CN114057490A - Method for preparing large-size ceramic - Google Patents
Method for preparing large-size ceramic Download PDFInfo
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- CN114057490A CN114057490A CN202111429465.5A CN202111429465A CN114057490A CN 114057490 A CN114057490 A CN 114057490A CN 202111429465 A CN202111429465 A CN 202111429465A CN 114057490 A CN114057490 A CN 114057490A
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- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000000843 powder Substances 0.000 claims abstract description 125
- 238000007639 printing Methods 0.000 claims abstract description 87
- 229920005989 resin Polymers 0.000 claims abstract description 58
- 239000011347 resin Substances 0.000 claims abstract description 58
- 238000005245 sintering Methods 0.000 claims abstract description 28
- 235000015895 biscuits Nutrition 0.000 claims abstract description 26
- 239000007787 solid Substances 0.000 claims abstract description 21
- 238000005507 spraying Methods 0.000 claims abstract description 19
- 238000000465 moulding Methods 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 238000001723 curing Methods 0.000 claims abstract description 14
- 239000007921 spray Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
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- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims abstract description 4
- 238000001125 extrusion Methods 0.000 claims abstract description 3
- 230000001678 irradiating effect Effects 0.000 claims abstract description 3
- 238000003892 spreading Methods 0.000 claims abstract description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 14
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 12
- 239000005011 phenolic resin Substances 0.000 claims description 12
- 229920001568 phenolic resin Polymers 0.000 claims description 12
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 12
- 229910052580 B4C Inorganic materials 0.000 claims description 8
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 8
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 claims description 7
- ZDHCZVWCTKTBRY-UHFFFAOYSA-N omega-Hydroxydodecanoic acid Natural products OCCCCCCCCCCCC(O)=O ZDHCZVWCTKTBRY-UHFFFAOYSA-N 0.000 claims description 7
- 102100026735 Coagulation factor VIII Human genes 0.000 claims description 5
- 101000911390 Homo sapiens Coagulation factor VIII Proteins 0.000 claims description 5
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 5
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 5
- 239000007849 furan resin Substances 0.000 claims description 5
- 229920000647 polyepoxide Polymers 0.000 claims description 5
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000243 solution Substances 0.000 description 16
- 238000005516 engineering process Methods 0.000 description 15
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- JIRHAGAOHOYLNO-UHFFFAOYSA-N (3-cyclopentyloxy-4-methoxyphenyl)methanol Chemical compound COC1=CC=C(CO)C=C1OC1CCCC1 JIRHAGAOHOYLNO-UHFFFAOYSA-N 0.000 description 2
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 238000007641 inkjet printing Methods 0.000 description 2
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- ZZXDRXVIRVJQBT-UHFFFAOYSA-N 2,3-dimethylbenzenesulfonic acid Chemical compound CC1=CC=CC(S(O)(=O)=O)=C1C ZZXDRXVIRVJQBT-UHFFFAOYSA-N 0.000 description 1
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- 238000009851 ferrous metallurgy Methods 0.000 description 1
- 239000012943 hotmelt Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 238000012703 microemulsion polymerization Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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Abstract
The invention provides a method for preparing large-size ceramic, which comprises the following steps: s1, coating and mixing the solid resin powder and the ceramic powder to enable the surface of the ceramic powder to be uniformly coated with a layer of solid resin, adding a photoinitiator and a curing agent into the ceramic powder material coated with the solid resin, and stirring and mixing at a high speed to obtain printing powder; s2, placing the printing powder in a printing device for printing and molding, adopting a layer-by-layer printing and molding method, generating a corresponding printing path for each layer of model through a computer, spreading powder in a roller extrusion mode, scanning the powder by a laser in the molding process of each layer of powder, respectively spraying light-cured resin and glue-sprayed resin to the powder by two spray heads, irradiating the powder by ultraviolet light for curing and molding, and accumulating layer by layer to form a printing biscuit; and S3, sintering the printing biscuit in a sintering furnace to obtain a ceramic body. The method is suitable for preparing large-size ceramic blanks, and can greatly improve the structural strength of the material and reduce the deformation amount.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a method for preparing large-size ceramic.
Background
The ceramic material has excellent mechanical property, thermal property and chemical stability, and is widely applied to the industrial fields of petrochemical industry, ferrous metallurgy, mechanical electronics, aerospace, energy environmental protection, nuclear energy, automobiles, high-temperature kilns and the like at present. The preparation of the ceramic usually needs four links of powder processing, green body forming, solid sintering and processing and manufacturing, wherein the green body forming technology plays an important role in the structure and the performance of the ceramic material. The traditional ceramic material forming method mainly comprises the following steps: the dry pressing, extrusion, injection molding, isostatic pressing, casting, etc. are used to prepare the structural member, and the mold with corresponding shape is prepared according to the shape of the structural member.
The rapid prototyping technology is a novel prototyping technology which is rapidly developed in recent years, and the technology utilizes computer CAD software to design components, utilizes a software layering dispersion and numerical control prototyping system, and utilizes laser beams, hot melt nozzles and other modes to stack and bond ceramic powder layer by layer, and finally forms the ceramic powder in an overlaying mode to manufacture solid products. The existing rapid prototyping technology is mainly Selective Laser Sintering (SLS), inkjet printing (3DP), photo-curing technology (SLA, DLP) and the like, but the structural strength of a blank prepared by the existing rapid prototyping technology is low, the strength of the blank prepared by the selective laser sintering technology and the photo-curing technology is 2-3Mpa, and the strength of the blank prepared by the inkjet printing technology is 3-5 Mpa. This limits the rapid prototyping technology from being used to produce large-sized ceramic products, and especially when the size of the ceramic product is larger than 700mm, the strength of the blank produced by the prior rapid prototyping technology is not enough, the product will crack or deform seriously, and the structure and size of the produced ceramic product are different from the designed structure.
Disclosure of Invention
Aiming at the defects of the prior art, the invention mainly aims to provide a new rapid forming technology, improve the strength of a ceramic blank and meet the requirement of preparing a large-size ceramic product.
In order to solve the above technical problems, the present invention provides a method for preparing a large-sized ceramic, comprising the steps of:
s1, coating and mixing the solid resin powder and the ceramic powder to enable the surface of the ceramic powder to be uniformly coated with a layer of solid resin, adding a photoinitiator and a curing agent into the ceramic powder material coated with the solid resin, and stirring and mixing at a high speed to obtain printing powder;
s2, placing the printing powder in a printing device for printing and molding, adopting a layer-by-layer printing and molding method, generating a corresponding printing path for each layer of model through a computer, spreading powder in a roller grinding mode, scanning the powder by a laser in the molding process of each layer of powder, respectively spraying photocureable resin and glue spraying resin to the powder by two spray heads, irradiating the powder by ultraviolet light for curing and molding, and accumulating layer by layer to form a printing biscuit;
and S3, sintering the printing biscuit in a sintering furnace to obtain a ceramic body.
Further, the amount of the light-cured resin in each layer of the blank in the step S2 is 2% -10% of the mass of the printing powder.
Further, the amount of the glue spraying resin in each layer of the blank body in the step S2 is 3-15% of the mass of the printing powder.
Further, the light-cured resin is selected from one or more of HEMA, HDDA and TMPTA, and the glue spraying resin is selected from one or more of phenolic resin solution, furan resin solution, PVA resin solution and PVP resin solution.
Further, the laser power of the laser in the step S2 is 5-60W.
Further, the ultraviolet irradiation power in step S2 is 5-30W.
Further, the layer height of each layer model in the step S2 is 0.01-5 mm.
Further, the sintering temperature of the sintering furnace in the step S3 is 1000-1900 ℃.
Further, the printing powder material in the step S1 includes the following components in parts by mass: 5-20 parts of solid resin powder, 75-90 parts of ceramic powder, 0.1-5 parts of photoinitiator and 0.1-5% of curing agent. .
Further, in the step S1, the solid resin powder is selected from one or more of phenolic resin, epoxy resin and unsaturated polyester resin, and the ceramic powder is selected from one or more of silicon carbide, boron carbide, alumina and zirconia.
Compared with the prior art, the preparation method is suitable for preparing large-size ceramic blanks, the structural strength of the material is greatly improved in the forming process through the modes of laser scanning, glue resin spraying and ultraviolet irradiation, the structural strength of the printed biscuit can reach 10-20MPa, and the prepared ceramic product has small deformation and good application prospect.
Drawings
FIG. 1 is a structural view of a boron carbide ceramic member in example 2 of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, specific embodiments thereof are described in detail below. It should be noted that the following examples are only used to illustrate the implementation method and typical parameters of the present invention, and are not used to limit the scope of the parameters of the present invention, so that the reasonable variation can be extended and still fall within the protection scope of the claims of the present invention.
It is noted that the endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and that such ranges or values are understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to yield one or more new ranges of values, which ranges of values are to be considered as specifically disclosed herein.
An embodiment of the present invention discloses a method for preparing a large-sized ceramic, as shown in fig. 1, the method including the steps of:
s1 preparation of powder
And (3) coating and mixing the solid resin powder and the ceramic powder to uniformly wrap a layer of solid resin on the surface of the ceramic powder. The ceramic powder can be coated by mechanical mixing, or by atomization process, sol-gel method, precipitation method, and microemulsion polymerization method. The surface of the ceramic powder is coated with the solid resin, so that the refractive index of the ceramic powder is close to that of the photosensitive resin, the curing effect in the subsequent forming process can be improved, and the forming efficiency is improved. The solid resin powder is selected from one or more of phenolic resin, epoxy resin and unsaturated polyester resin, and the ceramic powder is selected from one or more of silicon carbide, boron carbide, alumina and zirconia according to the requirements of products.
Adding a photoinitiator and a curing agent into the ceramic powder material wrapped with the solid resin, and stirring and mixing at a high speed to obtain printing powder. The photoinitiator is added for catalyzing the light-cured resin to generate a curing reaction in the subsequent forming process, and is selected from any one of TPO, 907 photoinitiator and 184 photoinitiator. The curing agent is used for promoting the subsequent resin curing and improving the biscuit strength, and is selected from any one of urotropine, p-benzenesulfonic acid and xylene sulfonic acid.
The method comprises the following steps of controlling the dosage of solid resin powder, ceramic powder and photoinitiator, wherein the printing powder comprises the following components in percentage by mass: 5-20% of solid resin powder, 75-90% of ceramic powder, 0.1-5% of photo initiator and 0.1-5% of curing agent, thereby ensuring that a high-strength biscuit can be obtained in the subsequent printing and forming step.
S2, printing and forming
And (4) placing the printing powder in printing equipment for printing and forming. The printing equipment used in the step comprises a workbench, a roller grinding machine, a laser, an ultraviolet light source and two spray heads. And a layer-by-layer printing forming method is adopted, each layer of model generates a corresponding printing path through a computer, and powder paving is carried out by adopting roller grinding, so that the uniform thickness is ensured.
The forming process of each layer of powder is as follows:
s201, scanning powder by a laser, and sintering and molding the powder by laser scanning. The laser power of the laser is 5W-60W.
S202, respectively spraying light-cured resin and glue-spraying resin to the powder by two spray heads while scanning by the laser. The glue spraying resin can improve the bonding effect among the powder materials, so that the material strength is improved, the glue spraying resin is selected from one or more of phenolic resin solution, furan resin solution, PVA resin solution and PVP resin solution, the use amount of the glue spraying resin in each layer of blank body is controlled to be 3% -15% of the mass of the printing powder materials, and the structural strength of the ceramic material is improved under the condition of keeping the performance of the ceramic material. The photocuring resin is used for subsequent photocuring reinforcement, the photocuring resin is selected from one or more of HEMA, HDDA and TMPTA, the dosage of the photocuring resin in each layer of blank is controlled to be 2% -10% of the mass of the printing powder, and the structural strength of the ceramic material is improved under the condition of keeping the performance of the ceramic material.
S203, after the laser scanning and glue spraying are finished, the powder is irradiated by the ultraviolet light source, and the photoinitiator catalyzes the photocuring resin to react, cure and form, so that the strength of the material is further enhanced. The irradiation power of the ultraviolet light source is 5-30W.
In the steps, the layer height of each layer of model is controlled to be 0.01-5mm, the laser power of the laser and the irradiation power of the ultraviolet light source are higher, the powder forming speed can be accelerated, and the forming efficiency is improved. The molding step combines laser scanning, glue resin spraying and ultraviolet irradiation technologies, each step can reinforce the material, the layer height of each layer of model can be controlled to be larger, and the preparation of large-size ceramics is facilitated.
And after one layer of powder is formed, repeating the steps, and stacking layer by layer to finally obtain the printing biscuit.
S3, sintering
And sintering the printing biscuit in a sintering furnace to obtain a ceramic body, wherein the sintering temperature is 1000-1900 ℃, and the sintering time is 1-5h, so as to obtain the ceramic body.
Tests show that the strength of the printed biscuit prepared by the method can reach 10-20MPa, the strength is obviously higher than that of a ceramic material prepared by the existing rapid forming technology, the printed biscuit is suitable for preparing large-size ceramic products, the structure and the size of the prepared ceramic products are basically consistent with those of target products, and the deformation amount is small.
The present invention will be described in detail below by way of specific examples.
Example 1
This example produced a large-size silicon carbide ceramic member having a disk structure and a diameter of 1500 mm.
The preparation method of the silicon carbide ceramic component comprises the following steps:
s1, heating and mechanically mixing 10 parts of phenolic resin powder and 90 parts of silicon carbide powder to obtain silicon carbide powder coated with phenolic resin; then adding 2 parts of TPO photoinitiator and 2 parts of urotropine, and stirring and mixing at a high speed to obtain the printing powder.
And S2, placing the printing powder in a printing device for printing and molding. And (3) adopting a layer-by-layer printing and forming method, generating a corresponding printing path for each layer of model through a computer, and paving powder by adopting a roller grinding method, wherein the layer height of each layer of model is 0.1mm, and the printing speed is 1000 mm/s. The forming process of each layer of powder is as follows: scanning powder by a laser, wherein the laser power is 20W; simultaneously, two spray heads respectively spray HEMA and phenolic resin solution to the powder, wherein the dosage of the HEMA is 2% of the mass of the printing powder, and the dosage of the phenolic resin solution is 3% of the mass of the printing powder; after the laser scanning and glue spraying are finished, the powder is irradiated by an ultraviolet light source, and the irradiation power is 5W. And repeating the steps after forming a layer of powder, and stacking layer by layer to finally obtain the printing biscuit.
S3, placing the printing biscuit in a sintering furnace for reaction siliconizing sintering, wherein the sintering temperature is 1600 ℃, and keeping the temperature for 3h to obtain the structural component shown in figure 1.
The biscuit structural strength is tested to be 15.6Mpa, the finally sintered ceramic product conforms to the size of the designed product, and the deformation amount is less than 1.5 mm.
Example 2
This example produced a large-sized boron carbide ceramic member having a structure as shown in FIG. 1, which was a tubular structure having a diameter of 700mm and a height of 850 mm.
The preparation method of the boron carbide ceramic component comprises the following steps:
s1, heating and mechanically mixing 15 parts of epoxy resin powder and 83 parts of boron carbide powder to obtain boron carbide powder wrapped with epoxy resin; then 2 parts of 907 light initiator and 1 part of p-benzenesulfonic acid are added, and the mixture is stirred and mixed at high speed to obtain the printing powder.
And S2, placing the printing powder in a printing device for printing and molding. And (3) adopting a layer-by-layer printing and forming method, generating a corresponding printing path for each layer of model through a computer, and paving powder by adopting a roller grinding method, wherein the layer height of each layer of model is 0.3mm, and the printing speed is 5000 mm/s. The forming process of each layer of powder is as follows: scanning powder by a laser, wherein the laser power is 30W; simultaneously, two spray heads respectively spray low-viscosity HDDA and furan resin solution to the powder, wherein the amount of the HDDA is 5% of the mass of the printing powder, and the amount of the furan resin solution is 10% of the mass of the printing powder; after the laser scanning and glue spraying are finished, the powder is irradiated by an ultraviolet light source, and the irradiation power is 15W. And repeating the steps after forming a layer of powder, and stacking layer by layer to finally obtain the printing biscuit.
And S3, placing the printing biscuit in a sintering furnace for siliconizing reaction sintering, wherein the sintering temperature is 1550 ℃, and keeping the temperature for 4 hours to obtain the structural member.
The strength of the structural biscuit is tested to be 17.8Mpa, the structural biscuit conforms to the size of a designed product, and the deformation amount is less than 0.5 mm.
Example 3
This example prepared a large-size zirconia ceramic structure having a cubic structure with a side length of 1000 mm.
The preparation method of the zirconia ceramic component comprises the following steps:
s1, mixing 20 parts of unsaturated polyester resin powder and 79 parts of zirconia powder in a heating machine to obtain zirconia powder wrapping the unsaturated polyester resin; then 0.1 part of 184 photoinitiator and 0.5 part of dimethylbenzene sulfonic acid are added, and the mixture is stirred and mixed at high speed to obtain printing powder.
And S2, placing the printing powder in a printing device for printing and molding. And (3) adopting a layer-by-layer printing and forming method, generating a corresponding printing path for each layer of model through a computer, and paving powder by adopting a roller grinding method, wherein the layer height of each layer of model is 0.2mm, and the printing speed is 2000 mm/s. The forming process of each layer of powder is as follows: scanning powder by a laser, wherein the laser power is 25W; simultaneously, two spray heads respectively spray low-viscosity TMPTA and PVA resin solution to the powder, wherein the amount of the TMPTA is 10% of the mass of the printing powder, and the amount of the PVA resin solution is 4% of the mass of the printing powder; after the laser scanning and glue spraying are finished, the powder is irradiated by an ultraviolet light source, and the irradiation power is 10W. And repeating the steps after forming a layer of powder, and stacking layer by layer to finally obtain the printing biscuit.
And S3, sintering the printing biscuit in a sintering furnace at 1760 ℃ for 3 hours to obtain the structural member.
The structural strength of the biscuit is tested to be 15.0Mpa, the biscuit conforms to the size of a designed product, and the deformation amount is less than 1 mm.
Example 4
This example produced a large-sized silicon carbide ceramic structural member having a plate-like structure with a thickness of 50mm, a length of 1000mm and a width of 300 mm.
The preparation method of the silicon carbide ceramic component comprises the following steps:
s1, heating and mechanically mixing 10 parts of phenolic resin powder and 85 parts of silicon carbide powder to obtain silicon carbide powder wrapped with phenolic resin; then adding 2 parts of TPO photoinitiator and 3 parts of xylene sulfonic acid, and stirring and mixing at high speed to obtain printing powder.
And S2, placing the printing powder in a printing device for printing and molding. And (3) adopting a layer-by-layer printing and forming method, generating a corresponding printing path for each layer of model through a computer, and paving powder by adopting a roller grinding method, wherein the layer height of each layer of model is 0.3mm, and the printing speed is 4000 mm/s. The forming process of each layer of powder is as follows: scanning powder by a laser, wherein the laser power is 30W; simultaneously, two spray heads respectively spray low-viscosity HDDA and PVA resin solutions to the powder, wherein the amount of the HDDA is 8% of the mass of the printing powder, and the amount of the PVA resin solution is 12% of the mass of the printing powder; after the laser scanning and glue spraying are finished, the powder is irradiated by an ultraviolet light source, and the irradiation power is 20W. And repeating the steps after forming a layer of powder, and stacking layer by layer to finally obtain the printing biscuit.
And S3, placing the printed biscuit in a sintering furnace for siliconizing reaction sintering, wherein the sintering temperature is 1600 ℃, and preserving heat for 3 hours to obtain the silicon carbide ceramic structural member.
Although the present invention is disclosed above, the present invention is not limited thereto. Various changes and modifications may be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method for preparing a large-size ceramic, comprising the steps of:
s1, coating and mixing the solid resin powder and the ceramic powder to enable the surface of the ceramic powder to be uniformly coated with a layer of solid resin, adding a photoinitiator and a curing agent into the ceramic powder material coated with the solid resin, and stirring and mixing at a high speed to obtain printing powder;
s2, placing the printing powder in a printing device for printing and molding, adopting a layer-by-layer printing and molding method, generating a corresponding printing path for each layer of model through a computer, spreading powder in a roller extrusion mode, scanning the powder by a laser in the molding process of each layer of powder, respectively spraying light-cured resin and glue-sprayed resin to the powder by two spray heads, irradiating the powder by ultraviolet light for curing and molding, and accumulating layer by layer to form a printing biscuit;
and S3, sintering the printing biscuit in a sintering furnace to obtain a ceramic body.
2. The method for preparing large-size ceramics according to claim 1, wherein the amount of the photocurable resin used in each layer of the green body in step S2 is 2% -10% by mass of the printing powder.
3. The method for preparing large-size ceramics according to claim 2, wherein the amount of the spray resin in each layer of the green body in the step S2 is 3% -15% of the mass of the printing powder.
4. The method for preparing large-size ceramic according to claim 3, wherein the light-cured resin is selected from one or more of HEMA, HDDA and TMPTA, and the glue-spraying resin is selected from one or more of phenolic resin solution, furan resin solution, PVA resin solution and PVP resin solution.
5. The method for preparing large-sized ceramic according to claim 1, wherein the laser power of the laser in the step S2 is 5-60W.
6. The method for preparing large-sized ceramics according to claim 1, wherein the ultraviolet irradiation power in step S2 is 5-30W.
7. The method for preparing large-sized ceramic according to claim 1, wherein the layer height of each layer pattern in the step S2 is 0.01-5 mm.
8. The method for preparing large-size ceramics according to claim 1, wherein the sintering temperature of the sintering furnace in the step S3 is 1000-1900 ℃.
9. The method for preparing large-size ceramics according to any of claims 1 to 8, wherein the printing powder in the step S1 comprises the following components by mass: 5 to 20 percent of solid resin powder, 75 to 90 percent of ceramic powder, 0.1 to 5 percent of photoinitiator and 0.1 to 5 percent of curing agent.
10. The method for preparing large-size ceramic according to claim 9, wherein the solid resin powder in step S1 is selected from one or more of phenolic resin, epoxy resin and unsaturated polyester resin, and the ceramic powder is selected from one or more of silicon carbide, boron carbide, alumina and zirconia.
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| CN116041065A (en) * | 2022-11-28 | 2023-05-02 | 中南大学 | Preparation method of 3D printing B4C-based composite ceramic |
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Application publication date: 20220218 |