CN109970439B - Preparation method of light ceramic composite sheet - Google Patents

Preparation method of light ceramic composite sheet Download PDF

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CN109970439B
CN109970439B CN201910196069.9A CN201910196069A CN109970439B CN 109970439 B CN109970439 B CN 109970439B CN 201910196069 A CN201910196069 A CN 201910196069A CN 109970439 B CN109970439 B CN 109970439B
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ceramic
fiber
vacuum
powder
binder
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CN109970439A (en
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萧礼标
欧阳海波
黄玲艳
汪庆刚
黄剑锋
李嘉胤
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Monalisa Group Co Ltd
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Abstract

The invention provides a preparation method of a light ceramic composite sheet. The method comprises the following steps: (1) uniformly mixing polycrystalline mullite fiber, a binder and water to prepare a fiber dispersion liquid; (2) adding ceramic powder into the obtained fiber dispersion liquid to prepare mixed suspension; (3) pouring the obtained mixed suspension into a vacuum filtration device, and carrying out vacuum filtration to obtain a fiber reinforced ceramic biscuit; (4) biscuit firing the obtained fiber reinforced ceramic biscuit to obtain a ceramic sheet blank; (5) putting the obtained ceramic sheet blank into a vacuum filtration device, and pouring a suspension containing ceramic powder and a binder into the vacuum filtration device for vacuum infiltration treatment to obtain a vacuum infiltrated ceramic sheet blank; (6) sintering the ceramic sheet blank subjected to vacuum infiltration to obtain the light ceramic composite sheet. The invention can greatly improve the volume fraction of the fibers in the ceramic sheet, effectively avoid the damage of the fibers and improve the toughening effect of the fibers.

Description

Preparation method of light ceramic composite sheet
Technical Field
The invention belongs to the technical field of ceramic material preparation, and particularly relates to a light ceramic composite sheet and a preparation method thereof.
Background
The ceramic sheet has the characteristics of energy conservation, consumption reduction, cleanness, environmental protection, light weight, high strength and the like, so that the traditional building ceramic is greatly changed, and the thinning of the building ceramic becomes the future development trend of the industry. However, the existing ceramic sheet mainly depends on adjusting the proportion of raw materials, and the strength and toughness of the sheet are improved by reducing the porosity of a ceramic blank by adopting a high-tonnage press, so that the cost of the raw materials is high, the requirement on equipment is high, and the popularization and application of the ceramic sheet are limited. Fiber reinforcement is an effective means of improving the strength and toughness of ceramic materials. Chinese patent ZL201510266745.7 (CN 104926344B) discloses alumina silicate fiber reinforced oxide ceramic and a preparation method thereof, wherein oxide sol is used as a precursor, alumina silicate fiber fabric is subjected to vacuum impregnation, then gelation is carried out, and high-temperature ceramic is carried out to obtain the alumina silicate fiber reinforced oxide ceramic. But the cost and the preparation process of the composite material are difficult to apply in the building ceramic industry.
Disclosure of Invention
In view of the above drawbacks, the present invention provides a lightweight ceramic composite sheet and a method for manufacturing the same, wherein the ceramic composite sheet has a low density, a high strength, and a gradient pore structure, and is simple and low in cost, and suitable for the production of functional ceramic sheets.
In one aspect, the present invention provides a lightweight ceramic composite sheet comprising a ceramic sheet matrix and polycrystalline mullite fibers distributed in the ceramic sheet matrix, the lightweight ceramic composite sheet having a gradient pore structure in a thickness direction.
Preferably, in the lightweight ceramic composite sheet, the volume fraction of the polycrystalline mullite fibers is 10-30%.
Preferably, the density of the light ceramic composite sheet is 1.5-2.0 g/cm3The bending strength is more than 80 MPa.
On the other hand, the invention provides a preparation method of the light ceramic composite sheet, which comprises the following steps:
(1) uniformly mixing polycrystalline mullite fiber, a binder and water to prepare a fiber dispersion liquid;
(2) adding ceramic powder into the obtained fiber dispersion liquid to prepare mixed suspension;
(3) pouring the obtained mixed suspension into a vacuum filtration device, and carrying out vacuum filtration to obtain a fiber reinforced ceramic biscuit;
(4) biscuit firing the obtained fiber reinforced ceramic biscuit to obtain a ceramic sheet blank;
(5) putting the obtained ceramic sheet blank into a vacuum filtration device, and pouring a suspension containing ceramic powder and a binder into the vacuum filtration device for vacuum infiltration treatment to obtain a vacuum infiltrated ceramic sheet blank;
(6) sintering the ceramic sheet blank subjected to vacuum infiltration to obtain the light ceramic composite sheet.
According to the method, polycrystalline mullite fiber is used as a reinforcement, a binder is introduced, ceramic powder is used as a substrate, a porous ceramic sheet blank is prepared by vacuum infiltration (vacuum filtration) -low-temperature sintering (biscuit firing), and the fiber and the substrate are integrated by the low-temperature sintering, so that the strength of the biscuit is improved, and cracking and deformation of the biscuit in the infiltration process are avoided. And then selecting a suspension containing ceramic powder and a binder as a raw material, filling the ceramic powder and the binder in the surface gaps of the porous ceramic sheet blank by using a secondary vacuum infiltration treatment method to form a gradient pore structure, and sintering at high temperature to obtain the lightweight ceramic composite sheet with the gradient pore structure. The existence of the binder enables the ceramic powder and the ceramic thin plate blank to be tightly combined.
Preferably, in the step (1), the polycrystalline mullite fiber has a use temperature of more than 1400 ℃, a diameter of 3-5 μm and a length of 5-10 mm; the binder is silica sol, preferably SiO in silica sol2The mass concentration of (A) is 20-30%.
Preferably, in the step (1), the mass ratio of the polycrystalline mullite fiber to the binder in the fiber dispersion liquid is (3-1): 1, and the mass ratio of the polycrystalline mullite fiber to the water is 1: (10-20).
Preferably, in the step (2), the mass ratio of the polycrystalline mullite fiber to the ceramic powder is 1 (2-5).
Preferably, in the step (2), the ceramic powder includes: 35 to 45 weight percent of SiO235 to 45 weight percent of mullite and 10 to 30 weight percent of corundum powder; preferably, the particle size of the ceramic powder is less than 100 meshes.
Preferably, in the step (3), the thickness of the fiber reinforced ceramic biscuit is 5-8 mm.
Preferably, in the step (4), the temperature of the bisque firing is 600-800 ℃, and the bisque firing time is 0.5-1.0 hour.
Preferably, in the step (5), the mass ratio of the binder to the ceramic powder in the suspension containing the ceramic powder and the binder is 1 (2-5). The quality ratio of the adhesive to the ceramic powder in the suspension affects the depth of the subsequent secondary vacuum infiltration and the effect of filling the pores. Within the range of the ratio, the depth of the subsequent secondary vacuum infiltration and the effect of filling the pores are better. The content of the binder affects the temperature and time of high-temperature sintering. At the above binder content, the temperature and time for high-temperature sintering are suitable. Preferably, the binder is a silica sol, more preferably, SiO in silica sol2The mass concentration of (A) is 20-30%; the ceramic powder comprises: 35 to 45 weight percent of SiO235 to 45 weight percent of mullite and 10 to 30 weight percent of corundum powder; preferably, the particle size of the ceramic powder is less than 100 meshes.
Preferably, in the step (3), the vacuum degree of the vacuum filtration is 10-100 Pa, and the filtration time is 5-10 minutes; in the step (5), the vacuum degree of the vacuum suction and infiltration treatment is 10-100 Pa, and the suction filtration time is 10-20 minutes.
Preferably, the obtained fiber reinforced ceramic biscuit is subjected to static pressure forming in a press before biscuit firing, and the pressure of the static pressure forming is 3-5 MPa.
Preferably, in the step (6), the sintering temperature is 1100-1300 ℃ and the time is 1-2 hours.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the invention, the ceramic sheet biscuit is prepared by selecting a vacuum filtration mode, the volume fraction of fibers in the ceramic sheet can be greatly improved, the damage of the fibers is effectively avoided, the fiber toughening effect is improved, the gradient pore structure formed by the ceramic sheet is realized by utilizing secondary vacuum infiltration, the section of the ceramic sheet is compact to a porous structure, the self weight of the ceramic sheet is effectively reduced, the consumption of raw materials is reduced, the construction difficulty is also greatly reduced, and the application field of the ceramic sheet biscuit can be effectively expanded. In addition, the pore structure of the ceramic sheet can be applied in the fields of heat insulation, noise reduction and the like, and the functions of the ceramic sheet are enriched.
Drawings
FIG. 1 is a schematic view of a light ceramic composite sheet prepared by the vacuum infiltration process of the present invention;
FIG. 2 is a schematic structural view of a lightweight composite ceramic sheet according to the present invention;
FIG. 3 is a SEM image of the porous surface of a lightweight composite ceramic sheet made in example 2;
FIG. 4 is a SEM image of the dense surface of a lightweight composite ceramic sheet made in example 2;
fig. 5 is an SEM image of the reinforcing fibers inside the plate of the lightweight composite ceramic sheet prepared in example 2.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive. The following percentages are by mass unless otherwise specified.
In the present disclosure, a lightweight ceramic composite sheet includes a ceramic sheet matrix and polycrystalline mullite fibers distributed in the ceramic sheet matrix. Also, the lightweight ceramic composite sheet has a gradient pore structure in the thickness direction.
The polycrystalline mullite fiber is one of polycrystalline alumina fibers, wherein Al is contained in the fibers2O3The content is between 72 and 75 percent. The polycrystalline mullite fiber can enhance the strength and toughness of the sheet. In a preferred embodiment, the polycrystalline mullite fiber has a diameter of 3 to 5 μm and a length of 5 to 10 mm.
The gradient pore structure effectively reduces the dead weight of the ceramic sheet, not only reduces the consumption of raw materials, but also greatly reduces the construction difficulty and can effectively expand the application field of the ceramic sheet. In addition, the pore structure of the ceramic sheet can be applied in the fields of heat insulation, noise reduction and the like, and the functions of the ceramic sheet are enriched.
Fig. 2 is a schematic cross-sectional structure view of a lightweight ceramic composite sheet according to an embodiment, and as shown in fig. 2, the lightweight ceramic composite sheet has a structure ranging from a dense structure to a porous structure in a thickness direction, and includes a dense layer, a transition layer, and a porous layer in this order. In some embodiments, the lightweight ceramic composite sheet has a porosity that gradually increases from side to side in a thickness direction. In some embodiments, the porous layer has a pore size distribution of 10 to 200 microns.
In the light ceramic composite sheet, the polycrystalline mullite fibers can be uniformly distributed, and the volume fraction of the polycrystalline mullite fibers can be 10-30%.
The raw material formula of the ceramic sheet substrate can be as follows: 35 to 45 weight percent of SiO235 to 45 weight percent of mullite and 10 to 30 weight percent of corundum powder, wherein the sum of the mass percent of the components is 100 weight percent. By adopting the formula, the sintering temperature can be effectively reduced, the reaction of the reinforcing fiber and the ceramic powder at high temperature can be avoided, and the sintered ceramic sheet has higher strength.
In some embodiments, the lightweight ceramic composite sheets of the present disclosure may be obtained by gradient-filling ceramic powders in a porous ceramic sheet blank and sintering. In addition, the light ceramic composite sheet can also contain a binder, which enables the ceramic powder filled in the holes to be tightly combined with the ceramic sheet blank.
In some embodiments, the density of the lightweight ceramic composite sheet of the present disclosure can be 1.5-2.0 g/cm3The bending strength is more than 80 MPa. In the present disclosure, the bending strength of the resulting lightweight ceramic composite sheet was tested by a three-point bending method.
In some embodiments, the thickness of the lightweight ceramic composite sheet of the present disclosure may be 5 to 8mm, and further may be 5mm or less.
In some embodiments of the present disclosure, polycrystalline mullite fiber is used as a reinforcement, silica sol is used as a binder, ceramic powder is used as a matrix, a porous ceramic sheet is prepared by vacuum infiltration-low temperature sintering, secondary vacuum infiltration is used for filling up gaps on the surface layer of the porous ceramic sheet, and the lightweight ceramic composite sheet with a gradient pore structure is prepared by high temperature sintering. The following exemplarily illustrates a method for preparing a lightweight ceramic composite sheet.
And uniformly stirring and dispersing the polycrystalline mullite fiber, the silica sol and the water to prepare a fiber dispersion liquid. It is composed ofIn the middle, the polycrystalline mullite fiber is used at a temperature of more than 1400 ℃. Mullite fiber is generally used as a refractory material, and the use temperature means that the mullite fiber does not undergo phase change or melting at a certain temperature. The diameter of the polycrystalline mullite fiber can be 5-10 mu m, and the length can be 5-10 mm. SiO in silica sol2The concentration is 20-30%. In an optional embodiment, the mass ratio of the polycrystalline mullite fiber to the silica sol in the fiber dispersion is controlled within a range of 3:1 to 1: 1. The proportion range can effectively ensure the dispersion of mullite fiber and the strength of ceramic cellulose blank. The mass ratio of the polycrystalline mullite fiber to the water in the fiber dispersion liquid can be controlled within the range of 1: 10-1: 20. The dispersion may be by mechanical agitation.
Adding the ceramic powder into the fiber dispersion liquid, and continuously stirring in the adding process to prepare mixed suspension (slurry). If the ceramic powder, the polycrystalline mullite fiber, the silica sol and the water are directly added together, the slurry is too thick and is not beneficial to the dispersion of the fibers, and the ceramic powder is preferably added after the fibers are dispersed. Wherein the ceramic powder may contain SiO2Mullite and corundum powder. In an alternative embodiment, the SiO in the ceramic powder2The content of the powder is 35-45 percent, the content of the mullite is 35-45 percent, the content of the corundum powder is 10-30 percent, and the total mass content of all the components is 100 percent. The grain diameter of the ceramic powder after ball milling and granulation is less than 100 meshes. In the particle size range, the dispersion of slurry is facilitated, and a uniform pore structure is constructed. In an optional embodiment, the ratio of the polycrystalline mullite fiber to the ceramic powder is controlled to be 1: 2-1: 5.
And pouring the mixed suspension into a vacuum filtration device by adopting a vacuum filtration method, and carrying out vacuum filtration to obtain the fiber reinforced ceramic biscuit. In an alternative embodiment, the thickness of the fiber reinforced ceramic biscuit is controlled within the range of 5-8 mm. In the vacuum filtration, the vacuum degree and the filtration time can be selected according to the required thickness and pore structure, for example, the vacuum degree can be 10-100 Pa, and the filtration time can be 5-10 minutes.
In an alternative embodiment, the fiber reinforced ceramic greenbody is press formed in a press. The thickness of the obtained fiber reinforced ceramic biscuit after the static pressure forming is controlled to be 5-8 mm. The static pressure forming can reduce the thickness of the blank by 10-20%. The static pressure forming pressure of the fiber reinforced ceramic biscuit in the press can be controlled to be 3-5 MPa, so that the fiber volume fraction and the biscuit strength of the biscuit can be improved.
And (4) carrying out biscuit firing (low-temperature sintering) on the fiber reinforced ceramic biscuit to obtain a ceramic sheet biscuit. Wherein, the low-temperature sintering temperature can be 600-800 ℃, and the sintering time can be 0.5-1.0 hour. The porosity of the obtained ceramic sheet blank can be 25-40%.
The silica sol and the ceramic powder are prepared into a suspension. Wherein the mass ratio of the silica sol to the ceramic powder in the suspension is controlled within the range of 1: 2-1: 5. The proportion range is favorable for dispersing the ceramic powder, and simultaneously, the viscosity of the slurry is ensured to be favorable for permeating into the biscuit. The solvent in the suspension may be water or the like. SiO in silica sol2The concentration can be 20-30%. The ceramic powder and the ceramic powder for preparing the ceramic sheet blank can have the same or different, preferably the same composition, and can ensure the consistency of material proportions when the ceramic powder and the ceramic powder are the same, so that the deformation and cracking of the ceramic sheet caused by stress caused by inconsistent proportions in the sintering process are avoided. In some embodiments, the ceramic powder comprises SiO2Mullite and corundum powder. Preferably, SiO is contained in the ceramic powder2The content can be 35-45%, the mullite content can be 35-45%, the corundum powder content can be 10-30%, and the total mass content of all the components is 100%. In a preferred embodiment, the ceramic powder has a particle size of < 100 mesh. The grain size range is favorable for ceramic powder to permeate into the surface layer of the ceramic sheet blank.
As shown in fig. 1, the low-temperature sintered ceramic thin plate blank is placed into a vacuum filtration device, the suspension is poured into the vacuum filtration device, vacuum pumping is performed to perform vacuum infiltration treatment, so that ceramic powder and silica sol are infiltrated into the surface layer of the ceramic thin plate blank to fill the surface pores, and redundant slurry deposited on the surface of the ceramic thin plate blank is removed to obtain the ceramic thin plate blank subjected to vacuum infiltration treatment. In the vacuum suction infiltration treatment, the vacuum degree and the suction filtration time can be selected according to the required pore structure, for example, the vacuum degree can be 10-100 Pa, and the suction filtration time can be 10-20 minutes.
Sintering the ceramic blank subjected to vacuum infiltration treatment at high temperature to obtain the light composite ceramic sheet. Wherein the high-temperature sintering temperature can be 1100-1300 ℃, and the time can be 1-2 hours. In the above embodiment, the binder is silica sol, but it should be understood that the binder in the present invention is not limited thereto, and may be aluminum sol, water glass, nano silica or alumina water-based suspension, etc. The silica sol is preferred, and is a good dispersing agent for ceramic powder due to low price, so that the cost performance is high.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below. In the following examples, unless otherwise specified, the polycrystalline mullite fiber is obtained from Zhejiang oshi romance crystal fiber Co., Ltd, and is F-1600, with a diameter of 3-5 μm and a length of 5-10 mm; the silica sol is purchased from Shandong Baite New Material Co Ltd, the model is PI2020, and SiO in the silica sol2The mass concentration of (2) is 20%. In the following examples, the density of the lightweight ceramic composite sheet was measured using the archimedes drainage method. And (4) measuring the bending strength of the light ceramic composite sheet by using a three-point bending method.
Example 1
A light ceramic composite sheet and a preparation method thereof comprise the following steps:
1) adding 100g of polycrystalline mullite fiber and 100g of silica sol into 2000ml of water, stirring and dispersing to prepare a fiber dispersion liquid;
2) mixing SiO2After ball milling and granulation are carried out on the ceramic powder with the content of 35 percent, the content of 35 percent of mullite and the content of 30 percent of corundum powder, the powder with the grain size less than 100 meshes is selected through screening. Pottery (porcelain)Adding 300g of porcelain powder into the fiber dispersion liquid, and continuously stirring in the adding process to prepare a mixed suspension;
3) vacuum filtration is adopted, the mixed suspension is poured into a vacuum filtration device, the vacuum degree is 10Pa, the filtration time is 5 minutes, and the fiber reinforced ceramic biscuit is obtained after filtration, and the thickness is controlled to be 8 mm;
4) carrying out static pressure forming on the fiber reinforced ceramic biscuit in a press, wherein the applied pressure is 5Mpa, and the thickness is 5.8 mm;
5) sintering the molded fiber reinforced ceramic biscuit at 800 ℃ for 1 hour to obtain a low-temperature sintered ceramic sheet blank with the porosity of 28%;
6) 100g of silica sol and 300g of ceramic powder (the composition of which is the same as that of the ceramic powder in the step 2) are added with 1000ml of water to prepare suspension;
7) putting the low-temperature sintered ceramic sheet blank into a vacuum filtration device (as shown in figure 1), pouring the suspension into the vacuum filtration device, wherein the vacuum degree is 10Pa, vacuumizing for 15 minutes to ensure that ceramic powder permeates into the surface of the fiber reinforced ceramic blank, filling surface pores, and removing redundant slurry deposited on the surface of the ceramic sheet blank;
8) sintering the ceramic sheet blank subjected to vacuum infiltration treatment at the high temperature of 1300 ℃ for 1 hour to obtain the light composite ceramic sheet with the thickness of 4.9 mm.
The density of the lightweight ceramic composite sheet obtained in example 1 was 1.98 g/cm3The bending strength is 98 MPa. Wherein the volume fraction of polycrystalline mullite fibers is 21%.
Example 2
A light ceramic composite sheet and a preparation method thereof comprise the following steps:
1) adding 100g of polycrystalline mullite fiber and 50g of silica sol into 1000ml of water, stirring and dispersing to prepare a fiber dispersion liquid;
2) mixing SiO2After ball milling and granulation of ceramic powder with the powder content of 45 percent, the mullite powder content of 45 percent and the corundum powder content of 10 percent, the powder with the grain size of less than 100 meshes is selected through screening. Adding 200g of ceramic powder into the fiber dispersion liquidContinuously stirring in the process to prepare mixed suspension;
3) vacuum filtration is adopted, the mixed suspension is poured into a vacuum filtration device, the vacuum degree is 100Pa, the filtration time is 10 minutes, and the fiber reinforced ceramic biscuit is obtained after filtration, and the thickness is controlled to be 5 mm;
4) carrying out static pressure forming on the fiber reinforced ceramic biscuit in a press, wherein the applied pressure is 3Mpa, and the thickness is 4.5 mm;
5) sintering the molded fiber reinforced ceramic biscuit at 600 ℃ for 1 hour to obtain a low-temperature sintered ceramic sheet blank, wherein the porosity is 35%;
6) 100g of silica sol and 200g of ceramic powder (the composition of which is the same as that of the ceramic powder in the step 2) are added with 1000ml of water to prepare suspension;
7) putting the low-temperature sintered ceramic sheet blank into a vacuum filtration device (as shown in figure 1), pouring the suspension into the vacuum filtration device, wherein the vacuum degree is 100Pa, vacuumizing for 10 minutes to ensure that ceramic powder permeates into the surface of the fiber reinforced ceramic blank, filling surface pores, and removing redundant slurry deposited on the surface of the ceramic sheet blank;
8) sintering the ceramic sheet blank subjected to vacuum infiltration treatment at the high temperature of 1100 ℃ for 1 hour to obtain the light composite ceramic sheet with the thickness of 4.5 mm.
The density of the lightweight ceramic composite sheet obtained in example 2 was 1.62 g/cm3The bending strength is 85 MPa. Wherein the volume fraction of polycrystalline mullite fibers is 28%.
Example 3
A light ceramic composite sheet and a preparation method thereof comprise the following steps:
1) adding 100g of polycrystalline mullite fiber and 40g of silica sol into 1500ml of water, stirring and dispersing to prepare a fiber dispersion liquid;
2) mixing SiO2After ball milling and granulation of ceramic powder with the powder content of 40%, the mullite powder content of 40% and the corundum powder content of 20%, screening is carried out, and powder with the particle size of less than 100 meshes is selected. Adding 500g of ceramic powder into the fiber dispersion liquid, and continuously stirring in the adding process to prepare a mixed suspension;
3) vacuum filtration is adopted, the mixed suspension is poured into a vacuum filtration device, the vacuum degree is 50Pa, the filtration time is 8 minutes, and the fiber reinforced ceramic biscuit is obtained after filtration, and the thickness is controlled to be 8 mm;
4) carrying out static pressure forming on the fiber reinforced ceramic biscuit in a press, wherein the applied pressure is 4Mpa, and the thickness is 7.2 mm;
5) sintering the molded fiber reinforced ceramic biscuit at 700 ℃ for 1 hour to obtain a low-temperature sintered ceramic sheet blank with the porosity of 32 percent;
6) 100g of silica sol and 500g of ceramic powder (the composition of which is the same as that of the ceramic powder in the step 2) are added with 2000ml of water to prepare suspension;
7) putting the low-temperature sintered ceramic sheet blank into a vacuum filtration device (as shown in figure 1), pouring the suspension into the vacuum filtration device, wherein the vacuum degree is 40Pa, vacuumizing for 20 minutes to ensure that ceramic powder permeates into the surface of the fiber reinforced ceramic blank, filling surface pores, and removing redundant slurry deposited on the surface of the ceramic sheet blank;
8) sintering the ceramic sheet blank subjected to vacuum infiltration treatment at the high temperature of 1200 ℃ for 1 hour to obtain the light composite ceramic sheet with the thickness of 7.2 mm.
The density of the lightweight ceramic composite sheet obtained in example 3 was 1.78 g/cm3The flexural strength (bending strength) was 80 MPa. Wherein the volume fraction of polycrystalline mullite fibers is 15%.
Example 4
A light ceramic composite sheet and a preparation method thereof comprise the following steps:
1) adding 100g of polycrystalline mullite fiber and 60g of silica sol into 1500ml of water, stirring and dispersing to prepare a fiber dispersion liquid;
2) mixing SiO2After ball milling and granulation of ceramic powder with the powder content of 40%, the mullite powder content of 35% and the corundum powder content of 25%, screening is carried out, and powder with the particle size of less than 100 meshes is selected. Adding 400g of ceramic powder into the fiber dispersion liquid, and continuously stirring in the adding process to prepare a mixed suspension;
3) vacuum filtration is adopted, the mixed suspension is poured into a vacuum filtration device, the vacuum degree is 40Pa, the filtration time is 6 minutes, and the fiber reinforced ceramic biscuit is obtained after filtration, and the thickness is controlled to be 7.2 mm;
4) carrying out static pressure forming on the fiber reinforced ceramic biscuit in a press, wherein the applied pressure is 3Mpa, and the thickness is 6.9 mm;
5) sintering the molded fiber reinforced ceramic biscuit at the low temperature of 750 ℃ for 1 hour to obtain a low-temperature sintered ceramic sheet blank, wherein the porosity is 27%;
6) 100g of silica sol and 400g of ceramic powder (the composition of which is the same as that of the ceramic powder in the step 2) are added with 2000ml of water to prepare suspension;
7) putting the low-temperature sintered ceramic sheet blank into a vacuum filtration device (as shown in figure 1), pouring the suspension into the vacuum filtration device, wherein the vacuum degree is 40Pa, vacuumizing for 20 minutes to ensure that ceramic powder permeates into the surface of the fiber reinforced ceramic blank, filling surface pores, and removing redundant slurry deposited on the surface of the ceramic sheet blank;
8) sintering the ceramic sheet blank subjected to vacuum infiltration treatment at the high temperature of 1200 ℃ for 1 hour to obtain the light composite ceramic sheet with the thickness of 6.9 mm.
The density of the lightweight ceramic composite sheet obtained in example 4 was 1.85 g/cm3The bending strength is 85 MPa. Wherein the volume fraction of polycrystalline mullite fibers is 19%.
FIG. 3 is an SEM image of the porous surface of the lightweight composite ceramic sheet prepared in example 2, which shows that the ceramic sheet has a porous structure and the pore size is 10-200 μm;
FIG. 4 is a SEM image of the dense surface of the lightweight composite ceramic sheet prepared in example 2, which shows that the ceramic powder permeates the surface of the fiber-reinforced ceramic blank to form a dense layer, and the pores are sealed by the secondary infiltration member;
fig. 5 is an SEM image of the reinforcing fibers inside the plate of the lightweight composite ceramic sheet prepared in example 2, and it can be seen that the polycrystalline mullite fiber junctions still maintain a large aspect ratio, the fiber surface damage is small, and the bonding between the fibers and the ceramic matrix is tight.

Claims (9)

1. The preparation method of the light ceramic composite sheet is characterized in that the light ceramic composite sheet is prepared by using polycrystalline mullite fiber as a reinforcement, silica sol as a binder and ceramic powder as a matrix, preparing a porous ceramic sheet blank by adopting vacuum infiltration-biscuit firing, filling gaps on the surface layer of the porous ceramic sheet by using secondary vacuum infiltration, and sintering at high temperature to obtain the light ceramic composite sheet with a gradient pore structure; the preparation method comprises the following steps:
(1) uniformly mixing polycrystalline mullite fiber, a binder and water to prepare a fiber dispersion liquid;
(2) adding ceramic powder into the obtained fiber dispersion liquid to prepare mixed suspension;
(3) pouring the obtained mixed suspension into a vacuum filtration device, and carrying out vacuum filtration to obtain a fiber reinforced ceramic biscuit;
(4) biscuit firing the obtained fiber reinforced ceramic biscuit at the temperature of 600-800 ℃ for 0.5-1.0 hour to obtain a ceramic sheet blank; the porosity of the obtained ceramic sheet blank is 25-40%;
(5) putting the obtained ceramic sheet blank into a vacuum filtration device, and pouring a suspension containing ceramic powder and a binder into the vacuum filtration device for vacuum infiltration treatment to obtain a vacuum infiltrated ceramic sheet blank;
(6) sintering the obtained ceramic sheet blank subjected to vacuum infiltration at the sintering temperature of 1100-1300 ℃ for 1-2 hours to obtain the lightweight ceramic composite sheet.
2. The preparation method according to claim 1, wherein in the step (1), the polycrystalline mullite fiber is used at a temperature of more than 1400 ℃, has a diameter of 3-5 μm and a length of 5-10 mm; the binder is silica sol.
3. The preparation method according to claim 1, wherein in the step (1), the mass ratio of the polycrystalline mullite fiber to the binder in the fiber dispersion is (3-1): 1, and the mass ratio of the polycrystalline mullite fiber to the water is 1: (10-20).
4. The preparation method according to claim 1, wherein in the step (2), the mass ratio of the polycrystalline mullite fiber to the ceramic powder is 1 (2-5).
5. The method according to claim 1, wherein in the step (2), the ceramic powder comprises: 35 to 45 weight percent of SiO235 to 45 weight percent of mullite and 10 to 30 weight percent of corundum powder.
6. The method according to claim 1, wherein in the step (3), the thickness of the fiber-reinforced ceramic green body is 5 to 8 mm.
7. The production method according to claim 1, wherein in the step (4), the obtained fiber-reinforced ceramic greenbody is subjected to static pressure forming in a press at a pressure of 3 to 5MPa before bisque firing.
8. The preparation method according to claim 1, wherein in the step (5), the mass ratio of the binder to the ceramic powder in the suspension containing the ceramic powder and the binder is 1 (2-5); the binder is silica sol; the ceramic powder comprises: 35 to 45 weight percent of SiO235 to 45 weight percent of mullite and 10 to 30 weight percent of corundum powder.
9. The preparation method according to claim 1, wherein in the step (3), the vacuum degree of the vacuum filtration is 10-100 Pa, and the filtration time is 5-10 minutes; in the step (5), the vacuum degree of the vacuum suction and infiltration treatment is 10-100 Pa, and the suction filtration time is 10-20 minutes.
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