CN116199505B - Lamellar interface reinforced photocuring 3D printing ceramic core and preparation method thereof - Google Patents
Lamellar interface reinforced photocuring 3D printing ceramic core and preparation method thereof Download PDFInfo
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- CN116199505B CN116199505B CN202211445224.4A CN202211445224A CN116199505B CN 116199505 B CN116199505 B CN 116199505B CN 202211445224 A CN202211445224 A CN 202211445224A CN 116199505 B CN116199505 B CN 116199505B
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 18
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- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 8
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- PSGCQDPCAWOCSH-UHFFFAOYSA-N (4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl) prop-2-enoate Chemical compound C1CC2(C)C(OC(=O)C=C)CC1C2(C)C PSGCQDPCAWOCSH-UHFFFAOYSA-N 0.000 claims description 5
- IQQVCMQJDJSRFU-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.CCC(CO)(CO)CO IQQVCMQJDJSRFU-UHFFFAOYSA-N 0.000 claims description 5
- 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 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
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- 235000012241 calcium silicate Nutrition 0.000 claims description 5
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 5
- 229910052839 forsterite Inorganic materials 0.000 claims description 5
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052863 mullite Inorganic materials 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 4
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- OTRIMLCPYJAPPD-UHFFFAOYSA-N methanol prop-2-enoic acid Chemical compound OC.OC.OC(=O)C=C.OC(=O)C=C OTRIMLCPYJAPPD-UHFFFAOYSA-N 0.000 claims description 3
- FSAJWMJJORKPKS-UHFFFAOYSA-N octadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C=C FSAJWMJJORKPKS-UHFFFAOYSA-N 0.000 claims description 3
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- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- B33—ADDITIVE MANUFACTURING TECHNOLOGY
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- 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
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Abstract
The invention relates to a laminar interface reinforced photo-curing 3D printing ceramic core and a preparation method thereof, wherein the preparation method comprises the following steps: and preparing the ceramic mixed powder and the liquid phase curing agent into the photo-curing 3D printing ceramic slurry. The ceramic mixed powder comprises a framework material and a first reinforcing agent; the first reinforcing agent is used for improving the interface strength between any two adjacent layers in the layered structure in the photocuring 3D printing ceramic core; wherein, the first enhancer is one or more of La 2O3、Y2O3、SiO2、ZrO2; the particle size of the first enhancer is 5-35nm; performing photocuring 3D printing forming on the photocuring 3D printing ceramic slurry to obtain a photocuring 3D printing ceramic biscuit; degreasing treatment and sintering treatment are carried out on the photo-curing 3D printing ceramic biscuit to obtain the photo-curing 3D printing ceramic core. The method is used for strengthening the interface between any two adjacent layers in the layered structure in the photocuring 3D printing ceramic core, and improving the strength of the photocuring 3D printing ceramic core.
Description
Technical Field
The invention relates to the technical field of ceramic cores for additive manufacturing, in particular to a photocuring 3D printing ceramic core with strengthened lamellar interfaces and a preparation method thereof.
Background
With the progress of technology and the development of times, the technical fields of high-end equipment, semiconductors, clean energy, fine chemical engineering, advanced manufacturing, aerospace and the like provide higher requirements on the complex structure and the structural precision of the precise ceramic component, so that the development of the complex structure and the preparation technology of the high-precision ceramic component based on the photo-curing 3D printing technology is particularly important.
At present, application attempts of photocuring 3D printing ceramic cores have been made in the fields of complex structures, high-precision large-scale components (for example, ceramic pump impellers, ceramic casting molds for turbine blade complex castings and the like) and small-scale components (for example, alumina ceramic cleavers, microchannel reactors and the like).
Since the photo-curing 3D printing technology is a three-dimensional entity constructed by mixing photosensitive resin and ceramic powder and curing and forming the mixture layer by using ultraviolet light, a typical layered structure exists in the photo-curing 3D printing ceramic core. Thus, the photocured 3D-printed ceramic cores exhibit significant anisotropic sintering shrinkage and performance, which greatly limits the molding accuracy of the technique. In addition, due to the appearance of the lamellar interfaces, the interfaces are the weakest areas of the overall material, becoming the preferred areas for sintering cracking and crack propagation. Based on this problem, it is widely accepted in the art that this interface is formed because the sedimentation of the ceramic powder in the slurry forms a transition layer, which, after degreasing, forms a layered structure. The sheets are indirectly connected by discrete ceramic particles, resulting in interfaces that are the weakest areas of the overall material.
At present, most research work is focused on preparing ceramic slurries with higher and more stable solids content, and inhibiting sedimentation. For example, the printing speed is optimized by designing and optimizing the content of the surfactant or dispersant in the slurry, the printing thickness of the monolayer, adjusting the ceramic particle size and the volume fraction of the content, and the like. Although these methods improve the layered structure of the 3D printed ceramic core to some extent, the interface of the layered structure still exists, which is a weak area of the whole material, restricting the wider use of the whole technology, and further improvement and reinforcement are needed.
Disclosure of Invention
In view of this, the present invention provides a photocuring 3D printing ceramic core with reinforced lamellar interfaces and a preparation method thereof, and is mainly aimed at reinforcing interfaces between any two adjacent layers in a lamellar structure in the photocuring 3D printing ceramic core so as to improve the strength of the photocuring 3D printing ceramic core.
In order to achieve the above purpose, the present invention mainly provides the following technical solutions:
In one aspect, an embodiment of the present invention provides a method for preparing a laminar interface-reinforced photo-cured 3D printing ceramic core, including the steps of:
preparing a photo-curing 3D printing ceramic slurry: preparing the ceramic mixed powder and a liquid phase curing agent into photo-curing 3D printing ceramic slurry; wherein the ceramic mixed powder comprises a framework material and a first reinforcing agent; the first reinforcing agent is used for improving the interface strength between any two adjacent layers in the layered structure in the photocuring 3D printing ceramic core; wherein the first enhancer is one or more of La 2O3、Y2O3、SiO2、ZrO2; the particle size of the first enhancer is 5-35nm;
Preparing a photo-curing 3D printing ceramic biscuit: performing photocuring 3D printing forming treatment on the photocuring 3D printing ceramic slurry to obtain a photocuring 3D printing ceramic biscuit;
Degreasing and sintering: and degreasing and sintering the photocuring 3D printing ceramic biscuit to obtain the photocuring 3D printing ceramic core.
Preferably, the framework material comprises a framework propping agent, a framework reinforcing agent and a framework filling agent; wherein the framework propping agent is one or more of SiO 2、Al2O3, mullite powder and zircon powder; the skeleton enhancer is one or more of SiO 2、ZrO2、ZrSiO4; the skeleton filler is one or more of CuO, tiO 2、MnO2、SiO2, caO and MgO.
Preferably, the particle size of the framework proppants is 25-55 μm; and/or the particle size of the skeleton reinforcing agent is 0.5-5 mu m; and/or the particle size of the skeleton filler is 0.5-2 μm.
Preferably, the ceramic mixed powder further comprises a second enhancer for improving the high-temperature creep resistance of the photocuring 3D printing ceramic core; wherein the second strengthening agent comprises one or more of Al 2O3, magnesia-alumina spinel, magnesia-chrome spinel, calcium metasilicate and forsterite; preferably, the particle size of the second enhancer is 10-30 μm.
Preferably, the ceramic mixed powder comprises the following components in parts by weight:
35-40 parts of framework propping agent;
10-20 parts of skeleton reinforcing agent;
15-25 parts of framework filler;
14-28 parts by weight of a first reinforcing agent;
preferably, when the ceramic mixed powder further includes a second reinforcing agent, the second reinforcing agent is 2 to 6 parts by weight.
Preferably, in the photocuring 3D printing ceramic slurry, the mass of the liquid phase curing agent is 25-50% of the mass of the ceramic mixed powder.
Preferably, the liquid phase curing agent is formed by mixing 65-78% of photosensitive resin, 20-30% of viscosity regulator and 2-5% of photoinitiator in percentage by volume; preferably, the photosensitive resin is selected from one or more of trimethylolpropane triacrylate, trimethylolpropane tetraacrylate and tricyclodecyl dimethanol diacrylate; preferably, the viscosity modifier is one or more of 1, 6-hexanediol diacrylate, isobornyl acrylate and octadecyl acrylate; preferably, the photoinitiator is selected from the group consisting of basf 184, basf 819 and basf 1173.
Preferably, in the step of preparing the photo-cured 3D printed ceramic greenware: the process parameters of the photo-curing 3D printing forming treatment are set as follows: the slurry knife coating speed is 0.02-0.1m/s, the spreading thickness is 100-150 mu m, the curing power is 3-20nW/cm 2, and the single-layer curing time is 5-15s.
Preferably, in the degreasing process, the step of: heating the photocuring 3D printing ceramic biscuit to 350-650 ℃, preserving heat for 180-360min, and then cooling to obtain a degreased photocuring 3D printing ceramic biscuit; preferably, the heating rate is 1-5 ℃/min, and the cooling rate is 1-5 ℃/min.
Preferably, in the step of sintering treatment: heating the degreased photocuring 3D printing ceramic biscuit to 1200-1650 ℃, preserving heat for 360-660min, and cooling to obtain the photocuring 3D printing ceramic core; preferably, the heating rate is 1-3 ℃/min, and the cooling rate is 1-3 ℃/min.
On the other hand, the embodiment of the invention provides a photocuring 3D printing ceramic core with strengthened lamellar interfaces, wherein the photocuring 3D printing ceramic core is provided with a lamellar structure; wherein the interface strength between any two layers in the layered structure is 10-50MPa; the crack rate of the photo-curing 3D printing ceramic core is 0.1-5%, and the bending strength is 10-40MPa; preferably, the layered interface-reinforced photo-curing 3D printing ceramic core is prepared by the preparation method of the layered interface-reinforced photo-curing 3D printing ceramic core.
Compared with the prior art, the laminar interface reinforced photo-curing 3D printing ceramic core and the preparation method thereof have at least the following beneficial effects:
The embodiment of the invention provides a preparation method of a layered interface reinforced photocuring 3D printing ceramic core, which comprises the steps of adding a first reinforcing agent (one or more of La 2O3、Y2O3、SiO2、ZrO2 with the particle size of 5-35 nm) when preparing photocuring 3D printing ceramic slurry; the first reinforcing agent with the particle size is enriched at the interface between adjacent layers in the layered structure under the action of fluid by utilizing the slurry flow characteristic in the spreading process of the photocuring 3D printing ceramic technology, and the first reinforcing agent is ceramic powder with low melting point, small particle size and more activity, and is easy to react with other ceramic cores to generate refractory ceramic phases with excellent high-temperature mechanical properties, so that the layered interface in the ceramic cores can be reinforced. Here, the reinforced layered interface is to solve the problem of "the ceramic chip layered structure is easily cracked, sintered shrinkage, and anisotropy of mechanical properties" existing in the prior art. Wherein, the anisotropy of the ceramic core can lead to cracking, deformation and reduced precision of the ceramic core in the sintering process. Therefore, the scheme of the embodiment of the invention ensures the strength and the precision of the photocuring 3D printing ceramic core by strengthening the layered interface in the ceramic core.
Further, the embodiment of the invention provides a preparation method of a layered interface reinforced photo-curing 3D printing ceramic core, which is characterized in that a framework material is designed to comprise a framework propping agent (the grain diameter is 25-55 mu m, one or more of SiO 2、Al2O3, mullite powder and zircon powder are selected), a framework reinforcing agent (the grain diameter is 0.5-5 mu m, one or more of SiO 2、ZrO2、ZrSiO4 are selected), and a framework filling agent (the grain diameter is 0.5-2 mu m, and one or more of CuO, tiO 2、MnO2、SiO2, caO and MgO are selected); the framework is reinforced by the conception of framework design, framework reinforcement and framework filling, so that the strength of the ceramic core is enhanced and the compactness of the ceramic core is controllable.
Meanwhile, the skeleton filler comprises metal oxide and glass phase filling oxide, crystal lattice vacancies are introduced, so that the diffusion is easy, the sintering activation energy is reduced, a solid solution is formed, and the internal structure of the ceramic is further strengthened; in addition, the glass phase filling oxide is easy to generate liquid phase in the sintering process, so that a mass transfer machine is changed from solid phase diffusion to liquid phase diffusion, and the sintering temperature is reduced.
Further, the embodiment of the invention provides a preparation method of a layered interface reinforced photo-curing 3D printing ceramic core, which fully utilizes the fluid rule in the slurry blade coating process to fully enrich a first reinforcing agent (interface reinforcing agent) through the coordination of the particle size design of the first reinforcing agent (interface reinforcing agent) with printing parameters and sintering parameters, and finally fully plays the reinforcing role of the layered interface reinforcing agent and a skeleton filler by utilizing the cooperative control of the sintering parameters.
Further, the embodiment of the invention provides a preparation method of the photocuring 3D printing ceramic core with strengthened lamellar interfaces, and a second strengthening agent is added in the preparation of the photocuring 3D printing ceramic slurry. The second reinforcing agent is an oxide which is stable at high temperature and has high melting point. The use of the second reinforcing agent can significantly improve the high-temperature creep resistance of the ceramic core and increase the high-temperature casting temperature limit of the ceramic core.
The foregoing description is only an overview of the present invention, and is intended to provide a better understanding of the present invention, as it is embodied in the following description, with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
Fig. 1 is a back-scattered SEM inspection photograph of a cross-sectional layered structure of a photo-cured 3D printing ceramic core prepared in example 1.
Fig. 2 is a graph showing the element distribution detection result of the printing stack surface of the photo-cured 3D printing ceramic core prepared in example 1 of the present invention.
Detailed Description
In order to further describe the technical means and effects adopted for achieving the preset aim of the invention, the following detailed description refers to the specific implementation, structure, characteristics and effects according to the application of the invention with reference to the accompanying drawings and preferred embodiments. In the following description, different "an embodiment" or "an embodiment" do not necessarily refer to the same embodiment. Furthermore, the particular features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.
Based on the problems of the background technology, the inventor of the invention considers that from the other thinking, namely from the angle of strengthening the interface, the formation of the layered interface in the layered structure is more important, in the process of doctor-blading the photocuring 3D printing slurry, small-size particles are enriched on the interface and large particles remain in the middle area of the slurry layer due to the flow velocity difference of different positions of the slurry layer, so that the interface sintering is compact, and the pores of the middle layer are larger to form an obvious layered structure. Based on the thought, the invention provides a novel photocuring 3D printing ceramic core with strengthened lamellar interfaces and a preparation method by utilizing the flow characteristic of photocuring 3D printing slurry in the knife coating process, so as to solve the problems of interfacial cracking and crack propagation of the photocuring 3D printing ceramic lamellar structure.
The specific scheme of the invention is as follows:
In one aspect, the embodiment of the invention provides a preparation method of a laminar interface reinforced photo-curing 3D printing ceramic core, which comprises the following steps:
Preparing a photo-curing 3D printing ceramic slurry: preparing the ceramic mixed powder and a liquid phase curing agent into photo-curing 3D printing ceramic slurry; wherein the ceramic mixed powder comprises a framework material and a first reinforcing agent; wherein the first reinforcing agent is used for improving the strength of a lamellar interface in the photo-cured 3D printing ceramic core (the lamellar interface refers to an interface between any two adjacent layers in a lamellar structure in the photo-cured 3D printing ceramic core); wherein the first enhancer is one or more of La 2O3、Y2O3、SiO2、ZrO2; the particle size of the first enhancer is 5-35nm.
Preferably, the framework material comprises a framework proppant, a framework enhancer, and a framework filler; wherein, the skeleton propping agent is one or more of SiO 2、Al2O3, mullite powder and zircon powder; the skeleton enhancer is one or more of SiO 2、ZrO2、ZrSiO4; the skeleton filler is one or more of CuO, tiO 2、MnO2、SiO2, caO and MgO. Preferably, the particle size of the framework proppants is 25-55 μm; the grain diameter of the skeleton strengthening agent is 0.5-5 mu m; the particle size of the skeleton filler is 0.5-2 mu m.
Preferably, the ceramic mixed powder further comprises a second enhancer for improving the high-temperature creep resistance of the photocuring 3D printing ceramic core; wherein the second strengthening agent comprises one or more of Al 2O3, magnesia-alumina spinel, magnesia-chrome spinel, calcium metasilicate and forsterite; preferably, the particle size of the second enhancer is 10-30 μm.
Preferably, the ceramic mixed powder comprises the following components in parts by weight: 35-40 parts of framework propping agent; 10-20 parts of skeleton reinforcing agent; 15-25 parts of framework filler; 14-28 parts by weight of a first reinforcing agent; preferably, when the ceramic mixed powder further includes a second reinforcing agent, the second reinforcing agent is 2 to 6 parts by weight.
Preferably, in the photocuring 3D printing ceramic slurry, the mass of the liquid phase curing agent is 25-50% of the mass of the ceramic mixed powder.
Preferably, the liquid phase curing agent is formed by mixing 65-78% of photosensitive resin, 20-30% of viscosity regulator and 2-5% of photoinitiator in percentage by volume; preferably, the photosensitive resin is selected from one or more of trimethylolpropane triacrylate, trimethylolpropane tetraacrylate and tricyclodecyl dimethanol diacrylate; preferably, the viscosity modifier is one or more of 1, 6-hexanediol diacrylate, isobornyl acrylate and octadecyl acrylate; preferably, the photoinitiator is selected from the group consisting of basf 184, basf 819 and basf 1173.
Preferably, the steps are as follows: mechanically stirring a framework propping agent, a framework reinforcing agent, a framework filling agent, a first reinforcing agent and a second reinforcing agent to obtain ceramic mixed powder; and adding the 3D printing ceramic mixed powder into a liquid phase curing agent, and carrying out heat preservation and stirring to obtain the photo-curing 3D printing ceramic slurry.
Preparing a photo-curing 3D printing ceramic biscuit: and (3) performing photocuring 3D printing forming on the photocuring 3D printing ceramic slurry to obtain a photocuring 3D printing ceramic biscuit.
The method specifically comprises the following steps: setting photocuring 3D printing technological parameters, and carrying out photocuring forming treatment on the photocuring 3D printing ceramic slurry by utilizing a photocuring 3D printer to obtain a photocuring 3D printing ceramic biscuit.
Wherein, the photo-curing 3D printing process parameters are as follows: the slurry knife coating speed is 0.02-0.1m/s, the spreading thickness is 100-150 mu m, the curing power is 3-20nW/cm 2, and the single-layer curing time is 5-15s.
Degreasing and sintering: degreasing treatment and sintering treatment are carried out on the photo-curing 3D printing ceramic biscuit to obtain the photo-curing 3D printing ceramic core.
In this step, the degreasing treatment is specifically: heating the photocuring 3D printing ceramic biscuit to 350-650 ℃, preserving heat for 180-360min, and then cooling; preferably, the heating rate is 1-5 ℃/min, and the cooling rate is 1-5 ℃/min.
The sintering treatment is specifically as follows: heating the photo-cured 3D printing ceramic biscuit subjected to degreasing treatment to 1200-1650 ℃, preserving heat for 360-660min, and then cooling; preferably, the heating rate is 1-3 ℃/min, and the cooling rate is 1-3 ℃/min.
On the other hand, the embodiment of the invention also provides a layered interface reinforced photo-curing 3D printing ceramic core, wherein the layered interface reinforced photo-curing 3D printing ceramic core is prepared by the preparation method of the layered interface reinforced photo-curing 3D printing ceramic core. Wherein, the photocuring 3D printing ceramic core is provided with a layered structure; wherein the interface strength between any two layers in the layered structure is 10-50MPa; the crack rate of the photo-curing 3D printing ceramic core is 0.1-5%, and the bending strength is 10-40MPa.
Here, the above-described aspects of the present invention are described as follows:
(1) According to the method, by utilizing the slurry flow characteristic of the photocuring 3D printing ceramic technology in the spreading process, through selection and design of powder with different particle sizes, the nano lamellar interface enhancer (first enhancer) is enriched on lamellar interfaces (interfaces between adjacent layers in a lamellar structure) under the action of fluid, the first enhancer is ceramic powder with low melting point, small granularity and more activity, is easy to react with other ceramic cores to generate a refractory ceramic phase with excellent high-temperature mechanical property, and improves the high-temperature strength of the material while strengthening the interfaces of the ceramic cores.
(2) The method strengthens the framework through the conception of framework design, framework strengthening and framework filling, wherein the strengthening effect of the framework enhances the strength of the ceramic core and the density of the ceramic core is controllable.
(3) The skeleton filler selected by the method comprises metal oxide and glass phase filling oxide, and crystal lattice vacancies are introduced, so that the skeleton filler is easy to diffuse, reduces sintering activation energy, forms solid solution and further strengthens internal structure of ceramic; in addition, the glass phase filling oxide is easy to generate liquid phase in the sintering process, so that a mass transfer machine is changed from solid phase diffusion to liquid phase diffusion, and the sintering temperature is reduced.
(4) According to the invention, through coordination of the grain size design of the reinforcing agent, the printing parameters and the sintering parameters, the interface reinforcing agent is fully enriched by fully utilizing the fluid rule in the slurry blade coating process, and the reinforcing effect of the layered interface reinforcing agent and the skeleton filler is fully exerted by utilizing the cooperative control of the sintering parameters.
The invention is further illustrated by the following specific examples:
example 1
The embodiment provides a preparation method of a laminar interface reinforced photo-curing 3D printing ceramic core, wherein the ceramic mixed powder comprises the following components in parts by weight: the framework material (40 parts by weight of framework propping agent, 10 parts by weight of framework reinforcing agent, 25 parts by weight of framework filling agent), 5 parts by weight of second reinforcing agent and 20 parts by weight of first reinforcing agent. Wherein the addition amount of the liquid phase curing agent is 30% of the weight of the ceramic mixed powder (wherein the liquid phase curing agent comprises 78% of photosensitive resin, 20% of viscosity modifier and 2% of photoinitiator in terms of volume fraction), wherein the skeleton propping agent is SiO 2 with the particle size of 55 mu m, and the skeleton strengthening agent is mixed powder of ZrSiO 4 and SiO 2 with the particle size of 5 mu m (the mass ratio of ZrSiO 4 to SiO 2 is 3:1); the skeleton filler is mixed powder of CuO and SiO 2 (the mass ratio of CuO to SiO 2 is 1:1) with the thickness of 2 mu m; the second strengthening agent (high temperature strengthening agent) was 30 μm of Al 2O3 and magnesia-alumina spinel (the mass ratio of Al 2O3 and magnesia-alumina spinel was 4:3). The first reinforcing agent (lamellar interface reinforcing agent) was ZrO 2 at 35 nm. The photosensitive resin is trimethylolpropane triacrylate, the viscosity modifier is 1, 6-hexanediol diacrylate, and the photoinitiator is Basoff 819.
The preparation method of the laminar interface reinforced photo-curing 3D printing ceramic core provided by the embodiment specifically comprises the following steps:
(1) Weighing the framework propping agent, the framework reinforcing agent, the framework filling agent, the second reinforcing agent and the first reinforcing agent, and mechanically stirring and uniformly mixing to obtain ceramic mixed powder.
And (3) weighing trimethylolpropane triacrylate, 1, 6-hexanediol diacrylate and basf 819, adding the obtained mixture into ceramic mixed powder, and stirring for 90 minutes at the temperature of 80 ℃ to obtain the photo-curing 3D ceramic slurry.
(2) Setting 3D printing parameters (slurry knife coating speed is 0.02m/s, spreading thickness is 100 mu m, curing power is 3.8nW/cm 2, single-layer curing time is 5 s), and performing photo-curing molding on photo-curing ceramic slurry to obtain photo-curing 3D printing ceramic biscuit.
(3) Degreasing and sintering the photo-curing 3D printing ceramic biscuit to obtain the photo-curing 3D printing ceramic core. Wherein, the degreasing treatment conditions are as follows: heating the photocuring 3D printing ceramic biscuit to 550 ℃ in air, preserving heat for 360min, and then cooling to obtain a degreased photocuring 3D printing ceramic biscuit; wherein, the heating speed and the cooling speed are both 1 ℃/min. The sintering treatment conditions are as follows: heating the photo-cured 3D printing ceramic biscuit subjected to degreasing treatment to 1250 ℃ in air, and preserving heat for 600min to obtain photo-cured 3D printing ceramic slurry; wherein, the heating speed and the cooling speed are 3 ℃/min.
Fig. 1 is a back-scattered SEM inspection photograph of a layered structure in a cross section of a photo-cured 3D printing ceramic core prepared in example 1, wherein the cross section thereof is enriched with large-sized ceramic particles and small-sized particles are enriched at an interface of the layered structure due to a difference in flow characteristics of slurry during slurry blade coating. The small-size ceramic particles are easy to sinter, the vicinity of the interface is relatively compact, and the inside of the sheet layer is formed into macropores due to the enrichment of the ceramic particles with larger sizes. In example 1, the first reinforcing agent (interface reinforcing agent) added was mainly ZrO 2, and it was observed to appear bright white by back-scattered SEM. The formulation and process design of this example are expected to meet the requirements from SEM pictures. By means of the flow state difference of the sizing agent at different positions in the sizing agent knife coating process of the photo-curing 3D printing process, enrichment and sintering reinforcement of the first reinforcing agent (interface reinforcing agent) on the interface are achieved.
Fig. 2 is a graph showing the element distribution detection result of the printing stack face of the photo-cured 3D printing ceramic core prepared in example 1. From the element distribution, zr element is enriched near the layered interface, and Si element is enriched inside the sheet layer. It can be judged that nano ZrO 2 is enriched on the interface, and large-particle SiO 2 is taken as a framework in the layer.
Example 2
The embodiment provides a preparation method of a laminar interface reinforced photo-curing 3D printing ceramic core, wherein the ceramic mixed powder comprises the following components in parts by weight: 35 parts of framework material (framework propping agent, 20 parts of framework reinforcing agent and 15 parts of framework filling agent), 6 parts of second reinforcing agent (high-temperature reinforcing agent) and 24 parts of first reinforcing agent (lamellar interface reinforcing agent). Wherein the addition amount of the liquid phase curing agent is 50% of the weight of the ceramic mixed powder. The liquid phase additive comprises 65% of photosensitive resin, 30% of viscosity modifier and 5% of photoinitiator by volume fraction. Wherein, the framework propping agent is Al 2O3 and SiO 2 with the grain diameter of 25 μm, wherein, al 2O3 and SiO 2 are mixed according to the mass ratio of 3:1. The skeleton strengthening agent is ZrSiO 4 and ZrO 2 powder with the particle size of 0.5 mu m according to the following weight ratio of 4:1. The skeleton filler is TiO 2 and MgO powder with the mass ratio of TiO 2 to MgO being 2:1. The second strengthening agent (high temperature strengthening agent) is 10 mu m of calcium metasilicate and forsterite powder, wherein the calcium metasilicate and the forsterite are mixed according to the mass ratio of 5:1; the first reinforcing agent (lamellar interface reinforcing agent) is Y 2O3 and SiO 2 with a mass ratio of Y 2O3 to SiO 2 of 3:1; the photosensitive resin is trimethylolpropane tetra-acrylate, the viscosity modifier is isobornyl acrylate, and the photoinitiator is basf 819.
The preparation method of the laminar interface reinforced photo-curing 3D printing ceramic core provided by the embodiment specifically comprises the following steps:
(1) Weighing the framework propping agent, the framework reinforcing agent, the framework filling agent, the second reinforcing agent and the first reinforcing agent, and mechanically stirring and uniformly mixing to obtain ceramic mixed powder.
Weighing trimethylolpropane tetra-acrylate, isobornyl acrylate and basf 819, adding into ceramic mixed powder, preserving heat at 80 ℃ and stirring for 90 minutes to prepare the photo-curing 3D printing ceramic slurry.
(2) Setting 3D printing parameters (slurry knife coating speed is 0.1m/s, spreading thickness is 150 mu m, curing power is 20nW/cm 2, single-layer curing time is 5 s), and curing and forming the photo-curing 3D printing ceramic slurry obtained in the step (1) to obtain a photo-curing 3D printing ceramic biscuit.
(3) And (3) degreasing and sintering the photo-curing 3D printing ceramic biscuit obtained in the step (2) to obtain the photo-curing 3D printing ceramic core. The degreasing treatment condition is that in air, the photo-curing 3D printing ceramic biscuit is heated to 650 ℃, and the temperature is kept for 180 minutes and then is reduced to obtain the photo-curing 3D printing ceramic biscuit after the degreasing treatment; wherein, the heating speed and the cooling speed are 5 ℃/min; the sintering treatment condition is that in the air, the temperature of the photo-curing 3D printing ceramic biscuit after degreasing treatment is raised to 1650 ℃, and the temperature is kept for 360 minutes, so as to obtain photo-curing 3D printing ceramic slurry; wherein, the heating speed and the cooling speed are both 1 ℃/min.
Comparative example 1
Comparative example 1a method for preparing a photo-cured 3D printing ceramic core, comparative example 1 differs from example 1 in that: (1) The photocuring 3D printing ceramic slurry is not added with a lamellar interface enhancer (first enhancer); (2) The framework material is selected from conventional framework materials, in particular SiO 2 with the particle size of 55 mu m; the others are exactly the same as in example 1.
Here, comparative example 1 is a prior art scheme.
Comparative example 2
Comparative example 2a method of preparing a photo-cured 3D printing ceramic core, comparative example 2 differs from example 1 in that: the photocuring 3D printing ceramic slurry is not added with a lamellar interface enhancer (first enhancer); the others are exactly the same as in example 1.
In addition, the invention also provides a comparative example 3 and a comparative example 4; here, comparative examples 3 and 4 are main concepts employing the present invention, but do not employ the preferred embodiments of the present invention.
Comparative example 3
Comparative example 3a method of preparing a photo-cured 3D printing ceramic core, comparative example 3 differs from example 1 in that: the framework material is selected from conventional framework materials, in particular SiO 2 with the particle size of 55 mu m; the others are exactly the same as in example 1.
Comparative example 4
Comparative example 4a method of preparing a photo-cured 3D printing ceramic core, comparative example 4 differs from example 1 in that: (1) setting the photo-curing 3D printing parameters as follows: the slurry blade coating speed is 1m/s, the thickness of the spreading material is 200 mu m, the curing power is 2nW/cm 2, and the single-layer curing time is 20s. (2) setting the sintering process to: heating the degreased photocuring 3D printing ceramic biscuit to 1100 ℃, preserving heat for 300min, and then cooling to obtain a photocuring 3D printing ceramic core; wherein, the heating rate is 10 ℃/min, and the cooling rate is 10 ℃/min. The others are exactly the same as in example 1.
Comparative example 5
Comparative example 5 a method of preparing a photo-cured 3D printing ceramic core, comparative example 5 differs from example 1 in that: no second strengthening agent (i.e., high temperature strengthening agent) is added to the photo-cured 3D printing ceramic slurry. The other points are the same as in example 1.
For test data of indexes such as crack rate and bending strength of the photo-cured 3D printing ceramic cores prepared in the above examples 1 and 2 and comparative examples 1 to 5, the test data are shown in table 1.
TABLE 1
| Detecting items | Crack rate | Flexural Strength | Open porosity | Layered interfacial strength |
| Example 1 | 0.8％ | 38MPa | 38％ | 45MPa |
| Example 2 | 1.4％ | 34MPa | 41％ | 38MPa |
| Comparative example 1 | 21％ | 2.5MPa | 61％ | 8MPa |
| Comparative example 2 | 16％ | 3MPa | 58％ | 7MPa |
| Comparative example 3 | 17％ | 4MPa | 54％ | 18MPa |
| Comparative example 4 | 19％ | 1.8MPa | 59％ | 15MPa |
| Comparative example 5 | 4.3％ | 18MPa | 25％ | 28MPa |
Note that: the layered interface strength in table 1 refers to the interface strength between any two layers in the layered structure of the ceramic core.
As can be seen from the data in table 1:
(1) The cracks in the photo-cured 3D printing ceramic core prepared in the embodiment 1-2 of the invention are obviously reduced, and the bending strength is obviously increased. The layered interface in the layered structure resists crack propagation well during the bending test. In addition, the ceramic core generally needs to ensure about 35% of the open porosity, and the performance parameters are optimal, so that the ceramic core prepared by the embodiment of the invention has excellent performance.
The increase in the open porosity of the ceramic cores prepared in comparative examples 1-2 was due to the cleavage of the layered structure interface.
(2) Compared with comparative examples 1 and 2, the method of the embodiment of the invention can strengthen the lamellar interface in the ceramic core and improve the strength of the photo-cured 3D printing ceramic core by adding the first strengthening agent (lamellar strengthening agent with set grain size) when preparing the photo-cured 3D printing ceramic slurry.
(3) By comparing examples 1-2, comparative examples 1-3, it can be seen that:
The framework material provided by the invention comprises a framework propping agent, a framework reinforcing agent and a framework filling agent; the framework is reinforced by the conception of framework design, framework reinforcement and framework filling, so that the strength of the material can be enhanced and the compactness of the ceramic core can be controlled.
On the basis of adding the first reinforcing agent, the performance of the photocuring 3D printing ceramic core can be further improved by further designing the framework material.
(4) From comparative examples 1 and 4, it can be seen that: the first strengthening agent (interfacial strengthening agent) has a synergistic effect with the printing parameters and sintering parameters. Through setting of printing parameters, the fluid rule in the slurry blade coating process can be fully utilized to fully enrich the first reinforcing agent, and finally, the synergistic control of sintering parameters is utilized to fully play the reinforcing effect of the layered interface reinforcing agent and the skeleton filler.
(5) As can be seen from comparative examples 1 and 5; the second reinforcing agent is added into the photo-curing 3D printing ceramic slurry, so that the performance of the photo-curing 3D printing ceramic core can be further improved.
In summary, compared with the prior art (comparative example 1), the preparation method of the laminar interface-reinforced photo-curing 3D printing ceramic core provided by the invention can reduce the crack rate and improve the laminar interface strength by adding the first reinforcing agent into the photo-curing 3D printing ceramic slurry (compared with comparative example 1, examples 1-2 and comparative examples 3-5 reduce the crack rate and improve the laminar interface strength). But on the basis of adding the first reinforcing agent, the photocuring 3D printing ceramic core is particularly excellent in performance (compared with comparative examples 3-5, the crack rate of examples 1-2 is remarkably reduced, and the bending strength and the lamellar interface strength are remarkably improved) by further cooperating with the design of the framework material, the second reinforcing agent, the photocuring printing parameters and the sintering parameters.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention in any way, but any simple modification, equivalent variation and modification made to the above embodiments according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (14)
1. The preparation method of the laminar interface reinforced photo-curing 3D printing ceramic core is characterized by comprising the following steps of:
preparing a photo-curing 3D printing ceramic slurry: preparing the ceramic mixed powder and a liquid phase curing agent into photo-curing 3D printing ceramic slurry; wherein the ceramic mixed powder comprises a framework material and a first reinforcing agent; the first reinforcing agent is used for improving the interface strength between any two adjacent layers in the layered structure in the photocuring 3D printing ceramic core; wherein the first enhancer is one or more of La 2O3、Y2O3、SiO2、ZrO2; the particle size of the first enhancer is 5-35nm;
Preparing a photo-curing 3D printing ceramic biscuit: performing photocuring 3D printing forming treatment on the photocuring 3D printing ceramic slurry to obtain a photocuring 3D printing ceramic biscuit;
Degreasing and sintering: degreasing and sintering the photocuring 3D printing ceramic biscuit to obtain a photocuring 3D printing ceramic core;
wherein the framework material comprises a framework propping agent, a framework reinforcing agent and a framework filling agent; wherein the framework propping agent is one or more of SiO 2、Al2O3, mullite powder and zircon powder; the skeleton enhancer is one or more of SiO 2、ZrO2、ZrSiO4; the skeleton filler is one or more of CuO, tiO 2、MnO2、SiO2, caO and MgO; the particle size of the framework propping agent is 25-55 mu m; the grain diameter of the skeleton strengthening agent is 0.5-5 mu m; the particle size of the skeleton filler is 0.5-2 mu m;
Wherein, calculated by weight portion, the ceramic mixed powder comprises: 35-40 parts of framework propping agent; 10-20 parts of skeleton reinforcing agent; 15-25 parts of framework filler; 14-28 parts by weight of a first reinforcing agent;
Wherein, in the step of sintering treatment: and heating the degreased photocuring 3D printing ceramic biscuit to 1200-1650 ℃, preserving heat for 360-660min, and cooling to obtain the photocuring 3D printing ceramic core.
2. The method for preparing the laminar interface-reinforced photo-curing 3D printing ceramic core according to claim 1, wherein the ceramic mixed powder further comprises a second reinforcing agent for improving the high-temperature creep resistance of the photo-curing 3D printing ceramic core; wherein,
The second strengthening agent comprises one or more of Al 2O3, magnesia-alumina spinel, magnesia-chrome spinel, calcium metasilicate and forsterite.
3. The method of preparing a laminar interface-reinforced photo-curable 3D printing ceramic core according to claim 2, characterized in that the particle size of the second reinforcing agent is 10-30 μm.
4. The method of preparing a laminar interface-reinforced photo-curable 3D printing ceramic core according to claim 2, characterized in that the second reinforcing agent is 2-6 parts by weight.
5. The method for producing a laminar interface-reinforced photocurable 3D printing ceramic core according to any one of claims 1-4, characterized in that in the photocurable 3D printing ceramic slurry, the mass of the liquid phase curing agent is 25-50% of the mass of the ceramic mixed powder.
6. The method for preparing a laminar interface-reinforced photo-cured 3D printing ceramic core according to claim 5, characterized in that the liquid phase curing agent is mixed by 65-78% of photosensitive resin, 20-30% of viscosity regulator and 2-5% of photoinitiator by volume percent.
7. The method for preparing the laminar interface strengthening photo-curing 3D printing ceramic core according to claim 6, wherein the photosensitive resin is one or more of trimethylolpropane triacrylate, trimethylolpropane tetra-acrylate and tricyclodecyl dimethanol diacrylate.
8. The method for preparing the laminar interface strengthening photo-curing 3D printing ceramic core according to claim 6, wherein the viscosity modifier is one or more of 1, 6-hexanediol diacrylate, isobornyl acrylate and octadecyl acrylate.
9. The method for preparing the laminar interface strengthening photo-curing 3D printing ceramic core according to claim 6, wherein the photoinitiator is selected from the group consisting of Basoff 184, basoff 819 and Basoff 1173.
10. The method of preparing a laminar interface-reinforced photocurable 3D-printable ceramic core according to any one of claims 1-4, characterized in that in the step of preparing a photocurable 3D-printable ceramic green body:
the process parameters of the photo-curing 3D printing forming treatment are set as follows: the slurry knife coating speed is 0.02-0.1m/s, the spreading thickness is 100-150 mu m, the curing power is 3-20nW/cm 2, and the single-layer curing time is 5-15s.
11. The method of producing a laminar interface-reinforced photocurable 3D printing ceramic core according to any one of claims 1-4, characterized in that in the step of degreasing treatment:
And heating the photocuring 3D printing ceramic biscuit to 350-650 ℃, preserving heat for 180-360min, and then cooling to obtain the degreased photocuring 3D printing ceramic biscuit.
12. The method of preparing a laminar interface-reinforced photo-curable 3D printing ceramic mandrel according to claim 11, characterized in that in the step of degreasing treatment:
The temperature rising rate is 1-5 ℃/min, and the temperature reducing rate is 1-5 ℃/min.
13. The method of preparing a laminar interface-reinforced photo-curable 3D printing ceramic mandrel according to claim 1, characterized in that in the step of sintering treatment: the temperature rising rate is 1-3 ℃/min, and the temperature reducing rate is 1-3 ℃/min.
14. The photocuring 3D printing ceramic core with the strengthened lamellar interface is characterized in that the photocuring 3D printing ceramic core is provided with a lamellar structure; wherein the interface strength between any two layers in the layered structure is 10-50MPa; the crack rate of the photo-curing 3D printing ceramic core is 0.1-5%, and the bending strength is 10-40Mpa;
Wherein the laminar interface-reinforced photo-curing 3D printing ceramic core is prepared by the preparation method of the laminar interface-reinforced photo-curing 3D printing ceramic core as claimed in any one of claims 1 to 13.
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