CN114507079B - Mullite fiber reinforced metal-based composite ceramic sheet and preparation method thereof - Google Patents
Mullite fiber reinforced metal-based composite ceramic sheet and preparation method thereof Download PDFInfo
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Abstract
The invention provides a mullite fiber reinforced metal matrix composite ceramic sheet and a preparation method thereof, wherein calcined alumina, magnesia soil, nanoscale fused quartz, monazite, bentonite, pyrophyllite, black talc, potash feldspar, aluminum powder and sodium tripolyphosphate are mixed and then subjected to ball milling treatment to obtain mixed powder, and the mixed powder is subjected to pulping and spray granulation to obtain blank powder; and pressing and molding the blank powder into a ceramic plate-shaped green body, sintering the ceramic plate-shaped green body to obtain a ceramic sheet blank, and glazing, surface grinding and polishing the ceramic sheet blank to obtain the mullite fiber reinforced metal matrix composite ceramic sheet. The invention has simple preparation process and low raw material cost, and can be applied to the commercial fields of architectural decoration ceramics, protective materials and the like. By optimizing a solid-phase reaction sintering system and regulating and controlling the precipitation rate and precipitation amount of the internal mullite crystal phase, the prepared large-size ceramic sheet has excellent mechanical properties and wide potential commercial market.
Description
Technical Field
The invention belongs to the technical field of metal-based composite ceramic sheets, and relates to a mullite fiber reinforced metal-based composite ceramic sheet and a preparation method thereof.
Background
In recent years, with the gradual rise of building ceramics in the field of home decoration, the building ceramic sheet has attracted attention due to the advantages of lightness, thinness, low energy consumption, few raw materials and the like, becomes the key research direction of the traditional building ceramic sheet, has 1000 million yuan in the international market share in 2020, and has huge development potential.
Compared with the traditional architectural ceramic plate, the thickness of the architectural ceramic plate is only 3-5mm, which can save 30-50% of the raw material consumption, reduce 20-40% of production emission and reduce 20-30% of production energy consumption, and becomes an important outlet of the traditional architectural ceramic plate industry. However, according to the mechanical relationship between the thickness of the brittle material and the failure strength, the mechanical strength of the building ceramic plate is suddenly reduced along with the reduction of the thickness of the building ceramic plate, so that the building ceramic plate is difficult to form and difficult to meet the requirements of daily home decoration and safety protection. Therefore, how to develop systematic strengthening and toughening research based on the structural characteristics of the traditional architectural ceramic plate is the key to realize the thinning of the traditional large-size architectural ceramic plate.
At present, aiming at the difficult problem of the traditional large-specification architectural ceramic plate thinning, a scientific researcher mainly adjusts blank formula parameters such as aluminum content, plasticity and the like, so that the comprehensive mechanical property of the material is improved, and the large-specification architectural ceramic plate thinning is realized. In addition, by optimizing the formula composition of the blank, reinforcing phase substances such as mullite and the like can be precipitated in the system to reinforce the building ceramic plate. However, because the blank of the building ceramic plate contains dozens of oxides, the components of a formula system are complex, the solid-phase reaction is uncontrollable, and the uniform precipitation of reinforcing phases such as mullite, wax feldspar and the like in a matrix phase is difficult to effectively regulate and control. The Euglena sea wave and the like take mullite ceramic fiber felts as reinforcements, adopt traditional building ceramic powder as a matrix, and prepare the mullite fiber reinforced ceramic sheet by means of a vacuum infiltration method. Researches find that reinforcing phase substances such as mullite and cerasus feldspar can be separated out from the internal molten glass phase, so that the comprehensive mechanical property of the composite ceramic sheet is improved, but the internal self-growing substances are not uniformly dispersed.
Disclosure of Invention
Aiming at the problems in the prior art, the invention develops a technology for generating the mullite fiber reinforced metal-based composite ceramic sheet by in-situ induction, and the large-size ceramic sheet prepared by optimizing a solid-phase reaction sintering system and regulating and controlling the precipitation rate and precipitation amount of an internal mullite phase has excellent mechanical properties and low cost.
The invention is realized by the following technical scheme:
a method for preparing a mullite fiber reinforced metal matrix composite ceramic sheet comprises the following steps,
step 1, uniformly mixing calcined alumina, magnesia, nanoscale fused quartz, monazite, bentonite, pyrophyllite, black talc, potash feldspar, aluminum powder and sodium tripolyphosphate, performing ball milling treatment, screening and drying to obtain mixed powder A;
step 2, pretreating the mixed powder A prepared in the step 1, and then pulping and spray granulating to obtain blank powder B;
and 3, pressing and forming the blank powder B prepared in the step 2 into a ceramic plate-shaped green body, sintering the ceramic plate-shaped green body to obtain a ceramic sheet blank C, glazing, grinding the surface and polishing the ceramic sheet blank C to obtain the mullite fiber reinforced metal matrix composite ceramic sheet.
Preferably, the mass ratio of the calcined alumina, the magnesia, the nano fused quartz, the monazite, the bentonite, the pyrophyllite, the black talc and the potash feldspar in the step 1 is (30-35): (5-10): (20-25): (10-15): (1-3): (5-10): (5-10): (10-15); the aluminum powder and the sodium tripolyphosphate account for 5-10% and 0.5-1.2% of the mixed powder A by mass respectively.
Preferably, the particle size of the aluminum powder is 100 to 300nm.
Preferably, the pretreatment in step 2 is to remove iron and screen the mixed powder A prepared in step 1.
Preferably, the moisture content of the green body powder B in the step 2 is 5-8%.
Preferably, the length, width and thickness of the ceramic plate-like green body in step 3 are 700 to 900mm, 1500 to 1700mm and 2 to 5mm, respectively.
Preferably, the specific process of the compression molding in the step 3 is as follows: pressurizing the blank powder B from 0MPa to 30-40MPa, keeping the pressure for 10-15s, and then pressurizing to 60-80MPa, and keeping the pressure for 25-30s.
Preferably, the sintering in step 3 comprises the following specific steps: under the condition of reducing atmosphere, heating from room temperature to 1200-1300 ℃ at the heating rate of 8-10 ℃/min, preserving heat for 5-10min, then, under the oxidizing atmosphere, reducing the temperature to 1000-1100 ℃ at the cooling rate of 5-8 ℃/min, preserving heat for 15-20min, and finally, naturally cooling along with the furnace. .
Preferably, the reducing atmosphere is a mixed gas of methane and hydrogen, and the volume ratio of methane to hydrogen is 1; the oxidizing atmosphere is oxygen.
A mullite fiber reinforced metal matrix composite ceramic sheet is prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention provides an in-situ induced mullite fiber reinforced metal matrix composite ceramic sheet and a preparation method thereof, wherein an in-situ internal toughening formula system is developed by introducing a low-cost nano-scale sintering aid; selecting low-cost potash albite as a sintering aid, strictly regulating and controlling the aluminum-silicon ratio according to a crystallization route, promoting a high-temperature molten glass phase to reach a supersaturated crystallization state, and inducing an internal in-situ and high-efficiency precipitation of a high-strength acicular mullite phase; meanwhile, low-cost nanoscale fused quartz is selected as a sintering aid, has the characteristics of high specific surface area and high reactivity, can be melted into a flowing state glass phase at high temperature, can be dissipated by virtue of osmosis and uniformly distributed in a blank body to form a reticular flowing state melting structure, and promotes internal pore exhaust and particle rearrangement; in addition, low-cost micron-sized calcined alumina is selected as a dispersive particle reinforcing phase and can cooperate with a high-strength acicular mullite phase grown in situ to construct a particle-fiber multi-dimensional common reinforcing system, when the composite ceramic sheet bears external stress, the high-strength granular alumina and the acicular mullite phase which are uniformly distributed in the composite ceramic sheet can deflect internal microcrack expansion paths to timely transmit external load and absorb load energy, so that the comprehensive mechanical property of the composite ceramic sheet is effectively improved, and material failure is avoided.
Furthermore, the invention also introduces nano-scale aluminum powder as a high-quality aluminum source to participate in constructing an internal silicon-oxygen tetrahedron, promotes particle rearrangement, reduces the number of internal pores, and improves the mechanical structure stability of the composite ceramic sheet; the nanoscale aluminum powder has the characteristics of high surface energy, high specific surface area and low melting point, is adsorbed into a glass phase in a molten state at high temperature to generate a supersaturated molten glass phase with high aluminum and low silicon, and separates out a high-aluminum low-silicon and high-strength acicular mullite phase in the cooling process, so that the content of a green body reinforcing phase is increased, and the mechanical property of the composite ceramic plate is favorably improved; the nano-scale aluminum powder has the grain diameter of 100-300nm and high dispersion efficiency, can be uniformly distributed at each position of a matrix and is filled among the micro-scale powder particles, thereby promoting the densification process of the system, being beneficial to separating out high-strength crystalline phase from the matrix phase in an omnibearing and high-efficiency manner, and avoiding the fracture failure of the material due to the uneven distribution of the internal crystalline phase; the invention controls the introduction amount of the nano-scale aluminum powder, can promote the internal crystallization reaction process, synchronously ensures the density and the mechanical strength of the composite ceramic sheet, and is difficult to achieve the beneficial effect when the introduction amount is too high/low.
Furthermore, a reduction-oxidation multi-stage co-sintering system is developed based on the characteristics of a metal-based blank formula, the reduction-oxidation multi-stage co-sintering system is carried out in a reducing atmosphere in the first stage, the ratio of methane to hydrogen is regulated and the sintering temperature is controlled, high-temperature thermodynamic power can be used as reaction driving force, an aluminum oxide wrapping layer of an aluminum source can be reduced into elemental aluminum, the aluminum source breaks through the limitation of the wrapping layer, the aluminum source permeates into a glass phase in a liquid phase form to generate a supersaturated molten glass phase with high aluminum and low silicon, and the precipitation efficiency of high-strength phases such as acicular mullite is improved; the second stage is carried out in an oxidizing atmosphere, can promote the oxidative decomposition of substances such as internal phosphate, sulfate and the like, accelerates the transmission rate of internal substances under the combined action of liquid-phase mass transfer and gas-phase mass transfer, and promotes the process of structure densification. In addition, the sintering temperature is reduced to 1000-1100 ℃ in the second stage, so that secondary growth of internal particles caused by overhigh thermal driving energy can be prevented, the internal porosity is reduced, the density of the material is improved, and the comprehensive mechanical property of the metal-based ceramic sheet is ensured.
Furthermore, the invention has simple preparation process and low raw material cost, and can be applied to the commercial fields of architectural decoration ceramics, protective materials and the like. By optimizing a solid-phase reaction sintering system and regulating and controlling the precipitation rate and precipitation amount of the internal mullite crystal phase, the prepared large-size ceramic sheet has excellent mechanical properties and wide potential commercial market.
Drawings
FIG. 1 is a scanning electron microscope test chart (by etching) of a cross section of a metal matrix composite ceramic thin plate in example 1;
FIG. 2 is an X-ray energy spectrum analysis of a cross-section of a metal matrix composite ceramic thin plate according to example 1;
FIG. 3 is a scanning electron microscope test chart (by etching) of the cross section of the metal matrix composite ceramic sheet in example 2;
FIG. 4 is a scanning electron microscope test pattern (by etching) of a cross section of the metal matrix composite ceramic thin plate in comparative example 1;
FIG. 5 is a scanning electron microscope test chart (by etching) of a cross section of the metal matrix composite ceramic sheet in comparative example 2;
FIG. 6 is a scanning electron microscope test chart (by etching) of a cross section of the metal matrix composite ceramic thin plate in comparative example 3.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The specific technical scheme is as follows: a method for generating a mullite fiber reinforced metal matrix composite ceramic sheet by in-situ induction comprises the following steps:
1) According to a specific stoichiometric ratio, 8 raw materials of calcined alumina, magnesia, nano fused quartz, monazite, bentonite, pyrophyllite, black talc and potash feldspar are uniformly mixed. And then adding nano-scale aluminum powder and sodium tripolyphosphate into the mixed raw materials based on the mass of the mixed raw materials, performing ball milling treatment, screening the ball-milled products by a screen of 80-120 meshes, collecting screened materials, and drying to obtain mixed powder A. Wherein the mass ratio of the calcined alumina to the magnesia to the nano fused quartz to the monazite to the bentonite to the pyrophyllite to the black talc to the potash feldspar is (30-35): (5-10): (20-25): (10-15): (1-3): (5-10): (5-10): (10-15). The mixed powder A is added with 5 to 10 mass percent of aluminum powder, the particle size is 100 to 300nm, and the added mass percent of sodium tripolyphosphate is 0.5 to 1.2 percent.
2) And performing iron removal, sieving, pulping, spray granulation and other processes on the powder A to obtain green body powder B with the water content of 5-8%.
3) And (3) forming the blank powder B into ceramic plate-shaped green bodies with the length, width and thickness of 700-900mm, 1500-1700mm and 2-5mm respectively, and then transferring the ceramic plate-shaped green bodies into a high-temperature atmosphere furnace for sintering to obtain compact ceramic sheet blanks C. Wherein, the powder molding system is as follows: pressurizing from 0MPa to 30-40MPa, keeping the pressure for 10-15s, then pressurizing to 60-80MPa, and keeping the maximum pressure for 25-30s. The green body sintering system is as follows: in terms of volume fraction methane: heating the mixture from room temperature to 1200-1300 ℃ at a heating rate of 8-10 ℃/min under a reducing atmosphere of hydrogen = (1.
4) And glazing, surface grinding, polishing and other processes are carried out on the ceramic sheet blank C to obtain the mullite fiber reinforced metal-based composite ceramic sheet through in-situ induction.
The following detailed description is illustrative of the embodiments and is intended to provide further details of the invention. Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention.
Example 1:
1) According to a specific stoichiometric ratio, 8 raw materials of calcined alumina, magnesia, nano fused quartz, monazite, bentonite, pyrophyllite, black talc and potash feldspar are uniformly mixed. And then adding nanoscale aluminum powder and sodium tripolyphosphate into the mixed raw materials based on the mass of the mixed raw materials, performing ball milling treatment, screening the ball milled product with a 80-mesh screen, collecting screened materials, and drying to obtain powder A. Wherein the mass ratio of the calcined alumina, the magnesia, the nano fused quartz, the monazite, the bentonite, the pyrophyllite, the black talc and the potash feldspar is 30:5:20:10:1:5:5:10, adding 5 mass percent of aluminum powder into the mixed powder A, wherein the particle size is 100nm, and the mass percent of the added sodium tripolyphosphate is 0.5%.
2) And performing iron removal, sieving, pulping, spray granulation and other processes on the powder A to obtain green body powder B with the water content of 5%.
3) And (3) forming the blank powder B into ceramic plate-shaped green bodies with the length, width and thickness of 700mm, 1500mm and 2mm respectively, and then transferring the ceramic plate-shaped green bodies into a high-temperature atmosphere furnace for sintering to obtain compact ceramic sheet blanks C. Wherein the powder molding system is as follows: pressurizing from 0MPa to 30MPa, keeping the pressure for 10s, then pressurizing to the maximum pressure of 60MPa, and keeping the maximum pressure for 25s. The green body sintering system is as follows: in terms of volume fraction methane: hydrogen =1:1, heating to 1200 ℃ from room temperature at the heating rate of 8 ℃/min and preserving heat for 5min, then reducing to 1000 ℃ at the cooling rate of 5 ℃/min and preserving heat for 15min in the oxidizing atmosphere, and finally naturally cooling along with the furnace.
4) And glazing, surface grinding, polishing and other processes are carried out on the ceramic sheet blank C to obtain the mullite fiber reinforced metal-based composite ceramic sheet through in-situ induction.
Example 2:
1) According to a specific stoichiometric ratio, 8 raw materials of calcined alumina, magnesia, nano fused quartz, monazite, bentonite, pyrophyllite, black talc and potash albite are uniformly mixed. And then adding nano-scale aluminum powder and sodium tripolyphosphate into the mixed raw materials based on the mass of the mixed raw materials, performing ball milling treatment, screening the ball-milled products by a 120-mesh screen, collecting screened materials, and drying to obtain mixed powder A. Wherein the mass ratio of the calcined alumina, the magnesia, the nano fused quartz, the monazite, the bentonite, the pyrophyllite, the black talc and the potash feldspar is 35:10:25:15:3:10:10:15, adding 10 mass percent of aluminum powder into the mixed powder A, wherein the particle size of the particles is 300nm, and the mass percent of the added sodium tripolyphosphate is 1.2%.
2) And performing iron removal, sieving, pulping, spray granulation and other processes on the powder A to obtain green body powder B with the water content of 8%.
3) And (3) forming the blank powder B into ceramic plate-shaped green bodies with the length, width and thickness of 900mm, 1700mm and 5mm respectively, and then transferring the ceramic plate-shaped green bodies into a high-temperature atmosphere furnace for sintering to obtain compact ceramic sheet blanks C. Wherein the powder molding system is as follows: pressurizing from 0MPa to 40MPa, keeping the pressure for 15s, then pressurizing to the maximum pressure of 80MPa, and keeping the maximum pressure for 30s. The green body sintering system is as follows: in terms of volume fraction methane: heating from room temperature to 1300 ℃ at a heating rate of 10 ℃/min and preserving heat for 10min under a reducing atmosphere of hydrogen = (3).
4) And glazing, surface grinding, polishing and other processes are carried out on the ceramic sheet blank C to obtain the mullite fiber reinforced metal-based composite ceramic sheet through in-situ induction.
Example 3:
1) According to a specific stoichiometric ratio, 8 raw materials of calcined alumina, magnesia, nano fused quartz, monazite, bentonite, pyrophyllite, black talc and potash albite are uniformly mixed. And then adding nanoscale aluminum powder and sodium tripolyphosphate into the mixed raw materials based on the mass of the mixed raw materials, performing ball milling treatment, screening the ball-milled products with a 100-mesh screen, collecting screened materials, and drying to obtain powder A. Wherein the mass ratio of the calcined alumina, the magnesia, the nano fused quartz, the monazite, the bentonite, the pyrophyllite, the black talc and the potash feldspar is 32:8:22:12:2:8:7:13. the mass percent of the aluminum powder added into the mixed powder A is 8%, the particle diameter is 220nm, and the mass percent of the sodium tripolyphosphate is 0.7%.
2) And performing iron removal, sieving, pulping, spray granulation and other processes on the powder A to obtain green body powder B with the water content of 6%.
3) And (3) forming the blank powder B into ceramic plate-shaped green bodies with the length, width and thickness of 800mm, 1600mm and 3mm respectively, and then transferring the ceramic plate-shaped green bodies into a high-temperature atmosphere furnace for sintering to obtain compact ceramic sheet blanks C. Wherein, the powder molding system is as follows: pressurizing from 0MPa to 36MPa, keeping the pressure for 12s, then pressurizing to the maximum pressure of 72MPa, and keeping the maximum pressure of 28s. The green body sintering system is as follows: in terms of volume fraction methane: heating from room temperature to 1220 ℃ at a heating rate of 9 ℃/min and preserving heat for 8min under a reducing atmosphere of hydrogen = (2.
4) And glazing, surface grinding, polishing and other processes are carried out on the ceramic sheet blank C to obtain the mullite fiber reinforced metal matrix composite ceramic sheet through in-situ induction.
Comparative example 1:
comparative example 1 core modifications compared to example 1 are as follows: the preparation process was the same as in example 1 except that nano-sized fused silica was not introduced as a sintering aid.
1) According to a specific stoichiometric ratio, 8 raw materials of calcined alumina, magnesia, glass frit, monazite, bentonite, pyrophyllite, black talc and potash albite are uniformly mixed. And then adding nano-scale aluminum powder and sodium tripolyphosphate into the mixed raw materials based on the mass of the mixed raw materials, performing ball milling treatment, screening the ball-milled products by a screen of 80-120 meshes, collecting screened materials, and drying to obtain powder A. Wherein the mass ratio of the calcined alumina, the magnesia, the glass frit, the monazite, the bentonite, the pyrophyllite, the black talc and the potash feldspar is 28:42:3:8:1:5:8:0.7:0.2:0.1. the mass percent of the aluminum powder added into the mixed powder is 5 percent, the particle diameter is 100nm, and the mass percent of the sodium tripolyphosphate added is 0.5 percent.
Comparative example 2:
compared with example 2, the core modification of comparative example 2 is as follows: the preparation process is the same as that of example 2 except that nanoscale aluminum powder is not introduced as a mineralizer.
1) According to a specific stoichiometric ratio, 8 raw materials of calcined alumina, magnesia, nano fused quartz, monazite, bentonite, pyrophyllite, black talc and potash albite are uniformly mixed. And then adding sodium tripolyphosphate into the mixed raw materials based on the mass of the mixed raw materials, performing ball milling treatment, sieving the ball-milled products with a 80-120-mesh sieve, collecting sieved materials, and drying to obtain powder A. Wherein the mass ratio of the calcined alumina, the magnesia, the nano fused quartz, the monazite, the bentonite, the pyrophyllite, the black talc and the potash feldspar is 30:45:5:10:3:8:10:1.2:0.5:0.3. the mass percent of sodium tripolyphosphate added into the mixed raw materials is 1.2%.
Comparative example 3:
compared with example 3, the core modification content of comparative example 3 is as follows: the conventional sintering system was adopted, and the reduction-oxidation multi-stage co-sintering system was not adopted, and the rest of the preparation process was the same as in example 3.
3) And forming the blank powder B into ceramic plate-shaped green bodies with the length, width and thickness of 800mm, 1600mm and 3mm respectively, and then transferring the ceramic plate-shaped green bodies into a high-temperature atmosphere furnace for sintering to obtain a compact ceramic sheet blank C. Wherein, the powder molding system is as follows: pressurizing from 0MPa to 36MPa, keeping the pressure for 12s, pressurizing to 60-80MPa, and keeping the maximum pressure for 28s. The green body sintering system is as follows: heating from room temperature to 1220 ℃ at the heating rate of 9 ℃/min, preserving heat for 18min, and naturally cooling along with the furnace.
Table 1 lists some of the mechanical property test data for examples 1, 2, 3 and comparative examples 1, 2, 3:
TABLE 1 comparison of mechanical Properties of examples and comparative examples
FIG. 1 is a scanning electron microscope test chart (by etching) of a cross section of a metal matrix composite ceramic sheet according to example 1. As can be seen from FIG. 1, the cross-section structure after etching has no large pores, the structure is relatively compact, and a large amount of needle-like and cluster-like substances are uniformly grown in situ in the matrix. According to the X-ray energy spectrum analysis result in fig. 2, the acicular and cluster-like substances are phases with high aluminum and low silicon, and are presumed to be high-strength mullite whiskers, which shows that the formula system developed by the invention is beneficial to the omnibearing and high-efficiency precipitation of high-strength mullite crystal phases on the matrix, and is closely related to the introduction of nano-scale fused quartz and aluminum powder.
FIG. 3 is a scanning electron microscope (etched) test pattern of the cross section of the metal matrix composite ceramic thin plate in example 1. As can be seen from fig. 3, a large amount of fibrous mullite phase and granular corundum phase are uniformly distributed in the matrix. When the microcracks expand in the matrix, the expansion path of the microcracks obviously deflects, which shows that the particle-fiber multi-dimensional common enhancement system constructed by the invention can cooperatively bear external load, is beneficial to absorbing load energy and improving the comprehensive mechanical property of the composite ceramic sheet.
FIG. 4 is a scanning electron microscope test chart (etched) of the cross section of the metal matrix composite ceramic sheet in comparative example 1. As can be seen from FIG. 4, when the nano-fused quartz is not introduced as the sintering aid, the acicular or clustered mullite phase substances precipitated inside the nano-fused quartz are not uniformly distributed and the number of the acicular or clustered mullite phase substances is obviously reduced, which indicates that the nano-fused quartz is beneficial to omnibearing and high-efficiency precipitation of a high-strength crystalline phase from the matrix.
FIG. 5 is a scanning electron microscope test chart (etched) of the cross section of the metal matrix composite ceramic sheet in comparative example 2. It can be seen from table 1 and fig. 5 that, when the nano-scale aluminum powder is not introduced as a mineralizer, acicular or clustered mullite phase substances are rarely precipitated in the matrix, an enough strengthening and toughening system is lacked in the matrix, and the expansion path of the microcracks is single long crack diffusion. In addition, the mechanical strength of the material is obviously reduced due to blank delamination, the bending strength of the composite ceramic sheet is only 26.68MPa, and the fracture toughness is 2.21MPa/m 2 。
FIG. 6 is a scanning electron microscope test chart (etched) of the cross section of the metal matrix composite ceramic sheet in comparative example 3. As can be seen from FIG. 6, when the conventional sintering system in the market is adopted, no high-strength crystalline phase such as mullite whisker is generated inside, and the grains are obviously abnormally grown, which indicates that the conventional sintering system in the market is unreasonable, and the beneficial effect of the conventional sintering system is not as good as the reduction-oxidation multi-stage co-sintering system developed by the invention.
(1) Compared with the comparative example 1, the in-situ internal toughening formula system is developed by introducing the low-cost nano-scale sintering aid. The method has the following beneficial effects: one, based on K 2 O/Na 2 O-Al 2 O 3 -SiO 2 Selecting a mullite phase as a specific crystallization area, selecting low-cost potash-soda feldspar as a sintering aid, strictly regulating and controlling the aluminum-silicon ratio according to a crystallization route, promoting a high-temperature molten glass phase to reach a supersaturated crystallization state, and inducing an internal in-situ and high-efficiency precipitation of a high-strength acicular mullite phase; secondly, low-cost nano-scale fused quartz is selected as a sintering aid, has the characteristics of high specific surface area and high reaction activity, can be fused into a flowing state glass phase at 700-900 ℃, can be dissipated by virtue of osmosis and uniformly distributed in a blank body to form a reticular flowing state fused structure, and promotes internal pore exhaust and particle rearrangement; thirdly, selecting low-cost micron-grade calcined alumina as a dispersible particle reinforcing phase, and constructing a 'particle-fiber' multi-dimensional common reinforcing system by cooperating with a high-strength acicular mullite phase grown in situ. When the composite ceramic sheet bears external stress, the high-strength granular alumina and the acicular mullite which are uniformly distributed inside can deflect the internal microcrack expansion path, external load is transmitted in time, and load energy is absorbed, so that the comprehensive mechanical property of the composite ceramic sheet is effectively improved, and material failure is avoided.
(2) Comparing example 2 with comparative example 2, it can be known that the metal matrix composite ceramic system is constructed by introducing the nano-scale aluminum powder as the mineralizer. The traditional ceramics mainly have a silicon-oxygen tetrahedral network structure inside, 60-80% of aluminum source exists in a bonding structure, and the traditional ceramics are difficult to melt in a glass phase to generate a specific phase, so that the crystallization reaction efficiency is low. The invention introduces 5-10% of nano-scale aluminum powder as a mineralizer, and has the following four beneficial effects: firstly, the nanoscale aluminum powder can be used as a high-quality aluminum source to participate in constructing an internal silicon-oxygen tetrahedron, so that particle rearrangement is promoted, the number of internal pores is reduced, and the mechanical structure stability of the composite ceramic sheet is improved; secondly, the nanoscale aluminum powder has the characteristics of high surface energy, high specific surface area and low melting point, is adsorbed into a glass phase in a molten state at 800-1000 ℃ to generate a supersaturated molten glass phase with high aluminum and low silicon, and separates out a high-aluminum low-silicon and high-strength acicular mullite phase in the cooling process, so that the content of a green body reinforcing phase is increased, and the mechanical property of the composite ceramic plate is favorably improved; thirdly, the nano-scale aluminum powder has the particle size of 100-300nm, high dispersion efficiency, can be uniformly distributed at each position of the matrix and is filled among the micron-scale powder particles, the densification process of the system is promoted, the omnibearing and high-efficiency precipitation of high-strength crystalline phase from the matrix phase is facilitated, and the material fracture failure caused by the uneven distribution of the internal crystalline phase is avoided; fourthly, the invention controls the introduction amount of the nano-scale aluminum powder to be 5 to 10 percent, can promote the internal crystallization reaction process, synchronously ensure the compactness and the mechanical strength of the composite ceramic sheet, and cannot achieve the beneficial effect when the introduction amount is too high/low.
(3) As can be seen from the comparison of example 3 with comparative example 3, a "reduction-oxidation" multi-stage co-sintering system was developed based on the formulation characteristics of the metal-based green body. The traditional ceramic sheet mostly adopts a solid-phase sintering process, has a relatively single production mode, and cannot meet the sintering requirement of the invention. Therefore, the invention optimizes the sintering process system, develops the reduction-oxidation multi-section type co-sintering system, and has the following two beneficial effects: first, the first stage is carried out in a reducing atmosphere by regulating and controlling the optimal ratio of methane: hydrogen = (1) - (3), the sintering temperature is controlled to be 1200-1300 ℃, high-temperature thermal power can be used as a reaction driving force, an alumina wrapping layer of an aluminum source can be reduced to be simple-substance aluminum, the aluminum source can break through the limitation of the wrapping layer and permeate into a glass phase in a liquid phase form, a supersaturated molten state glass phase with high aluminum and low silicon is generated, and the precipitation efficiency of high-strength phases such as acicular mullite is improved; the second stage is carried out in an oxidizing atmosphere, so that the oxidative decomposition of substances such as internal phosphate, sulfate and the like can be promoted, the transmission rate of internal substances is accelerated under the combined action of liquid-phase mass transfer and gas-phase mass transfer, and the process of structure densification is promoted. In addition, the sintering temperature is reduced to 1000-1100 ℃ in the second stage, so that secondary growth of internal particles caused by overhigh thermal driving energy can be prevented, the internal porosity is reduced, the density of the material is improved, and the comprehensive mechanical property of the metal-based ceramic sheet is ensured.
(4) A multi-step vented compression molding process was developed. The prior art for disclosing the ceramic thin plate on the market is mostly a one-step dry pressing forming process, which is very easy to have structural defects of layering, blank surface damage and the like, is difficult to form a low-plasticity blank formula, and has poor mechanical strength of a product. Based on the developed formula of the low-plasticity metal-based ceramic blank, the invention optimizes the water content of the blank to 5-8%, develops a multi-step exhaust pressing forming process applicable to the formula of the low-plasticity blank, and has the following two beneficial effects: firstly, the multi-step exhaust pressing process is divided into two stages: in the first stage, residual gas among powder materials can be rapidly discharged under the pressure of 30-40MPa, so that blank particles are promoted to be tightly attached, and mechanical structure defects such as powder material layering and the like are prevented; in the second stage, the forming pressure is set to be 60-80MPa, plastic substances can be fully filled to the periphery of the barren substances under the forming pressure, an integrated network bonding structure is constructed, the forming efficiency of ceramic sheet green bodies with the thickness of less than 3mm is improved, and apparent defects such as green surface breakage and the like are avoided, so that the mechanical strength of the green bodies is guaranteed; secondly, the multi-step exhaust pressing forming process method developed by the invention is simple, can be debugged based on the existing production equipment, and has strong industrialization replaceability and extremely wide market application prospect.
In conclusion, the invention provides the mullite fiber reinforced metal matrix composite ceramic sheet and the preparation method thereof, the preparation process is simple, the raw material cost is low, and the mullite fiber reinforced metal matrix composite ceramic sheet can be applied to the commercial fields of building decoration ceramics, protective materials and the like. By optimizing a solid-phase reaction sintering system and regulating and controlling the precipitation rate and precipitation amount of the mullite crystal phase in the ceramic thin plate, the prepared large-size ceramic thin plate has excellent mechanical properties and wide potential commercial market.
Claims (7)
1. A method for preparing a mullite fiber reinforced metal matrix composite ceramic sheet is characterized by comprising the following steps of,
step 1, uniformly mixing calcined alumina, magnesia, nanoscale fused quartz, monazite, bentonite, pyrophyllite, black talc, potash feldspar, aluminum powder and sodium tripolyphosphate, performing ball milling treatment, screening and drying to obtain mixed powder A;
step 2, pretreating the mixed powder A prepared in the step 1, and then pulping and spray granulating to obtain blank powder B;
step 3, pressing and molding the blank powder B prepared in the step 2 into a ceramic plate-shaped green body, then sintering the ceramic plate-shaped green body to obtain a ceramic sheet blank C, and glazing, surface grinding and polishing the ceramic sheet blank C to obtain the mullite fiber reinforced metal matrix composite ceramic sheet;
the mass ratio of calcined alumina, magnesia, nanoscale fused silica, monazite, bentonite, pyrophyllite, black talc and potash feldspar in the step 1 is (30-35): (5-10): (20-25): (10-15): (1-3): (5-10): (5-10): (10-15); the aluminum powder and the sodium tripolyphosphate account for 5-10% and 0.5-1.2% of the mixed powder A by mass respectively;
the particle size of the aluminum powder is 100-300nm;
the sintering process in the step 3 comprises the following specific steps: heating from room temperature to 1200-1300 ℃ at a heating rate of 8-10 ℃/min under the condition of a reducing atmosphere, preserving heat for 5-10min, then reducing the temperature to 1000-1100 ℃ at a cooling rate of 5-8 ℃/min under the condition of an oxidizing atmosphere, preserving heat for 15-20min, and finally naturally cooling along with the furnace.
2. The method for preparing the mullite fiber reinforced metal matrix composite ceramic sheet according to claim 1, wherein the step 2 is carried out by performing iron removal and screening on the mixed powder A prepared in the step 1.
3. The method for preparing the mullite fiber reinforced metal matrix composite ceramic sheet according to claim 1, wherein the moisture content of the blank powder B in the step 2 is 5-8%.
4. The method for preparing the mullite fiber reinforced metal matrix composite ceramic sheet as claimed in claim 1, wherein the ceramic plate-shaped green compact in step 3 has a length, a width and a thickness of 1500-1700mm, 700-900mm and 2-5mm, respectively.
5. The method for preparing the mullite fiber reinforced metal matrix composite ceramic sheet according to claim 1, wherein the specific process of the compression molding in the step 3 is as follows: pressurizing the blank powder B from 0MPa to 30-40MPa, keeping the pressure for 10-15s, and then pressurizing to 60-80MPa, and keeping the pressure for 25-30s.
6. The method for preparing the mullite fiber-reinforced metal-matrix composite ceramic sheet according to claim 1, wherein the reducing atmosphere is a mixed gas of methane and hydrogen, and the volume ratio of the methane to the hydrogen is 1; the oxidizing atmosphere is oxygen.
7. A mullite fiber-reinforced metal-matrix composite ceramic sheet produced by the production method according to any one of claims 1 to 6.
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