CN114436632A - High-temperature thermal shock resistant ceramic material and preparation method thereof - Google Patents
High-temperature thermal shock resistant ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-temperature thermal shock resistant ceramic material, which comprises the following steps: mixing ceramic powder with an organic binder to obtain a ceramic feed; forming the ceramic feed, removing the glue and sintering to obtain the ceramic material; wherein the ceramic powder comprises the following components in parts by weight: 31-53 parts of fused quartz, 25-45 parts of tabular corundum powder, 20-35 parts of alumina micro powder and 0.5-1.5 parts of silicon nitride micro powder. The ceramic material prepared by the method has good high-temperature thermal shock resistance.
Description
Technical Field
The invention belongs to the field of ceramic materials, and particularly relates to a high-temperature thermal shock resistant ceramic material and a preparation method thereof.
Background
The aerospace development has higher and higher requirements on the smelting industry, such as smelting refractory metals, preparing special alloys or ultra-pure metals and the like, and smelting appliances are required to be continuously subjected to cold and thermal shock and slag corrosion of smelting materials in the using process.
As one of the common materials of smelting appliances, ceramic materials are required to have good thermal shock stability, erosion resistance and spalling resistance. However, the ceramic material produced at present has poor high-temperature thermal shock resistance, short service life and poor erosion resistance, is difficult to meet the requirements, and greatly restricts the development of the research on the aviation material in China.
Disclosure of Invention
Aiming at the problems, the invention provides a high-temperature thermal shock resistant ceramic material and a preparation method thereof, and aims to solve the problems of poor high-temperature thermal shock resistance, poor erosion resistance, easiness in cracking and stripping, short service life and the like of the ceramic material prepared by the prior art.
The invention provides a preparation method of a high-temperature thermal shock resistant ceramic material, which comprises the following steps: mixing ceramic powder with an organic binder to obtain a ceramic feed; forming the ceramic feed, removing the glue and sintering to obtain the ceramic material; wherein, according to the weight portion, the ceramic powder comprises: 31-53 parts of fused quartz, 25-45 parts of tabular corundum powder, 20-35 parts of alumina micro powder and 0.5-1.5 parts of silicon nitride micro powder.
Compared with the prior art, the technical scheme has the following beneficial effects: according to the technical scheme, silicon nitride is introduced as a reaction auxiliary agent, and is sintered in an air atmosphere to form free silicon dioxide, so that the internal structure of a product is filled, the frame shape of the product is changed, the conversion degree of a synthetic ceramic crystal phase can be improved, the crystal phase synthesis temperature is reduced, and the strength of a ceramic matrix is improved.
In the synthesis process, along with temperature change and different acting forces among molecules, fused quartz reacts with alumina, tabular corundum and silicon nitride to generate a mixed crystal phase, the mixed crystal phase has a single-substance crystal phase and a mullite crystal phase, the reaction degree of the fused quartz with the alumina and the tabular corundum powder is different at different temperatures, and different crystal phases can be formed, and the mixed crystal phase is beneficial to improving the resistance of the material to different temperatures.
Preferably, the organic binder comprises organic glass, polystyrene, high-density polyethylene, microcrystalline wax powder and a dispersing agent in a weight ratio of (35-50) to (10-20) to (10-15) to (3-10). The organic binder has strong coating capability, is beneficial to improving the loading capacity of ceramic powder, has high strength of a formed blank body, and is easy to remove glue and sinter.
Preferably, the dispersing agent is one or more of stearic acid, oleic acid and carboxyl stearic acid, has a good dispersing effect, and is helpful for removing organic binders in the sintering process.
Preferably, in the plate-shaped corundum powder, the weight ratio of the plate-shaped corundum powder with the particle size of 0.18-0.1 mm to the plate-shaped corundum powder with the particle size of 0.045mm is (10-20): (15-25). Corundum of different particle sizes, different specific surface areas, and different combinations with fused silica reaction at the same temperature.
Preferably, the fused quartz comprises a first fused quartz, a second fused quartz, a third fused quartz and a fourth fused quartz in a weight ratio of (10-18): (15-20): (5-10): (1-5), wherein the particle size of the first fused quartz is 0.27-0.18 mm, the particle size of the second fused quartz is 0.15-0.1 mm, the particle size of the third fused quartz is smaller than 0.1mm and not smaller than 0.075mm, and the particle size of the fourth fused quartz is smaller than 0.045 mm. The fused quartz with different grain sizes is selected to form staggered tension of the product.
Preferably, the molding is injection molding, the injection pressure is 20-80 MPa, and the injection temperature is 120-180 ℃. By adopting the molding method of the preferred scheme, namely high-pressure injection molding, the manufactured product has high precision, the near-net-size molding of the product can be realized without any processing, the traditional ceramic injection process can only realize the product with the weight of less than 400 g and the wall thickness of less than 5mm, and the process provided by the invention realizes the batch production of the product with the weight of more than 2000 g, the height of more than 240 mm and the wall thickness of more than 10 mm.
Preferably, the rubber discharging comprises the steps of heating the ceramic feed at the speed of 10-20 ℃/h to 450-550 ℃ after the ceramic feed is formed, and preserving the heat for 5-7 h.
Preferably, the sintering comprises: the sintering comprises the following steps: and after the ceramic feed is molded and the rubber is discharged, heating to 1150-1320 ℃ at the speed of 120-180 ℃/h, and preserving heat for 2-6 h.
Preferably, the ceramic powder and the organic binder are mixed according to the weight ratio of 1: 0.1-0.2 to obtain the ceramic feed.
The invention also provides a high-temperature thermal shock resistant ceramic material prepared by the method. Preheating the obtained ceramic material to 200 ℃, pouring 1650 ℃ high-temperature metal solution into the ceramic material, repeatedly using the ceramic material for more than 10 times without explosion and peeling, and the normal temperature compressive strength is more than 90 MPa.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
The invention provides a preparation method of a high-temperature thermal shock resistant ceramic material, which comprises the following steps: mixing ceramic powder and an organic binder according to the weight ratio of 1: 0.1-0.2 to obtain a ceramic feed; the ceramic feed is molded by adopting an injection molding method, wherein the injection pressure is 20-80 MPa, and the injection temperature is 120-180 ℃; after the ceramic feed is formed, heating the obtained blank to 450-550 ℃ at the speed of 10-20 ℃/h, preserving heat for 5-7 h, and carrying out degumming treatment; after glue discharging, heating to 1150-1320 ℃ at the speed of 120-180 ℃/h, and carrying out heat preservation for 2-6 h for sintering to obtain the ceramic material.
The organic binder comprises organic glass, polystyrene, high-density polyethylene, microcrystalline wax powder and a dispersing agent in a weight ratio of (35-50) to (10-20) to (10-15) to (3-10). The dispersant is one or more of stearic acid, oleic acid and carboxyl stearic acid. The ceramic powder comprises the following components in parts by weight: 31-53 parts of fused quartz, 25-45 parts of tabular corundum powder, 20-35 parts of alumina micro powder and 0.5-1.5 parts of silicon nitride micro powder. The plate-shaped corundum powder has the weight ratio of the plate-shaped corundum powder with the particle size of 0.18-0.1 mm to the plate-shaped corundum powder with the particle size of 0.045mm of (10-20) to (15-25). The fused quartz comprises a first fused quartz, a second fused quartz, a third fused quartz and a fourth fused quartz in a weight ratio of (10-18): (15-20): (5-10): (1-5), wherein the particle size of the first fused quartz is 0.27-0.18 mm, the particle size of the second fused quartz is 0.15-0.1 mm, the particle size of the third fused quartz is smaller than 0.1mm and not smaller than 0.075mm, and the particle size of the fourth fused quartz is smaller than 0.045 mm. By the combination of the selection of the organic binder and the grain composition of the ceramic powder, low-deformation sintering can be realized under the condition of ensuring the strength of the green body.
The invention also provides a high-temperature thermal shock resistant ceramic material prepared by the method.
Example 1
The embodiment provides a preparation method of a high-temperature thermal shock resistant ceramic material, which comprises the following steps:
according to parts by weight, taking 14 parts of first fused quartz, 16 parts of second fused quartz, 5 parts of third fused quartz, 2 parts of fourth fused quartz, 12 parts of plate-shaped corundum powder with the particle size of 0.18-0.1 mm, 20 parts of plate-shaped corundum powder with the particle size of 0.045mm, 30 parts of alumina micro powder and 1 part of silicon nitride micro powder, and putting the ceramic powder into a horizontal ceramic ball mill for ball milling for 5 hours to obtain the premix.
Adding an organic binder into the premix, uniformly banburying at the temperature of 150 ℃, and carrying out banburying and then granulating into granules with the diameter of 1-3 mm and the height of 1-5 mm to obtain a ceramic feed; wherein the weight of the organic binder is 10 percent of the total mass of the ceramic powder, and the weight ratio of the organic glass, the polystyrene, the high-density polyethylene, the microcrystalline wax powder and the stearic acid in the organic binder is 35: 20: 15: 8.
Feeding the ceramic feed into a hopper of a high-pressure injection molding machine, injecting the ceramic feed into a precise mold under the conditions that the injection pressure is 20MPa and the injection temperature is 150 ℃, and opening the mold to obtain a molded ceramic blank;
putting the formed ceramic blank into an electric furnace, heating to 500 ℃ at the rate of 15 ℃, and preserving heat for 6 hours to carry out glue removal treatment; and then, heating to 1250 ℃ at the rate of 150 ℃ and preserving heat for 3h for sintering to obtain the ceramic material.
The embodiment also provides a high-temperature thermal shock resistant ceramic material prepared by the method.
Example 2
The embodiment provides a preparation method of a high-temperature thermal shock resistant ceramic material, which comprises the following steps:
according to parts by weight, taking 10 parts of first fused quartz, 18 parts of second fused quartz, 8 parts of third fused quartz, 3 parts of fourth fused quartz, 15 parts of plate-shaped corundum powder with the particle size of 0.18-0.1 mm, 18.5 parts of plate-shaped corundum powder with the particle size of 0.045mm, 26 parts of alumina micro powder and 1.5 parts of silicon nitride micro powder, and putting the ceramic powder into a horizontal ceramic ball mill for ball milling for 5 hours to obtain the premix.
Adding an organic binder into the premix, uniformly banburying at 180 ℃, and carrying out banburying and then granulating into granules with the diameter of 1-3 mm and the height of 1-5 mm to obtain a ceramic feed; wherein the weight of the organic binder is 15 percent of the total mass of the ceramic powder, and the weight ratio of the organic glass, the polystyrene, the high-density polyethylene, the microcrystalline wax powder and the oleic acid in the organic binder is 50: 10: 3.
Feeding the ceramic feed into a hopper of a high-pressure injection molding machine, injecting the ceramic feed into a precise mold under the conditions that the injection pressure is 50MPa and the injection temperature is 120 ℃, and opening the mold to obtain a molded ceramic blank;
putting the formed ceramic blank into an electric furnace, heating to 450 ℃ at the speed of 10 ℃, and preserving heat for 7 hours to carry out glue removal treatment; and then, heating to 1320 ℃ at the rate of 180 ℃ and preserving heat for 2h for sintering to obtain the material.
The embodiment also provides a high-temperature thermal shock resistant ceramic material prepared by the method.
Example 3
The embodiment provides a preparation method of a high-temperature thermal shock resistant ceramic material, which comprises the following steps:
according to parts by weight, 18 parts of first fused quartz, 15 parts of second fused quartz, 10 parts of third fused quartz, 1 part of fourth fused quartz, 18 parts of plate-shaped corundum powder with the particle size of 0.18-0.1 mm, 15 parts of plate-shaped corundum powder with the particle size of 0.045mm, 22.5 parts of alumina micro powder and 0.5 part of silicon nitride micro powder are taken, and the ceramic powder is put into a horizontal ceramic ball mill for ball milling for 8 hours to obtain the premix.
Adding an organic binder into the premix, uniformly banburying at the temperature of 200 ℃, and carrying out banburying and then granulating into granules with the diameter of 1-3 mm and the height of 1-5 mm to obtain a ceramic feed; wherein the weight of the organic binder is 20 percent of the total mass of the ceramic powder, and the weight ratio of the organic glass, the polystyrene, the high-density polyethylene, the microcrystalline wax powder and the carboxyl stearic acid in the organic binder is 40: 15: 12: 13: 10.
Feeding the ceramic feed into a hopper of a high-pressure injection molding machine, injecting the ceramic feed into a precise mold under the conditions that the injection pressure is 80MPa and the injection temperature is 180 ℃, and opening the mold to obtain a molded ceramic blank;
putting the formed ceramic blank into an electric furnace, heating to 550 ℃ at the rate of 20 ℃, and preserving heat for 5 hours to carry out glue removal treatment; and then raising the temperature to 1150 ℃ at the rate of 120 ℃ and preserving the heat for 6h for sintering to obtain the ceramic material.
The embodiment also provides a high-temperature thermal shock resistant ceramic material prepared by the method.
Comparative example
Experiment 1: preparing the ceramic material prepared by the method of example 1 into a container, which is marked as number X;
experiment 2: the preparation method of the experiment is different from that of the example 1 in that the particle sizes of the fused quartz and the plate-shaped corundum powder in the experiment are 0.15-0.1 mm, the other conditions are the same as those of the example 1, a container which is the same as the experiment 1 is manufactured, and the obtained ceramic material is marked as a number Y1;
experiment 3: the preparation method of the experiment is different from that of the example 1 in that the particle sizes of the fused silica and the plate-shaped corundum powder in the experiment are both 0.27-0.18 mm, the fused silica and the plate-shaped corundum powder are prepared into a container shape which is the same as that of the experiment 1 under the same conditions as the example 1, and the obtained ceramic material is marked as a number Y2;
experiment 4: the preparation method of the experiment is different from that of the example 1 in that the organic binder in the experiment consists of paraffin, polyethylene and stearic acid, the other conditions are the same as the example 1, the container is made as the same as the experiment 1, and the obtained ceramic material is marked as the number Y3;
experiment 5: the preparation method of this experiment differs from that of example 1 in that casting molding was used as the molding method in this experiment, the same vessel as in experiment 1 was prepared under the same conditions as in example 1, and the obtained ceramic material was designated as Y4.
The properties of the ceramic material obtained in the above experiments 1 to 5 are as follows:
the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; all other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the high-temperature thermal shock resistant ceramic material is characterized by comprising the following steps of:
mixing ceramic powder with an organic binder to obtain a ceramic feed;
forming the ceramic feed, removing the glue and sintering to obtain the ceramic material;
wherein the ceramic powder comprises the following components in parts by weight: 31-53 parts of fused quartz, 25-45 parts of tabular corundum powder, 20-35 parts of alumina micro powder and 0.5-1.5 parts of silicon nitride micro powder.
2. The preparation method of claim 1, wherein the organic binder comprises organic glass, polystyrene, high-density polyethylene, microcrystalline wax powder and a dispersing agent in a weight ratio of (35-50) to (10-20) to (10-15) to (3-10).
3. The method of claim 2, wherein the dispersant is one or more of stearic acid, oleic acid, and carboxystearic acid.
4. The method according to claim 1, wherein the plate-like corundum powder has a weight ratio of (10-20) to (15-25) of plate-like corundum powder having a particle size of 0.18-0.1 mm to plate-like corundum powder having a particle size of 0.045 mm.
5. The preparation method according to claim 1, wherein the fused quartz comprises a first fused quartz, a second fused quartz, a third fused quartz and a fourth fused quartz in a weight ratio of (10-18) to (15-20) to (5-10) to (1-5), wherein the particle size of the first fused quartz is 0.27-0.18 mm, the particle size of the second fused quartz is 0.15-0.1 mm, the particle size of the third fused quartz is less than 0.1mm and not less than 0.075mm, and the particle size of the fourth fused quartz is less than 0.045 mm.
6. The preparation method according to claim 1, wherein the molding is injection molding, the injection pressure is 20 to 80MPa, and the injection temperature is 120 to 180 ℃.
7. The preparation method of claim 1, wherein the rubber discharging comprises heating the ceramic feed at a rate of 10-20 ℃/h to 450-550 ℃ and maintaining the temperature for 5-7 h after the ceramic feed is formed.
8. The method of manufacturing according to claim 1, wherein the sintering comprises: and after the ceramic feed is molded and the rubber is discharged, heating to 1150-1320 ℃ at the speed of 120-180 ℃/h, and preserving heat for 2-6 h.
9. The preparation method of claim 1, wherein the ceramic powder and the organic binder are mixed in a weight ratio of 1: 0.1-0.2.
10. A high temperature thermal shock resistant ceramic material prepared by the method of any one of claims 1 to 9.
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