CN114082896A - Photocuring 3D printing aluminum-based ceramic core and preparation method thereof - Google Patents
Photocuring 3D printing aluminum-based ceramic core and preparation method thereof Download PDFInfo
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- CN114082896A CN114082896A CN202111397616.3A CN202111397616A CN114082896A CN 114082896 A CN114082896 A CN 114082896A CN 202111397616 A CN202111397616 A CN 202111397616A CN 114082896 A CN114082896 A CN 114082896A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
- B22C9/10—Cores; Manufacture or installation of cores
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C1/00—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds
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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
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
- B33Y40/20—Post-treatment, e.g. curing, coating or polishing
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention relates to a photocuring 3D printing aluminum-based ceramic core and a preparation method thereof, and relates to the technical field of additive manufacturing ceramic materials. The main technical scheme adopted is as follows: the preparation method of the photocuring 3D printing aluminum-based ceramic core comprises the following steps: mixing the through-hole agent and the pore-forming agent, and drying to obtain a mixed fiber material; wherein the through-hole agent is organic fiber; the pore-forming agent is starch; mixing the mixed fiber material, mixed powder containing framework powder and filler and a light-cured resin pre-polymerization liquid to obtain light-cured 3D printing aluminum-based ceramic core slurry; carrying out photocuring 3D printing treatment on the photocuring 3D printing aluminum-based ceramic core slurry to obtain an aluminum-based ceramic core biscuit; and (4) degreasing and sintering the biscuit of the aluminum-based ceramic core to obtain the photocuring 3D printing aluminum-based ceramic core. The method improves the porosity of the aluminum-based ceramic core and improves the removal performance of the aluminum-based ceramic core on the basis of ensuring the strength and sintering precision of the aluminum-based ceramic core.
Description
Technical Field
The invention relates to the technical field of additive manufacturing ceramic materials, in particular to a photocuring 3D printing aluminum-based ceramic core and a preparation method thereof.
Background
The high-temperature alloy hollow turbine blade is a key component of an aeroengine and a gas turbine, and the ceramic core is an indispensable high-technology product for preparing a complex air-cooled hollow inner cavity structure of the hollow turbine blade and is known as a core. The performance of the ceramic core directly affects the dimensional accuracy and the qualification rate of the inner cavity of the blade.
At present, ceramic cores for hollow turbine blades mainly include silica-based ceramic cores and alumina-based ceramic cores. Compared with the silicon dioxide-based ceramic core, the alumina-based ceramic core has higher fire resistance and high-temperature stability; however, alumina-based ceramic cores suffer from low flexural strength, low porosity, and are difficult to remove. Therefore, it is urgent to widen the range of use of the aluminum-based ceramic core: the strength of the aluminum-based ceramic core is ensured, and the porosity of the aluminum-based ceramic core is improved, so that the problem of removing the aluminum-based ceramic core after the alloy parts are cast is solved.
After the casting of the alloy part is completed, the ceramic core needs to be removed, and specifically, in a high-temperature and high-pressure core-removing reaction kettle, corrosive liquid in the reaction kettle has an opportunity to enter the ceramic core through an opening gap in the ceramic core so as to dissolve and remove the ceramic core. Therefore, open porosity has a greater impact on the removal performance of the ceramic core. However, an increase in the open porosity of the ceramic core may decrease the strength of the ceramic core.
In the prior art, in order to ensure the strength of the ceramic core and improve the porosity of the ceramic core, the sintering degree of ceramic particles is mainly controlled by controlling the technological parameters of degreasing and sintering, so that the balance between the porosity and the strength is obtained; however, the method has the defects of high operation difficulty and unstable process.
In addition, there are also prior art methods to improve the removal performance of ceramic cores by preparing internal topologies of ceramic cores to increase porosity. However, this method has the following problems: the topological structure can greatly reduce the strength of the ceramic core; in the photocuring 3D printing process, due to the fact that the exterior of the topological structure is closed, slurry is difficult to clean; the sintering shrinkage of the topological structure is difficult to control in the degreasing and sintering processes, so that the dimensional accuracy of the ceramic core is poor, and even a compact surface layer on the surface of the ceramic core is cracked.
Disclosure of Invention
In view of this, the invention provides a photocuring 3D printing aluminum-based ceramic core and a preparation method thereof, and mainly aims to improve the porosity of the aluminum-based ceramic core on the basis of ensuring the strength of the aluminum-based ceramic core.
In order to achieve the purpose, the invention mainly provides the following technical scheme:
in one aspect, an embodiment of the present invention provides a method for preparing a photocuring 3D printing aluminum-based ceramic core, which includes the following steps:
preparing photocuring 3D printing aluminum-based ceramic core slurry: mixing the through-hole agent and the pore-forming agent, and drying to obtain a mixed fiber material; wherein the through-hole agent is organic fiber; the pore-forming agent is starch; mixing the mixed fiber material, mixed powder containing framework powder and filler and a light-cured resin pre-polymerization liquid to obtain light-cured 3D printing aluminum-based ceramic core slurry;
photocuring 3D printing treatment: carrying out photocuring 3D printing treatment on the photocuring 3D printing aluminum-based ceramic core slurry to obtain an aluminum-based ceramic core biscuit;
degreasing and sintering treatment: and degreasing and sintering the aluminum-based ceramic core biscuit to obtain the photocuring 3D printing aluminum-based ceramic core.
Preferably, the organic fiber is one or more of polyacrylic fiber, polyethylene fiber, polypropylene alcohol fiber, polyacrylonitrile fiber, polyester fiber, acrylic fiber, cotton fiber, polypropylene fiber and aramid fiber.
Preferably, the organic fiber is chopped fiber with the length of 1-10mm and the diameter of 5-10 μm.
Preferably, the skeleton powder is Al2O3。
Preferably, the particle size of the skeleton powder is 50-100 μm.
Preferably, the filler is SiO2、ZrO2、Y2O3、ZrSiO4One or two of them.
Preferably, the particle size of the filler is 20 to 80 nm.
Preferably, the particle size of the starch is 10-100 nm.
Preferably, the light-curable resin premix comprises a photosensitive resin and a diluent; wherein, the volume fraction of the photosensitive resin is 70-80%, and the volume fraction of the diluent is 20-30%; preferably, the photosensitive resin is one or more of urethane acrylate, polyester acrylate and methacrylate; preferably, the diluent is 1, 6-hexanediol diacrylate.
Preferably, the photocuring 3D printing aluminum-based ceramic core slurry comprises, in parts by weight: 50-70 parts of framework powder, 10-25 parts of filler, 1-5 parts of through-hole agent, 5-10 parts of pore-forming agent and 10-30 parts of light-cured resin premix.
Preferably, in the step of formulating the photocurable 3D-printed aluminum-based ceramic core paste: mixing and stirring the through-hole agent, the pore-forming agent and deionized water, and drying to obtain a mixed fiber material; preferably, the dosage of the deionized water is 5-10% of the sum of the mass of the through hole agent and the mass of the pore-forming agent; preferably, the time for mixing and stirring treatment is 1-2 h.
Preferably, the preparation steps of the mixed powder are as follows: mixing the framework powder, the filler and the absolute ethyl alcohol, and drying to obtain mixed powder; preferably, the using amount of the absolute ethyl alcohol is 10-15% of the sum of the mass of the framework powder and the mass of the filler; preferably, the time for mixing and stirring the skeleton powder, the filler and the absolute ethyl alcohol is 2-3 h.
Preferably, in the step of formulating the photocurable 3D-printed aluminum-based ceramic core paste: and mixing the mixed powder, the mixed fiber material and the light-cured resin premix, and stirring at the temperature of 80-120 ℃ for 8-12 h.
Preferably, in the step of the photocuring 3D printing process, the photocuring 3D printing process parameters are set as: the curing thickness is set to be 50-150 μm, and the curing power is set to be 25-45nW/cm2The monolayer curing time was set to 5-20 s.
Preferably, in the step of degreasing and sintering treatment:
the step of degreasing treatment comprises: in the air atmosphere, heating the aluminum-based ceramic core biscuit to the temperature of 550-600 ℃, and cooling after heat preservation for 180 min; preferably, the heating rate is 60-100 ℃/h, and the cooling rate is 60-100 ℃/h; and/or
The sintering treatment step comprises: in the air atmosphere, heating the degreased aluminum-based ceramic core biscuit to 1300 ℃ and 1500 ℃, preserving the heat for 180min and cooling; preferably, the heating rate is 60-120 ℃/h, and the cooling rate is 60-120 ℃/h.
In another aspect, embodiments of the present invention provide a photocuring 3D printing aluminum-based ceramic core, wherein the bending strength of the photocuring 3D printing aluminum-based ceramic core is 15-25MPa, and the porosity of the opening is 25-40%.
Preferably, the photocuring 3D printing aluminum-based ceramic core is prepared by any one of the preparation methods of the photocuring 3D printing aluminum-based ceramic core.
Compared with the prior art, the photocuring 3D printing aluminum-based ceramic core and the preparation method thereof have at least the following beneficial effects:
on one hand, according to the preparation method of the photocuring 3D printing aluminum-based ceramic core provided by the embodiment of the invention, the pore-forming agent starch and the through-hole agent organic fiber are added into the photocuring 3D printing slurry, so that a large number of small and concentrated closed holes are generated in the degreasing and sintering processes of the small-size pore-forming agent starch, and the through-hole agent organic fiber is decomposed and oxidized into gas to overflow in the degreasing and sintering processes, so that the small holes are communicated, and the porosity of the aluminum-based ceramic core is greatly improved. In addition, the embodiment of the invention can ensure the strength of the aluminum-based ceramic core by adding the mixed powder containing the skeleton powder and the filler into the photocuring 3D printing slurry. Therefore, the preparation method of the photocuring 3D printing aluminum-based ceramic core provided by the embodiment of the invention can improve the porosity of the aluminum-based ceramic core on the basis of ensuring the strength of the aluminum-based ceramic core, thereby improving the removal performance of the aluminum-based ceramic core and enabling the aluminum-based ceramic core to be easily removed after metal parts are cast.
Further, according to the preparation method of the photocuring 3D printing aluminum-based ceramic core provided by the embodiment of the invention, the through-hole agent with the set weight part is added into the photocuring 3D printing slurry, so that the inherent closed pores in the aluminum-based ceramic core are communicated, and the porosity of the aluminum-based ceramic core is obviously improved; in addition, in the degreasing and sintering process, the channels formed by oxidizing and decomposing the organic fibers in a gas form provide channels for the overflow of the generated gas such as resin, pore-forming agent and the like, so that the sintering precision of the aluminum-based ceramic core is ensured, the sintering cracking tendency (difficult cracking in the sintering process) of the aluminum-based ceramic core is reduced, and the strength of the aluminum-based ceramic core is improved.
Further, according to the preparation method of the photocuring 3D printing aluminum-based ceramic core provided by the embodiment of the invention, by adding the pore-forming agent starch in the set weight part, the number of micro pores in the aluminum-based ceramic core can be increased, and the pore-forming agent starch is combined with the organic fiber of the pore-forming agent, so that the porosity of the aluminum-based ceramic core is greatly improved. Preferably, in the mixing treatment process of the pore-forming agent, the through-hole agent and the deionized water, the pore-forming agent can wrap the through-hole agent, so that the through-hole agent is more easily dispersed in the slurry, and thus, in the aluminum-based ceramic biscuit, the pore-forming agent can be intensively distributed around the through-hole agent, and the porosity of the aluminum-based ceramic core can be further improved after degreasing and sintering treatment.
On the other hand, the bending strength of the aluminum-based ceramic core is 15-25MPa, and the porosity is 25-40%, so that the aluminum-based ceramic core provided by the embodiment of the invention has excellent strength performance and high porosity, and is easy to remove after a metal piece is poured.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
Fig. 1 is a process flow diagram of a method for preparing a photocuring 3D printing aluminum-based ceramic core according to an embodiment of the invention.
Fig. 2 is a SEM ceramic core open pore distribution plot taken after the photocured 3D printed aluminum-based ceramic core prepared in example 1 of the present invention was ground and polished.
Detailed Description
To further explain the technical means and effects of the present invention adopted to achieve the predetermined object, the following detailed description of the embodiments, structures, features and effects according to the present invention will be made with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
According to the invention, by utilizing the characteristic that photocuring 3D printing aluminum-based ceramic core slurry is subjected to curing molding by using a photocuring 3D printing technology, through-hole agent organic fibers and pore-forming agent starch are added into the photocuring 3D printing aluminum-based ceramic core slurry; the pore-forming agent can generate a large number of fine holes in the degreasing and sintering processes, and the fibrous organic through-hole agent can be decomposed and oxidized into gas to overflow in the degreasing and sintering processes, so that fine pores are communicated, and the porosity of the ceramic core is greatly improved. On the basis of ensuring the strength and the precision of the aluminum-based ceramic core, the invention increases the porosity of the aluminum-based ceramic core and improves the dissolution loss of the aluminum-based ceramic core.
The scheme of the invention is as follows:
the invention provides a preparation method of a photocuring 3D printing aluminum-based ceramic core, which mainly comprises the following steps as shown in figure 1:
1) and preparing the photocuring 3D printing aluminum-based ceramic core slurry. The method comprises the following steps:
adding absolute ethyl alcohol into the framework powder and the filler, mixing and stirring for 2-3h, and drying to obtain mixed powder; adding deionized water into the through-hole agent and the pore-forming agent, mixing and stirring for 1-2h, and drying to obtain a mixed fiber material; and sequentially adding the mixed powder and the mixed fiber material into the light-cured resin premix, and stirring for 8-12h at the temperature of 80-120 ℃ in a heat preservation manner to obtain the light-cured 3D printing ceramic core slurry.
The through-hole agent is organic fiber, preferably one or more of polyacrylic fiber, polyethylene fiber, polypropylene alcohol fiber, polyacrylonitrile fiber, polyester fiber, acrylic fiber, cotton fiber, polypropylene fiber and aramid fiber. Preferably, the through-hole agent is chopped fiber with the length of 1-10mm and the diameter of 5-10 μm.
Wherein the pore-forming agent is starch.
Wherein the skeleton powder is Al2O3. The skeleton powder is ceramic powder with particle size of 50-100 μm.
Wherein the filler is SiO2、ZrO2、Y2O3、ZrSiO4One or two of them. Preferably, the filler is ceramic powder with the grain diameter of 20-80 nm.
Wherein the light-cured resin premix comprises a photosensitive resin and a diluent; wherein, the volume fraction of the photosensitive resin is 70-80%, and the volume fraction of the diluent is 20-30%. Preferably, the photosensitive resin is one or more of urethane acrylate, polyester acrylate and methacrylate; the diluent is 1, 6-hexanediol diacrylate.
Wherein the photocuring 3D printing ceramic core slurry comprises the following components in parts by weight: 50-70 parts of framework powder, 10-25 parts of filler, 1-5 parts of through-hole agent, 5-10 parts of pore-forming agent and 10-30 parts of light-cured resin premix.
2) A photocuring 3D printing processing step; and carrying out photocuring 3D printing treatment on the photocuring 3D printing aluminum-based ceramic core slurry to obtain an aluminum-based ceramic core biscuit.
In this step, the photocuring 3D printing process parameters are set to: the curing thickness is set to 50-150 μm, and the curing power is set to 25-45nW/cm2The monolayer curing time was set to 5-20 s.
3) Degreasing and sintering treatment: and (4) degreasing and sintering the biscuit of the aluminum-based ceramic core to obtain the photocuring 3D printing aluminum-based ceramic core.
Wherein the step of degreasing comprises: in the air atmosphere, heating the aluminum-based ceramic core biscuit to the temperature of 550-600 ℃, and cooling after heat preservation for 180 min; preferably, the heating rate is 60-100 ℃/h, and the cooling rate is 60-100 ℃/h; and/or
Wherein the step of sintering treatment comprises: in the air atmosphere, heating the degreased aluminum-based ceramic core biscuit to 1300 ℃ and 1500 ℃, preserving the heat for 180min and cooling; preferably, the heating rate is 60-120 ℃/h, and the cooling rate is 60-120 ℃/h.
In the preparation method of the photocuring 3D printing aluminum-based ceramic core provided by the embodiment of the invention, the through-hole agent organic fiber is added into the photocuring 3D printing aluminum-based ceramic core slurry, so that not only can the inherent closed pores in the aluminum-based ceramic core be communicated, and the porosity of the ceramic core be obviously improved, but also in the degreasing sintering process, the channels formed by the oxidation and decomposition of the organic fiber in the form of gas overflow provide channels for the gas overflow generated by resin, pore-forming agent and the like, the sintering precision of the aluminum-based ceramic core is ensured, the sintering cracking tendency of the aluminum-based ceramic core is reduced, and the strength of the aluminum-based ceramic core is improved. In addition, the pore-forming agent starch can increase the number of micro pores in the aluminum-based ceramic core, and is combined with the organic fiber of the pore-forming agent, so that the porosity of the ceramic core is greatly improved. In addition, in the process of mixing and stirring the pore-forming agent, the through-hole agent and the deionized water, the pore-forming agent wraps the through-hole agent, so that the through-hole agent is more easily dispersed in the slurry, and the pore-forming agent is intensively distributed around the through-hole agent in the aluminum-based ceramic biscuit, so that the open porosity can be further improved after degreasing and sintering. In addition, the framework powder and the filler in the slurry for the photocuring 3D printing aluminum-based ceramic core in set amounts can further ensure the strength of the aluminum-based ceramic core.
The invention is further illustrated below by means of specific examples:
example 1
The embodiment prepares a photocuring 3D printing aluminum-based ceramic core, wherein the raw materials used are as follows: 60 parts of framework powder, 20 parts of filler, 3 parts of through-hole agent, 7 parts of pore-forming agent and 10 parts of light-cured resin pre-polymerized liquid (wherein the light-cured resin pre-polymerized liquid comprises 80% of photosensitive resin and 20% of diluent in terms of volume fraction). Wherein the skeleton powder is Al with particle size of 100 μm2O3The powder and the filler are SiO with the particle size of 20nm2And ZrO2Powder (of which SiO is2And ZrO2The mass ratio of the powder is 2: 1); the pore-forming agent is polyacrylic acid fiber and polyethylene fiber with the length of 1mm and the diameter of 5 mu m (wherein, the mass ratio of the polyacrylic acid fiber to the polyethylene fiber is 1: 1); the pore-forming agent is starch (the grain diameter of the starch is 50 nm); the volume ratio of the photosensitive resin is 3: 2 urethane acrylates and polyester acrylates; the diluent is 1, 6-hexanediol diacrylate.
The method specifically comprises the following steps:
1) to Al2O3Powder of SiO2Powder, ZrO2Adding absolute ethyl alcohol into the powder, mixing and stirring for 2 hours, and drying to obtain mixed powder; wherein the addition amount of the absolute ethyl alcohol is Al2O3Powder, SiO2Powder, ZrO210% of the total mass of the powder.
Adding deionized water into polyacrylic acid fiber, polyethylene fiber and starch, mixing and stirring for 2h, and drying to obtain a mixed fiber material; wherein, the adding amount of the deionized water is 10 percent of the total mass of the polyacrylic acid fiber, the polyethylene fiber and the starch.
And sequentially adding the obtained mixed powder and the mixed fiber material into the photocuring resin premix, and stirring for 12 hours at the temperature of 80 ℃ to obtain the photocuring 3D printing aluminum-based ceramic core slurry.
2) Setting photocuring 3D printing parameters: the curing thickness was set at 150 μm and the curing power was set at 35nW/cm2Setting the single-layer curing time to be 5 s; and curing the photocuring 3D printing aluminum-based ceramic core slurry through photocuring 3D printing equipment to obtain an aluminum-based ceramic core biscuit.
3) And (4) degreasing and sintering the biscuit of the aluminum-based ceramic core to obtain the photocuring 3D printing aluminum-based ceramic core.
The conditions of the degreasing treatment are as follows: under the air atmosphere, the heating rate and the cooling rate are both 60 ℃/h, the temperature of degreasing treatment is 600 ℃, and the heat preservation time at 600 ℃ is 180 min.
The conditions of the sintering treatment are as follows: in the air atmosphere, the heating rate and the cooling rate are both 120 ℃/h, the sintering treatment temperature is 1400 ℃, and the heat preservation time at 1400 ℃ is 240 min.
Fig. 2 is a graph showing the open pore distribution of the SEM ceramic core prepared by this example, after being ground and polished. As can be seen from fig. 2: in the ceramic core, the through-hole agent and the pore-forming agent act synergistically, the pore-forming agent generates a large amount of fine closed pores, and the closed pores are stringed into open pores by the through-hole agent, so that the photocuring 3D printing ceramic core with the bending strength of 24.3MPa and the porosity of 30.1% and low sintering crack incidence is prepared.
Example 2
This example prepares a photocuring 3D printing aluminum-based ceramic core, wherein, the raw materials that use are as follows: 50 parts of framework powder, 15 parts of filler, 5 parts of through-hole agent, 10 parts of pore-forming agent and 20 parts of light-cured resin pre-mixed liquid (wherein the light-cured resin pre-mixed liquid comprises 70% of photosensitive resin and 30% of diluent by volume fraction). Wherein the skeleton powder is Al with particle size of 80 μm2O3The powder and the filler are ZrSiO with the grain diameter of 50nm4Powder; the through-hole agent is prepared from 5mm long polyester fiber and 8 μm diameter acrylic fiber (wherein the mass ratio of the polyester fiber to the acrylic fiber is 2)1); the pore-forming agent is starch (the grain diameter of the starch is 100 nm); the volume ratio of the photosensitive resin is 4: 1 urethane acrylates and polyester acrylates; the diluent is 1, 6-hexanediol diacrylate.
The method specifically comprises the following steps:
1) to Al2O3Powder, ZrSiO2Adding absolute ethyl alcohol into the powder, mixing and stirring for 2 hours, and drying to obtain mixed powder; wherein the addition amount of the absolute ethyl alcohol is Al2O3Powder, ZrSiO28% of the total mass of the powder.
Adding deionized water into the polyester fiber, the acrylic fiber and the starch, mixing and stirring for 2 hours, and drying to obtain a mixed fiber material; wherein, the adding amount of the deionized water is 5 percent of the total mass of the polyacrylic acid fiber, the polyethylene fiber and the starch.
And sequentially adding the obtained mixed powder and the mixed fiber material into the photocuring resin premix, and stirring for 8 hours at the temperature of 120 ℃ to obtain the photocuring 3D printing aluminum-based ceramic core slurry.
2) Setting photocuring 3D printing parameters: the curing thickness was set at 100 μm and the curing power was set at 25nW/cm2Setting the single-layer curing time to be 15 s; and curing the photocuring 3D printing aluminum-based ceramic core slurry through photocuring 3D printing equipment to obtain an aluminum-based ceramic core biscuit.
3) And (4) degreasing and sintering the biscuit of the aluminum-based ceramic core to obtain the photocuring 3D printing aluminum-based ceramic core.
The conditions of the degreasing treatment are as follows: under the air atmosphere, the heating rate and the cooling rate are both 100 ℃/h, the temperature of degreasing treatment is 550 ℃, and the heat preservation time at 550 ℃ is 120 min.
The conditions of the sintering treatment are as follows: under the air atmosphere, the heating rate and the cooling rate are 100 ℃/h, the sintering treatment temperature is 1300 ℃, and the heat preservation time at 1300 ℃ is 180 min.
Example 3
This example prepared a photocuring 3D printing aluminum-based ceramic core, which differs from example 1 in that: in this example, the weight fraction of the raw material pore-forming agent was 1 part by weight, the pore-forming agent was 5 parts by weight, and the particle size of the pore-forming agent was 10 nm.
The other steps and parameters were exactly the same as in example 1.
Example 4
This example prepares a photocured 3D printed aluminum-based ceramic core, differing from example 1 in that: the raw material through-hole agent in the embodiment is polypropylene alcohol fiber, namely, the step 1) is as follows:
to Al2O3Powder, SiO2Powder, ZrO2Adding absolute ethyl alcohol into the powder, mixing and stirring for 2 hours, and drying to obtain mixed powder; wherein the addition amount of the absolute ethyl alcohol is Al2O3Powder of SiO2Powder, ZrO210% of the total mass of the powder.
Adding deionized water into the polypropylene alcohol fiber and the starch, mixing and stirring for 2 hours, and drying to obtain a mixed fiber material; wherein the adding amount of the deionized water is 10 percent of the total mass of the polypropylene alcohol fiber and the starch.
And sequentially adding the obtained mixed powder and the mixed fiber material into the photocuring resin premix, and stirring for 12 hours at the temperature of 80 ℃ to obtain the photocuring 3D printing aluminum-based ceramic core slurry.
The other steps and parameters were exactly the same as in example 1.
Example 5
This example prepared a photocuring 3D printing aluminum-based ceramic core, which differs from example 1 in that: the length of the raw material through-hole agent in this example was 10mm and the diameter was 10 μm.
The other steps and parameters were exactly the same as in example 1.
Comparative example 1
Comparative example 1 a photocuring 3D printed aluminum-based ceramic core was prepared, differing from example 1 in that: the raw materials of comparative example 1 did not contain a through-hole agent and a pore-forming agent.
The preparation method comprises the following specific steps:
the embodiment prepares a photocuring 3D printing aluminum-based ceramic core, wherein the raw materials used are as follows: 60 parts by weight of skeleton powderAnd 20 parts by weight of a filler, and 10 parts by weight of a photocurable resin premix (wherein the photocurable resin premix comprises 80% of a photosensitive resin and 20% of a diluent in terms of volume fraction). Wherein the skeleton powder is Al with particle size of 100 μm2O3The powder and the filler are SiO with the particle size of 20nm2And ZrO2Powder (of which SiO is2And ZrO2The mass ratio of the powder is 2: 1); the volume ratio of the photosensitive resin is 3: 2 urethane acrylates and polyester acrylates; the diluent is 1, 6-hexanediol diacrylate.
The method specifically comprises the following steps:
1) to Al2O3Powder, SiO2Powder, ZrO2Adding absolute ethyl alcohol into the powder, mixing and stirring for 2 hours, and drying to obtain mixed powder; wherein the addition amount of the absolute ethyl alcohol is Al2O3Powder of SiO2Powder, ZrO210% of the total mass of the powder.
And adding the obtained mixed powder into a light-cured resin premix, and stirring for 12 hours at a temperature of 80 ℃ to obtain light-cured 3D printing aluminum-based ceramic core slurry.
2) Setting photocuring 3D printing parameters: the curing thickness was set at 150 μm and the curing power was set at 35nW/cm2Setting the single-layer curing time to be 5 s; and curing the photocuring 3D printing aluminum-based ceramic core slurry through photocuring 3D printing equipment to obtain an aluminum-based ceramic core biscuit.
3) And (4) degreasing and sintering the biscuit of the aluminum-based ceramic core to obtain the photocuring 3D printing aluminum-based ceramic core.
The conditions of the degreasing treatment are as follows: under the air atmosphere, the heating rate and the cooling rate are both 60 ℃/h, the temperature of degreasing treatment is 600 ℃, and the heat preservation time at 600 ℃ is 180 min.
The conditions of the sintering treatment are as follows: under the air atmosphere, the heating rate and the cooling rate are 120 ℃/h, the sintering treatment temperature is 1400 ℃, and the heat preservation time at 1400 ℃ is 240 min.
Comparative example 2
Comparative example 2 a photocuring 3D printed aluminum-based ceramic core was prepared, differing from example 1 in that: the raw material of comparative example 2 contained no pore-forming agent.
The method specifically comprises the following steps:
the embodiment prepares a photocuring 3D printing aluminum-based ceramic core, wherein the raw materials used are as follows: 60 parts of framework powder, 20 parts of filler, 3 parts of through hole agent and 10 parts of light-cured resin pre-polymerized liquid (wherein the light-cured resin pre-polymerized liquid comprises 80% of photosensitive resin and 20% of diluent in volume fraction). Wherein the skeleton powder is Al with particle size of 100 μm2O3The powder and the filler are SiO with the particle size of 20nm2And ZrO2Powder (of which SiO is2And ZrO2The mass ratio of the powder is 2: 1); the pore-forming agent is polyacrylic acid fiber and polyethylene fiber with the length of 1mm and the diameter of 5 mu m (wherein, the mass ratio of the polyacrylic acid fiber to the polyethylene fiber is 1: 1); the volume ratio of the photosensitive resin is 3: 2 urethane acrylates and polyester acrylates; the diluent is 1, 6-hexanediol diacrylate.
The method specifically comprises the following steps:
1) to Al2O3Powder, SiO2Powder, ZrO2Adding absolute ethyl alcohol into the powder, mixing and stirring for 2 hours, and drying to obtain mixed powder; wherein the addition amount of the absolute ethyl alcohol is Al2O3Powder of SiO2Powder, ZrO210% of the total mass of the powder.
And adding the mixed powder, polyacrylic acid fibers and polyethylene fibers into the photocuring resin premix, and stirring for 12 hours at the temperature of 80 ℃ to obtain the photocuring 3D printing aluminum-based ceramic core slurry.
2) Setting photocuring 3D printing parameters: the curing thickness was set at 150 μm and the curing power was set at 35nW/cm2Setting the single-layer curing time to be 5 s; and curing the photocuring 3D printing aluminum-based ceramic core slurry through photocuring 3D printing equipment to obtain an aluminum-based ceramic core biscuit.
3) And (4) degreasing and sintering the biscuit of the aluminum-based ceramic core to obtain the photocuring 3D printing aluminum-based ceramic core.
The conditions of the degreasing treatment are as follows: under the air atmosphere, the heating rate and the cooling rate are both 60 ℃/h, the temperature of degreasing treatment is 600 ℃, and the heat preservation time at 600 ℃ is 180 min.
The conditions of the sintering treatment are as follows: under the air atmosphere, the heating rate and the cooling rate are 120 ℃/h, the sintering treatment temperature is 1400 ℃, and the heat preservation time at 1400 ℃ is 240 min.
The photocuring 3D printing silicon-based ceramic cores prepared in the above examples 1-5 and comparative examples 1 and 2 were tested for room temperature bending strength, open porosity, sintering crack occurrence rate, dissolution rate and other indexes, and the test data are shown in Table 1.
TABLE 1
| Detecting items | Bending strength at room temperature | Open porosity | Incidence of sintering cracks | Rate of dissolution |
| Example 1 | 24.3MPa | 30.1％ | 3.5％ | 0.034g/min |
| Example 2 | 21.8MPa | 31.5％ | 2.8％ | 0.037g/min |
| Example 3 | 23.4MPa | 30.3％ | 4.1％ | 0.031g/min |
| Example 4 | 22.1MPa | 31.2％ | 3.3％ | 0.028g/min |
| Example 5 | 24.1MPa | 29.5％ | 4.8％ | 0.038g/min |
| Comparative example 1 | 17.8MPa | 18.2％ | 9.8％ | 0.011g/min |
| Comparative example 2 | 18.5MPa | 20.3％ | 7.3％ | 0.016g/min |
Note: the room temperature bending strength in the table is tested according to the aviation industry standard HB 5353.3-2004; the open porosity is tested according to the aviation industry standard HB 5353.1-2004; the loss rate is tested according to the aviation industry standard HB 5353.6-2004; the incidence of the sintering cracks adopts a GB/T25995-2010 fine ceramic density and apparent porosity test method.
As can be seen from the data in table 1: the photocuring 3D printing aluminum-based ceramic core prepared by the embodiment of the invention has high open porosity, strong room-temperature bending strength and good solvent loss property. The scheme of the embodiment of the invention reduces the sintering cracking tendency of the aluminum-based ceramic core, ensures that the aluminum-based ceramic core has higher strength and simultaneously improves the open porosity of the core. Therefore, the photocuring 3D printing aluminum-based ceramic core prepared by the embodiment of the invention has excellent mechanical properties and high porosity, and is easy to remove after metal pieces are poured.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (10)
1. The preparation method of the photocuring 3D printing aluminum-based ceramic core is characterized by comprising the following steps:
preparing photocuring 3D printing aluminum-based ceramic core slurry: mixing the through-hole agent and the pore-forming agent, and drying to obtain a mixed fiber material; wherein the through-hole agent is organic fiber; the pore-forming agent is starch; mixing the mixed fiber material, mixed powder containing framework powder and filler and a light-cured resin pre-polymerization liquid to obtain light-cured 3D printing aluminum-based ceramic core slurry;
photocuring 3D printing treatment: carrying out photocuring 3D printing treatment on the photocuring 3D printing aluminum-based ceramic core slurry to obtain an aluminum-based ceramic core biscuit;
degreasing and sintering treatment: and degreasing and sintering the biscuit of the aluminum-based ceramic core to obtain the photocuring 3D printing aluminum-based ceramic core.
2. The preparation method of the photocuring 3D printing aluminum-based ceramic core according to claim 1, wherein the organic fiber is one or more of polyacrylic fiber, polyethylene fiber, polyallyl alcohol fiber, polyacrylonitrile fiber, polyester fiber, acrylic fiber, cotton fiber, polypropylene fiber and aramid fiber; and/or
The organic fiber is chopped fiber with the length of 1-10mm and the diameter of 5-10 mu m; and/or
The particle size of the starch is 10-100 nm.
3. The method for preparing the photocuring 3D printing aluminum-based ceramic core according to claim 1, wherein the framework powder is Al2O3(ii) a And/or
The grain diameter of the skeleton powder is 50-100 mu m; and/or
The filler is SiO2、ZrO2、Y2O3、ZrSiO4One or two of them; and/or
The particle size of the filler is 20-80 nm; and/or
The light-cured resin premix comprises a photosensitive resin and a diluent; wherein, the volume fraction of the photosensitive resin is 70-80%, and the volume fraction of the diluent is 20-30%; preferably, the photosensitive resin is one or more of urethane acrylate, polyester acrylate and methacrylate; preferably, the diluent is 1, 6-hexanediol diacrylate.
4. The method for preparing a photocuring 3D printing aluminum-based ceramic core as recited in any one of claims 1 to 3, wherein the photocuring 3D printing aluminum-based ceramic core slurry comprises, in parts by weight: 50-70 parts of framework powder, 10-25 parts of filler, 1-5 parts of through-hole agent, 5-10 parts of pore-forming agent and 10-30 parts of light-cured resin premix.
5. The method for preparing a photocuring 3D printed aluminum-based ceramic core as recited in any one of claims 1 to 4, wherein in the step of formulating a photocuring 3D printed aluminum-based ceramic core slurry: mixing and stirring the through-hole agent, the pore-forming agent and deionized water, and drying to obtain a mixed fiber material;
preferably, the dosage of the deionized water is 5-10% of the sum of the mass of the through hole agent and the mass of the pore-forming agent;
preferably, the time for mixing and stirring treatment is 1-2 h.
6. The preparation method of the photocuring 3D printing aluminum-based ceramic core as recited in any one of claims 1 to 5, wherein the preparation steps of the mixed powder are as follows:
mixing the framework powder, the filler and the absolute ethyl alcohol, and drying to obtain mixed powder;
preferably, the use amount of the absolute ethyl alcohol is 10-15% of the sum of the mass of the framework powder and the mass of the filler;
preferably, the time for mixing and stirring the skeleton powder, the filler and the absolute ethyl alcohol is 2-3 h.
7. The method for preparing a photocuring 3D printed aluminum-based ceramic core as recited in any one of claims 1 to 6, wherein in the step of formulating a photocuring 3D printed aluminum-based ceramic core slurry:
and mixing the mixed powder, the mixed fiber material and the light-cured resin premix, and stirring at the temperature of 80-120 ℃ for 8-12 h.
8. The method for preparing the photocuring 3D printing aluminum-based ceramic core according to any one of claims 1-7, wherein in the step of photocuring 3D printing processing, the photocuring 3D printing process parameters are set as follows:
the curing thickness is set to 50-150 μm, and the curing power is set to 25-45nW/cm2The monolayer curing time was set to 5-20 s.
9. The method for preparing a photocuring 3D printing aluminum-based ceramic core according to any one of claims 1 to 8, wherein in the step of degreasing and sintering treatment:
the step of degreasing treatment comprises: under the air atmosphere, heating the biscuit of the aluminum-based ceramic core to the temperature of 550-600 ℃, and cooling after heat preservation for 180 min; preferably, the heating rate is 60-100 ℃/h, and the cooling rate is 60-100 ℃/h; and/or
The sintering treatment step comprises: in the air atmosphere, heating the degreased aluminum-based ceramic core biscuit to 1300 ℃ and 1500 ℃, preserving the heat for 180min and cooling; preferably, the heating rate is 60-120 ℃/h, and the cooling rate is 60-120 ℃/h.
10. The photocuring 3D printing aluminum-based ceramic core is characterized in that the bending strength of the photocuring 3D printing aluminum-based ceramic core is 15-25MPa, and the porosity of a hole is 25-40%.
Preferably, the photocuring 3D printing aluminum-based ceramic core is prepared by the preparation method of the photocuring 3D printing aluminum-based ceramic core as claimed in any one of claims 1 to 9.
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