CN112125686A - Method for preparing silicon carbide coated graphite by molten salt isolation - Google Patents
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Abstract
A method for preparing silicon carbide coated graphite by molten salt isolation comprises the steps of weighing silicon powder, crystalline flake graphite powder and molten salt according to a set proportion, uniformly mixing the silicon powder, the crystalline flake graphite powder and the molten salt in a ball milling tank to obtain mixed slurry, drying the mixed slurry in an oven, and sieving the dried powder to obtain granulated powder A; placing the granulated powder A in a mould to be pressed and molded to obtain a blank body B, then using a large mould to wrap the blank body B by using molten salt as a filler, and pressing and molding to obtain a salt packaging sample C; placing the salt-sealed sample C in an alumina crucible, adding enough molten salt into the crucible to completely cover the salt-sealed sample C, covering the crucible, placing the crucible in a high-temperature furnace, heating to 1300 plus materials and 1400 ℃, keeping the temperature for 1-5h, roasting, and naturally cooling to room temperature; and washing the product with deionized water to remove salt in a salt layer and a blank, and filtering and drying to obtain the graphite powder which is uniformly dispersed and completely coated with SiC. The method has the advantages of wide raw material source, low cost, short time consumption, no need of expensive argon as protective atmosphere in the preparation process and the like.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a method for preparing silicon carbide coated graphite by molten salt isolation.
Background
In order to improve the high temperature slag erosion resistance and thermal shock resistance of oxide-based castable materials, it is often desirable to add carbon materials to achieve this goal. The crystalline integrity of the flake graphite and the non-wettability of the flake graphite with the slag are the preferred carbon source of the carbon-containing castable, but the graphite is not wetted with water, and the poor fluidity and the poor dispersibility of the graphite cause the water addition amount of the carbon-containing castable to be greatly increased, so that the normal temperature performance and the high temperature performance of the castable are obviously reduced, the porosity is obviously improved, and the improvement of the slag resistance of the material is not facilitated. To address this problem, graphite is often surface modified to improve its wettability and dispersibility.
The method for modifying the graphite surface mainly comprises introducing a surfactant, a graphite granulation method, a surface coating and the like. The technical process of the surfactant is simple and convenient, the cost is low, but the improvement on the wettability and the dispersibility of the graphite is limited, the water adding amount required by the molding of the casting material is still high, the performance of the casting material is poor, and the use requirement cannot be met; the graphite granulation method can obviously reduce the water demand, but the granulated graphite has larger size and is in millimeter level, which is not beneficial to the uniform distribution of the graphite in the casting material and has limited improvement on the slag resistance of the casting material.
The graphite is coated on the surface by chemical or physical means, the coating layer generally has better wettability and dispersibility, and the existence of the coating layer can prevent the graphite from contacting with oxygen so as to slow down the oxidation speed of the graphite. Chinese patent (CN 101565848A) entitled "method for preparing gradient silicon carbide coating by electrophoretic codeposition" provides a method for preparing gradient silicon carbide coating by electrophoretic codeposition, which adopts the technical scheme that silicon powder, carbon black, polyvinyl butyral, acetone and n-butylamine are mixed and ultrasonically treated to prepare suspension, graphite material is used as an anode, deposition is carried out in a constant potential mode, and the suspension is dried and then sintered at 1200-1600 ℃. The process comprises electrophoretic deposition and sintering processes, and has the defects of high power consumption, high cost and the like.
The Chinese patent (CN 110615682A) with the patent name of 'a graphite surface modification method for carbon-containing refractory castable and application thereof' discloses a graphite surface modification method for carbon-containing refractory castable, which adopts the technical scheme that crystalline flake graphite powder and titanium powder are used as raw materials, and a self-propagating sintering method is adopted to prepare titanium carbide coated crystalline flake graphite.
Chinese patent (CN 107793164A) entitled "preparation method of granulated graphite of refractory castable material" provides a preparation method of granulated graphite for refractory castable material, which adopts the technical scheme that zirconium oxychloride octahydrate is used as a precursor, and a sol-gel method is adopted to coat the surface of graphite, but the graphite coating prepared by the method is weaker in combination with the graphite, and the coating is easy to peel off. This results in limited improvement in the wettability and dispersibility of the graphite and does not effectively reduce the actual water demand of the castable.
Compared with the traditional solid-phase sintering technology, the molten salt method has the advantages of low synthesis temperature, small environmental pollution, adjustable morphology and size, reusability of salts and the like, is applied to preparation of oxide powder and non-oxide powder, and has also been reported for preparation of graphite coated with molten salt in an auxiliary way, but the synthesis of the graphite coated with molten salt usually needs flowing argon as protective atmosphere.
The Chinese patent (CN 109942297A) entitled "silicon carbide nanowire reinforced high-orientation graphite composite material and preparation method" provides a preparation method of a silicon carbide nanowire reinforced graphite composite material, and the technical scheme is that silicon carbide nanowire coated flake graphite powder is prepared from silicon powder and flake graphite by a molten salt method, and discharge plasma sintering is carried out at 1600-2000 ℃ after pre-pressing molding. The technical scheme is simple in process, and the spark plasma sintering has the advantages of high heating rate, high efficiency and the like, but in the powder synthesis step, circulating argon is needed to be used as a protective atmosphere for protecting silicon powder and graphite from being oxidized.
The Chinese patent (CN 108640117A) with the name of 'synthesizing a two-dimensional SiC ultrathin nanostructure by using a graphene as a template molten salt method and a preparation method thereof' discloses a method for synthesizing a two-dimensional SiC ultrathin nanostructure by using a graphene as a template molten salt method and a preparation method thereof. In the method, flowing argon is still required to be introduced to serve as a protective atmosphere for protecting the silicon powder and the graphite from being oxidized.
Therefore, a preparation technology of coated graphite with low cost, environmental friendliness and uniform product size is urgently needed to be developed to solve the problem of poor wettability of crystalline flake graphite and water.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides the method for preparing the silicon carbide coated graphite by molten salt isolation, which has the advantages of low preparation cost, environmental friendliness, uniform product size, no need of expensive argon as a protective atmosphere and easiness in large-scale preparation.
The object of the invention can be achieved by the following technical measures:
the method for preparing the silicon carbide coated graphite by molten salt isolation comprises the following steps:
a. weighing silicon powder, crystalline flake graphite powder and molten salt according to the mass ratio of 7: 6-24: 13-31, and uniformly mixing by using a ball mill in a wet grinding mode to obtain mixed slurry, wherein the mass ratio of the material to balls to ethanol is 1:2: 2;
b. putting the mixed slurry into an oven for drying, and sieving and granulating the dried powder to obtain granulated powder A;
c. placing the granulated powder A in a mould to be pressed and molded to obtain a blank body B, then wrapping the blank body B by using a mould larger than the blank body B and using molten salt as a filler, and then pressing and molding to obtain a salt packaging sample C;
d. placing a salt packaging sample C in an alumina crucible, putting molten salt capable of completely covering the salt packaging sample C in the crucible as a salt bed, covering the molten salt, putting the crucible in a high-temperature furnace, heating to 1300-;
e. and d, washing the blank obtained in the step d by deionized water to remove salt layers and salt in the blank, crushing the blank to dissolve the salt in the blank, filtering, and finally drying to obtain the target powder.
Furthermore, in the step a, the purity of the silicon powder is more than 98%, and the particle size is less than 75 microns; the purity of the flake graphite powder is more than 95 percent, and the granularity is less than 100 microns; the fused salt is analytically pure and has a particle size of less than 100 microns.
The mass ratio of the silicon powder to the crystalline flake graphite in the step a is 7: 6-24; the mass ratio of the total mass of the silicon powder and the crystalline flake graphite powder to the molten salt is 1: 1.
In the step a, the molten salt is one of potassium chloride, potassium bromide or sodium chloride.
And C, placing the granulated powder A in a mould to be pressed and molded to obtain a blank B with the pressure of 200MPa, then wrapping the blank B by using a mould larger than the blank B and using molten salt as a filler, and pressing and molding to obtain a salt packaging sample C with the pressure of 200 MPa.
And d, placing the cover into a high-temperature furnace for firing at the temperature of 1300-1400 ℃ at the speed of 5 ℃/min, and keeping the temperature for 1-5h, wherein the firing atmosphere is air atmosphere and does not need to be protected by introducing argon.
The invention has the following beneficial effects:
the synthesis process of preparing the silicon carbide coated graphite by using the method does not need expensive argon as protective atmosphere, and the synthesized powder has good dispersibility and uniform size and does not need extra grinding.
More particularly to
1) The used molten salt has low price, wide source, no toxicity and environmental protection.
2) The synthesis temperature in the synthesis process is 100-200 ℃ lower than the traditional solid phase sintering temperature.
3) And expensive argon is not used as protective atmosphere in the synthesis process, so that the preparation cost is low.
4) The surface of the synthesized graphite powder is uniformly coated by SiC, and the powder has good wettability with water.
Drawings
Fig. 1 is an X-ray diffraction pattern of the prepared silicon carbide-coated graphite powder.
Fig. 2 and 3 are scanning electron micrographs of the prepared silicon carbide-coated graphite powder.
Detailed Description
The invention will be further described with reference to the following examples:
the method for preparing the silicon carbide coated graphite by molten salt isolation comprises the following steps:
a. weighing silicon powder, crystalline flake graphite powder and molten salt according to the mass ratio of 7: 6-24: 13-31, and uniformly mixing by using a ball mill in a wet grinding mode to obtain mixed slurry, wherein the mass ratio of the material to balls to ethanol is 1:2: 2;
b. putting the mixed slurry into an oven for drying, and sieving and granulating the dried powder to obtain granulated powder A;
c. placing the granulated powder A in a mould to be pressed and molded to obtain a blank body B, then wrapping the blank body B by using a mould larger than the blank body B and using molten salt as a filler, and then pressing and molding to obtain a salt packaging sample C;
d. placing a salt packaging sample C in an alumina crucible, putting molten salt capable of completely covering the salt packaging sample C in the crucible as a salt bed, covering the molten salt, putting the crucible in a high-temperature furnace, heating to 1300-;
e. and d, washing the blank obtained in the step d by deionized water to remove salt layers and salt in the blank, crushing the blank to dissolve the salt in the blank, filtering, and finally drying to obtain the target powder.
Furthermore, in the step a, the purity of the silicon powder is more than 98%, and the particle size is less than 75 microns; the purity of the flake graphite powder is more than 95 percent, and the granularity is less than 100 microns; the fused salt is analytically pure and has a particle size of less than 100 microns.
The mass ratio of the silicon powder to the crystalline flake graphite in the step a is 7: 6-24; the mass ratio of the total mass of the silicon powder and the crystalline flake graphite powder to the molten salt is 1: 1.
In the step a, the molten salt is one of potassium chloride, potassium bromide or sodium chloride.
And C, placing the granulated powder A in a mould to be pressed and molded to obtain a blank B with the pressure of 200MPa, then wrapping the blank B by using a mould larger than the blank B and using molten salt as a filler, and pressing and molding to obtain a salt packaging sample C with the pressure of 200 MPa.
And d, placing the cover into a high-temperature furnace for firing at the temperature of 1300-1400 ℃ at the speed of 5 ℃/min, and keeping the temperature for 1-5h, wherein the firing atmosphere is air atmosphere and does not need to be protected by introducing argon.
Example 1
Weighing 7 parts of silicon powder and 6 parts of crystalline flake graphite powder according to mass fraction, weighing 13 parts of potassium chloride, putting the potassium chloride into a ball milling tank, adding grinding balls and industrial ethanol liquid into the ball milling tank for ball milling for 4 hours, putting the mixed slurry after ball milling into an oven for drying for 12 hours at the temperature of 80 ℃, and sieving through a 40-mesh sieve after drying to obtain granulation powder A; putting the granulation powder A into a phi 20mm mould, and performing compression molding under the uniaxial pressure of 200MPa, and putting the initial sample into a phi 36mm mould full of potassium chloride, and performing compression molding under the uniaxial pressure of 200 MPa; placing the pressed salt packaging sample in an alumina crucible, putting sufficient potassium chloride in the crucible as a salt bed to fully immerse the sample, covering the crucible with a cover, putting the crucible in a high-temperature furnace, roasting to 1400 ℃ at the heating rate of 5 ℃/min, preserving heat for 3h, and naturally cooling to room temperature; and finally, repeatedly washing the product with deionized water for several times to remove salt in a salt layer and the initial sample, filtering, and drying for 12 hours to obtain the silicon carbide coated graphite powder which is dispersed and uniform in size.
Example 2
Weighing 7 parts of silicon powder and 12 parts of crystalline flake graphite powder according to mass fraction, then weighing 19 parts of potassium bromide, putting the potassium bromide into a ball milling tank, adding grinding balls and industrial ethanol liquid into the ball milling tank for ball milling for 4 hours, putting the mixed powder after ball milling into a drying oven for drying for 12 hours at the temperature of 80 ℃, and screening through a 40-mesh sieve after drying to obtain granulation powder A; putting the granulation powder A into a phi 20mm mould, and performing compression molding under the uniaxial pressure of 200MPa, and putting the initial sample into a phi 36mm mould full of potassium bromide, and performing compression molding under the uniaxial pressure of 200 MPa; placing the pressed salt packaging sample in an alumina crucible, putting sufficient potassium bromide in the crucible as a salt bed to fully immerse the sample, covering the crucible, putting the crucible in a high-temperature furnace, roasting to 1350 ℃ at the heating rate of 5 ℃/min, preserving heat for 4h, and naturally cooling to room temperature; and finally, repeatedly washing the product with deionized water for several times to remove salt in a salt layer and the initial sample, filtering, and drying for 12 hours to obtain the silicon carbide coated graphite powder which is dispersed and uniform in size.
Example 3
Weighing 7 parts of silicon powder and 24 parts of crystalline flake graphite powder according to mass fraction, weighing 31 parts of sodium chloride, putting the sodium chloride into a ball milling tank, adding grinding balls and industrial ethanol liquid into the ball milling tank for ball milling for 4 hours, putting the mixed powder after ball milling into an oven for drying at 80 ℃ for 12 hours, and sieving through a 40-mesh sieve after drying to obtain granulation powder A; putting the granulation powder A into a phi 20mm mould, pressing and molding at the uniaxial pressure of 200MPa, putting the initial sample into a phi 36mm mould full of sodium chloride, and pressing and molding at the uniaxial pressure of 200 MPa; placing the pressed salt packaging sample in an alumina crucible, putting sufficient sodium chloride in the crucible as a salt bed to fully immerse the sample, covering the crucible, putting the crucible in a high-temperature furnace, roasting to 1300 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 5h, and naturally cooling to room temperature; and finally, repeatedly washing the product with deionized water for several times to remove salt in a salt layer and the initial sample, filtering, and drying for 12 hours to obtain the silicon carbide coated graphite powder which is dispersed and uniform in size.
The crystal structure and chemical composition of the sample were analyzed by X-ray diffraction, and the results are shown in fig. 1, which shows that the product was graphite and silicon carbide composite powder.
The shape, size and characteristics of the sample are analyzed by a scanning electron microscope, and the results are shown in fig. 2 and fig. 3, and the test results show that the graphite surface is successfully coated with the silicon carbide.
Compared with other preparation methods, the method uses the molten salt which has low price, wide source, no toxicity and environmental protection; the synthesis temperature in the synthesis process is 100-200 ℃ lower than the traditional solid phase sintering temperature, so that the energy is saved; expensive argon is not used as protective atmosphere in the synthesis process, so that the preparation cost is low; the synthesized powder has good dispersibility and uniform size; the prepared SiC-coated crystalline flake graphite powder has good wettability with water.
Claims (6)
1. A method for preparing silicon carbide coated graphite by molten salt isolation is characterized by comprising the following steps: the method comprises the following steps:
a. weighing silicon powder, crystalline flake graphite powder and molten salt according to the mass ratio of 7: 6-24: 13-31, and uniformly mixing by using a ball mill in a wet grinding mode to obtain mixed slurry, wherein the mass ratio of the material to balls to ethanol is 1:2: 2;
b. putting the mixed slurry into an oven for drying, and sieving and granulating the dried powder to obtain granulated powder A;
c. placing the granulated powder A in a mould to be pressed and molded to obtain a blank body B, then wrapping the blank body B by using a mould larger than the blank body B and using molten salt as a filler, and then pressing and molding to obtain a salt packaging sample C;
d. placing a salt packaging sample C in an alumina crucible, putting molten salt capable of completely covering the salt packaging sample C in the crucible as a salt bed, covering the molten salt, putting the crucible in a high-temperature furnace, heating to 1300-;
e. and d, washing the blank obtained in the step d by deionized water to remove salt layers and salt in the blank, crushing the blank to dissolve the salt in the blank, filtering, and finally drying to obtain the target powder.
2. The method of molten salt isolation for preparing silicon carbide coated graphite according to claim 1, characterized in that: in the step a, the purity of the silicon powder is more than 98%, and the particle size is less than 75 microns; the purity of the flake graphite powder is more than 95 percent, and the granularity is less than 100 microns; the fused salt is analytically pure and has a particle size of less than 100 microns.
3. The method of molten salt isolation for preparing silicon carbide coated graphite according to claim 1, characterized in that: the mass ratio of the silicon powder to the crystalline flake graphite in the step a is 7: 6-24; the mass ratio of the total mass of the silicon powder and the crystalline flake graphite powder to the molten salt is 1: 1.
4. The method of molten salt isolation for preparing silicon carbide coated graphite according to claim 1, characterized in that: in the step a, the molten salt is one of potassium chloride, potassium bromide or sodium chloride.
5. The method of molten salt isolation for preparing silicon carbide coated graphite according to claim 1, characterized in that: and C, placing the granulated powder A in a mould to be pressed and molded to obtain a blank B with the pressure of 200MPa, then wrapping the blank B by using a mould larger than the blank B and using molten salt as a filler, and pressing and molding to obtain a salt packaging sample C with the pressure of 200 MPa.
6. The method of molten salt isolation for preparing silicon carbide coated graphite according to claim 1, characterized in that: and d, placing the cover into a high-temperature furnace for firing at the temperature of 1300-1400 ℃ at the speed of 5 ℃/min, and keeping the temperature for 1-5h, wherein the firing atmosphere is air atmosphere and does not need to be protected by introducing argon.
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| CN115215654A (en) * | 2022-07-01 | 2022-10-21 | 偃师中岳耐火材料有限公司 | Preparation method of high-wettability graphite-based composite powder |
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