CN113264771B - Method for rapidly preparing high-strength carbon foam - Google Patents
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- CN113264771B CN113264771B CN202110669352.6A CN202110669352A CN113264771B CN 113264771 B CN113264771 B CN 113264771B CN 202110669352 A CN202110669352 A CN 202110669352A CN 113264771 B CN113264771 B CN 113264771B
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Abstract
A method for rapidly preparing light high-strength carbon foam comprises the following steps: mechanically stirring commercial phenolic resin and 2000-mesh quartz powder for more than 30 min to uniformly mix; adding a small amount of benzenesulfonic acid serving as a curing agent, and continuously stirring for about 10 min to uniformly mix to obtain mixed slurry; pouring the mixed slurry into a cylindrical mold, and curing for 2 hours in a box-type resistance furnace at the temperature of 100 ℃; placing the foam blank solidified in the step (4) in a vacuum tube type resistance heating furnace, wherein the vacuum degree is-0.1 MPa, the temperature is increased to 1000 ℃ at the heating rate of 5-15 ℃/min, and the temperature is kept for 3 h and then the foam blank is cooled to room temperature along with the furnace to complete carbonization of the foam blank; and (5) placing the carbonized foam blank in HF acid for ultrasonic etching for more than 48 h to filter out the quartz template, thereby obtaining the final carbon foam product.
Description
Technical Field
The invention relates to an inorganic porous material technology, in particular to a preparation technology of carbon foam with low density and high strength characteristics.
Background
Carbon foam is widely applied to the industrial fields of aerospace, nuclear industry, supercapacitors, catalyst carriers and the like due to the special organization structure, low density, high porosity, low thermal expansion coefficient, larger specific surface area, excellent oxidation resistance, low cost, excellent sound absorption performance, excellent electromagnetic shielding performance and the like.
Carbon foams exist in two major microstructures, one being an open, reticulated vitreous structure and the other being a spherical porous structure. Different structures endow the carbon foam with different characteristics, for example, the reticular glassy carbon foam is generally in an open-cell structure, open pores are favorable for exerting the adsorption effect of the carbon foam, and in addition, the carbon foam has the characteristics of wave absorption and the like; and the carbon foam with the spherical pore structure is more beneficial to the application of the characteristics of heat conduction, electric conduction and the like.
The development of carbon foams at present mainly utilizes the functional and structural properties of the carbon foams, and no matter which type of carbon foams is improved and developed for countless times, but the most remarkable defects of the carbon foams are that the strength is generally low, and the differences of mechanical properties are caused by the structures and densities of different foams. The compressive strength of common carbon foam is generally low, and the common carbon foam has serious mechanical property defects in the aspect of being used as a structural or heavy-duty material. In other words, their widespread use is limited due to the specific nature of the porous structure that limits the development of high strength carbon foams. In addition, the prior art processes often require tens or even hundreds of hours to produce carbon foams, increasing production costs.
Disclosure of Invention
The object of the present invention is to provide a method for rapidly preparing a lightweight high-strength carbon foam.
The invention relates to a method for quickly preparing light high-strength carbon foam, which comprises the following steps:
respectively mechanically stirring commercial phenolic resin and 2000-mesh quartz powder for more than 30 min according to four proportions of 3:1, 2:1, 1:1 and 1:2, and uniformly mixing;
adding a small amount of benzenesulfonic acid serving as a curing agent into the mixture, and continuously stirring the mixture for about 10 min to uniformly mix the mixture to obtain mixed slurry;
pouring the mixed slurry into a cylindrical mold, and curing for 2 hours in a box-type resistance furnace at the temperature of 100 ℃;
placing the foam blank solidified in the step (4) in a vacuum tube type resistance heating furnace, wherein the vacuum degree is-0.1 MPa, the temperature is increased to 1000 ℃ at the heating rate of 5-15 ℃/min, and the temperature is kept for 3 h and then the foam blank is cooled to room temperature along with the furnace to complete carbonization of the foam blank;
and (5) placing the carbonized foam blank in HF acid for ultrasonic etching for more than 48 hours to filter out a quartz template, and obtaining a final carbon foam product.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method has simple process route in the preparation process, only needs four steps, and greatly shortens the preparation period in the prior art; the equipment is less in strict requirement, and the preparation can be carried out only by a box-type resistance furnace and a vacuum heating furnace; the raw materials for preparing the carbon foam are low in cost and easy to obtain, and the preparation cost is greatly reduced in the aspects of raw materials, process route design and equipment conditions.
(2) The density of the carbon foam prepared by the process from foam blanks with different proportions (phenolic resin/quartz template) is 0.947 g/cm3、0.781 g/cm3、0.471 g/cm3And 0.306 g/cm3The compression strength is respectively 106.4 MPa, 76.5 MPa, 40.4 MPa and 21.6 MPa, which is obviously higher than the carbon foam with the same density level in the existing research at home and abroad at present.
(3) The carbon foam prepared by the invention has controllable volume shrinkage, and the geometric effect of the sample is smaller in the isothermal carbonization environment, so that the requirement of customizing the product can be met.
(4) According to the invention, the quartz templates with different specific gravities are added into different resin blanks, so that the pore size, pore size distribution, porosity and the like of the final carbon foam can be changed under the condition of a certain proportion of resin and curing agent, and the purpose of pore control is achieved.
Drawings
FIG. 1 is a flow chart of the inventive process for carbon foam, FIG. 2 is a 3:1 solidified foam green body macro-topography, FIG. 3 is an enlarged view of a yellow box of FIG. 2, FIG. 4 is a 2:1 solidified foam green body macro-topography, FIG. 5 is an enlarged view of a yellow box of FIG. 4, FIG. 6 is a 1:1 solidified foam green body macro-topography, FIG. 7 is an enlarged view of a yellow box of FIG. 6, FIG. 8 is a 1:2 solidified foam green body macro-topography, FIG. 9 is an enlarged view of a yellow box of FIG. 8, FIG. 10 is a 3:1 carbonized foam green body macro-topography, FIG. 11 is an enlarged view of FIG. 10, FIG. 12 is a 2:1 carbonized foam green body macro-topography, FIG. 13 is an enlarged view of FIG. 12, FIG. 14 is a 1:1 carbonized foam green body macro-topography, FIG. 15 is an enlarged view of FIG. 14, FIG. 16 is a 1:2 carbonized foam green body macro-topography, FIG. 17 is an enlarged view of FIG. 16, FIG. 18 is a microscopic topography of a 3:1 carbon foam, FIG. 19 is an enlarged view of the yellow box of FIG. 18, FIG. 20 is a microscopic topography of a 2:1 carbon foam, FIG. 21 is an enlarged view of the yellow box of FIG. 20, FIG. 22 is a microscopic topography of a 1:1 carbon foam, FIG. 23 is an enlarged view of the yellow box of FIG. 22, FIG. 24 is a microscopic topography of a 1:2 carbon foam, FIG. 25 is an enlarged view of the yellow box of FIG. 24, and FIG. 26 is a compressive strength of a different carbon foam.
Detailed Description
As shown in fig. 1, the present invention is a method for rapidly preparing a light-weight high-strength carbon foam, comprising the steps of:
respectively mechanically stirring commercial phenolic resin and 2000-mesh quartz powder for more than 30 min according to four proportions of 3:1, 2:1, 1:1 and 1:2, and uniformly mixing;
adding a small amount of benzenesulfonic acid serving as a curing agent into the mixture, and continuously stirring the mixture for about 10 min to uniformly mix the mixture to obtain mixed slurry;
pouring the mixed slurry into a cylindrical mold, and curing for 2 hours in a box-type resistance furnace at the temperature of 100 ℃;
placing the foam blank solidified in the step (4) in a vacuum tube type resistance heating furnace, wherein the vacuum degree is-0.1 MPa, the temperature is increased to 1000 ℃ at the heating rate of 5-15 ℃/min, and the temperature is kept for 3 h and then the foam blank is cooled to room temperature along with the furnace to complete carbonization of the foam blank;
and (5) placing the carbonized foam blank in HF acid for ultrasonic etching for more than 48 h to filter out the quartz template, thereby obtaining the final carbon foam product.
According to the relevant regulations of GB/T34559 and 2017, the compression strength of different carbon foams is tested, and the geometric dimension of a sample to be tested is 10 mm multiplied by 10 mm.
The mechanical mixing of step (1) described above does not involve grinding, otherwise the crystal form of the quartz template is destroyed. And (2) mechanically mixing, namely stirring for not less than 30 min at room temperature.
The mechanical mixing time after the curing agent is added in the step (2) is not longer than 20 min, continuous stirring is beneficial to curing, but the too long stirring time can cause the curing molding to be not uniform.
And (4) naturally standing the mixed slurry obtained in the step (3) at room temperature for 24 hours to shape the blank.
The variation error of the vacuum pressure in the carbonization process in the step (4) is +/-0.01 MPa.
In the ultrasonic etching process in the step (5), the filtrate needs to be replaced every 10 hours, and the filtrate with high saturation degree is difficult to filter out the residual template, so that the filtrate needs to be replaced in time.
As can be seen from the carbon foam green body graphs with different proportions in the graphs of fig. 2 to fig. 9, the spherical pores formed in the curing process are reduced along with the increase of the quartz concentration, and the pore diameter is gradually and uniformly changed.
The macroscopic morphology of fig. 8 shows that the color distribution between red and white phases is mainly caused by the fact that the viscosity of the resin is reduced due to the increase of the concentration of quartz, the mechanical mixing difficulty is increased, and the green slurry before curing is not uniform enough.
As can be seen from the diagrams of the carbon foam blank after carbonization at different ratios in fig. 13 to fig. 19, the progress of the carbonization process causes uniform shrinkage of the sample, and the larger the quartz concentration is, the smaller the volume shrinkage rate is, and the spherical pore volume is also reduced correspondingly.
As can be seen from the carbon foam microstructures with different proportions in the figures 18-25, the concentration of quartz in the blank is increased, the aperture of the spherical hole is reduced, the aperture distribution is gradually uniform, the hole wall is thinned, the columnar ligament is thinned, and the spherical closed hole embedded in the ligament is reduced.
As can be seen from the compression performance histogram of the carbon foam with different ratios in fig. 26, the quartz concentration in the green body is increased, and the density, the compression strength and the specific compression strength are all linearly decreased, but the carbon creep mold under any density condition has unique performance advantages.
The process flow of the invention is shown in fig. 1, and the preparation process of the invention is described in detail below with reference to specific examples.
Example 1:
(1) a carbon foam having a specific gravity of 3:1 of resin and quartz is prepared by first preparing 15 g of a thermosetting phenol resin (viscosity: 16000-19000 MP/25 ℃, residual carbon rate: 40-45%, purity: 99%) and 5 g of quartz powder (main component: SiO) having a particle size of 2000 mesh2Purity: 99 percent) and quartz powder are dried in a box type resistance furnace at the temperature of 100 ℃ for 1 hour for later use;
(2) pouring phenolic resin into a mortar, slowly adding quartz powder, continuously stirring for more than 30 min, stopping stirring, adding a trace amount of curing agent (benzenesulfonic acid), continuously stirring for 8-10 min until the mixed slurry is viscous, and pouring the mixed slurry into a prefabricated cylindrical mold;
(3) placing the prefabricated blank slurry in air at room temperature, and standing for 24h until the blank slurry is solidified and shaped;
(4) placing the cured foam blank body in a box-type resistance heating furnace, heating to 100 ℃, keeping for 2 hours, and naturally cooling to room temperature along with the furnace to finish the final curing process of the foam blank;
(5) polishing burrs and the surface of the solidified foam blank to be flat by a grinder, abrasive paper and the like, then placing the blank in a tubular resistance heating furnace, rapidly heating the blank to 1000 ℃ from room temperature at a heating rate of 10 ℃/min, keeping the temperature for 3 h, then finishing the heating procedure, cooling the blank to room temperature along with the furnace, and finishing the carbonization process of the blank;
(6) polishing the surface of the carbonized foam blank body to be flat, completely immersing the foam blank body into filtrate HF acid, soaking for more than 48 hours, wherein the HF acid is replaced every 6 hours, and ultrasonically oscillating for 15 min in an ultrasonic cleaning instrument;
(7) the carbon foam after the filtering process is firstly cleaned by absolute ethyl alcohol in an ultrasonic mode for 15 min, and the operation is repeated for 3 times, so that the carbon foam with the ratio of 3:1 (phenolic resin: quartz powder) is finally prepared.
Tests show that the density of the carbon foam prepared by the process is 0.947 g/cm3A compressive strength of 106.4 MPa and a specific compressive strength of 112.35 MPa cm3/g。
Example 2:
(1) a carbon foam having a specific gravity of resin and quartz of 1:1 is prepared by first preparing 10 g of a thermosetting phenol resin (viscosity: 16000-19000 MP/25 ℃, residual carbon rate: 40-45%, purity: 99%) and 10 g of quartz powder (main component: SiO) having a particle size of 2000 mesh2Purity: 99 percent) and quartz powder are dried in a box type resistance furnace at the temperature of 100 ℃ for 1 hour for later use;
(2) pouring phenolic resin into a mortar, slowly adding quartz powder, continuously stirring for more than 30 min, stopping stirring, adding a trace amount of curing agent (benzenesulfonic acid), continuously stirring for 8-10 min until the mixed slurry is viscous, and pouring the mixed slurry into a prefabricated cylindrical mold;
(3) placing the prefabricated blank slurry in air at room temperature, and standing for 24h until the blank slurry is solidified and shaped;
(4) placing the cured foam blank body in a box-type resistance heating furnace, heating to 100 ℃, keeping for 2 hours, and naturally cooling to room temperature along with the furnace to finish the final curing process of the foam blank;
(5) polishing burrs and the surface of the solidified foam blank to be flat by a grinder, abrasive paper and the like, then placing the blank in a tubular resistance heating furnace, rapidly heating the blank to 1000 ℃ from room temperature at a heating rate of 10 ℃/min, keeping the temperature for 3 h, then finishing the heating procedure, cooling the blank to room temperature along with the furnace, and finishing the carbonization process of the blank;
(6) polishing the surface of the carbonized foam blank body to be flat, completely immersing the foam blank body into filtrate HF acid, soaking for more than 48 hours, wherein the HF acid is replaced every 6 hours, and ultrasonically oscillating for 15 min in an ultrasonic cleaning instrument;
(7) the carbon foam after the filtering process is firstly cleaned by absolute ethyl alcohol in an ultrasonic way for 15 min and is repeatedly operated for 3 times, and finally the carbon foam with the ratio of 1:1 (phenolic resin: quartz powder) is prepared.
Tests show that the density of the carbon foam prepared by the process is 0.471 g/cm3A compressive strength of 40.4 MPa and a specific compressive strength of 85.77 MPa cm3/g。
The invention has not been described in detail in part of the common general knowledge of those skilled in the art.
Claims (6)
1. A method for rapidly preparing high-strength carbon foam is characterized by comprising the following steps:
step (1) mechanically stirring commercial phenolic resin and 2000-mesh quartz powder for more than 30 min according to four proportions of 3:1, 2:1, 1:1 and 1:2 respectively and uniformly mixing;
adding a small amount of benzenesulfonic acid serving as a curing agent, and continuously stirring for 10 min to uniformly mix to obtain mixed slurry;
pouring the mixed slurry into a cylindrical mold, and curing for 2 hours in a box-type resistance furnace at the temperature of 100 ℃;
placing the solidified foam blank in the step (4) in a vacuum tube type resistance heating furnace, wherein the vacuum degree is-0.1 MPa, the temperature is increased to 1000 ℃ at the heating rate of 5-15 ℃/min, and the temperature is kept for 3 h and then is cooled to room temperature along with the furnace to complete carbonization of the foam blank;
and (5) placing the carbonized foam blank in HF acid for ultrasonic etching for more than 48 h to dissolve and leach out the quartz template, thereby obtaining the final carbon foam product.
2. The method for rapid production of high strength carbon foam according to claim 1, wherein the mechanical mixing of step (1) does not include milling.
3. The method for rapidly preparing a high strength carbon foam according to claim 1, wherein the step (1) of mechanically mixing is performed for not less than 30 min under a room temperature environment.
4. The method for rapidly preparing high strength carbon foam according to claim 1, wherein the mechanical mixing time after the addition of the curing agent in the step (2) is not more than 20 min, and the continuous stirring is used for facilitating the curing.
5. The method for rapidly preparing high-strength carbon foam according to claim 1, wherein the mixed slurry in the step (3) is placed in the air at room temperature after being poured into the cylindrical mold, and is left for 24 hours until the blank slurry is solidified and molded.
6. The method for rapidly preparing high-strength carbon foam according to claim 1, wherein the dissolution solution is replaced every 10 hours during the ultrasonic etching in the step (5).
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