CN111004026A - Preparation method of forsterite-based foamed ceramic spherical shell for civil air defense engineering - Google Patents
Preparation method of forsterite-based foamed ceramic spherical shell for civil air defense engineering Download PDFInfo
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Abstract
The invention relates to a preparation method of a forsterite-based foamed ceramic spherical shell for civil air defense engineering. The technical scheme is as follows: taking 67-85 wt% of forsterite powder, 5-10 wt% of sericite powder and 3-13 wt% of silicon micropowder as raw materials, adding 10-15 wt% of a bonding agent, 10-30 wt% of water and 8-15 wt% of a pore-forming agent, and uniformly mixing to obtain a pug; filling the pug into a hemispherical shell mold with the outer diameter of 6-10 cm and the inner diameter of 3-5 cm, pressing under 5-10 Mpa to prepare a hemispherical shell green body, butting the side openings of the hemispherical shells under the same pressure to combine into a hollow sphere, and demolding. Curing at 25 ℃ for 2-5 h, drying at 60-110 ℃ for 6-12 h, placing in an air atmosphere, heating to 800-1000 ℃ at a speed of 1-10 ℃/min, and preserving heat for 1-2 h, sintering and sealing to obtain the forsterite-based foamed ceramic spherical shell. The forsterite-based foamed ceramic spherical shell prepared by the method has the advantages of uniform wall thickness, high strength, controllable density, wall thickness and sphere size, and low cost and easy obtainment of raw materials, low sintering temperature and high production efficiency, and can realize automatic production.
Description
Technical Field
The invention belongs to the technical field of foam ceramic spherical shells. In particular to a preparation method of a forsterite-based foamed ceramic spherical shell for civil air defense engineering.
Background
The foamed ceramic spherical shell has the double characteristics of high-efficiency clipping energy absorption of porous materials and high structural strength of the shell, not only has strong attenuation effect on explosion waves, but also has the capability of withstanding multiple times of strikes, and because the cavity therein has diffraction and isolation effects on stress waves, the dispersion and attenuation effects of the materials on the waves are enhanced under the condition of keeping the strength, so that the foamed ceramic spherical shell has wide application space in the fields of impact dynamics, civil air defense engineering and the like.
Cao Yan et Al (Zengyan, Sangyuan Hualin, et Al. preparation of millimeter-level translucent Al by template method2O3Hollow ball [ J]The silicate science report, 2013(12): 1644-1649.) adopts a centrifugal pressurization physical coating method to prepare a polystyrene-alumina composite spherical shell, then the temperature is kept at 1300 ℃ for 2h to obtain an alumina hollow spherical shell, and finally the alumina hollow spherical shell is sintered at 1800 ℃ under a vacuum condition to obtain the semitransparent alumina hollow sphere. The technology has high sintering temperature, complex process and high cost; the spherical shell prepared by the technology has high density, and the thickness of the spherical shell is difficult to control.
The Chinese patent of invention-a ceramic hollow buoyancy ball and its manufacturing method, 201710399976.4, discloses the following technology: firstly, manufacturing a semi-spherical shell biscuit, sintering for the first time to obtain a semi-spherical shell, then precisely processing the side openings of the semi-spherical shell to ensure that the two semi-spherical shell side openings can be completely jointed when being close to each other, then carrying out hot isostatic pressing treatment on the semi-spherical shell after the precise processing, and grinding and polishing the semi-spherical shell side openings after the hot isostatic pressing treatment; and finally, butting and combining the side openings of the two hemispherical shells into a complete hollow sphere, and sintering for the second time to obtain the complete hollow sphere. The preparation method of the semi-spherical shell biscuit in the technology is 3D printing, and a product formed by the method is rough in surface, long in forming period and high in equipment cost. The technology needs two times of sintering treatment, and the sintered hollow ball also needs subsequent treatment to eliminate the stress at the sealing position.
The parameter indexes corresponding to the national standard (GB/T3994-2013) of the clay heat-insulating refractory brick which is also the foamed ceramic material show that when the volume density of the material is 0.8 g/cm3In the process, the static strength at normal temperature is 2.5MPa, and the low density and the high strength of the foamed ceramic material are in contradiction, so that the technical requirements of the civil air defense engineering on the low density and the high strength of the foamed ceramic spherical shell cannot be met.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a forsterite-based foamed ceramic spherical shell for civil air defense engineering.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
a preparation method of a forsterite-based foamed ceramic spherical shell for civil air defense engineering comprises the following steps:
step one, taking 67-85 wt% of forsterite powder, 5-10 wt% of sericite powder and 3-13 wt% of silicon micropowder as raw materials, adding 10-15 wt% of a bonding agent, 10-30 wt% of water and 8-15 wt% of a pore-forming agent, and uniformly mixing to obtain a pug;
and step two, filling the pug into a hemispherical shell mold with the outer diameter of 6-10 cm and the inner diameter of 3-5 cm, pressing the mixture into a hemispherical shell green body under the pressure of 5-10 Mpa, butting and combining the side openings of the hemispherical shells into a hollow sphere under the same pressure, and demolding. Curing at 25 ℃ for 2-5 h, and drying at 60-110 ℃ for 6-12 h to obtain a forsterite-based foamed ceramic spherical shell blank;
and step three, placing the forsterite-based foamed ceramic spherical shell blank in an air atmosphere, heating to 800-1000 ℃ at the speed of 1-10 ℃/min, preserving heat for 1-2 hours, and cooling to room temperature to obtain the forsterite-based foamed ceramic spherical shell.
The particle size of the forsterite is 10-90 mu m.
The particle size of the sericite powder is 10-90 mu m.
The particle size of the silicon micro powder is 10-90 mu m.
The pore-forming agent is at least one of starch, carbon powder and plastic microspheres
The binder is at least one of water glass, calcium aluminate cement and polyvinyl alcohol.
The molding mode is compression molding, and the molding pressure is 5-10 MPa.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages:
the invention relates to a preparation method of a forsterite-based foamed ceramic spherical shell for civil air defense engineering, which uses natural mineral powder as a main raw material, and has the advantages of cheap and easily-obtained raw materials, low cost and excellent normal-temperature mechanical property; the invention adopts a compression molding process, has simple operation, can realize automatic production and high production efficiency, and can further control the sphere size and the wall thickness of the forsterite-based foamed ceramic spherical shell by controlling the cavity of the mold. According to the invention, the forsterite-based foamed ceramic spherical shell is prepared by adopting a pore-forming agent adding method, and the porosity, density and pore size of the forsterite-based foamed ceramic spherical shell and the corresponding normal-temperature mechanical property thereof can be controlled by controlling the addition amount of the pore-forming agent and the particle size of the pore-forming agent.
Therefore, the method has the characteristics of simple process, low sintering temperature, low cost, high production efficiency, easy product forming and easy process control, and the forsterite-based foamed ceramic spherical shell prepared by the method has high strength and controllable sphere size, spherical shell wall thickness, porosity, density, pore size and normal-temperature mechanical properties.
Drawings
FIG. 1 is a green forsterite-based ceramic foam hemispherical shell for civil air defense engineering prepared by the present invention;
FIG. 2 is a diagram of a forsterite-based ceramic foam spherical shell for civil air defense engineering prepared by the present invention.
Detailed Description
The invention is further described with reference to specific embodiments, without limiting its scope. The starting materials and reagents required in the embodiments are commercially available.
In order to avoid repetition, the raw materials of the present specific embodiment are described as follows, and are not described in the embodiments again:
the particle size of the forsterite is 10-90 mu m.
The particle size of the sericite powder is 10-90 mu m.
The particle size of the silicon micro powder is 10-90 mu m.
The pore-forming agent is at least one of starch, carbon powder and plastic microspheres
The binder is at least one of water glass, calcium aluminate cement and polyvinyl alcohol.
Example 1
Step one, taking 67-75 wt% of forsterite powder, 8-15 wt% of sericite powder and 8-13 wt% of silicon micropowder as raw materials, adding 10-15 wt% of a bonding agent, 10-15 wt% of water and 8-15 wt% of a pore-forming agent, and uniformly mixing to obtain a pug;
filling the pug into a hemispherical shell mold with the outer diameter of 6-10 cm and the inner diameter of 3-5 cm, pressing under 5-7 Mpa to prepare a hemispherical shell green body 1, wherein the middle part of the hemispherical shell green body 1 is a hollow hemisphere 3, and the cross section of the hemispherical shell green body 1 is of an annular structure 2;
and (3) combining the side openings of the hemispherical shells into a hollow sphere 4 under the same pressure, and demolding. Curing at 25 ℃ for 2-3 h, and drying at 60-80 ℃ for 6-12 h to obtain a forsterite-based foamed ceramic spherical shell blank;
and step three, placing the forsterite-based foamed ceramic spherical shell blank in an air atmosphere, heating to 800-900 ℃ at the speed of 1-3 ℃/min, preserving heat for 1-2 hours, and cooling to room temperature to obtain the forsterite-based foamed ceramic spherical shell.
The pore-forming agent is starch; the binding agent is water glass. The volume density of the obtained forsterite-based foamed ceramic spherical shell matrix material is 1.0-1.5 g/cm3And the normal-temperature compressive strength is 8-12 MPa.
Example 2
A forsterite-based foamed ceramic spherical shell for civil air defense engineering and a preparation method thereof. In this example, the procedure is the same as in example 1 except for step three:
and step three, placing the forsterite-based foamed ceramic spherical shell blank in an air atmosphere, heating to 900-1000 ℃ at the speed of 1-3 ℃/min, preserving heat for 1-2 hours, and cooling to room temperature to obtain the forsterite-based foamed ceramic spherical shell.
The pore-forming agent is starch; the binding agent is water glass. The volume density of the obtained forsterite-based foamed ceramic spherical shell matrix material is 1.2-1.7 g/cm3And the normal-temperature compressive strength is 10-15 MPa.
Example 3
Step one, taking 75-80 wt% of forsterite powder, 8-15 wt% of sericite powder and 5-8 wt% of silicon micropowder as raw materials, adding 10-15 wt% of a bonding agent, 15-20 wt% of water and 8-15 wt% of a pore-forming agent, and uniformly mixing to obtain a pug;
and step two, filling the pug into a hemispherical shell mold with the outer diameter of 6-10 cm and the inner diameter of 3-5 cm, pressing under 7-8 Mpa to prepare a hemispherical shell green body, butting and combining the side openings of the hemispherical shells into a hollow sphere under the same pressure, and demolding. Curing at 25 ℃ for 3-4 h, and drying at 80-100 ℃ for 6-12 h to obtain a forsterite-based foamed ceramic spherical shell blank;
and step three, placing the forsterite-based foamed ceramic spherical shell blank in an air atmosphere, heating to 800-900 ℃ at the speed of 3-7 ℃/min, preserving heat for 1-2 hours, and cooling to room temperature to obtain the forsterite-based foamed ceramic spherical shell.
The pore-forming agent is carbon powder; the binder is calcium aluminate cement. The volume density of the obtained forsterite-based foamed ceramic spherical shell matrix material is 1.2-1.5 g/cm3And the normal-temperature compressive strength is 10-12 MPa.
Example 4
A forsterite-based foamed ceramic spherical shell for civil air defense engineering and a preparation method thereof. This example is the same as example 3 except for the third step:
and step three, placing the forsterite-based foamed ceramic spherical shell blank in an air atmosphere, heating to 900-1000 ℃ at the speed of 3-7 ℃/min, preserving heat for 1-2 hours, and cooling to room temperature to obtain the forsterite-based foamed ceramic spherical shell.
The pore-forming agent is carbon powder; the binder is calcium aluminate cement. The obtained forsterite-based foamed ceramic spherical shellThe bulk density of the matrix material is 1.5-1.9 g/cm3And the normal-temperature compressive strength is 12-20 MPa.
Example 5
Step one, taking 80-85 wt% of forsterite powder, 5-8 wt% of sericite powder and 3-5 wt% of silicon micropowder as raw materials, adding 10-15 wt% of a bonding agent, 20-30 wt% of water and 8-15 wt% of a pore-forming agent, and uniformly mixing to obtain a pug;
and step two, filling the pug into a hemispherical shell mold with the outer diameter of 6-10 cm and the inner diameter of 3-5 cm, pressing under 8-10 Mpa to prepare a hemispherical shell green body, butting and combining the side openings of the hemispherical shells into a hollow sphere under the same pressure, and demolding. Curing at 25 ℃ for 4-5 h, and drying at 100-1110 ℃ for 6-12 h to obtain a forsterite-based foamed ceramic spherical shell blank;
and step three, placing the forsterite-based foamed ceramic spherical shell blank in an air atmosphere, heating to 800-900 ℃ at the speed of 7-10 ℃/min, preserving heat for 1-2 hours, and cooling to room temperature to obtain the forsterite-based foamed ceramic spherical shell.
The pore-forming agent is plastic microspheres; the binder is polyvinyl alcohol. The volume density of the obtained forsterite-based foamed ceramic spherical shell matrix material is 0.6-1.2 g/cm3And the normal-temperature compressive strength is 5-8 MPa.
Example 6
A forsterite-based foamed ceramic spherical shell for civil air defense engineering and a preparation method thereof. This example is the same as example 5 except for step three:
and step three, placing the forsterite-based foamed ceramic spherical shell blank in an air atmosphere, heating to 900-1000 ℃ at the speed of 7-10 ℃/min, preserving heat for 1-2 hours, and cooling to room temperature to obtain the forsterite-based foamed ceramic spherical shell.
The pore-forming agent is plastic microspheres; the binder is polyvinyl alcohol. The volume density of the obtained forsterite-based foamed ceramic spherical shell matrix material is 0.8-1.2 g/cm3And the normal-temperature compressive strength is 8-12 MPa.
Compared with the prior art, the specific implementation mode has the following positive effects:
the main raw materials used by the invention are natural minerals such as forsterite powder, sericite powder, silicon micropowder and the like, and the raw materials are cheap and easy to obtain, low in cost and excellent in normal-temperature mechanical property. Adding a bonding agent, water and a certain amount of pore-forming agent into the raw materials, and uniformly mixing to obtain the pug. Pressing the pug into a semi-spherical shell green body, then butting and combining the side openings of the semi-spherical shells into a hollow sphere under the same pressure, and demoulding. And firing the forsterite-based foamed ceramic spherical shell blank at 800-1000 ℃ to obtain the forsterite-based foamed ceramic spherical shell. The invention adopts a compression molding process, has simple operation, can realize automatic production and high production efficiency, and can further control the sphere size and the wall thickness of the forsterite-based foamed ceramic spherical shell by controlling the cavity of the mold. According to the invention, the forsterite-based foamed ceramic spherical shell is prepared by adopting a pore-forming agent adding method, and the porosity, density and pore size of the forsterite-based foamed ceramic spherical shell and the corresponding normal-temperature mechanical property thereof can be controlled by controlling the addition amount of the pore-forming agent and the particle size of the pore-forming agent.
Therefore, the invention has the characteristics of simple process, low sintering temperature, low cost, high production efficiency, easy product forming and easy process control. The forsterite-based foamed ceramic ball shell prepared by the method has uniform wall thickness, high strength, and controllable density, wall thickness and ball size.
Claims (8)
1. A forsterite-based foamed ceramic spherical shell for civil air defense engineering is characterized in that the preparation method comprises the following steps:
step one, taking 67-85 wt% of forsterite powder, 5-10 wt% of sericite powder and 3-13 wt% of silicon micropowder as raw materials, adding 10-15 wt% of a bonding agent, 10-30 wt% of water and 8-15 wt% of a pore-forming agent, and uniformly mixing to obtain a pug;
filling the pug into a hemispherical shell mold with the outer diameter of 6-10 cm and the inner diameter of 3-5 cm, pressing under 5-10 Mpa to prepare a hemispherical shell green body 1, wherein the middle part of the hemispherical shell green body 1 is a hollow hemisphere 3, and the cross section of the hemispherical shell green body 1 is of an annular structure 2;
the side openings of the hemispherical shells are butted and combined into a hollow sphere 4 under the same pressure, and demoulding is carried out; curing at 25 ℃ for 2-5 h, and drying at 60-110 ℃ for 6-12 h to obtain a forsterite-based foamed ceramic spherical shell blank;
placing the forsterite-based foamed ceramic spherical shell blank in an air atmosphere, heating to 800-1000 ℃ at the speed of 1-10 ℃/min, preserving heat for 1-2 hours, and cooling to room temperature to obtain a forsterite-based foamed ceramic spherical shell;
the pore-forming agent is starch; the binding agent is water glass, and the volume density of the obtained forsterite-based foamed ceramic spherical shell base material is 1.0-1.5 g/cm3And the normal-temperature compressive strength is 8-12 MPa.
2. The method for preparing the forsterite-based ceramic foam ball shell for civil air defense engineering as claimed in claim 1, wherein: the particle size of the forsterite is 10-90 mu m.
3. The method for preparing the forsterite-based ceramic foam ball shell for civil air defense engineering as claimed in claim 1, wherein: the particle size of the sericite powder is 10-90 mu m.
4. The method for preparing the forsterite-based ceramic foam ball shell for civil air defense engineering as claimed in claim 1, wherein: the particle size of the silicon micro powder is 10-90 mu m.
5. The method for preparing the forsterite-based ceramic foam ball shell for civil air defense engineering as claimed in claim 1, wherein: the pore-forming agent is at least one of starch, carbon powder and plastic microspheres.
6. The method for preparing the forsterite-based ceramic foam ball shell for civil air defense engineering as claimed in claim 1, wherein: the binder is at least one of water glass, calcium aluminate cement and polyvinyl alcohol.
7. The method for preparing the forsterite-based ceramic foam ball shell for civil air defense engineering as claimed in claim 1, wherein: the molding mode is compression molding, and the molding pressure is 5-10 MPa.
8. A forsterite-based foamed ceramic spherical shell for civil air defense engineering is characterized in that: the forsterite-based foamed ceramic spherical shell for civil air defense engineering is prepared by the preparation method of the forsterite-based foamed ceramic spherical shell for civil air defense engineering according to any one of claims 1 to 7.
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