firstly heating to 700 ℃ under the condition of nitrogen, keeping the temperature for 4 hours, and then continuously heating to 1200 ℃ and keeping the temperature for 3 hours.
And S3, reducing the temperature to 450 ℃, introducing air or oxygen, and calcining for 3 hours.
Example 3
The embodiment provides a preparation method of a diatom-based silicon carbide material, which comprises the following steps:
s1, artificially culturing the granular rhombohedral algae in an f/2 culture medium, and adding ferrous sulfate to the culture solution until the concentration of ferrous ions in the culture solution is 50nmol/L in the culturing process to obtain the high-iron diatom with the iron content of 0.98%. The cultured living diatoms are taken out of the culture pond by a screen, and most of the water contained in the living diatoms is drained.
S2, directly placing the drained granular rhombohedral algae in a closed heating device, firstly heating to 500 ℃ under the condition of nitrogen, keeping the temperature for 2 hours, and then continuously raising the temperature to 1100 ℃ and keeping the temperature for 1 hour.
And S3, reducing the temperature to 400 ℃, introducing air or oxygen, and calcining for 2 hours.
Example 4
The embodiment provides a preparation method of a diatom-based silicon carbide material, which comprises the following steps:
s1, artificially culturing the granular rhombohedral algae in an f/2 culture medium, and adding ferrous sulfate to the culture solution until the concentration of ferrous ions in the culture solution is 500nmol/L in the culturing process to obtain the high-iron diatom with the iron content of 2.36%. The cultured living diatoms are taken out of the culture pond by a screen, and most of the water contained in the living diatoms is drained.
S2, directly placing the drained granular rhombohedral algae in a closed heating device, firstly heating to 700 ℃ under the condition of nitrogen, keeping the temperature for 4 hours, and then continuously raising the temperature to 1200 ℃ and keeping the temperature for 3 hours.
And S3, reducing the temperature to 450 ℃, introducing air or oxygen, and calcining for 3 hours.
Example 5
This embodiment is substantially the same as embodiment 4 except that step S3 of embodiment 4 is omitted.
Example 6
This example is substantially the same as example 4, except that in step S2, the temperature is directly raised to 700 ℃ and maintained for 7 hours.
Example 7
This example is substantially the same as example 4, except that in step S2, the temperature is raised directly to 1200 ℃ and maintained for 7 hours.
Comparative example 1
The Mei Ni chlorella of example 1 was cultured directly in f/2 medium without adding ferrous sulfate to adjust the concentration of ferrous ions in the culture broth, at which time diatoms with an iron content of 0.15% were obtained.
Comparative example 2
The artificially cultured Mei Ni Cyclotella in example 1 was directly used as Mei Ni Cyclotella, and purchased from the institute of aquatic organism (or Shanghai plain Biotechnology Co., ltd.) of Chinese academy of sciences.
Comparative example 3
The ferrous ion concentration in example 1 was replaced with 700nmol/L, at which time diatoms with an iron content of 2.38% were obtained.
The silicon carbide obtained in the above examples 1 to 7 and comparative examples 1 to 3 was examined by a method comprising:
specific surface area detection method: the test instrument is ASAP2020 manufactured by Michmark corporation, the method is a nitrogen adsorption method, and the analysis method is a BET method.
Pore volume detection method: the testing instrument is ASAP2020 manufactured by McMac corporation, the method is a nitrogen adsorption method, and the analysis method is a DR method.
The purity calculation method comprises the following steps: and (4) XRF testing.
The detection results are as follows:
as can be seen from the above table, the iron ion concentration is increased in examples 1 to 4, which is beneficial to increase the specific surface area and pore volume, and the product performance is obviously reduced in example 5 compared with example 4, which shows that the aerobic heat treatment in step S3 can calcine the carbon which is not completely reacted in the diatom shell, thereby increasing the purity of the silicon carbide. As can be seen from example 6, when the oxygen-free heat treatment is performed only at a relatively low temperature of 700 ℃, iron oxide contained in the high-iron diatom cannot be effectively reduced to elemental iron, and thus carbon cannot be promoted to react with the diatom shell to form silicon carbide. It can be seen from example 7 that when the oxygen-free heat treatment is carried out only at a higher temperature of 1200 c, without a low temperature hold at 700 c, the resulting carbon has poor catalytic activity and less contact with iron, which significantly reduces product performance. Further, it can be seen from comparative examples 1 and 2 that the product performance is significantly reduced when the iron content in diatom is low, while comparative example 3 shows that the product performance is not significantly improved but the production cost is increased by continuously increasing the concentration of ferrous ions in the medium. Therefore, the method and corresponding parameters adopted by the application can meet the preparation requirement of the diatom silicon carbide material, and the quality of the corresponding product cannot be improved for a longer time or at a higher temperature.
To sum up, the preparation method of diatom base silicon carbide material that this application provided is through adopting the high-iron diatom that the iron content is high as raw materials preparation silicon carbide material, because the high-iron diatom is the iron content that self increases in the growth process, the iron that increases can evenly distributed in the diatom, carries out anaerobic heat treatment to the iron-containing diatom after that, and organic matter in the high-iron diatom shell takes place reduction reaction and becomes carbon. Because diatoms are enriched with divalent and trivalent iron, carbon can promote iron oxides contained in diatoms to be reduced to elemental iron during anaerobic heat treatment. The iron simple substance can be used as a catalyst to promote the carbon to react with the diatom shell to generate silicon carbide. The iron-containing oxide uniformly distributed in the diatom shell is reduced into the iron simple substance capable of serving as the catalyst during heat treatment, other metals do not need to be added to serve as a reducing agent or a catalyst, impurities cannot be introduced, and the obtained carbonized diatom isThe silicon purity is higher. In addition, this application still carries out heat treatment under the aerobic condition after preparing and obtaining carborundum, can calcine the carbon that does not react completely in the diatom casing to promote carborundum's purity. The preparation method has the advantages of high efficiency, easy operation, low cost, easy popularization and the like. The diatom-based silicon carbide material prepared by the preparation method has the specific surface area of 140-220m 2 (ii)/g, total pore volume of 0.12-0.25cm 3 Per gram, purity > 96%. The diatom-based silicon carbide material can be widely used as a functional material in national defense, aviation, metallurgy or chemical engineering, and the functional material comprises a heat exchanger material, an electronic material or a sensing material.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a diatom-based silicon carbide material is characterized by comprising the following steps: placing the high-iron diatom in a closed heating device, heating to 500-1200 ℃ under an anaerobic condition, and carrying out heat treatment for 3-7 hours, wherein the mass percentage content of ferrous in the high-iron diatom is 0.98% -2.4%;
the high-ferrum diatom is artificially cultured fresh water diatom, and the concentration of ferrous ions in the culture solution is kept to be 50-500nmol/L in the artificial culture;
heating to 500-1200 deg.C in the absence of oxygen for 3-7 hours comprising: heating to 500-700 deg.C under oxygen-free condition, maintaining the temperature for 2-4 hr, and then continuously raising the temperature to 1100-1200 deg.C and maintaining the temperature for 1-3 hr.
2. The method for preparing the diatom-based silicon carbide material according to claim 1, wherein the fresh water diatoms of the living bodies after cultivation are removed from the culture solution and drained before the ferric diatoms are placed in the closed heating device.
3. The method of producing a diatom-based silicon carbide material of claim 1, wherein said freshwater diatoms comprises at least one of Mei Ni Cyclotella tenella and Phyllostachys granulosa.
4. The method for preparing a diatom-based silicon carbide material of claim 1 wherein said oxygen-free conditions are inert gas conditions.
5. The method for preparing a diatom-based silicon carbide material according to claim 4 wherein said inert gas in said inert gas conditions comprises at least one of nitrogen and argon.
6. The method of claim 1, further comprising reducing the temperature to 350-450 ℃ after the heat treatment under anaerobic conditions, and calcining the diatom-based silicon carbide material under aerobic conditions for 1-3 hours after introducing at least one of air and oxygen.
7. A diatom-based silicon carbide material prepared by the method of any one of claims 1-6.
8. The diatomic silicon carbide material of claim 7, wherein the diatomic silicon carbide material has a specific surface area of 140-220m 2 (iv)/g, total pore volume of 0.12-0.25cm 3 The purity is more than 96 percent per gram.
9. Use of the diatom-based silicon carbide material of claim 8 as a functional material in defense, aviation, metallurgy or chemical industry.
10. Use according to claim 9, wherein the functional material comprises a heat exchanger material, an electronic material or a sensing material.
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| CN101306816A (en) * | 2008-06-24 | 2008-11-19 | 陕西科技大学 | Method for synthesizing beta-SiC nano-wire |
| CN102303866A (en) * | 2011-08-16 | 2012-01-04 | 浙江大学 | Method for preparing SiC from natural diatom |
| CN102303867A (en) * | 2011-08-16 | 2012-01-04 | 浙江大学 | Method for preparing porous silicon carbide by utilizing diatomite |
| CN106753196A (en) * | 2016-12-25 | 2017-05-31 | 常州创索新材料科技有限公司 | A kind of preparation method of high temperature resistant dimensional stability Metal adhesive |
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