CN115784751B - Method for preparing high-toughness ceramic based on laser etching technology - Google Patents
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Abstract
The invention discloses a method for preparing high-toughness ceramic based on a laser etching technology, and belongs to the technical field of ceramic materials and preparation thereof. The invention comprises the following steps: (1) preparing ceramic slurry with good fluidity; (2) The ceramic slurry is not limited to be manufactured into a green sheet (3) with a certain thickness by using a tape casting technology, and the green sheet is subjected to patterning etching by using a laser etching technology. (4) The green sheets are arranged in a certain arrangement including lamination, rotation, etc. And (5) discharging glue and sintering to obtain the high-toughness ceramic material. The invention can also be based on (1), 2 and 3) to obtain the high-toughness ceramic material by firstly sintering the sheet layers, and then laminating and treating again. The invention can prepare the laminar material with full ceramic components, obviously improves the toughness of the ceramic material, can be applied to extreme environments such as high temperature and the like, and has the advantages of simple preparation, wide applicability and excellent comprehensive performance.
Description
Technical Field
The invention relates to a preparation method of high-toughness ceramic, in particular to a method for preparing high-toughness ceramic based on a laser etching technology, and belongs to the technical field of ceramic materials and preparation thereof.
Background
The ceramic material generally has the advantages of high strength, high temperature resistance, oxidation resistance, low friction coefficient, creep resistance, thermal shock resistance, corrosion resistance and the like, so that the ceramic material has wide application prospect, and can be especially used as a structural material in a high-temperature environment. However, the chemical bond of the ceramic material is usually covalent bond or ionic bond, which lacks plastic deformation mechanism, and the material has large brittleness and is easy to have catastrophic failure under the action of external force. This greatly limits the range of applications for ceramic materials. Therefore, the development of high-toughness and damage-resistant ceramic materials has become a hot point of research.
The toughening means of ceramic materials generally include toughening with a second phase to effect zone shielding of cracks; extending crack propagation length and crack deflection times; and the crack resistance is improved by utilizing grain boundary friction, bridging and other modes. Wherein the brittle fracture problem of the ceramic material cannot be fundamentally solved only by means of component change or simple combination of a plurality of components. The introduction of the second phase often requires consideration of the dispersibility and thermal matching properties of the material, and therefore the types of materials that can be used as the second phase are limited and generally costly. The improvement of the toughness of the material by a structural design method is an effective approach. The layered ceramic material based on the bionic shell structure design can greatly improve the fracture toughness of the material, but the layered ceramic material usually needs to be introduced with organic matters as a weak interface layer, and the use temperature range of the material is limited and can not be used in a high-temperature environment. Therefore, it is necessary to develop a high-toughness ceramic that can be used in a high-temperature environment.
Disclosure of Invention
In order to overcome the existing defects, the main object of the invention is to provide a method for preparing high-toughness ceramic based on laser etching technology, which is characterized in that the ceramic green body is subjected to pattern etching, the etching layers are rotated through stacking arrangement, crack growth of the material in the breaking process is induced, the energy dissipation is improved, and the high-toughness ceramic material (the breaking toughness is more than 12 MP.m) 1/2 ). The invention can obviously improve the toughness of the ceramic material, can be applied to extreme environments such as high temperature and the like, and has the advantages of simple preparation and wide applicability.
In order to achieve the purpose of the invention, the method comprises the following steps:
the invention discloses a method for preparing high-toughness ceramic based on a laser etching technology, which comprises the following steps:
1. preparing ceramic slurry: dissolving a dispersing agent with the mass fraction of 5-10% in a solvent, sequentially adding sintering auxiliary agents with the mass fraction of 5-20% after the dispersing agent is completely dissolved, and then adding ceramic powder for dispersing, wherein the ratio of the total mass of the powder to the mass of the solvent is 0.1-10. Finally, 10-30% of binder and plasticizer are added in mass fraction, and ball milling or stirring is continued until complete dissolution is achieved.
2. Preparing a ceramic green body: pouring the ceramic slurry into a trough of a casting forming machine, keeping the height of a scraper to be 20-2000 mu m and the casting speed to be 10-100cm/min. Drying in a drying oven at room temperature for 0.5-72h, and stripping from the substrate to obtain the green sheet with thickness of 10-1500 μm.
3. And (3) laser etching: and etching the green sheet by utilizing laser according to the pre-designed pattern to obtain the patterned green sheet, wherein the etching depth of the pattern is 10% -90% of the thickness of the green sheet.
4. Structural design: the green sheets are arranged in a predetermined manner including stacking of the green sheets and twisting each layer of the patterned green sheets by rotating the current layer at an angle to the previous layer. After a certain number of layers are arranged, cold pressing is carried out to obtain a green body block. The green sheet includes a patterned green sheet and an unpatterned green sheet.
Fifth step: and (3) discharging glue and sintering: the glue discharging process is to discharge glue at the temperature rising rate of 0.5-10 ℃/min and the temperature is kept at 500-800 ℃ for 0-24 hours to obtain a glue-free green body; and then placing the glue-free green body into a sintering furnace, preserving heat at a temperature rising rate of 5-500 ℃/min at 1000-2500 ℃ and then sintering to obtain a ceramic block, namely realizing the preparation of high-toughness ceramic based on a laser etching technology.
The ceramic powder in the first step contains one or more additives; the additive comprises boron nitride, graphene oxide, graphene, carbon nanotubes or silicon carbide whiskers.
The pattern types include straight line structures, branch structures, polygonal structures, corrugated structures, triangular structures.
In the third step, the laser processing equipment is not specific, and the etching depth is controlled by adjusting the laser emission power.
The green sheet material to be etched is not limited to a single body material, but may be a composite of multiple materials in different proportions.
And laminating and pressing the green sheets into a green body block according to a preset arrangement mode, including but not limited to laminating arrangement of green sheets with the same etching pattern, laminating arrangement of green sheets with different etching patterns, laminating arrangement of green sheets with the same etching depth with the same pattern, laminating arrangement of green sheets with different etching depths with different etching patterns, and laminating of green sheets with different etching patterns and the same etching depth.
The green sheets are laminated in a predetermined arrangement to form a green block including, but not limited to, etched layers and unetched sheets in a stacked arrangement.
The arrangement includes, but is not limited to, etched blanks of different materials being arranged in a stack with unetched blanks.
The beneficial effects are that:
1. according to the method for preparing the high-toughness ceramic based on the laser etching technology, the ceramic block body is used for reasonably patterning and processing a ceramic green body single layer by the laser etching technology, and then crack deflection of a ceramic material in a fracture process is induced by stacking arrangement in a certain mode, so that the fracture toughness of the ceramic block body can be remarkably improved compared with that of a laminated ceramic body and a compact ceramic block body which are not etched.
2. The invention discloses a method for preparing high-toughness ceramic based on a laser etching technology, wherein the ceramic material is subjected to green body single-layer structure design by using the laser etching technology, and then a complete ceramic block is obtained by a laminating and sintering mode. Unlike conventional layered materials that utilize organic substances as weak interfacial layers. The full ceramic material has higher strength and can be applied in high-temperature environment.
3. The method for preparing the high-toughness ceramic based on the laser etching technology disclosed by the invention has the advantages that the laser etching technology is utilized to carry out patterning design on the surface of the green sheet, the requirement on laser equipment is low, most laser processing equipment can be realized, and the processing difficulty is low.
4. According to the method for preparing the high-toughness ceramic based on the laser etching technology, disclosed by the invention, the patterning structure is optimized by utilizing the laser etching technology, so that the controllability of the structure can be realized, the uniformity of the structure can be ensured, and the reliability of the material can be improved.
Drawings
FIG. 1 is an R graph of the samples prepared in examples 1-3 based on the SENB method.
FIG. 2 is an R-graph of the sample prepared in comparative examples 1-2 based on the SENB method.
FIG. 3 is an optical photograph of the parallel stripe etched pattern of examples 1-3
Fig. 4 is an optical photograph of a parallel hexagonal etching pattern of example 4.
Fig. 5 is an optical image of an etched pattern of the parallel-branched structure of example 5.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples, but is not intended to limit the scope of the patent.
Specific embodiments of the present invention are described below by way of specific examples, but are not limiting to the invention.
Example 1
(1) Configuration of silicon nitride slurry: and dissolving the polyethylenimine with the mass fraction of 2% in 60g of absolute ethyl alcohol, adding 100g of powder for ball milling after the polyethylenimine is completely dissolved, adding 10% and 10% of polyethylenglycol butyral and polyethylene glycol after 6 hours, and continuing ball milling for 12 hours.
(2) Preparation of a silicon nitride green sheet: pouring the slurry into a trough of a casting forming machine, setting a scraper with the height of 500 mu m and the casting speed of 30cm/min, drying the slurry in a drying box for 1h at room temperature, and then cutting the green sheet into a wafer.
(3) And (3) patterning and designing a green sheet: and (3) etching parallel stripes on the surface of the green sheet by using a laser etching technology, wherein the depth is 40% of the thickness of the green sheet, and the intervals between the stripes are 1mm.
(4) Stacking arrangement: and (3) alternately arranging the etched green sheets and the unetched green sheets, and simultaneously deflecting a certain angle when the etched green sheets are placed, wherein each etched layer ensures an included angle of 15 degrees with the previous layer. Cold pressing at 20MPa for 15min after lamination
(5) And (3) discharging glue and sintering: and (3) carrying out heat preservation on the green briquettes in an air atmosphere for 1h at 600 ℃ at a heating rate of 1 ℃/min to carry out glue discharging. Then placing the mixture in a nitrogen atmosphere at a heating rate of 10 ℃/min, and carrying out sintering under the condition of heat preservation at 1750 ℃ for 1 h. Finally, the ceramic block is obtained.
The results of fracture toughness testing of the ceramic blocks prepared in this example using the SENB method are shown in fig. 1.
Example 2
The present embodiment is different from embodiment 1 in that
(4) Stacking arrangement: and (3) alternately arranging the etched green sheets and the unetched green sheets, and simultaneously deflecting a certain angle when the etched green sheets are placed, wherein each etched layer ensures an included angle of 30 degrees with the previous layer. And (3) cold pressing for 15min under 20MPa after lamination and arrangement.
The rest of the procedure is the same as in example 1.
The results of fracture toughness testing of the ceramic blocks prepared in this example using the SENB method are shown in fig. 1.
Example 3
The present embodiment is different from embodiment 1 in that
(4) Stacking arrangement: and (3) alternately arranging the etched green sheets and the unetched green sheets, and simultaneously deflecting a certain angle when the etched green sheets are placed, wherein each etched layer ensures an included angle of 90 degrees with the previous layer. And (3) cold pressing for 15min under 20MPa after lamination and arrangement.
The rest of the procedure is the same as in example 1.
The results of fracture toughness tests of the ceramic blocks prepared in the embodiment by using the SENB method are shown in FIG. 1
Example 4
The present embodiment is different from embodiment 1 in that
(3) And (3) patterning and designing a green sheet: and etching a hexagonal structure which is arranged in parallel on the green sheet by using a laser etching technology, wherein the depth is 40% of the thickness of the green sheet.
The rest of the procedure is the same as in example 1.
Example 5
The present embodiment is different from embodiment 1 in that
(3) And (3) patterning and designing a green sheet: and (3) etching a parallel branch structure on the green sheet by using a laser etching technology, wherein the depth is 40% of the thickness of the green sheet, and the interval between the stripes is 3mm.
The rest of the procedure is the same as in example 1.
Example 6
(1) Configuration of silicon nitride slurry: and dissolving the polyethylenimine with the mass fraction of 2% in 60g of absolute ethyl alcohol, adding 100g of powder for ball milling after the polyethylenimine is completely dissolved, adding 10% and 10% of polyethylenglycol butyral and polyethylene glycol after 6 hours, and continuing ball milling for 12 hours.
(2) Configuration of silicon nitride/boron nitride slurry: and dissolving polyethylene imine with the mass fraction of 2% into 60g of absolute ethyl alcohol, adding 80g of silicon nitride and 20g of boron nitride for ball milling after the polyethylene imine is completely dissolved, adding 10% and 10% of polyethylene glycol respectively after 6 hours, and continuing ball milling for 12 hours.
(3) Preparation of a silicon nitride green sheet: pouring the slurry into a trough of a casting forming machine, setting a scraper with the height of 500 mu m and the casting speed of 30cm/min, drying the slurry in a drying box for 1h at room temperature, and then cutting the green sheet into a wafer.
(4) Preparation of a silicon nitride/boron nitride green sheet: pouring the slurry into a trough of a casting forming machine, setting a scraper with the height of 300 mu m and the casting speed of 30cm/min, drying the slurry in a drying box for 1h at room temperature, and then cutting the green sheet into a wafer.
(5) And (3) patterning and designing a green sheet: and (3) etching a parallel stripe structure on the green sheet by using a laser etching technology, wherein the depth is 40% of the thickness of the green sheet, and the stripe interval is 1mm.
(6) Stacking arrangement: and alternately stacking the unetched silicon nitride green sheet, the etched silicon nitride green sheet and the silicon nitride/boron nitride green sheet, wherein the included angle between the etched green sheet and the etched green sheet of the previous layer is kept at 15 degrees. And (3) cold pressing for 15min under 20MPa after lamination and arrangement.
(7) And (3) discharging glue and sintering: and (3) carrying out heat preservation on the green briquettes in an air atmosphere for 1h at 600 ℃ at a heating rate of 1 ℃/min to carry out glue discharging. Then placing the mixture in a nitrogen atmosphere at a heating rate of 10 ℃/min, and carrying out sintering under the condition of heat preservation at 1750 ℃ for 1 h. Finally, the ceramic block is obtained.
Example 7
(1) Configuration of silicon nitride slurry: and dissolving the polyethylenimine with the mass fraction of 2% in 60g of absolute ethyl alcohol, adding 100g of powder for ball milling after the polyethylenimine is completely dissolved, adding 10% and 10% of polyethylenglycol butyral and polyethylene glycol after 6 hours, and continuing ball milling for 12 hours.
(2) Configuration of silicon nitride/graphene oxide slurry: and dissolving polyethylene imine with the mass fraction of 2% in 60g of absolute ethyl alcohol, adding 99g of silicon nitride and 1g of graphene oxide after the polyethylene imine is completely dissolved, performing ball milling, adding 10% and 10% of polyethylene glycol after 6 hours, and then continuing ball milling for 12 hours.
(3) Preparation of a silicon nitride green sheet: pouring the slurry into a trough of a casting forming machine, setting a scraper with the height of 500 mu m and the casting speed of 30cm/min, drying the slurry in a drying box for 1h at room temperature, and then cutting the green sheet into a wafer.
(4) Preparation of a silicon nitride/graphene oxide green sheet: pouring the slurry into a trough of a casting forming machine, setting a scraper with the height of 300 mu m and the casting speed of 30cm/min, drying the slurry in a drying box for 1h at room temperature, and then cutting the green sheet into a wafer.
(5) And (3) patterning and designing a green sheet: and etching a polygonal structure which is arranged in parallel on the green sheet by using a laser etching technology, wherein the etching depth is 40% of the thickness of the green sheet.
(6) Stacking arrangement: and arranging the unetched silicon nitride green sheet, the etched green sheet and the silicon nitride/graphene oxide green sheet in sequence, repeating the arrangement for a plurality of times, and ensuring that the included angles between the etched green sheet and the etched green sheet of the previous layer are all kept at 15 degrees. Cold pressing at 20MPa for 15min after lamination
(7) And (3) discharging glue and sintering: and (3) carrying out heat preservation on the green briquettes in an air atmosphere for 1h at 600 ℃ at a heating rate of 1 ℃/min to carry out glue discharging. Then placing the mixture in a nitrogen atmosphere at a heating rate of 10 ℃/min, and carrying out sintering under the condition of heat preservation at 1750 ℃ for 1 h. Finally, the ceramic block is obtained.
Example 8
(1) Configuration of silicon nitride slurry: and dissolving the polyethylenimine with the mass fraction of 2% in 60g of absolute ethyl alcohol, adding 100g of powder for ball milling after the polyethylenimine is completely dissolved, adding 10% and 10% of polyethylenglycol butyral and polyethylene glycol after 6 hours, and continuing ball milling for 12 hours.
(2) Configuration of silicon nitride/graphene slurry: and dissolving polyethylene imine with the mass fraction of 2% in 60g of absolute ethyl alcohol, adding 99g of silicon nitride and 1g of graphene for ball milling after the polyethylene imine is completely dissolved, adding 10% and 10% of polyethylene glycol after 6 hours, and continuing ball milling for 12 hours.
(3) Preparation of a silicon nitride green sheet: pouring the slurry into a trough of a casting forming machine, setting a scraper with the height of 500 mu m and the casting speed of 30cm/min, drying the slurry in a drying box for 1h at room temperature, and then cutting the green sheet into a wafer.
(4) Preparation of a silicon nitride/graphene green sheet: pouring the slurry into a trough of a casting forming machine, setting a scraper with the height of 300 mu m and the casting speed of 30cm/min, drying the slurry in a drying box for 1h at room temperature, and then cutting the green sheet into a wafer.
(5) And (3) patterning and designing a green sheet: and (3) etching a parallel-arranged branch structure on the green sheet by using a laser etching technology, wherein the etching depth is 40% of the thickness of the green sheet, and the interval is 3mm.
(6) Stacking arrangement: and arranging the unetched silicon nitride green sheets, the etched green sheets and the silicon nitride/graphene green sheets in sequence, repeating the arrangement for a plurality of times, and ensuring that the included angle between adjacent etched green sheets is 15 degrees. Cold pressing at 20MPa for 15min after lamination
(7) And (3) discharging glue and sintering: and (3) carrying out heat preservation on the green briquettes in an air atmosphere for 1h at 600 ℃ at a heating rate of 1 ℃/min to carry out glue discharging. Then placing the mixture in a nitrogen atmosphere at a heating rate of 10 ℃/min, and carrying out sintering under the condition of heat preservation at 1750 ℃ for 1 h. Finally, the ceramic block is obtained.
Example 9
(1) Configuration of silicon carbide slurry: and dissolving the polyethylenimine with the mass fraction of 2% in 60g of absolute ethyl alcohol, adding 100g of powder for ball milling after the polyethylenimine is completely dissolved, adding 10% and 10% of polyethylenglycol butyral and polyethylene glycol after 6 hours, and continuing ball milling for 12 hours.
(2) Preparation of a silicon carbide green sheet: pouring the slurry into a trough of a casting forming machine, setting a scraper with the height of 500 mu m and the casting speed of 30cm/min, drying the slurry in a drying box for 1h at room temperature, and then cutting the green sheet into a wafer.
(3) And (3) patterning and designing a green sheet: and (5) etching parallel stripes on the green sheet by using a laser etching technology, wherein the intervals are 2mm.
(4) Stacking arrangement: and stacking and arranging the etched green sheets, and ensuring that the included angle between adjacent etched green sheets is 20 degrees. Cold pressing at 20MPa for 15min after lamination
(5) And (3) discharging glue and sintering: and (3) carrying out heat preservation on the green briquettes in an air atmosphere for 1h at 600 ℃ at a heating rate of 0.5-1.5 ℃/min for discharging glue. Then placing the mixture in an argon atmosphere, and sintering the mixture under the condition of heat preservation at 1800 ℃ for 1h at a heating rate of 10 ℃/min. Finally, the ceramic block is obtained.
Example 10
(1) Configuration of silicon carbide slurry: and dissolving the polyethylenimine with the mass fraction of 2% in 60g of absolute ethyl alcohol, adding 100g of powder for ball milling after the polyethylenimine is completely dissolved, adding 10% and 10% of polyethylenglycol butyral and polyethylene glycol after 6 hours, and continuing ball milling for 12 hours.
(2) Configuration of silicon carbide/carbon nanotube slurry: and dissolving polyethylene imine with the mass fraction of 2% into 60g of absolute ethyl alcohol, adding 99g of silicon carbide and 1g of carbon nano tube for ball milling after the polyethylene imine is completely dissolved, adding 10% and 10% of polyethylene glycol after 6 hours, and continuing ball milling for 12 hours.
(3) Preparation of a silicon carbide green sheet: pouring the slurry into a trough of a casting forming machine, setting a scraper with the height of 500 mu m and the casting speed of 30cm/min, drying the slurry in a drying box for 1h at room temperature, and then cutting the green sheet into a wafer.
(4) Preparation of silicon carbide/carbon nanotube green sheets: pouring the slurry into a trough of a casting forming machine, setting a scraper with the height of 300 mu m and the casting speed of 30cm/min, drying the slurry in a drying box for 1h at room temperature, and then cutting the green sheet into a wafer.
(5) And (3) patterning and designing a green sheet: and (3) etching parallel stripes on the green sheet by using a laser etching technology, wherein the interval between the stripes is 0.5mm.
(6) Stacking arrangement: and arranging the unetched silicon carbide green sheet, the etched green sheet and the silicon carbide/carbon nanotube green sheet in sequence, repeating the arrangement for a plurality of times, and ensuring that the included angle of the adjacent etched green sheets is 20 degrees. Cold pressing at 20MPa for 15min after lamination
(7) And (3) discharging glue and sintering: and (3) carrying out heat preservation on the green briquettes in an air atmosphere for 1h at 600 ℃ at a heating rate of 1 ℃/min to carry out glue discharging. Then placing the mixture in an argon atmosphere, and sintering the mixture under the condition of heat preservation at 1800 ℃ for 1h at a heating rate of 10 ℃/min. Finally, the ceramic block is obtained.
Example 11
(1) Configuration of alumina slurry: and dissolving the polyethylenimine with the mass fraction of 2% in 60g of absolute ethyl alcohol, adding 100g of powder for ball milling after the polyethylenimine is completely dissolved, adding 10% and 10% of polyethylenglycol butyral and polyethylene glycol after 6 hours, and continuing ball milling for 12 hours.
(2) Preparation of alumina green sheet: pouring the slurry into a trough of a casting forming machine, setting a scraper with the height of 500 mu m and the casting speed of 30cm/min, drying the slurry in a drying box for 1h at room temperature, and then cutting the green sheet into a wafer.
(3) Alumina patterning design: and (3) etching parallel stripes on the green sheet by using a laser etching technology, wherein the interval between the stripes is 0.1-10mm.
(4) Stacking arrangement: and stacking and arranging the etched green sheets, and ensuring that the included angle of the adjacent etched green sheets is 25 degrees. Cold pressing at 20MPa for 15min after lamination
(5) And (3) discharging glue and sintering: and (3) carrying out heat preservation on the green briquettes in an air atmosphere for 1h at 600 ℃ at a heating rate of 0.5-1.5 ℃/min for discharging glue. Then placing the mixture in an air atmosphere at a heating rate of 10 ℃/min, and carrying out sintering under the condition of heat preservation at 1400 ℃ for 1 h. Finally, the ceramic block is obtained.
Example 12
(1) Configuration of alumina slurry: and dissolving the polyethylenimine with the mass fraction of 2% in 60g of absolute ethyl alcohol, adding 100g of powder for ball milling after the polyethylenimine is completely dissolved, adding 10% and 10% of polyethylenglycol butyral and polyethylene glycol after 6 hours, and continuing ball milling for 12 hours.
(2) Preparing alumina/silicon carbide whisker slurry: and dissolving polyethylene imine with the mass fraction of 2% into 60g of absolute ethyl alcohol, adding 90g of aluminum oxide and 10g of silicon carbide whisker for ball milling after the polyethylene imine is completely dissolved, adding 10% and 10% of polyethylene glycol after 6 hours, and continuing ball milling for 12 hours.
(3) Preparation of alumina green sheet: pouring the slurry into a trough of a casting forming machine, setting a scraper with the height of 500 mu m and the casting speed of 30cm/min, drying the slurry in a drying box for 1h at room temperature, and then cutting the green sheet into a wafer.
(4) Preparation of an alumina/silicon carbide whisker green sheet: pouring the slurry into a trough of a casting forming machine, setting a scraper with the height of 300 mu m and the casting speed of 30cm/min, drying the slurry in a drying box for 1h at room temperature, and then cutting the green sheet into a wafer.
(5) And (3) patterning and designing a green sheet: and etching a parallel branch structure on the green sheet by using a laser etching technology, wherein the interval between the stripes is 3mm.
(6) Stacking arrangement: and arranging the unetched aluminum oxide green body sheet, the etched green body sheet and the aluminum oxide/silicon carbide whisker green body sheet in sequence, repeating the arrangement for a plurality of times, and ensuring that the included angle of the adjacent etched green body sheets is 25 degrees. And (3) cold pressing for 15min under 20MPa after lamination and arrangement.
(7) And (3) discharging glue and sintering: and (3) carrying out heat preservation on the green briquettes in an air atmosphere for 1h at 600 ℃ at a heating rate of 1 ℃/min to carry out glue discharging. Then placing the ceramic block in an air atmosphere at a heating rate of 10 ℃/min, and carrying out sintering under the condition of heat preservation at 1400 ℃ for 1h to obtain the ceramic block.
Comparative example 1
(1) Configuration of silicon nitride slurry: and dissolving the polyethylenimine with the mass fraction of 2% in 60g of absolute ethyl alcohol, adding 100g of powder for ball milling after the polyethylenimine is completely dissolved, adding 10% and 10% of polyethylenglycol butyral and polyethylene glycol after 6 hours, and continuing ball milling for 12 hours.
(2) Preparation of a silicon nitride green sheet: pouring the slurry into a trough of a casting forming machine, setting a scraper with the height of 500 mu m and the casting speed of 30cm/min, drying the slurry in a drying box for 1h at room temperature, and then cutting the green sheet into a wafer.
(3) Stacking arrangement: cold pressing at 20MPa for 15min after stacking and arranging the green sheets
(5) And (3) discharging glue and sintering: and (3) carrying out heat preservation on the green briquettes in an air atmosphere for 1h at 600 ℃ at a heating rate of 1 ℃/min to carry out glue discharging. Then placing the mixture in a nitrogen atmosphere at a heating rate of 10 ℃/min, and carrying out sintering under the condition of heat preservation at 1750 ℃ for 1 h. Finally, the ceramic block is obtained.
The results of the fracture toughness test of the ceramic blocks prepared in this comparative example by the SENB method are shown in FIG. 2
Comparative example 2
(1) 20g of silicon nitride powder is weighed, 1g of PVA solution with the mass fraction of 10% is dripped into the powder, and the powder is stirred uniformly.
(2) Pouring the uniformly stirred powder into an indeterminate rigid mould, and cold pressing for 15min under 20 MPa.
(3) Taking out the formed block, placing the block in a nitrogen atmosphere, and sintering the block at 1750 ℃ for 1h under the condition of heat preservation at the heating rate of 10 ℃/min to obtain the ceramic block.
The results of the fracture toughness test of the ceramic blocks prepared in this comparative example by the SENB method are shown in FIG. 2
From examples and comparative examples, it was confirmed that the fracture toughness of the material can be remarkably improved by patterning etching of the green sheet under the same material, laminating and rotating the etched layers by a certain angle to press and sinter-mold. The effectiveness of the preparation method is demonstrated.
While the foregoing is directed to embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (8)
1. A method for preparing high-toughness ceramic based on a laser etching technology is characterized by comprising the following steps: comprises the following steps of the method,
1. preparing ceramic slurry: dissolving a dispersing agent with the mass fraction of 5-10% in a solvent, sequentially adding a sintering aid with the mass fraction of 5-20% after the dispersing agent is completely dissolved, and then adding ceramic powder for dispersion, wherein the ratio of the total mass of the powder to the mass of the solvent is 0.1-10; finally, adding 10-30% of binder and plasticizer by mass fraction, and continuing ball milling or stirring until completely dissolved;
2. preparing a ceramic green body: pouring the ceramic slurry into a trough of a casting forming machine, keeping the height of a scraper to be 20-2000 mu m and the casting speed to be 10-100cm/min; drying for 0.5-72h at room temperature in a drying oven, and stripping from the substrate after drying to obtain a green sheet with the thickness of 10-1500 mu m;
3. and (3) laser etching: etching the green sheet by using laser according to the pre-designed pattern to obtain a patterned green sheet, wherein the etching depth of the pattern is 10% -90% of the thickness of the green sheet;
4. structural design: arranging the green sheets according to a preset mode, wherein the arrangement mode comprises lamination and patterning of the green sheets, twisting each layer of the green sheets, and forming a certain included angle with the previous layer by rotating the current layer; arranging a certain number of layers and then cold-pressing to obtain a green body block; the green sheet comprises a patterned green sheet and a non-patterned green sheet;
fifth step: and (3) discharging glue and sintering: the glue discharging process is to discharge glue at the temperature rising rate of 0.5-10 ℃/min and the temperature is kept at 500-800 ℃ for 0-24 hours to obtain a glue-free green body; and then placing the glue-free green body into a sintering furnace, preserving heat at a temperature rising rate of 5-500 ℃/min at 1000-2500 ℃ and then sintering to obtain a ceramic block, namely realizing the preparation of high-toughness ceramic based on a laser etching technology.
2. The method for preparing high-toughness ceramic based on the laser etching technology as claimed in claim 1, wherein: the ceramic powder in the first step contains one or more additives; the additive comprises boron nitride, graphene oxide, graphene, carbon nanotubes or silicon carbide whiskers.
3. The method for preparing high-toughness ceramic based on the laser etching technology as claimed in claim 1, wherein: the pattern types include straight line structures, branch structures, polygonal structures, corrugated structures, triangular structures.
4. The method for preparing high-toughness ceramic based on the laser etching technology as claimed in claim 1, wherein: and step three, the laser processing equipment realizes the control of the etching depth by adjusting the laser emission power.
5. The method for preparing high-toughness ceramic based on the laser etching technology as claimed in claim 1, wherein: the etched green sheet material is a single body material or a material in which a plurality of materials are compounded in different proportions.
6. The method for preparing high-toughness ceramic based on the laser etching technology as claimed in claim 1, wherein: laminating the green sheets in a predetermined arrangement to form a green block body, including a laminated arrangement of etched pattern green sheets of the same type; stacking green sheets with different etching patterns, and stacking the green sheets with the same etching depth; the same pattern is arranged in a stacked manner with different etching depths.
7. The method for preparing high-toughness ceramic based on the laser etching technology as claimed in claim 1, wherein: and stacking and pressing the green sheets according to a preset arrangement mode to form a green block body, wherein the etched layers and the unetched green sheets are stacked and arranged according to the preset arrangement mode.
8. The method for preparing high-toughness ceramic based on the laser etching technology as claimed in claim 1, wherein: the arrangement mode is that etched blanks made of different materials and unetched blanks are stacked and arranged according to a preset mode.
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| JPH046166A (en) * | 1990-04-25 | 1992-01-10 | Mitsubishi Heavy Ind Ltd | Produciton of high-toughness ceramics |
| CN102503378A (en) * | 2011-10-14 | 2012-06-20 | 吕佳佳 | Thin chip ceramic substrate and manufacturing method thereof |
| CN113233875A (en) * | 2021-04-26 | 2021-08-10 | 广东工业大学 | Flexible high-electric-conductivity heat-conduction ceramic-based composite film and preparation method thereof |
| CN114988854A (en) * | 2022-07-19 | 2022-09-02 | 华中科技大学 | Alumina ceramic substrate and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150147710A1 (en) * | 2011-08-12 | 2015-05-28 | Ultradent Products, Inc. | Laser etched sintered ceramic orthodontic brackets |
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| JPH046166A (en) * | 1990-04-25 | 1992-01-10 | Mitsubishi Heavy Ind Ltd | Produciton of high-toughness ceramics |
| CN102503378A (en) * | 2011-10-14 | 2012-06-20 | 吕佳佳 | Thin chip ceramic substrate and manufacturing method thereof |
| CN113233875A (en) * | 2021-04-26 | 2021-08-10 | 广东工业大学 | Flexible high-electric-conductivity heat-conduction ceramic-based composite film and preparation method thereof |
| CN114988854A (en) * | 2022-07-19 | 2022-09-02 | 华中科技大学 | Alumina ceramic substrate and preparation method thereof |
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