CN114082896B - 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 PDF

Info

Publication number
CN114082896B
CN114082896B CN202111397616.3A CN202111397616A CN114082896B CN 114082896 B CN114082896 B CN 114082896B CN 202111397616 A CN202111397616 A CN 202111397616A CN 114082896 B CN114082896 B CN 114082896B
Authority
CN
China
Prior art keywords
ceramic core
based ceramic
photocuring
aluminum
printing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202111397616.3A
Other languages
Chinese (zh)
Other versions
CN114082896A (en
Inventor
李金国
李乔磊
梁静静
周亦胄
孙晓峰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institute of Metal Research of CAS
Original Assignee
Institute of Metal Research of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Institute of Metal Research of CAS filed Critical Institute of Metal Research of CAS
Priority to CN202111397616.3A priority Critical patent/CN114082896B/en
Publication of CN114082896A publication Critical patent/CN114082896A/en
Application granted granted Critical
Publication of CN114082896B publication Critical patent/CN114082896B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • 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
    • 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
    • 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
    • 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
    • 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 light-cured resin premix 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

Photocuring 3D printing aluminum-based ceramic core and preparation method thereof
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 part 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 a 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 high-pressure decoring 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 that the dissolution and removal of the ceramic core are realized. 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 porosity by preparing the internal topology of the ceramic core to improve the removal performance of the ceramic core. 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 premixed solution 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 mu m.
Preferably, the skeleton powder is Al 2 O 3 。
Preferably, the particle size of the skeleton powder is 50-100 μm.
Preferably, the filler is SiO 2 、ZrO 2 、Y 2 O 3 、ZrSiO 4 One or two of them.
Preferably, the particle size of the filler is 20 to 80nm.
Preferably, the particle size of the starch is 10-100nm.
Preferably, the photocurable 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 1-2h.
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 2-3h.
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 premixed solution, and stirring at the temperature of 80-120 ℃ for 8-12h.
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 50-150 μm, and the curing power is set to 25-45nW/cm 2 The monolayer curing time was set to 5-20s.
Preferably, in the step of degreasing and sintering treatment:
the step of degreasing treatment comprises: in the air atmosphere, heating the biscuit of the aluminum-based ceramic core to 550-600 ℃, preserving heat for 120-180min, and then cooling; 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 1300-1500 ℃, preserving the heat for 180-300min, and then 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 small-size pore-forming agent starch in the degreasing and sintering processes, and the through-hole agent organic fiber is decomposed and oxidized into gas to overflow in the degreasing and sintering processes to communicate fine holes, so that the open 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 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, is high in 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 photograph of an SEM ceramic core open pore distribution plot taken after grinding and polishing of a photocured 3D printed aluminum-based ceramic core prepared in example 1 of the invention.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description of the embodiments, structures, characteristics 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 fiber 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 holes 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 mu m.
Wherein the pore-forming agent is starch.
Wherein the skeleton powder is Al 2 O 3 . The skeleton powder is ceramic powder with particle size of 50-100 μm.
Wherein the filler is SiO 2 、ZrO 2 、Y 2 O 3 、ZrSiO 4 One or two of them. Preferably, the filler is ceramic powder with the grain diameter of 20-80nm.
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 pore-forming agent, 5-10 parts of pore-forming agent and 10-30 parts of light-cured resin premixed solution.
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 be 50-150 μm, and the curing power is set to be 25-45nW/cm 2 The monolayer curing time was set to 5-20s.
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 550-600 ℃, preserving heat for 120-180min, and then cooling; 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 1300-1500 ℃, preserving the heat for 180-300min, and then 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 open porosity of the ceramic core be obviously improved, but also in the degreasing and sintering process, the channels formed by the oxidation and decomposition of the organic fiber in a gas form overflow provide channels for the gas overflow generated by resin, pore-forming agent and the like, so that 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 with set amounts in the slurry for the photocuring 3D printing aluminum-based ceramic core 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 premix (wherein the light-cured resin premix comprises 80% of photosensitive resin and 20% of diluent by volume fraction). Wherein the skeleton powder is Al with particle size of 100 μm 2 O 3 The powder and the filler are SiO with the particle size of 20nm 2 And ZrO 2 Powder (of which SiO is 2 And ZrO 2 The mass ratio of the powder is 2); the perforating agent is selected from polyacrylic acid fiber and polyethylene fiber with length of 1mm and diameter of 5 μm (wherein the polyacrylic acid fiber and polyethylene fiberThe mass ratio of the polyethylene fibers is 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 Al 2 O 3 Powder, siO 2 Powder, zrO 2 Adding 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 Al 2 O 3 Powder, siO 2 Powder, zrO 2 10% 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/cm 2 Setting the single-layer curing time to be 5s; and (3) solidifying the photocuring 3D printed aluminum-based ceramic core slurry through photocuring 3D printing equipment to obtain an aluminum-based ceramic core biscuit.
3) And 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 180min.
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 240min.
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
The embodiment prepares a photocuring 3D printing aluminum-based ceramic core, wherein the raw materials used 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 premix (wherein the light-cured resin premix comprises 70% of photosensitive resin and 30% of diluent by volume fraction). Wherein the skeleton powder is Al with particle size of 80 μm 2 O 3 The powder and the filler are ZrSiO with the grain diameter of 50nm 4 Powder; the through-hole agent is prepared from 5 mm-long polyester fibers and 8 μm-long acrylic fibers (wherein the mass ratio of the polyester fibers to the acrylic fibers is 2; 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 Al 2 O 3 Powder, zrSiO 2 Adding 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 Al 2 O 3 Powder, zrSiO 2 8% 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 addition 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: curingThe thickness was set at 100 μm and the curing power was set at 25nW/cm 2 Setting the single-layer curing time to be 15s; and (3) solidifying the photocuring 3D printed aluminum-based ceramic core slurry through photocuring 3D printing equipment to obtain an aluminum-based ceramic core biscuit.
3) And 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: in the air atmosphere, the heating rate and the cooling rate are both 100 ℃/h, the temperature of degreasing treatment is 550 ℃, and the holding time at 550 ℃ is 120min.
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 180min.
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 former was 1 part by weight, the pore former was 5 parts by weight, and the particle diameter of the pore former was 10nm.
The other steps and parameters were exactly the same as in example 1.
Example 4
This example prepared a photocuring 3D printing aluminum-based ceramic core, which differs 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 Al 2 O 3 Powder of SiO 2 Powder, zrO 2 Adding 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 Al 2 O 3 Powder, siO 2 Powder, zrO 2 10% of the total mass of the powder.
Adding deionized water into the polypropylene alcohol fiber and 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 mixed fiber material into the photocuring resin premix, and stirring at the temperature of 80 ℃ for 12 hours in a heat preservation manner 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 prepares a photocured 3D printed aluminum-based ceramic core, differing 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 photo-cured 3D printed aluminum-based ceramic core was prepared, differing from example 1 in that: the raw material of comparative example 1 did not contain a pore-forming 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 of skeleton powder and 20 parts of filler, wherein the light-cured resin premix comprises 80% of photosensitive resin and 20% of diluent by volume fraction. Wherein the skeleton powder is Al with particle size of 100 μm 2 O 3 The powder and the filler are SiO with the particle size of 20nm 2 And ZrO 2 Powder (of which SiO is 2 And ZrO 2 The mass ratio of the powder is 2); 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 Al 2 O 3 Powder, siO 2 Powder, zrO 2 Adding 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 Al 2 O 3 Powder, siO 2 Powder, zrO 2 10% 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/cm 2 Setting the single-layer curing time to be 5s; 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: in 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 180min.
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 240min.
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 premixed liquid (wherein the light-cured resin premixed liquid comprises 80% of photosensitive resin and 20% of diluent in volume fraction). Wherein the skeleton powder is Al with particle size of 100 μm 2 O 3 The powder and the filler are SiO with the particle size of 20nm 2 And ZrO 2 Powder (of which SiO is 2 And ZrO 2 The mass ratio of the powder is 2); the pore-forming agent is prepared from polyacrylic fibers and polyethylene fibers with the length of 1mm and the diameter of 5 mu m (wherein the mass ratio of the polyacrylic fibers to the polyethylene fibers is 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 Al 2 O 3 Powder of SiO 2 Powder, zrO 2 Adding 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 Al 2 O 3 Powder of SiO 2 Powder, zrO 2 10% 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/cm 2 Setting the single-layer curing time to be 5s; and (3) solidifying the photocuring 3D printed aluminum-based ceramic core slurry through photocuring 3D printing equipment to obtain an aluminum-based ceramic core biscuit.
3) And 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 180min.
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 240min.
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 solution loss
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: in the table, the room-temperature bending strength 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 dissolution 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 a metal piece is 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 (13)

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 light-cured resin premix liquid to obtain light-cured 3D printing aluminum-based ceramic core slurry; wherein 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; the organic fiber is chopped fiber with the length of 1-10mm and the diameter of 5-10 mu m; the particle size of the starch is 10-100nm;
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 as claimed in claim 1, wherein the framework powder is Al 2 O 3 (ii) a And/or
The particle size of the skeleton powder is 50-100 mu m; and/or
The filler is SiO 2 、ZrO 2 、Y 2 O 3 、ZrSiO 4 One or two of (a) and (b); and/or
The particle size of the filler is 20-80nm.
3. The method for preparing a photocuring 3D-printed aluminum-based ceramic core according to claim 1, wherein the photocuring 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%.
4. The preparation method of the photocuring 3D printing aluminum-based ceramic core as claimed in claim 3, wherein the photosensitive resin is one or more of urethane acrylate, polyester acrylate and methacrylate; and/or
The diluent is 1, 6-hexanediol diacrylate.
5. The method for preparing a photocuring 3D printed aluminum-based ceramic core as recited in claim 1, wherein the photocuring 3D printed aluminum-based ceramic core paste 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.
6. The method for preparing a photocuring 3D printed aluminum-based ceramic core as recited in claim 1, wherein in the step of formulating a photocuring 3D printed aluminum-based ceramic core slurry: and mixing and stirring the through-hole agent, the pore-forming agent and deionized water, and drying to obtain the mixed fiber material.
7. The method of preparing a photocuring 3D printing aluminum-based ceramic core as recited in claim 6,
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; and/or
The time for mixing and stirring treatment is 1-2h.
8. The preparation method of the photocuring 3D printing aluminum-based ceramic core as recited in claim 1, wherein the mixed powder is prepared by the following steps:
and mixing the skeleton powder, the filler and the absolute ethyl alcohol, and drying to obtain mixed powder.
9. The method of preparing a photocuring 3D printing aluminum-based ceramic core as recited in claim 8,
the consumption of the absolute ethyl alcohol is 10-15% of the sum of the mass of the framework powder and the mass of the filler; and/or
The time for mixing and stirring the framework powder, the filler and the absolute ethyl alcohol is 2-3h.
10. The method for preparing a photocuring 3D printed aluminum-based ceramic core as recited in claim 1, 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 premixed solution, and stirring at the temperature of 80-120 ℃ for 8-12h.
11. The method for preparing the photocuring 3D printing aluminum-based ceramic core according to claim 1, 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 be 50-150 μm, and the curing power is set to be 25-45nW/cm 2 The monolayer curing time was set to 5-20s.
12. The method for preparing a photocuring 3D-printed aluminum-based ceramic core according to claim 1, wherein in the step of degreasing and sintering treatment:
the step of degreasing treatment comprises: in the air atmosphere, heating the biscuit of the aluminum-based ceramic core to 550-600 ℃, preserving heat for 120-180min, and then cooling; wherein the heating rate is 60-100 ℃/h, and the cooling rate is 60-100 ℃/h; and/or
The sintering treatment comprises the following steps: in the air atmosphere, heating the degreased aluminum-based ceramic core biscuit to 1300-1500 ℃, preserving the heat for 180-300min, and then cooling; wherein the heating rate is 60-120 ℃/h, and the cooling rate is 60-120 ℃/h.
13. 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%;
wherein 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 12.
CN202111397616.3A 2021-11-23 2021-11-23 Photocuring 3D printing aluminum-based ceramic core and preparation method thereof Active CN114082896B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111397616.3A CN114082896B (en) 2021-11-23 2021-11-23 Photocuring 3D printing aluminum-based ceramic core and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111397616.3A CN114082896B (en) 2021-11-23 2021-11-23 Photocuring 3D printing aluminum-based ceramic core and preparation method thereof

Publications (2)

Publication Number Publication Date
CN114082896A CN114082896A (en) 2022-02-25
CN114082896B true CN114082896B (en) 2022-12-13

Family

ID=80303537

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111397616.3A Active CN114082896B (en) 2021-11-23 2021-11-23 Photocuring 3D printing aluminum-based ceramic core and preparation method thereof

Country Status (1)

Country Link
CN (1) CN114082896B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114853450B (en) * 2022-05-23 2023-04-28 西北工业大学 Photo-curing 3D printing alumina-based ceramic core and preparation method thereof

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100560534C (en) * 2007-06-19 2009-11-18 西安交通大学 A kind of manufacture method of alumina based ceramic core
CN102746022B (en) * 2011-12-29 2013-12-04 西安建筑科技大学 Preparation method for Al2O3 ceramic material having controllable bimodal porous structure
US11230503B2 (en) * 2017-06-27 2022-01-25 General Electric Company Resin for production of porous ceramic stereolithography and methods of its use
CN108083777B (en) * 2017-11-10 2021-05-11 山东工业陶瓷研究设计院有限公司 Aluminum-based ceramic slurry for photocuring 3D printing and preparation method of ceramic core
CN111978074A (en) * 2020-07-31 2020-11-24 西安欧中材料科技有限公司 Carbon nanotube reinforced porous ceramic core and preparation method thereof
CN111995414B (en) * 2020-07-31 2022-06-17 西安欧中材料科技有限公司 Polyacrylonitrile-based carbon fiber reinforced ceramic core and preparation method thereof
CN112608136A (en) * 2020-12-19 2021-04-06 西北工业大学 Photocuring 3D printing manufacturing method of high-porosity ceramic core
CN112537948A (en) * 2020-12-19 2021-03-23 西北工业大学 Photocuring 3D printing manufacturing method of alumina-based ceramic core

Also Published As

Publication number Publication date
CN114082896A (en) 2022-02-25

Similar Documents

Publication Publication Date Title
CN105198449B (en) A kind of preparation method of the high ceramic of compact of Stereolithography
CN109734425B (en) Laser selective rapid forming method of complex phase ceramic casting mold and product thereof
CN114082896B (en) Photocuring 3D printing aluminum-based ceramic core and preparation method thereof
CN104326766A (en) Preparation method of porous silicon nitride ceramic material with spherical pore structure
CN108299001B (en) Silicon-based ceramic core forming method
CN110803915A (en) Ceramic photocuring material and preparation method thereof
CN114380583A (en) Preparation method of ceramic material
CN104387105A (en) Method for preparing porous alumina ceramic material through combination of 3D printing and reactive sintering
CN112250465A (en) 3D printing porous zirconia ceramic and preparation method thereof
KR20160005065A (en) Tape casting using slurry from a cavitation apparatus and methods of making same
CN106735241B (en) A kind of reinforced resin optical soliton interaction method
CN105802459B (en) Cobalt aluminate coating, cobalt aluminate preparation method for coating and ceramic core manufacturing method
JP4918227B2 (en) Method for producing multilayer ceramic shell mold and its use
CN113683425B (en) Photocuring silicon nitride ceramic and preparation method thereof with gradient structure
CN114085073B (en) Photocuring 3D printing silicon-based ceramic core and preparation method thereof
CN114085084A (en) High-strength silicon nitride ceramic and preparation method thereof
WO2023071842A1 (en) Ceramic atomization core, and preparation method therefor and use thereof
CN111266521A (en) Composite sand core for casting and preparation method thereof
CN106083005A (en) High porosity easily removes silicon-base ceramic core preparation method
CN114149253A (en) Photocuring 3D printing low-sintering-shrinkage ceramic core and preparation method thereof
CN114180945A (en) Additive manufacturing method for ceramic core-type shell integrated piece
CN116199505B (en) Lamellar interface reinforced photocuring 3D printing ceramic core and preparation method thereof
CN111004045B (en) Reinforcing method of fiber reinforced silicon carbide ceramic matrix composite
CN113979780A (en) Porous zirconia ceramic and preparation method thereof
CN112552776A (en) Hard alloy sintering anti-sticking coating and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant