CN112521138B - Diatomite porous body and preparation method thereof - Google Patents
Diatomite porous body and preparation method thereof Download PDFInfo
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- CN112521138B CN112521138B CN201910826074.3A CN201910826074A CN112521138B CN 112521138 B CN112521138 B CN 112521138B CN 201910826074 A CN201910826074 A CN 201910826074A CN 112521138 B CN112521138 B CN 112521138B
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/08—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/665—Local sintering, e.g. laser sintering
Abstract
The invention relates to an ordered cross-scale diatom shell porous body and a preparation method thereof, belonging to the field of bionic materials. The ordered diatom shell porous body has a four-level ordered porous structure, namely ordered millimeter and above scale layered pores, ordered 100 micrometer and above scale layered pores, ordered 10 micrometer and above scale round pores and ordered nanometer round pores. The aperture of the first three scales can be adjusted by software or laser parameters, and the fourth nanoscale hole is the hole of the frustules per se. The invention uses the diatom shell as a single raw material, and the diatom shell powder is sintered layer by layer in a selective area mode by a software-controlled powder paving device and a laser through a free forming method to obtain the porous body. The porous body of the present invention is used for air purification in a severe dust environment.
Description
Technical Field
The invention belongs to the field of new materials, and particularly belongs to the field of bionic materials.
Background
The diatom is aquatic unicellular algae, has various appearances and rich pore structures, takes round algae as an example, the size is about several micrometers to dozens of micrometers, the shell of the diatom is densely covered with pores for exchanging substances with the outside, the shape of the pores is round, the size of the pores is in submicron and nanometer scales, the main component of the shell of the diatom is amorphous silicon dioxide, the diatom belongs to natural biological glass materials, and sunlight penetrates through the glass shell of the diatom to participate in photosynthesis in the diatom shell. After the diatom dies, because the silicon dioxide is stable and is difficult to decompose, after thousands of years of accumulation, abundant and cheap kieselguhr is formed. The diatomite is mainly composed of diatom shells, some diatom shells are complete in shape, and some diatom shells are broken, but rich pore structures are reserved. Due to the high porosity, the diatomite is widely applied to the traditional fields of beverages, chemical engineering, home decoration and the like, and is also made into ceramic membranes, porous ceramics and the like for water treatment, photocatalysis and the like.
The existing diatomite-based porous ceramic material is not full diatomite but added with various organic or inorganic components, and the organic components are mainly added to play the roles of a binder, a pore-forming agent and a dispersing agent. However, the negative effect of adding organic matters is obvious, because the organic matters release toxic gas in the process of removing the glue (burning off the organic matters), and in order not to damage the porous structure in the glue removing process, the temperature rising process is very slow, the temperature rising speed is usually as low as 1 ℃/min, and the energy consumption is increased.
If the diatomite is sintered alone, the melting point is up to 1700 ℃ because the diatomite is silicon dioxide, and the pore structure is collapsed and damaged after high-temperature sintering. In the prior art, inorganic substances are added to form a low-melting-point glass phase, and the low-melting-point glass phase plays a role of a high-temperature binder. However, the presence of the low-melting-point glass phase has a large sintering shrinkage rate, which is not favorable for increasing the porosity, and the presence of the glass phase is also unfavorable for the pore connectivity because closed pores and ink bottle-shaped pores are easily formed.
The cross-scale diatomite-based multilevel porous structure ceramic material prepared in the prior art is mainly realized by compounding diatomite and other porous bodies with different pore sizes, typically zeolite is added, and the like, but the cross-scale porous structure is not realized by the diatomite singly. There are problems with material mixing uniformity and interactions during sintering, such as one porous body pore structure has collapsed at high temperatures and another has not achieved bonding.
The forming process for preparing the diatomite-based porous ceramic in the prior art mainly comprises a die pressing method, a pore-forming agent adding method, a foam impregnation method, a foaming method and the like, and free forming is difficult to realize. The sintering process is a conventional heating sintering process.
Disclosure of Invention
Problems to be solved by the invention
The invention discloses a porous body completely made of diatomite and a free forming preparation method thereof, wherein the diatomite porous body has a four-stage pore structure, specifically, a millimeter and above scale, a 100 micrometer and above scale layered pore, a 10 micrometer and above scale and a nanometer scale pore structure.
Technical scheme of the invention
The raw material used by the invention is the frustules, and the frustules can be obtained by removing organic matters of diatom or by purifying diatomite. The preparation process of the invention is a one-step forming and sintering process, and the process of the invention is a free forming process. The method specifically comprises a powder paving and laser layered sintering process controlled by software, wherein the thickness of a powder paving layer is 80-300 microns, preferably 100-200 microns, the laser is one of a solid laser, a fiber laser and a carbon dioxide laser, and preferably the carbon dioxide laser with the laser wavelength in an infrared region. The four-level pore structure, the pores of millimeter and above, of the invention are realized by selecting the laser area, the layered pores with the width of 100 microns and above are determined by the laser scanning resolution set by software, and the pores with the dimension of 10 microns and above are realized by the diameter of the laser beam and the pores with the dimension of nanometer are realized by the self-aperture of the frustules.
The invention has the advantages of
The only raw material of the invention is the diatom shell which can be designed by software and freely formed at will, and the ordered cross-scale full-diatomite porous body can be used for air purification under severe working conditions such as dust and the like, such as air purifiers, dust masks and other filter core materials.
Drawings
FIG. 1 is a regular and ordered 100-micron and above scale layered pore structure;
FIG. 2 is a regular and ordered circular hole with a size of 10 micrometers or more;
FIG. 3 is a regular ordered nanoscale circular hole.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example 1
The thickness of the diatom shell powder spreading layer is 100 micrometers, the holes in the laser selection area are round holes with the diameter of 10 millimeters through software design, the laser wavelength is 10.6 micrometers, the laser power is 30 watts, the light spot diameter is 10 micrometers, the laser scanning speed is 30cm/s, the resolution ratio is 500DPI, the obtained ordered diatom shell porous body has a four-level ordered porous structure which is respectively a round hole with the regular ordered diameter of 10 millimeters, a layered pore with the regular ordered width of about 80 micrometers, a round hole with the regular ordered width of about 10 micrometers, and a round hole with the regular ordered nanoscale.
Example 2
The thickness of the diatom shell powder spreading layer is 80 micrometers, the holes in the laser selection area are round holes with the diameter of 20 millimeters through software design, the laser wavelength is 10.6 micrometers, the laser power is 30 watts, the diameter of a light spot is 50 micrometers, the laser scanning speed is 40cm/s, the resolution is 500DPI, the obtained ordered diatom shell porous body has a four-level ordered porous structure which is respectively a round hole with the regular ordered diameter of 20 millimeters, a layered pore with the regular ordered width of about 80 micrometers, a round hole with the regular ordered width of about 50 micrometers, and a round hole with the regular ordered nanoscale.
Example 3
The thickness of the diatom shell powder spreading layer is 300 micrometers, the holes in the laser selection area are round holes with the diameter of 50 millimeters through software design, the laser wavelength is 9.2 micrometers, the laser power is 30 watts, the diameter of a light spot is 50 micrometers, the laser scanning speed is 50cm/s, the resolution is 250DPI, the obtained ordered diatom shell porous body has a four-level ordered porous structure which is respectively a round hole with the regular ordered diameter of 50 millimeters, a layered pore with the regular ordered width of about 200 micrometers, a round hole with the regular ordered width of about 50 micrometers, and a round hole with the regular ordered nanoscale.
Example 4
The thickness of the diatom shell powder blanket is 200 micrometers, the holes in the laser selection area are square holes with the side length of 1 mm through software design, the laser wavelength is 10.2 micrometers, the laser power is 50 watts, the diameter of a light spot is 30 micrometers, the laser scanning speed is 10cm/s, the resolution is 300DPI, the obtained ordered diatom shell porous body has a four-level ordered porous structure which is respectively a regular ordered square hole with the side length of 10 mm, a regular ordered layered hole with the width of about 150 micrometers, a regular ordered round hole with the diameter of about 30 micrometers and a regular ordered round hole with the dimension of nanometers.
Claims (6)
1. A preparation method of a diatomite porous body is characterized by comprising the following steps:
step one, preparing frustules: removing organic matters from diatom or purifying diatomite to obtain diatom shells;
step two, selecting and setting a laser: selecting a carbon dioxide laser, wherein the using power is 30-50W, the diameter of a light spot is 10-50 nm, the laser scanning speed is 10-50 cm/s, and the resolution is 250-500 DPI;
step three, controlling automatic area selection, powder paving and laser layered sintering by software: setting the diameter of a hole in a laser selection area to be 1-50 micrometers, spreading powder under software control, setting the thickness of the layer of the diatomite shell powder to be 80-300 micrometers, reserving macropores in the selection area by a carbon dioxide laser, and sintering layer by layer to obtain the diatomite porous body.
2. The method for producing a porous diatomaceous earth body according to claim 1, wherein: in the second step, the laser is a carbon dioxide laser in an infrared region, the laser wavelength is 10.6 microns, the using power is 30 watts, the diameter of a light spot is 10 microns, the laser scanning speed is 30cm/s, and the resolution is 500 DPI; in the third step, the thickness of the layer of the diatom shell powder is set to be 100 micrometers, and the diameter of the hole in the laser selection area is 10 micrometers.
3. The method for producing a porous diatomaceous earth body according to claim 1, wherein: in the second step, the laser is a carbon dioxide laser in an infrared region, the laser wavelength is 10.6 microns, the using power is 30 watts, the diameter of a light spot is 50 microns, the laser scanning speed is 40cm/s, and the resolution is 500 DPI; in the third step, the thickness of the layer of the diatom shell powder is set to be 80 micrometers, and the diameter of a hole in a laser selection area is 20 micrometers.
4. The method for producing a porous diatomaceous earth body according to claim 1, wherein: in the second step, the laser is a carbon dioxide laser in an infrared region, the laser wavelength is 9.2 microns, the using power is 30 watts, the diameter of a light spot is 50 microns, the laser scanning speed is 50cm/s, and the resolution is 250 DPI; in the third step, the thickness of the layer of the diatom shell powder is set to be 300 micrometers, and the diameter of the hole in the laser selection area is 50 micrometers.
5. The method for producing a porous diatomaceous earth body according to claim 1, wherein: in the second step, the laser is a carbon dioxide laser in an infrared region, the laser wavelength is 10.2 microns, the using power is 50 watts, the diameter of a light spot is 30 microns, the laser scanning speed is 10cm/s, and the resolution is 300 DPI; in the third step, the thickness of the layer of the diatom shell powder is set to be 200 micrometers, and the diameter of the hole in the laser selection area is 1 micrometer.
6. A porous diatomaceous earth prepared by the method according to any one of claims 1 to 5, wherein: the porous body has a pore structure including four-stage pores, specifically, millimeter-scale pores, layered micron-scale pores of 100 microns or more, micron-scale pores of 10 microns or more, and nanometer-scale pores.
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| CN102826556A (en) * | 2012-09-21 | 2012-12-19 | 海南大学 | Method for separating and extracting diatom shells from diatom |
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