CN115745655A - Preparation method of porous silicon carbide ceramic material and preparation method of phase-change heat storage material of porous silicon carbide ceramic material - Google Patents
Preparation method of porous silicon carbide ceramic material and preparation method of phase-change heat storage material of porous silicon carbide ceramic material Download PDFInfo
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Abstract
The invention discloses a preparation method of a porous silicon carbide ceramic material and a preparation method of a phase-change heat storage material thereof. The ceramic material is prepared from a matrix raw material which adopts NaOH-Na 2 SO 3 、H 2 O 2 Removing part of lignin and cellulose in the wood by chemical treatment to increase the porosity, carbonizing, reacting with molten silicon and removing redundant silicon to obtain porous silicon carbide ceramic, and changing the chemical treatment time to obtain silicon carbide ceramics with different pores, wherein the pore range of the prepared silicon carbide ceramic is 55-80%. Filling the polyethylene glycol phase-change material into pores of the porous silicon carbide by adopting a vacuum impregnation method to obtain the porous silicon carbide ceramic-based phase-change storageA thermal material. The porous silicon carbide ceramic-based phase change heat storage has the characteristics of high porosity and high heat conductivity, and provides an effective method for developing a higher-efficiency solar storage technology based on a phase change material.
Description
Technical Field
The invention relates to a preparation method of a ceramic material and a preparation method of a phase-change heat storage material, in particular to a preparation method of a porous silicon carbide ceramic material and a preparation method of a phase-change heat storage material thereof.
Background
Solar energy storage technology based on phase change materials is widely researched due to the fact that the solar radiation intermittency and fluctuation can be overcome, however, the bottleneck problem that the thermal conductivity of the phase change materials is low severely restricts the efficient and rapid storage of solar energy. The traditional method for improving the thermal conductivity of the phase change material is to prepare the composite phase change material by compounding the phase change material with a porous metal framework or a carbon framework, but the metal material is not resistant to molten salt corrosion, and the carbon material is not high-temperature resistant. Porous ceramic materials, especially porous silicon carbide ceramics, are considered to be good candidates for improving the thermal conductivity of phase change materials due to their high strength, high hardness, good thermal shock resistance, high thermal conductivity, and good chemical stability.
The biological material has a naturally communicated porous structure, and provides a new idea for preparing porous silicon carbide ceramic. However, the porosity of the biological material is fixed, and no regulation method is available, so that the heat storage requirements of different scenes are difficult to meet. Therefore, the silicon carbide ceramic based on the biological material has the characteristic of adjustable porosity, and becomes a key problem which needs to be solved urgently for improving the heat storage performance of the phase-change material.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a preparation method of a porous silicon carbide ceramic material with higher porosity;
the second purpose of the invention is to provide a preparation method of the porous silicon carbide ceramic-based phase change heat storage material with higher porosity and thermal conductivity.
The technical scheme is as follows: according to the preparation method of the porous silicon carbide ceramic material, the matrix raw material is subjected to chemical treatment to remove partial lignin and hemicellulose so as to increase the porosity, and then the matrix raw material is subjected to high-temperature carbonization, reacts with molten silicon and removes redundant silicon to obtain the porous silicon carbide ceramic.
Further, the method specifically comprises the following steps:
(1) Putting the matrix raw material in NaOH-Na 2 SO 3 Boiling the mixed aqueous solution to remove lignin and cellulose, and washing with boiling water;
(2) Putting the washed matrix raw material in H 2 O 2 Boiling in water solution to further remove lignin and cellulose, and washing with boiling water;
(3) Carrying out freeze drying and carbonization treatment on the matrix raw material washed in the step (2) to obtain a porous carbon precursor derived from the matrix raw material;
(4) And (3) taking the porous carbon precursor and molten silicon to generate the silicon carbide/silicon composite material under the high-temperature heating condition, and removing redundant silicon to obtain the silicon carbide ceramic material.
Furthermore, the matrix raw material of the invention is a mixture containing lignin, hemicellulose, cellulose and other components, and comprises any one of wood, bamboo, sugarcane, coconut shell and corn cob; the lignin and hemicellulose in the substances can be removed by sodium hydroxide-sodium sulfite and hydrogen peroxide solution to realize the function of adjusting the pores. Still further, the wood is preferably hardwood; the hardwood is preferably red oak; preferably, the wood is a block, and the block is 25-35 m long, 25-35 mm wide and 10-15 mm thick. The wood with the shape and the size can be fully mixed with NaOH-Na 2 SO 3 、H 2 O 2 And reacting to obtain the optimal delignification effect.
Furthermore, in the step (1), the boiling time is 7-14 h; the preferred NaOH concentration is 2.5 + -0.01M Na 2 SO 3 The concentration is 0.4 +/-0.01M; the delignification effect obtained under the conditions is optimal.
Further, in the step (2), H 2 O 2 H in aqueous solution 2 O 2 The mass fraction of (B) is 30 +/-1 wt%; the boiling time is 1-4 h. The wood block obtained under the condition has the best delignification effect and also has the best structural stability.
Further, in the step (3), the freeze-drying process parameters are as follows: the set temperature is-20 to-10 ℃, and the drying time is 36 to 48 hours. The drying effect obtained under this condition is the best.
Further, in the step (3), the carbonization process parameters are as follows: under the protection atmosphere, the heating rate is 1-2 ℃/min, the carbonization temperature is 900-1000 ℃, and the heat preservation time is 0.5-1 h. The wood block can be ensured to have higher structural stability at the temperature rising rate.
Further, in the step (4), the process parameters of silicon melting are as follows: in a vacuum state, the heating rate is 5-20 ℃/min, the reaction temperature is 1550-1600 ℃, and the heat preservation time is 1-2 h. Under the condition, the solid silicon is changed into a molten state, the molten silicon can be easily filled into the pores of the carbon precursor, and a fully reacted sample can be obtained.
Further, in the step (4), the process parameters of high-temperature heating are as follows: in a vacuum state, the heating rate is 5-20 ℃/min, the reaction temperature can be 1750-1850 ℃, and the heat preservation time can be 1-2 h. Silicon turns into silicon vapor at this temperature, which is more favorable than silicon removal, under which conditions the sintered silicon carbide grains are most dense.
Further, in the step (4), the process parameters of high-temperature heating are as follows: and (3) sufficiently spreading carbon powder at the bottom of the crucible, and reacting the carbon powder with the excess silicon to generate silicon carbide powder.
According to the method for preparing the phase change heat storage material by using the porous silicon carbide ceramic material prepared by the method, the phase change material is filled into the pores of the porous silicon carbide ceramic by adopting a vacuum impregnation method, so that the porous silicon carbide ceramic-based phase change heat storage material is obtained.
The method comprises the following specific steps: the parameters of the vacuum impregnation method are as follows: heating to 80-100 ℃ in a vacuum state, and keeping the temperature for 2-4 h. The best dipping effect can be obtained under the condition, and the filling rate of the phase-change material is highest.
When the porosity of the porous silicon carbide ceramic material is 55 +/-1%, the volume fraction of the phase change material is 55 +/-1%; when the porosity of the porous silicon carbide ceramic material is 80 +/-1%, the volume fraction of the phase-change material is 80 +/-1%; preferably, the phase change material is polyethylene glycol.
The invention principle is as follows: the method comprises the steps of selecting wood as a matrix raw material for preparing silicon carbide, wherein the wood has a naturally communicated pore structure, cutting the wood into thinner wood blocks, sequentially placing the wood blocks into boiling aqueous solutions of sodium hydroxide-sodium sulfite and hydrogen peroxide, boiling the wood blocks to remove part of lignin and hemicellulose in the wood blocks so as to increase the porosity of the wood blocks, controlling the degree of removing the lignin and the hemicellulose by controlling the boiling time so as to obtain the wood blocks with different porosities, and removing residual water in the wood blocks by adopting a freeze drying mode. And carbonizing the dried wood block in an inert atmosphere to obtain the porous carbon precursor with the wood block structure. The carbon precursor and the molten silicon are put in a high temperature environment then the silicon carbide-silicon composite material is generated by reaction. And removing redundant silicon by a high-temperature evaporation method, thereby obtaining the silicon carbide ceramics with different porosities.
And filling the phase change material into the pores of the porous silicon carbide ceramic by adopting a vacuum impregnation method to prepare the porous silicon carbide ceramic-based phase change heat storage material.
The natural red oak in the specific embodiment of the invention is directly carbonized into a porous carbon precursor, and then the porous carbon precursor reacts with molten silicon to obtain the silicon carbide ceramic with the porosity of only 55 percent. However, the porosity of the silicon carbide ceramic prepared by the method is too low, which results in that the volume fraction of the phase change material filled in the pores of the silicon carbide ceramic is only 55%, which further results in that the heat storage density of the composite material is too low. The porosity of the porous silicon carbide ceramic is effectively improved by the silicon carbide ceramic material prepared by the method, the volume fraction of the phase-change material is remarkably increased to 80%, and the heat storage density of the composite phase-change material is greatly improved; in addition, the thermal conductivity of the composite phase change material is as high as 31.2W/mK, and is remarkably improved compared with 0.2W/mK of a pure phase change material.
Has the advantages that: compared with the prior art, the invention has the following remarkable effects: (1) The porosity range of the porous silicon carbide ceramic is 55-80%, the porous silicon carbide ceramic has the advantage of adjustable height of pores, and the precursor is a biomass material and has the advantage of high communication of the pores. (2) The process method for preparing the porous silicon carbide ceramic has the advantages of high purity of the silicon carbide ceramic and good compactness of ceramic crystals. The high-temperature silicon removal method removes unreacted silicon, and the silicon carbide ceramic forms a compact structure at high temperature; carbon powder is introduced in the step of removing silicon, and the carbon powder can further react with more than silicon to generate silicon carbide powder, so that the removal of more than silicon is facilitated, and the prepared silicon carbide has high purity. (3) The invention adopts biomass materials, and has the advantages of environmental protection, rich raw materials, low price and suitability for batch production. (4) The silicon carbide ceramic prepared by the invention has the advantage of high thermal conductivity, and the thermal conductivity of the silicon carbide-polyethylene glycol composite phase change material can reach 31.2W/mK when the porosity of the silicon carbide ceramic is 80% owing to the characteristics of high-temperature sintering and directional structure.
Drawings
FIG. 1 is a schematic view of a process for preparing a ceramic-based phase-change heat storage material according to the present invention;
FIG. 2 is a schematic representation of a porous silicon carbide ceramic prepared in example 1;
FIG. 3 is an SEM image of a porous silicon carbide ceramic prepared in example 1;
FIG. 4 is an enlarged SEM image of grains of the porous silicon carbide ceramic prepared in example 1;
FIG. 5 is an SEM photograph of silicon carbide without lignin removal in comparative example 1;
FIG. 6 is a drawing of a silicon carbide ceramic real object prepared in comparative example 2 using Baer wood as a matrix raw material.
Detailed Description
The present invention is described in further detail below.
Example 1
Cutting red oak into wood blocks with length of 30mm, width of 30mm and thickness of 15mm, drying in oven at 70 deg.C for 2 days, adding 2.5M NaOH and 0.4M Na 2 SO 3 Boiling the mixed boiling water solution for 7h, and boiling in boiling deionized water for several times until the pH value of the solution is neutral. Then by boiling 30wt% 2 O 2 The wood block was treated for 1h to remove part of the lignin and hemicellulose, immersed in boiling deionized water to remove chemical residues, and then dried in a freeze dryer at-10 ℃ for 48h. And (3) carbonizing the wood block in a tube furnace in an argon atmosphere at the temperature rise rate of 1 ℃/min and the carbonization temperature of 900 ℃, and preserving the heat for 30 minutes to obtain the porous carbon precursor. And (3) taking the carbon precursor to react with the silicon particles at 1600 ℃ in vacuum for 1 hour to generate the silicon carbide-silicon composite material. Silicon carbideHeating the silicon composite material to 1800 ℃ in vacuum, keeping the temperature for 1.5 hours to remove the redundant silicon, and repeating the process for 3 times to obtain the porous silicon carbide ceramic. And (3) placing the porous silicon carbide ceramic coated with the polyethylene glycol phase-change material in an oven, heating to 80 ℃ in a vacuum state, and preserving heat for 2 hours to obtain the porous silicon carbide ceramic-based phase-change heat storage material.
Example 2
The specific preparation method is the same as that of example 1, except that the time of the hydrogen peroxide treatment is different.
Cutting red oak into wood blocks with length of 30mm, width of 30mm and thickness of 15mm, drying in oven at 70 deg.C for 2 days, adding 2.5M NaOH and 0.4M Na 2 SO 3 Boiling the mixed boiling water solution for 7h, and boiling in boiling deionized water for several times until the pH value of the solution is neutral. Then by boiling 30wt% 2 O 2 The wood pieces were treated for 4h to remove part of the lignin and hemicellulose, dipped in boiling deionized water to remove chemical residues, and then dried in a freeze dryer at-10 ℃ for 48h. And (3) putting the wood block into a tube furnace for carbonization in an argon atmosphere, wherein the heating rate is 1 ℃/min, the carbonization temperature is 900 ℃, and the temperature is kept for 30 minutes to obtain the porous carbon precursor. And taking the carbon precursor to react with the silicon particles for 1h at the temperature of 1600 ℃ in vacuum to generate the silicon carbide-silicon composite material. The silicon carbide-silicon composite material is heated to 1800 ℃ in vacuum, the temperature is kept for 1.5 hours, the redundant silicon is removed, the process is repeated for 3 times, and the porous silicon carbide ceramic is obtained. And (3) placing the porous silicon carbide ceramic coated with the polyethylene glycol phase-change material in an oven, heating to 80 ℃ in a vacuum state, and preserving heat for 2 hours to obtain the porous silicon carbide ceramic-based phase-change heat storage material.
The porosity of the silicon carbide ceramic increased from 55% to 80% with increasing hydrogen peroxide treatment time. Due to the removal of lignin and hemicellulose, the walls of the wood structure become thin and the structure becomes loose and porous, as shown in fig. 3. Therefore, by adjusting the time of the hydrogen peroxide treatment, silicon carbide ceramics with different porosities can be obtained.
Example 3
Cutting red oak into wood blocks with length of 30mm, width of 30mm and thickness of 15mm, drying in oven at 70 deg.C for 2 days, and placing 2.5M NaOH and 0.4M Na 2 SO 3 Boiling the mixed boiling water solution for 7h, and boiling in boiling deionized water for several times until the pH value of the solution is neutral. Then by boiling 30wt% 2 O 2 The wood block was treated for 1h to remove part of the lignin and hemicellulose, immersed in boiling deionized water to remove chemical residues, and then dried in a freeze dryer at-10 ℃ for 36h. And (3) putting the wood block into a tube furnace for carbonization in an argon atmosphere, wherein the heating rate is 1 ℃/min, the carbonization temperature is 900 ℃, and the temperature is kept for 30 minutes to obtain the porous carbon precursor. And (3) taking the carbon precursor to react with the silicon particles at 1550 ℃ in vacuum for 1.5h to generate the silicon carbide-silicon composite material. And (3) putting sufficient carbon powder into a crucible, heating the silicon carbide-silicon composite material to 1750 ℃ in vacuum, preserving the temperature for 2 hours to remove excessive silicon, and repeating the process for 3 times to obtain the porous silicon carbide ceramic. And (3) placing the porous silicon carbide ceramic coated with the polyethylene glycol phase-change material in an oven, heating to 80 ℃ in a vacuum state, and preserving heat for 4 hours to obtain the porous silicon carbide ceramic-based phase-change heat storage material.
Example 4
Cutting red oak into wood blocks with length of 30mm, width of 30mm and thickness of 15mm, drying in oven at 70 deg.C for 2 days, adding 2.5M NaOH and 0.4M Na 2 SO 3 Boiling the mixed boiling water solution for 14h, and boiling in boiling deionized water for several times until the pH value of the solution is neutral. Then by boiling 30wt% 2 O 2 The wood pieces were treated for 4h to remove part of the lignin and hemicellulose, dipped in boiling deionized water to remove chemical residues, and then dried in a freeze dryer at-20 ℃ for 48h. And (3) putting the wood block into a tube furnace for carbonization in an argon atmosphere, wherein the heating rate is 2 ℃/min, the carbonization temperature is 1000 ℃, and the temperature is kept for 60 minutes to obtain the porous carbon precursor. And (3) taking the carbon precursor to react with the silicon particles at 1600 ℃ in vacuum for 1 hour to generate the silicon carbide-silicon composite material. The silicon carbide-silicon composite material is heated up to 1850 ℃ in vacuum and is kept warm for 1 hour to remove the redundant silicon, the process was repeated 3 times to obtain porous silicon carbide ceramic. And (3) placing the porous silicon carbide ceramic coated with the polyethylene glycol phase-change material in an oven, heating to 100 ℃ in a vacuum state, and preserving heat for 2 hours to obtain the porous silicon carbide ceramic-based phase-change heat storage material.
Comparative example 1
The method is characterized in that lignin and hemicellulose are not removed, namely, the wood block is not boiled by using sodium hydroxide-sodium sulfite and hydrogen peroxide solution, the wood block is directly carbonized after being dried and reacts with molten silicon to remove the lignin to generate silicon carbide, the porosity of the prepared silicon carbide is only 55%, a microstructure diagram of the silicon carbide is shown in figure 5, and the porosity is fixed and unadjustable.
Comparative example 2
Instead of adopting the red oak with lower porosity as the matrix raw material, the Barre fir with higher porosity is adopted as the matrix raw material; the porosity of the balsa wood of this example was 75%. Cutting Baker fir wood into wood blocks with length of 30mm, width of 30mm and thickness of 15mm, drying in 70 deg.C oven for 48 hr, adding 2.5M NaOH and 0.4M Na 2 SO 3 Boiling the mixed boiling water solution for 7h, and boiling in boiling deionized water for several times until the pH value of the solution is neutral. Then by boiling 30wt% 2 O 2 The wood pieces were treated for 1h to remove part of the lignin and hemicellulose, dipped in boiling deionized water to remove chemical residues, and then dried in a freeze dryer at-10 ℃ for 2 days. And (3) putting the wood block into a tube furnace for carbonization in an argon atmosphere, wherein the heating rate is 1 ℃/min, the carbonization temperature is 900 ℃, and the temperature is kept for 30 minutes to obtain the porous carbon precursor. And taking the carbon precursor to react with the silicon particles for 1h at the temperature of 1600 ℃ in vacuum to generate the silicon carbide-silicon composite material. The silicon carbide-silicon composite material is heated to 1800 ℃ in vacuum and is kept warm for 1.5 hours to remove redundant silicon, and the process is repeated for 3 times to obtain the porous silicon carbide ceramic. And (3) placing the porous silicon carbide ceramic coated with the polyethylene glycol phase-change material in an oven, heating to 80 ℃ in a vacuum state, and preserving heat for 2 hours to obtain the porous silicon carbide ceramic-based phase-change heat storage material.
As shown in figure 6, the porous silicon carbide ceramic prepared by adopting the Baer fir as the matrix material has higher porosity, and the porosity is further improved after lignin is further removed, so that the structural strength is obviously reduced, and the porous silicon carbide ceramic prepared by adopting the Baer fir cannot keep the original structural shape.
Comparative example 3
Cutting red oak into wood blocks with length of 30mm, width of 30mm and thickness of 15mm, drying in oven at 70 deg.C for 48 hr, placing 2.5M NaOH and 0.4M Na 2 SO 3 Boiling the mixed boiling water solution for 7h, and boiling in boiling deionized water for several times until the pH value of the solution is neutral. Then by boiling 30wt% 2 O 2 The wood pieces were treated for 9h to remove lignin and hemicellulose, dipped into boiling deionized water to remove chemical residues, and then placed in a freeze dryer for 2 days at-10 ℃. And (3) putting the wood block into a tube furnace for carbonization in an argon atmosphere, wherein the heating rate is 1 ℃/min, the carbonization temperature is 900 ℃, and the temperature is kept for 30 minutes to obtain the porous carbon precursor. And taking the carbon precursor to react with the silicon particles for 1h at the temperature of 1600 ℃ in vacuum to generate the silicon carbide-silicon composite material. The silicon carbide-silicon composite material is heated to 1800 ℃ in vacuum, the temperature is kept for 1.5 hours, the redundant silicon is removed, the process is repeated for 3 times, and the porous silicon carbide ceramic is obtained. And (3) placing the porous silicon carbide ceramic coated with the polyethylene glycol phase-change material in an oven, heating to 80 ℃ in a vacuum state, and preserving heat for 2 hours to obtain the porous silicon carbide ceramic-based phase-change heat storage material.
The method is characterized in that 30wt% of hydrogen peroxide is adopted to boil the red oak for 9 hours, due to the fact that the boiling time is too long, lignin and cellulose structures are completely removed, the red oak structure is completely collapsed, the whole blocky structure cannot be kept, and therefore follow-up experiments cannot be carried out.
Claims (10)
1. A preparation method of a porous silicon carbide ceramic material is characterized in that a matrix raw material is subjected to chemical treatment to remove partial lignin and hemicellulose so as to increase porosity, and then is subjected to high-temperature carbonization, reacts with molten silicon and removes redundant silicon to obtain the porous silicon carbide ceramic.
2. The method for preparing the porous silicon carbide ceramic material according to claim 1, comprising the following steps:
(1) Putting the matrix raw material in NaOH-Na 2 SO 3 Boiling the mixed aqueous solution to remove lignin and cellulose, and washing with boiling water;
(2) Will washPlacing the substrate raw material in H 2 O 2 Boiling in water solution to further remove lignin and cellulose, and washing with boiling water;
(3) Carrying out freeze drying and carbonization treatment on the matrix raw material washed in the step (2) to obtain a porous carbon precursor derived from the matrix raw material;
(4) And (3) taking the porous carbon precursor and molten silicon to generate the silicon carbide/silicon composite material under the high-temperature heating condition, and removing redundant silicon to obtain the porous silicon carbide ceramic material.
3. The method for preparing a porous silicon carbide ceramic material according to claim 4, wherein the boiling time in step (1) is 7-14 h.
4. The method for preparing porous silicon carbide ceramic material according to claim 4, wherein in step (2), in H 2 O 2 The boiling time in the water solution is 1 to 4 hours.
5. The method for preparing a porous silicon carbide ceramic material according to claim 4, wherein: in the step (3), the carbonization process parameters are as follows: under the protective atmosphere, the heating rate is 1-2 ℃/min, the carbonization temperature is 900-1000 ℃, and the heat preservation time is 0.5-1 h.
6. The method for preparing a porous silicon carbide ceramic material according to claim 4, wherein: in the step (4), the silicon melting process parameters are as follows: in a vacuum state, the heating rate is 5-20 ℃/min, the reaction temperature is 1550-1600 ℃, and the heat preservation time is 1-2 h.
7. The method for preparing a porous silicon carbide ceramic material according to claim 4, wherein: in the step (4), the process parameters of high-temperature heating are as follows: in a vacuum state, the heating rate is 5-20 ℃/min, the reaction temperature can be 1750-1850 ℃, the heat preservation time can be 1-2 h, and the process is repeated for 3 times.
8. A method for preparing a phase change heat storage material by using the porous silicon carbide ceramic material prepared by the method of claim 1 is characterized in that the phase change material is filled in pores of the porous silicon carbide ceramic by a vacuum impregnation method to obtain the porous silicon carbide ceramic-based phase change heat storage material.
9. The method for preparing the phase-change heat storage material according to claim 8, comprising the following steps: the parameters of the vacuum impregnation method are as follows: heating to 80-100 ℃ in a vacuum state, and preserving heat for 2-4 h.
10. The method of claim 8, wherein when the porosity of the porous silicon carbide ceramic material is 55 ± 1%, the volume fraction of the phase change material is 55 ± 1%; when the porosity of the porous silicon carbide ceramic material is 80 +/-1%, the volume fraction of the phase-change material accounts for 80 +/-1%.
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