CN116813357B - Carbon dioxide atmosphere sintering molding method for simulating Mars soil - Google Patents

Carbon dioxide atmosphere sintering molding method for simulating Mars soil Download PDF

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CN116813357B
CN116813357B CN202310773909.XA CN202310773909A CN116813357B CN 116813357 B CN116813357 B CN 116813357B CN 202310773909 A CN202310773909 A CN 202310773909A CN 116813357 B CN116813357 B CN 116813357B
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simulated
soil
carbon dioxide
sintering
furnace
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CN116813357A (en
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刘琛
李勇
闫继宏
吴宜勇
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

A carbon dioxide atmosphere sintering molding method for simulating Mars soil relates to a sintering molding method for simulating Mars soil. The invention aims to solve the problem that the simulated Mars soil block material prepared by the existing method has poor mechanical properties. The method comprises the following steps: compacting the simulated spark soil into a cylindrical green body by adopting certain pressure and dwell time to obtain a simulated spark soil green body; 2. sintering the simulated marl soil green body in the carbon dioxide gas atmosphere to obtain the simulated marl soil block material. The compressive strength of the simulated marl soil block material prepared by the method is 129MPa, the maximum hardness reaches 10GPa, and compared with 51MPa of air atmosphere sintering reported in the literature, the performance is improved by 152 percent, so that the mechanical performance of the simulated marl soil sintered body can be greatly improved by adopting the method.

Description

Carbon dioxide atmosphere sintering molding method for simulating Mars soil
Technical Field
The invention relates to a sintering molding method for simulating Mars soil.
Background
Deep space exploration is one of the hot spot development directions of future aerospace activities of human beings. Future deep space exploration activities will be larger in scale and longer in period. In view of the high space transportation cost, how to fully utilize rich energy and mineral resources on the extraterrestrial, get rid of dependence on earth resources and transportation modes, and become a key technology for establishing and operating middle-long tasks such as an extraterrestrial base, and the like, and also are a basis for continuously and expandably developing residence and scientific research of the extraterrestrial celestial body. NASA in the united states first proposed the concept of space resource in situ utilization and its implementation approach, and developed this project as a priority technique. The space in-situ resource utilization technology refers to the technology of manufacturing water, oxygen, propellant, house and other necessities for constructing an extraterrestrial base by surveying, acquiring and utilizing natural resources of an extraterrestrial celestial body, such as the atmosphere, the soil and the like, so that the space self-sufficiency capability is enhanced, and the dependence on earth supply is reduced. Space in-situ manufacturing technology is a research hotspot in China and internationally at the present stage, and is also the field with the strongest current demand. Space in-situ fabrication techniques have significant technical and cost advantages over the manner in which they are sent to space after fabrication is completed on the ground.
Mars soil is used as a natural radiation-proof material, and is expected to provide a relatively safe environment for future human survival in Mars. However, the reported martin sintering studies mostly use protective atmosphere or air atmosphere sintering. However, mars atmosphere is mainly composed of carbon dioxide (95.3%), nitrogen (2.7%) and small amounts of other gases, with atmospheric pressure between 100 and 1500 Pa. The sintering atmosphere can greatly influence the type of solid phase reaction and physical and chemical changes possibly occurring in the high-temperature forming process, and particularly the chemical composition of the marten is extremely complex. Chow B J, chen T, methong Y, et al direct formation of structural components using a martian soil simulant scientific Reports,2017,7,1151, discloses: the bending strength of the simulated Mars soil block material prepared by adopting a dry pressing method is 50MPa; d Karl, F Kamutzki, A Zocca, et al Towards the colonization of Mars by in-situ resource utilization: slip cast ceramics frommartian soil simulan. PLoS ONE,2018,13 (10), e0204025 discloses that: the compressive strength of the simulated Mars soil block material sintered in the air atmosphere at 1130 ℃ is 51MPa; n Shiwei, dritsas S, fernandez J G.Marian biolith A bioinspired regolith composite for closed-loop extraterrestrial manufacturing. PLoS ONE,2020,15 (9), e0238606, discloses: adopting biological adhesive to form and simulate Mars soil, wherein the strength of the block material is 3.5MPa; from this, it can be seen that: the simulated Mars soil block material prepared by the existing method has the problem of poor mechanical properties.
Disclosure of Invention
The invention aims to solve the problem that the simulated Mars soil block material prepared by the existing method has poor mechanical properties, and provides a carbon dioxide atmosphere sintering molding method for the simulated Mars soil.
The carbon dioxide atmosphere sintering molding method for simulating the mars is specifically implemented according to the following steps:
1. compacting the simulated spark soil into a cylindrical green body by adopting certain pressure and dwell time to obtain a simulated spark soil green body;
2. placing the simulated marl green body in a tubular sintering furnace, continuously introducing carbon dioxide gas into the tubular sintering furnace, heating the tubular furnace to 1100-1200 ℃ at a certain heating rate, preserving heat for a certain time under the conditions of carbon dioxide gas atmosphere and 1100-1200 ℃, and finally cooling to room temperature along with the furnace to obtain the simulated marl block material.
The invention has the advantages that:
1. the invention sinters the simulated mars soil in the carbon dioxide atmosphere to obtain the simulated mars soil block material with good mechanical property;
2. the compressive strength of the simulated marl soil block material prepared by the method is 129MPa, the maximum hardness reaches 10GPa, and compared with 51MPa of air atmosphere sintering reported in the literature, the performance is improved by 152 percent, so that the mechanical performance of the simulated marl soil sintered body can be greatly improved by adopting the method.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention;
FIG. 2 is a macroscopic photograph and SEM image of simulated Mary soil as described in example 1, step one, wherein (a) is the macroscopic photograph and (b) is the SEM image;
FIG. 3 is a plot of the particle size distribution of the simulated spark-clay soil as described in example 1, step one;
FIG. 4 is a graph showing the comparison of simulated and actual soil components of the first step of example 1;
FIG. 5 is an SEM image of a simulated Mars loam material obtained in step two of example 1;
FIG. 6 is an XRD pattern of the simulated Mars loam material obtained in step two of example 1;
FIG. 7 is a compressive stress strain curve of the simulated Mars soil bulk material obtained in step two of example 1;
FIG. 8 shows the thermal expansion coefficients of the simulated Mars soil bulk material obtained in step two of example 1 in the temperature range of room temperature to 200deg.C.
Detailed Description
The first embodiment is as follows: the carbon dioxide atmosphere sintering molding method for simulating the Mars soil is specifically completed by the following steps:
1. compacting the simulated spark soil into a cylindrical green body by adopting certain pressure and dwell time to obtain a simulated spark soil green body;
2. placing the simulated marl green body in a tubular sintering furnace, continuously introducing carbon dioxide gas into the tubular sintering furnace, heating the tubular furnace to 1100-1200 ℃ at a certain heating rate, preserving heat for a certain time under the conditions of carbon dioxide gas atmosphere and 1100-1200 ℃, and finally cooling to room temperature along with the furnace to obtain the simulated marl block material.
The simulated mars soil described in step one of this embodiment is purchased from the institute of geochemistry, academy of sciences of china, model number: JMSS-1.
The second embodiment is as follows: the present embodiment differs from the specific embodiment in that: the particle size of the simulated mars soil in the first step is 1-100 mu m. The other steps are the same as in the first embodiment.
And a third specific embodiment: this embodiment differs from the first or second embodiment in that: the pressure in the first step is 8 MPa-15 MPa; the dwell time in the first step is 1 min-5 min. The other steps are the same as those of the first or second embodiment.
The specific embodiment IV is as follows: one difference between this embodiment and the first to third embodiments is that: in the first step, the pressure is maintained for 3min under the pressure of 12MPa, and the simulated Mars soil with the median particle size of 10 mu m is pressed into a cylindrical green body with the diameter of phi 20mm multiplied by 6.5 mm. The other steps are the same as those of the first to third embodiments.
Fifth embodiment: one to four differences between the present embodiment and the specific embodiment are: in the first step, the pressure is maintained for 1min under the pressure of 10MPa, and simulated Mars soil with the median particle size of 50 mu m is pressed into a cylindrical green body with the diameter of phi 10mm multiplied by 10 mm. Other steps are the same as those of the first to fourth embodiments.
Specific embodiment six: the present embodiment differs from the first to fifth embodiments in that: in the first step, the simulated Mars soil with the median particle diameter of 30 mu m is pressed into a cylindrical green body with the diameter of phi 25mm multiplied by 10mm under the pressure of 8MPa for 1 min. Other steps are the same as those of the first to fifth embodiments.
Seventh embodiment: one difference between the present embodiment and the first to sixth embodiments is that: the temperature rising rate in the second step is 3 ℃/min-5 ℃/min; and step two, the heat preservation time is 20-60 min. Other steps are the same as those of embodiments one to six.
Eighth embodiment: one difference between the present embodiment and the first to seventh embodiments is that: placing the simulated mars soil green body in a tubular sintering furnace, continuously introducing carbon dioxide gas into the tubular sintering furnace, heating the tubular furnace to 1100 ℃ at a heating rate of 5 ℃/min, preserving heat for 30min under the conditions of carbon dioxide gas atmosphere and 1100 ℃, and finally cooling to room temperature along with the furnace to obtain the simulated mars soil block material with the density of 83%. The other steps are the same as those of embodiments one to seven.
Detailed description nine: one of the differences between this embodiment and the first to eighth embodiments is: placing the simulated mars soil green body in a tubular sintering furnace, continuously introducing carbon dioxide gas into the tubular sintering furnace, heating the tubular furnace to 1130 ℃ at a heating rate of 3 ℃/min, preserving heat for 60min under the conditions of carbon dioxide gas atmosphere and 1130 ℃, and finally cooling to room temperature along with the furnace to obtain the simulated mars soil block material with 86% compactness. Other steps are the same as those of embodiments one to eight.
Detailed description ten: the present embodiment differs from the first to ninth embodiments in that: placing the simulated mars soil green body in a tubular sintering furnace, continuously introducing carbon dioxide gas into the tubular sintering furnace, heating the tubular furnace to 1200 ℃ at a heating rate of 1 ℃/min, preserving heat for 20min under the conditions of carbon dioxide gas atmosphere and 1200 ℃, and finally cooling to room temperature along with the furnace to obtain the simulated mars soil block material with the density of 80%. The other steps are the same as those of embodiments one to nine.
The following examples are used to verify the benefits of the present invention:
example 1: the carbon dioxide atmosphere sintering molding method for simulating the mars is specifically implemented according to the following steps:
1. pressing the simulated Mars soil with the median particle size of 12 mu m into a cylindrical green body with the diameter of phi 20mm multiplied by 10mm under the pressure of 15MPa for 5min to obtain a simulated Mars soil green body;
the simulated Mars soil described in the first step is purchased from the institute of geochemistry of the national academy of sciences, and has the model number: JMSS-1;
2. and (3) placing the simulated mar soil green body in a tubular sintering furnace, continuously introducing carbon dioxide gas into the tubular sintering furnace, heating the tubular furnace to 1130 ℃ at a heating rate of 5 ℃/min, preserving heat for 30min, and finally cooling to room temperature along with the furnace to obtain the simulated mar soil block material.
The microscopic morphology of the simulated marl soil described in step one of example 1 was analyzed by SEM as shown in fig. 2;
FIG. 2 is a macroscopic photograph and SEM image of simulated Mary soil as described in example 1, step one, wherein (a) is the macroscopic photograph and (b) is the SEM image;
as can be seen from fig. 2, the simulated mars soil exhibits irregular prisms or sub-prisms.
FIG. 3 is a plot of the particle size distribution of the simulated spark-clay soil as described in example 1, step one;
as can be seen from FIG. 3, the median particle diameter D50 of the simulated Mars soil was 12 μm, and the particle fractions of less than 100 μm were 98.86%, respectively.
FIG. 4 is a graph showing the comparison of simulated and actual soil components of the first step of example 1;
as can be seen from fig. 4: the main chemical component of the simulated mars soil is SiO 2 、FeO T 、Al 2 O 3 、MgO、TiO 2 、CaO、Na 2 O, etc., similar to real Mars soil in situ detection data, wherein Al 2 O 3 The content of MgO and CaO is lower than that of the true mars soil.
After sintering under the carbon dioxide atmosphere, the density of the simulated Mars soil block material obtained in the step two of the example 1 reaches 86%, and an SEM (scanning electron microscope) graph is shown in figure 5;
FIG. 5 is an SEM image of a simulated Mars loam material obtained in step two of example 1;
as can be seen from fig. 5: the internal pores of the simulated mars soil block material obtained in the step II of the example 1 are uniformly distributed, and the microstructure is formed by wrapping mineral grains with a silica glass phase.
FIG. 6 is an XRD pattern of the simulated Mars loam material obtained in step two of example 1;
as can be seen from fig. 6: the simulated Mars loam material obtained in example 1 step two had feldspar ((Ca) as the main component 0.78 Na 0.22 )(Al 1.78 Si 0.22 )Si 2 O 8 )、Fe 2 O 3 、TiO 2 、(Fe,Mg)SiO 4 MgO, etc.; (Fe, mg) SiO after sintering 4 The content of phases increases significantly, due to the chemical reaction of iron oxide, magnesium oxide and silicon dioxide, resulting in (Fe, mg) SiO 4 And (3) a mixture.
FIG. 7 is a compressive stress strain curve of the simulated Mars soil bulk material obtained in step two of example 1;
as can be seen from fig. 7: the average compressive strength of the simulated Mars soil block material obtained in the step II of the embodiment 1 can reach 129MPa, and compared with 51MPa of air atmosphere sintering reported in the literature, the performance is improved by 152 percent.
FIG. 8 shows the thermal expansion coefficients of the simulated Mars soil bulk material obtained in step two of example 1 in the temperature range of room temperature to 200deg.C;
as can be seen from fig. 8: the simulated Mars soil bulk material obtained in example 1 step II has a thermal expansion coefficient of (4.83-5.35) x 10 in the temperature range of room temperature to 200 DEG C -6-1
Table 1 shows the thermal conductivities of the simulated Mars soil bulk materials obtained in step two of example 1 at-80 ℃, -60 ℃ and 20 ℃;
TABLE 1
Temperature/. Degree.C Thermal conductivity (W/(m.K))
-80 0.98
-60 1.03
20 1.16

Claims (10)

1. The carbon dioxide atmosphere sintering molding method for simulating the mars is characterized by comprising the following steps of:
1. compacting the simulated spark soil into a cylindrical green body by adopting certain pressure and dwell time to obtain a simulated spark soil green body;
2. placing the simulated marl green body in a tubular sintering furnace, continuously introducing carbon dioxide gas into the tubular sintering furnace, heating the tubular furnace to 1100-1200 ℃ at a certain heating rate, preserving heat for a certain time under the conditions of carbon dioxide gas atmosphere and 1100-1200 ℃, and finally cooling to room temperature along with the furnace to obtain the simulated marl block material.
2. The method for sintering and forming the simulated marl under the carbon dioxide atmosphere according to claim 1, wherein the particle size of the simulated marl in the step one is 1-100 μm.
3. The method for sintering and forming the carbon dioxide atmosphere simulating the mars soil according to claim 1, wherein the pressure in the first step is 8-15 MPa; the dwell time in the first step is 1 min-5 min.
4. The method for sintering and forming the simulated marl under the carbon dioxide atmosphere according to claim 1, wherein in the first step, the simulated marl with the median particle size of 10 μm is pressed into a cylindrical green body with the diameter of phi 20mm multiplied by 6.5mm under the pressure of 12MPa for 3 min.
5. The method for sintering and forming the simulated marl under the carbon dioxide atmosphere according to claim 1, wherein in the first step, the simulated marl with the median particle size of 50 μm is pressed into a cylindrical green body with the diameter of phi 10mm multiplied by 10mm under the pressure of 10MPa for 1 min.
6. The method for sintering and forming the simulated marl under the carbon dioxide atmosphere according to claim 1, wherein in the first step, the simulated marl with the median particle size of 30 μm is pressed into a cylindrical green body with the diameter of phi 25mm multiplied by 10mm under the pressure of 8MPa for 1 min.
7. The method for sintering and forming the carbon dioxide atmosphere simulating the mars soil according to claim 1, wherein the heating rate in the second step is 3 ℃/min-5 ℃/min; and step two, the heat preservation time is 20-60 min.
8. The method for sintering and forming the simulated mar soil in the carbon dioxide atmosphere is characterized by comprising the steps of placing a simulated mar soil blank in a tubular sintering furnace, continuously introducing carbon dioxide gas into the tubular sintering furnace, heating the tubular furnace to 1100 ℃ at a heating rate of 5 ℃/min, preserving heat for 30min under the conditions of carbon dioxide gas atmosphere and 1100 ℃, and finally cooling to room temperature along with the furnace to obtain the simulated mar soil block material with the compactness of 83%.
9. The method for sintering and forming the simulated mar soil in the carbon dioxide atmosphere is characterized by comprising the steps of placing a simulated mar soil blank in a tubular sintering furnace, continuously introducing carbon dioxide gas into the tubular sintering furnace, heating the tubular furnace to 1130 ℃ at a heating rate of 3 ℃/min, preserving heat for 60min under the conditions of carbon dioxide gas atmosphere and 1130 ℃, and finally cooling to room temperature along with the furnace to obtain the simulated mar soil block material with 86% compactness.
10. The method for sintering and forming the simulated mar soil in the carbon dioxide atmosphere is characterized by comprising the steps of placing a simulated mar soil blank in a tubular sintering furnace, continuously introducing carbon dioxide gas into the tubular sintering furnace, heating the tubular furnace to 1200 ℃ at a heating rate of 1 ℃/min, preserving heat for 20min under the conditions of carbon dioxide gas atmosphere and 1200 ℃, and finally cooling to room temperature along with the furnace to obtain the simulated mar soil block material with the compactness of 80%.
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