CN113880563B - High-temperature creep-resistant ceramic material and preparation method thereof - Google Patents
High-temperature creep-resistant ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of a high-temperature creep-resistant ceramic material, which comprises the following steps: s1, weighing 50-90 parts by weight of high-purity alpha-Al 2 O 3 Powder, 25-50 parts of plate-shaped corundum powder, 1-3 parts of zirconia powder and 0.5-1 part of sintering aid, water is used as a solvent, a water-soluble dispersant is added, and slurry is obtained through ball milling; s2, removing bubbles of the slurry in vacuum, adding a catalyst and an initiator, stirring uniformly, injecting into a mold for curing, and demolding to obtain a blank; s3, drying the blank, softening, cutting into blank sheets and drying; and S4, sintering the dried blank sheet to obtain the ceramic material. The powder bulk density of the raw material components in different parts by weight is high, and the prepared ceramic material is a high-density material with high density and high hardness; through the mutual matching and distribution of the raw material components, the bridge support of the plate-shaped corundum in the material system, and the alpha-Al 2 O 3 And the combined action of phase change toughening of the zirconium oxide at a high temperature stage, so that the high-temperature creep resistance, the rupture strength and the erosion resistance of the prepared ceramic material are improved, the ceramic material is not easy to break and has long service life.
Description
Technical Field
The invention relates to the technical field of high-temperature ceramic materials, in particular to a high-temperature creep-resistant ceramic material and a preparation method thereof.
Background
In recent decades, high temperature technology has been rapidly developed, and the demand of metallurgy, chemical engineering, power, mechanical manufacturing, glass fiber and other industrial manufacturing for high temperature creep-resistant ceramic materials has increased dramatically, and the high temperature creep-resistant ceramic materials gradually occupy an important position. With the popularization and application of the new glass fiber technology, large, continuous and high-efficiency advanced equipment is gradually put into production, and the advanced equipment enables the working conditions of the high-temperature creep-resistant ceramic material to be worsened, so that the requirements on the mechanical strength, the erosion resistance, the high-temperature creep resistance and other properties of the ceramic material at high temperature in actual industrial production are higher. However, the existing ceramic products independently developed in China generally have the problems of poor high-temperature creep resistance, short service life, poor erosion resistance and the like, and the ceramic products are easy to crack and bend after being subjected to cold and thermal shock continuously in the use process, so that the existing ceramic products independently developed in China cannot meet the practical application of high-temperature industrial manufacturing of glass fibers and the like. In order to meet the application of some glass fiber industries, the glass fiber industry only depends on a large number of imports, and the development of China in the glass fiber industry is greatly restricted. Therefore, the ceramic material product with the characteristics of good high-temperature creep resistance, good erosion resistance, clean and fine appearance and the like is provided, and the ceramic material product has important significance for the glass fiber industry.
Disclosure of Invention
The invention provides a high-temperature creep-resistant ceramic material and a preparation method thereof, and aims to solve the problems of poor high-temperature creep resistance, poor erosion resistance, easy fracture, short service life and the like of the ceramic material prepared by the prior art.
In one aspect, the invention provides a method for preparing a high-temperature creep-resistant ceramic material, comprising the following steps: s1, weighing 50-90 parts by weight of high-purity alpha-Al 2 O 3 Powder, 25-50 parts of plate-shaped corundum powder, 1-3 parts of zirconia powder and 0.5-1 part of sintering aid, taking water as a solvent, adding a water-soluble dispersant, and performing ball milling for 15-24 hours to obtain ceramic slurry; s2, removing bubbles of the ceramic slurry in vacuum, adding a catalyst and an initiator, uniformly stirring, injecting into a mold for curing, and demolding to obtain a ceramic blank; s3, drying the ceramic blank, softening the dried ceramic blank, cutting the ceramic blank into blank sheets and drying the blank sheets; and S4, sintering the blank sheet processed in the step S3 to obtain the high-temperature creep-resistant ceramic material.
Compared with the prior art, the invention has the following beneficial effects: the ceramic slurry prepared by the invention comprises 50-90 parts of high-purity alpha-Al 2 O 3 Powder, 25-50 parts of tabular corundum powder, 1-3 parts of zirconia powder and 0.5-1 part of sintering aid, and the ceramic slurry has high solid phase content, good fluidity and uniform suspension property; the raw material components with different weight parts are uniformly mixed after the ball milling process of ball milling for 15-24h, all the powder is uniformly distributed, the powder has high bulk density, and the ceramic material obtained after curing, forming, drying, softening, drying and sintering is a high-density ceramic material with high density and high hardness, so that the ceramic material is favorable for obtaining high-temperature creep resistance; the invention designs the mutual matching of the raw material components with different weight parts, the distribution state of the raw material components, the bridge supporting effect of the plate-shaped corundum in a material system, and the high-purity alpha-Al 2 O 3 And the high-temperature creep resistance of the ceramic material prepared by taking the ceramic slurry prepared by the invention as the main raw material is improved under the combined action of a phase change toughening mechanism of zirconium oxide at a high temperature stage, so that the ceramic material is favorable for application in the high-temperature technical field (particularly the high-temperature technical field with the temperature of 1400-1600 ℃) such as glass fiber and the like, and the high-temperature creep resistance ensures that the ceramic material prepared by the invention can bear the gravity at a high temperature state and can be used as a load-bearing material in the high-temperature technical field. Tests prove that when the span of the ceramic material prepared by the method is 150mm, 0.76kg of load is applied to the ceramic material under the condition of 1400 ℃ (heat preservation for 40 h), and the ratio of the bending deformation of the ceramic material to the length of the ceramic material is less than 0.04; the normal-temperature rupture strength is improved to more than 450MPa from 250MPa, the erosion resistance is greatly improved, the fracture is not easy to occur, the service life is long, and the appearance is clean and fine; according to the invention, 0.5-1 part of sintering aid is introduced, so that the sintering temperature of the material system is reduced, the sintering range is widened, on one hand, the energy consumption is reduced, on the other hand, the controllability of sintering shrinkage is good, and the low-deformation sintering of the ceramic material of the system is realized.
In the present invention, the term "high purity alpha-Al 2 O 3 Powder "means alpha-Al 2 O 3 alpha-Al of not less than 99.5 percent by mass 2 O 3 And (3) pulverizing.
In some embodiments of the invention, the high purity alpha-Al is present in parts by weight 2 O 3 The powder comprises 30-50 parts of high-purity alpha-Al with the average grain diameter of 0.5-1.0 mu m 2 O 3 And 20-40 parts of high-purity alpha-Al with the average particle size of 3-5 mu m 2 O 3 。
The beneficial effect of adopting the further technical scheme is that the high-purity alpha-Al prepared by the preparation method of the invention 2 O 3 The powder comprises 30-50 parts of high-purity alpha-Al with the average grain diameter of 0.5-1.0 mu m 2 O 3 And 20-40 parts of high-purity alpha-Al with the average grain diameter of 3-5 mu m 2 O 3 The invention adopts high-purity alpha-Al with different particle sizes 2 O 3 Carrying out raw material grading and simultaneously carrying out high-purity alpha-Al of each granularity 2 O 3 The components in the ceramic slurry are mixed more compactly by designing the weight parts, so that the bulk density of powder in the ceramic material is further improved, and the high-density ceramic material with high density and high hardness is obtained.
In some embodiments of the present invention, the plate-shaped corundum powder includes, in parts by weight, 10 to 20 parts of plate-shaped corundum powder having an average particle size of 150 to 180 μm and 15 to 30 parts of plate-shaped corundum powder having an average particle size of 45 to 75 μm.
The plate-shaped corundum powder prepared by the preparation method disclosed by the invention comprises 10-20 parts of plate-shaped corundum powder with the average particle size of 150-180 micrometers and 15-30 parts of plate-shaped corundum powder with the average particle size of 45-75 micrometers, the plate-shaped corundum powder with different particle sizes is adopted for raw material grading, and meanwhile, the weight parts of the plate-shaped corundum powder with different particle sizes are designed, so that on one hand, the bridge supporting effect of the plate-shaped corundum powder in a material system is improved, the high-temperature creep resistance of the prepared ceramic material is further enhanced, on the other hand, all components in the ceramic slurry are mixed more compactly, the stacking density of powder in the ceramic material can be further improved, and the high-density and high-hardness high-density ceramic material is obtained. In addition, high-purity alpha-Al is mixed 2 O 3 The raw material grading of different particle sizes and the corresponding weight parts of the powder enable the components in the ceramic slurry to be mixed and further compacted, so that the powder bulk density of the ceramic slurry system prepared by the invention is greatly improved, and the ceramic material with higher density and higher hardness and higher compactness can be finally obtained.
In some embodiments of the invention, the sintering aid comprises one or more of yttria, magnesia, and lanthana.
The further technical scheme has the beneficial effect that the sintering aid prepared by the preparation method disclosed by the invention comprises one or more of yttrium oxide, magnesium oxide and lanthanum oxide. The invention combines the whole material system, selects the sintering aid as one or more of yttrium oxide, magnesium oxide and lanthanum oxide through the selection of the sintering aid, can reduce the sintering temperature of the material system and broaden the sintering range, on one hand, reduces the energy consumption, on the other hand, has good controllability of sintering contractibility, and realizes the low-deformation sintering of the ceramic material of the system.
In some embodiments of the present invention, the sintering aid comprises 0.3-0.5 parts by weight of yttrium oxide, 0.1-0.3 parts by weight of magnesium oxide, and 0.1-0.2 parts by weight of lanthanum oxide.
The further technical scheme has the beneficial effects that the sintering aid prepared by the preparation method comprises 0.3-0.5 part of yttrium oxide, 0.1-0.3 part of magnesium oxide and 0.1-0.2 part of lanthanum oxide. The invention adjusts the proportion of each sintering aid based on the whole material system, and the sintering aids are selected to comprise 0.3-0.5 part of yttrium oxide, 0.1-0.3 part of magnesium oxide and 0.1-0.2 part of lanthanum oxide, thereby further reducing the sintering temperature of the material system, widening the sintering range, reducing the energy consumption on one hand, having good controllability of sintering shrinkage on the other hand, and realizing the low-deformation sintering of the ceramic material of the system.
In some embodiments of the invention, the water soluble dispersant comprises one or more of ammonium polyacrylate, ammonium citrate, polyvinyl carboxylic acid.
The further technical scheme has the beneficial effects that the dispersant selected by the invention is water-soluble, and is selected from one or more of ammonium polyacrylate, ammonium citrate and polyvinyl carboxylic acid by combining with a ceramic slurry system, so that the prepared ceramic slurry has better fluidity and more uniform suspension property, good prerequisite conditions are provided for the subsequent preparation of ceramic materials, and the problems of uneven density, defect generation and the like of the prepared ceramic materials are prevented.
In some embodiments of the present invention, the pH of the ceramic slurry prepared in step S1 is 8 to 10.
The further technical scheme has the beneficial effects that the pH value of the ceramic slurry is mainly controlled by the water-soluble dispersing agent, the pH value of the ceramic slurry prepared by the method is 8-10, the ceramic slurry is alkalescent, the dispersing effect of the ceramic slurry is optimal, and the fluidity is best.
In some embodiments of the invention, the catalyst is tetramethylethylenediamine and the initiator is ammonium persulfate.
The ceramic slurry is prepared by using a water-soluble dispersant, a catalyst used in curing and forming is tetramethylethylenediamine, and an initiator is ammonium persulfate, namely, the ceramic slurry is formed by using water-based gel, does not use an organic solvent, can be directly sintered at high temperature without degreasing, and is energy-saving and environment-friendly.
In some embodiments of the present invention, the specific process of injecting the uniformly stirred slurry into the mold in the step S2 is: and applying pressure to the uniformly stirred slurry to control the slurry to be injected into the mold from a slurry injection port at the bottom of the mold, so that the slurry flows to fill the mold from bottom to top in the mold.
The preparation method has the advantages that the slurry which is uniformly stirred is injected into the die from bottom to top, the slurry is firstly injected into the bottom of the die, the slurry injected into the bottom of the die is pushed by the slurry injected subsequently to move from the bottom of the die to the top of the die, the problems of large density difference and large forming defect of a blank body obtained after solidification and forming due to the fact that materials with high specific gravity in the slurry are deposited at the bottom of the die are solved, net size forming of a product can be achieved, blank body defects caused in the forming process are avoided, and finally prepared ceramic materials are small in density difference, uniform in density and small in product defects.
In some embodiments of the present invention, in the step S2, after the uniformly stirred slurry is injected into the mold, the mold is removed after curing for 30 to 45min at a temperature of 25 ℃ to 40 ℃ and a humidity of 40 to 70%.
The further technical scheme has the beneficial effects that the technological parameters of curing and forming are researched based on the design of the ceramic slurry and the design of the injection molding mode, the curing condition is designed to be cured for 30-45min under the conditions that the temperature is 25-40 ℃ and the humidity is 40-70%, the density of a product obtained by demolding is higher, and the improvement of the high-temperature creep resistance is facilitated.
In some embodiments of the invention, in the step S4, before sintering, the green sheet processed in the step S3 is heated to 650-800 ℃ at a speed of 20-30 ℃/h, and is kept at the temperature for 5-10h to perform plastic removal treatment; heating the blank sheet after plastic removal treatment to 1540-1600 ℃ at the speed of 120-180 ℃/h, and preserving heat for 2-6h for sintering.
The method has the advantages that the temperature is raised to 650-800 ℃ at a speed of 20-30 ℃/h before sintering, the temperature is kept for 5-10h, the plastic removing treatment is completed, the temperature is raised to 1540-1600 ℃ at a speed of 120-180 ℃/h after plastic removing, the temperature is kept for 2-6h, and sintering is completed. The plastic-removing parameters and the sintering parameters are designed in a mode of firstly removing plastic and then sintering, and the finally obtained ceramic material has high density; the high-temperature creep resistance and erosion resistance are good, the high-temperature creep resistance and erosion resistance can bear the gravity at a high temperature, and the high-temperature creep resistance and erosion resistance can be used as a bearing material in the high-temperature technical field; difficult fracture, long service life and clean and fine appearance.
In another aspect, the present invention also provides a high temperature creep-resistant ceramic material prepared according to the method of any one of the above.
Compared with the prior art, the invention has the following beneficial effects: the high-temperature creep-resistant ceramic material is prepared by the preparation method of the high-temperature creep-resistant ceramic material, and the obtained ceramic material is a high-density ceramic material with high density and high hardness; the high-temperature creep resistance, mechanical strength and rupture strength are high, the erosion resistance is improved, the high-temperature creep resistance can bear the gravity at a high temperature, and the high-temperature creep resistance can be used as a bearing material in the high-temperature technical field; not easy to break, long service life and clean and fine appearance.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following detailed description of various aspects of the present invention is provided with specific examples, which are only used for illustrating the present invention and do not limit the scope and spirit of the present invention.
The invention provides a preparation method of a high-temperature creep-resistant ceramic material, which comprises the following steps:
s1, weighing 50-90 parts by weight of high-purity alpha-Al 2 O 3 Putting the powder, 25-50 parts of tabular corundum powder, 1-3 parts of zirconia powder and 0.5-1 part of sintering aid into a ball mill, adding a water-soluble dispersant by taking water as a solvent, grinding and mixing, and setting the ball milling time to be 15-24h to obtain ceramic slurry with high solid content, good fluidity and uniform suspension property; the ceramic slurry preferably has a weak alkaline pH, for example, a pH of 8 to 10.
S2, screening the ceramic slurry obtained in the S1, removing bubbles in vacuum, filling the ceramic slurry into a ceramic slurry barrel, adding a catalyst and an initiator, stirring uniformly, injecting the uniformly stirred slurry into a mold, curing, and demolding to obtain a ceramic blank;
s3, drying the ceramic blank obtained in the S2, softening the dried ceramic blank, cutting the ceramic blank into blank sheets, and naturally drying the blank sheets;
and S4, sintering the blank sheet processed in the step S3 to obtain the high-temperature creep-resistant ceramic material.
In the invention, the high-purity alpha-Al is calculated by weight parts 2 O 3 The powder comprises 30-50 parts of high-purity alpha-Al with the average grain diameter of 0.5-1.0 mu m 2 O 3 And 20-40 parts of high-purity alpha-Al with the average grain diameter of 3-5 mu m 2 O 3 。
In the present invention, the plate-shaped corundum powder includes, in parts by weight, 10 to 20 parts of plate-shaped corundum powder having an average particle size of 150 to 180 μm and 15 to 30 parts of plate-shaped corundum powder having an average particle size of 45 to 75 μm.
In the present invention, the sintering aid includes one or more of yttrium oxide, magnesium oxide, and lanthanum oxide. Preferably, in the present invention, the sintering aid comprises, by weight, 0.3 to 0.5 parts of yttrium oxide, 0.1 to 0.3 parts of magnesium oxide, and 0.1 to 0.2 parts of lanthanum oxide.
In the present invention, the water-soluble dispersant includes one or more of ammonium polyacrylate, ammonium citrate, polyvinyl carboxylic acid.
In the invention, the catalyst is tetramethyl ethylene diamine, and the initiator is ammonium persulfate.
In the invention, the concrete process of injecting the uniformly stirred slurry into the mold in the step S2 is as follows: and applying pressure to the uniformly stirred slurry to control the slurry to be injected into the mold from a slurry injection port at the bottom of the mold, so that the slurry flows in the mold from bottom to top until the mold is filled.
In the invention, in the step S2, after the evenly stirred slurry is injected into a mould, the mould is demoulded after being solidified for 30-45min under the conditions that the temperature is 25-40 ℃ and the humidity is 40-70%.
In the invention, in the step S4, before sintering, the blank sheet processed in the step S3 is heated to 650-800 ℃ at the speed of 20-30 ℃/h, and is kept warm for 5-10h to carry out plastic removal treatment; heating the blank sheet after plastic removal treatment to 1540-1600 ℃ at the speed of 120-180 ℃/h, and preserving heat for 2-6h for sintering.
The invention also provides a high-temperature creep-resistant ceramic material, which is prepared according to the preparation method of the invention.
Example 1:
the embodiment provides a preparation method of a high-temperature creep-resistant ceramic material, which comprises the following steps:
s1, weighing 50 parts by weight of high-purity alpha-Al 2 O 3 Putting the powder, 48.5 parts of tabular corundum powder, 1 part of zirconia powder and 0.5 part of sintering aid into a ball mill, adding a water-soluble dispersant into water serving as a solvent, and grinding and mixing for 15 hours to obtain ceramic slurry with high solid content, good fluidity and uniform suspension; the ceramic slurry preferably has a weak alkaline pH, for example, a pH of 8.
S2, screening the ceramic slurry obtained in the S1, removing bubbles in vacuum, filling the ceramic slurry into a ceramic slurry barrel, adding a catalyst and an initiator, stirring uniformly, injecting the uniformly stirred slurry into a mold, curing, and demolding to obtain a ceramic blank;
s3, drying the ceramic blank obtained in the S2, softening the dried ceramic blank, cutting the ceramic blank into blank sheets, and naturally drying the blank sheets;
and S4, sintering the blank sheet processed in the step S3 to obtain the high-temperature creep-resistant ceramic material.
In this example, high purity α -Al is present in parts by weight 2 O 3 The powder comprises 30 parts of high-purity alpha-Al with the average grain diameter of 0.5-1.0 mu m 2 O 3 And 20 parts of high-purity alpha-Al with the average grain diameter of 3-5 mu m 2 O 3 。
In this example, the plate-shaped corundum powder includes 20 parts by weight of plate-shaped corundum powder having an average particle size of 150 to 180 μm and 28.5 parts by weight of plate-shaped corundum powder having an average particle size of 45 to 75 μm.
In this example, the sintering aid was yttria.
In this embodiment, the water-soluble dispersant includes one or more of ammonium polyacrylate, ammonium citrate, polyvinyl carboxylic acid.
In this example, the catalyst was tetramethylethylenediamine and the initiator was ammonium persulfate.
In this embodiment, the specific process of injecting the uniformly stirred slurry into the mold in the step S2 is as follows: and applying pressure to the uniformly stirred slurry to control the slurry to be injected into the mold from a slurry injection port at the bottom of the mold, so that the slurry flows in the mold from bottom to top until the mold is filled.
In this example, in the step S2, the slurry stirred uniformly was poured into a mold, and then cured at 25 ℃ and 40% humidity for 30min, followed by demolding.
In the embodiment, in the step S4, before sintering, the green sheet processed in the step S3 is heated to 650 ℃ at a speed of 20 ℃/h, and is kept warm for 10h to perform plastic removal processing; and heating the blank sheet subjected to the plastic removal treatment to 1540 ℃ at the speed of 120 ℃/h, and preserving heat for 2h for sintering.
The present example also provides a high temperature creep resistant ceramic material prepared according to the method of preparation of the present example.
Example 2:
the embodiment provides a preparation method of a high-temperature creep-resistant ceramic material, which comprises the following steps:
s1, weighing 65 parts by weight of high-purity alpha-Al 2 O 3 Putting the powder, 33.5 parts of tabular corundum powder, 1.5 parts of zirconia powder and 0.65 part of sintering aid into a ball mill, adding a water-soluble dispersant by taking water as a solvent, and grinding and mixing, wherein the ball milling time is set to be 18 hours, so that ceramic slurry with high solid content, good fluidity and uniform suspension is obtained; the ceramic slurry preferably has a weak alkaline pH, for example, a pH of 9.
S2, screening the ceramic slurry obtained in the S1, removing bubbles in vacuum, filling the ceramic slurry into a ceramic slurry barrel, adding a catalyst and an initiator, stirring uniformly, injecting the uniformly stirred slurry into a mold, curing, and demolding to obtain a ceramic blank;
s3, drying the ceramic blank obtained in the S2, softening the dried ceramic blank, cutting the ceramic blank into blank sheets, and naturally drying the blank sheets;
and S4, sintering the blank sheet processed in the step S3 to obtain the high-temperature creep-resistant ceramic material.
In this example, high purity α -Al is present in parts by weight 2 O 3 The powder comprises 40 parts of high-purity alpha-Al with the average grain diameter of 0.5-1.0 mu m 2 O 3 And 25 parts of high-purity alpha-Al with the average grain diameter of 3-5 mu m 2 O 3 。
In this example, the plate-shaped corundum powder includes 13.5 parts by weight of plate-shaped corundum powder having an average particle size of 150 to 180 μm and 20 parts by weight of plate-shaped corundum powder having an average particle size of 45 to 75 μm.
In this embodiment, the sintering aid includes yttrium oxide and magnesium oxide. The sintering aid comprises 0.4 part of yttrium oxide and 0.25 part of magnesium oxide in parts by weight.
In this embodiment, the water-soluble dispersant includes one or more of ammonium polyacrylate, ammonium citrate, polyvinyl carboxylic acid.
In this example, the catalyst was tetramethylethylenediamine and the initiator was ammonium persulfate.
In this embodiment, the specific process of injecting the uniformly stirred slurry into the mold in the step S2 is as follows: and applying pressure to the uniformly stirred slurry to control the slurry to be injected into the mold from a slurry injection port at the bottom of the mold, so that the slurry flows to fill the mold from bottom to top in the mold.
In this example, in step S2, the slurry stirred uniformly was poured into a mold, and then cured at 35 ℃ and 50% humidity for 40min, followed by demolding.
In the embodiment, in the step S4, before sintering, the blank sheet processed in the step S3 is heated to 750 ℃ at the speed of 25 ℃/h, and is subjected to heat preservation for 8h to perform plastic removal treatment; and heating the blank sheet subjected to the plastic removal treatment to 1560 ℃ at the speed of 160 ℃/h, and preserving heat for 5h to sinter.
The present example also provides a high temperature creep resistant ceramic material prepared according to the method of preparation of the present example.
Example 3:
the embodiment provides a preparation method of a high-temperature creep-resistant ceramic material, which comprises the following steps:
s1, weighing 71 parts by weight of high-purity alpha-Al 2 O 3 Putting the powder, 25 parts of tabular corundum powder, 3 parts of zirconia powder and 1 part of sintering aid into a ball mill, adding a water-soluble dispersant into water serving as a solvent, grinding and mixing, and setting the ball milling time to be 24 hours to obtain ceramic slurry with high solid content, good fluidity and uniform suspension; the ceramic slurry preferably has a weak alkaline pH, for example, a pH of 10.
S2, screening the ceramic slurry obtained in the S1, removing bubbles in vacuum, filling the ceramic slurry into a ceramic slurry barrel, adding a catalyst and an initiator, stirring uniformly, injecting the uniformly stirred slurry into a mold, curing, and demolding to obtain a ceramic blank;
s3, drying the ceramic blank obtained in the S2, softening the dried ceramic blank, cutting the ceramic blank into blank sheets, and naturally drying the blank sheets;
and S4, sintering the blank sheet processed in the step S3 to obtain the high-temperature creep-resistant ceramic material.
In this example, high purity α -Al is present in parts by weight 2 O 3 The powder comprises 50 parts of high-purity alpha-Al with the average grain diameter of 0.5-1.0 mu m 2 O 3 And 21 parts of high-purity alpha-Al with the average grain diameter of 3-5 mu m 2 O 3 。
In this example, the plate-like corundum powder includes, in parts by weight, 10 parts of plate-like corundum powder having an average particle size of 150 to 180 μm and 15 parts of plate-like corundum powder having an average particle size of 45 to 75 μm.
In this embodiment, the sintering aid includes yttrium oxide, magnesium oxide, and lanthanum oxide. The sintering aid comprises, by weight, 0.5 part of yttrium oxide, 0.3 part of magnesium oxide and 0.2 part of lanthanum oxide.
In this embodiment, the water-soluble dispersant includes one or more of ammonium polyacrylate, ammonium citrate, polyvinyl carboxylic acid.
In this example, the catalyst was tetramethylethylenediamine and the initiator was ammonium persulfate.
In this embodiment, the specific process of injecting the uniformly stirred slurry into the mold in the step S2 is as follows: and applying pressure to the uniformly stirred slurry to control the slurry to be injected into the mold from a slurry injection port at the bottom of the mold, so that the slurry flows in the mold from bottom to top until the mold is filled.
In this example, in the step S2, the slurry stirred uniformly was poured into a mold, and then cured at 40 ℃ and 70% humidity for 45min, followed by demolding.
In the embodiment, in the step S4, before sintering, the blank sheet processed in the step S3 is heated to 800 ℃ at the speed of 30 ℃/h and is kept for 5h to carry out plastic removal processing; and heating the blank sheet subjected to the plastic removal treatment to 1600 ℃ at the speed of 180 ℃/h, and preserving heat for 6h to sinter.
The present example also provides a high temperature creep resistant ceramic material prepared according to the method of preparation of the present example.
The high-temperature creep-resistant ceramic materials prepared by the preparation methods of examples 1 to 3 and the conventional ceramic materials (hereinafter referred to as conventional materials) used in the high-temperature technical field such as glass fiber and the like are tested for high-temperature creep resistance, breaking strength, erosion resistance, surface appearance and the like. Specifically, the ceramic material prepared in examples 1 to 3 and the existing material were lapped on two pillars having a distance of 150mm (i.e., span of 150 mm) at both ends thereof, respectively, and heat-preserved at 1400 ℃ for 40 hours, and 0.76kg of load was applied to the ceramic material prepared in examples 1 to 3 and the existing material, respectively, and the ratio of the bending deformation of each material to the length of each material was measured to reflect the high-temperature creep resistance; the ceramic materials prepared in the embodiments 1-3 and the existing materials are subjected to flexural strength detection through a three-point bending test in GB/T6569-2006 'Fine ceramic flexural strength test method'; the erosion resistance test was carried out by observing the erosion situation after the ceramic materials prepared in examples 1 to 3 and the existing materials were placed in the same erosion environment for the same number of days; in addition, the surface appearance of the ceramic materials prepared in examples 1 to 3 and the conventional materials was observed. Specific results are shown in table 1:
TABLE 1
As can be seen from Table 1, when the span of the ceramic materials prepared in examples 1-3 is 150mm, and a load of 0.76kg is applied to the ceramic materials under the condition of heat preservation at 1400 ℃ for 40h, the ratios of the bending deformation of the ceramic materials to the length of the ceramic materials are both less than 0.04, while the existing materials are 0.08-0.20, i.e. the high-temperature creep resistance of the ceramic materials prepared in examples 1-3 is obviously higher than that of the existing materials; the breaking strength and the erosion resistance of the ceramic materials prepared in the examples 1 to 3 are obviously superior to those of the existing materials; the ceramic materials prepared in examples 1 to 3 are cleaner and finer in appearance, and more beautiful than the existing materials.
The present invention has been described in conjunction with specific embodiments which are intended to be exemplary only and are not intended to limit the scope of the invention, which is to be given the full breadth of the appended claims and any and all modifications, variations or alterations that may occur to those skilled in the art without departing from the spirit of the invention. Therefore, various equivalent changes made according to the present invention still fall within the scope covered by the present invention.
Claims (9)
1. The preparation method of the high-temperature creep-resistant ceramic material is characterized by comprising the following steps:
s1, weighing 50-90 parts by weight of high-purity alpha-Al 2 O 3 Powder, 25-50 parts of plate-shaped corundum powder, 1-3 parts of zirconia powder and 0.5-1 part of sintering aid, water is used as a solvent, a water-soluble dispersant is added, and ball milling is carried out for 15-24 hours to obtain ceramic slurry;
s2, removing bubbles of the ceramic slurry in vacuum, adding a catalyst and an initiator, uniformly stirring, injecting into a mold for curing, and demolding to obtain a ceramic blank;
s3, drying the ceramic body, softening the dried ceramic body, cutting into blank sheets and drying;
s4, sintering the blank sheet processed in the step S3 to obtain the high-temperature creep-resistant ceramic material;
in the step S4, before sintering, the blank sheet processed in the step S3 is heated to 650-800 ℃ at the speed of 20-30 ℃/h, and is subjected to heat preservation for 5-10h to carry out plastic removal treatment; heating the blank sheet after plastic removal treatment to 1540-1600 ℃ at the speed of 120-180 ℃/h, and preserving heat for 2-6h for sintering.
2. The method of claim 1, wherein the high purity α -Al is present in parts by weight 2 O 3 The powder comprises 30-50 parts of high-purity alpha-Al with the average grain diameter of 0.5-1.0 mu m 2 O 3 And 20-40 parts of high-purity alpha-Al with the average grain diameter of 3-5 mu m 2 O 3 。
3. The method according to claim 1, wherein the plate-shaped corundum powder comprises, in parts by weight, 10 to 20 parts of plate-shaped corundum powder having an average particle size of 150 to 180 μm and 15 to 30 parts of plate-shaped corundum powder having an average particle size of 45 to 75 μm.
4. The method of claim 1, wherein the sintering aid comprises one or more of yttria, magnesia, and lanthana.
5. The method of claim 4, wherein the sintering aid comprises, in parts by weight, 0.3 to 0.5 parts yttrium oxide, 0.1 to 0.3 parts magnesium oxide, and 0.1 to 0.2 parts lanthanum oxide.
6. The method of claim 1, wherein the water soluble dispersant comprises one or more of ammonium polyacrylate, ammonium citrate, polyvinyl carboxylic acid.
7. The method of claim 1, wherein the step S2 of injecting the uniformly stirred slurry into the mold comprises the following specific steps: and applying pressure to the uniformly stirred slurry to control the slurry to be injected into the mold from a slurry injection port at the bottom of the mold, so that the slurry flows in the mold from bottom to top until the mold is filled.
8. The method of claim 7, wherein in the step S2, the uniformly stirred slurry is injected into a mold, cured at a temperature of 25 ℃ to 40 ℃ and a humidity of 40% to 70% for 30 to 45min, and then demolded.
9. A high temperature creep-resistant ceramic material, characterized in that it is produced according to the method of any of claims 1 to 8.
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