CN113968738A - Ceramic precursor slurry for additive manufacturing and additive manufacturing process - Google Patents
Ceramic precursor slurry for additive manufacturing and additive manufacturing process Download PDFInfo
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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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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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/665—Local sintering, e.g. laser sintering
Abstract
The invention discloses ceramic precursor slurry for additive manufacturing and an additive manufacturing process, and belongs to the technical field of additive manufacturing of ceramic materials. The process comprises the steps of preparing a precursor solution by using bifunctional acrylate silicon resin with high silicon element content as a main raw material, simultaneously adding inert filler nano SiC powder with different mass fractions into the precursor liquid phase solution, utilizing photocuring and in-situ sintering ceramization technologies to realize direct molding of ceramic materials, firstly paving a layer of precursor material, utilizing the photocuring technology to realize material curing, then adopting an infrared light sintering mode to ceramize the material, and sequentially solidifying layer by layer and sintering layer by layer to finally realize direct integrated molding of a complex ceramic structure. Inert fillers are added into the precursor solution to reduce the volume shrinkage of the precursor ceramic in the sintering process, reduce the generation of cracks and pores and consider the maximization of efficiency and yield.
Description
Technical Field
The invention relates to the technical field of additive manufacturing of ceramic materials, in particular to ceramic precursor slurry for additive manufacturing and an additive manufacturing process.
Background
Ceramic materials are widely used in many fields because of their advantages such as high temperature resistance, corrosion resistance, oxidation resistance, excellent heat insulation and high temperature stability. Ceramic materials play an irreplaceable role, for example, in the field of aerospace. The main approach to increasing the thrust-to-weight ratio of an aircraft engine is to increase the turbine inlet temperature and reduce the structural weight. The ceramic and the composite material thereof have excellent performance and are the preferable good materials for the hot end part of the engine. With the rigorous service of engine components, higher demands are placed on ceramic and composite material structures thereof. Through technical innovation of decades, although various processes are improved, the traditional ceramic preparation method has long preparation period, high ceramic sintering temperature and poor processability in the whole process, and is difficult to manufacture ceramic components with high precision and complex geometric shapes, and the manufactured ceramic components can not meet the performance requirements of long-time reliable service in severe working environments (high temperature, corrosion and strong radiation). And the additive manufacturing technology provides a brand new way for the preparation of the structural and functional integration of the advanced ceramic component.
In recent years, ceramic additive manufacturing technology rises rapidly, and various manufacturing technology is derived, wherein a photocuring molding technology is one of effective means for ceramic additive manufacturing. The photocuring molding technology is characterized in that the prepared precursor solution initiates a crosslinking reaction under the radiation of ultraviolet light with specific wavelength, so that the precursor solution is cured and molded in a short time. The precursor conversion ceramic is a structural functional integrated ceramic component with excellent performance prepared by molding a precursor solution by using a ceramic additive manufacturing technology and performing pyrolysis. The precursor solution does not contain any ceramic component, but is a solution with certain fluidity and adjustable components prepared by organic photosensitive resin with higher silicon element content and other materials according to a certain proportion. The photocuring molding technology has the characteristics of high curing speed, high dimensional accuracy and high material utilization rate, but due to the chemical properties and characteristics of precursor solution components, the precursor polymer has not only chemical changes of conversion of the precursor polymer into precursor ceramic but also physical changes of macroscopic size in the sintering process, and mainly shows volume shrinkage and generation of pores.
The volume shrinkage not only can cause the reduction of the dimensional precision of parts, and causes various problems of deformation, fracture, workpiece warping and the like of materials, but also can seriously affect the mechanical property and the creep resistance of the materials. Therefore, how to control the volume shrinkage of the precursor polymer in the pyrolysis process has been an important issue of great concern for researchers
Disclosure of Invention
In order to prepare ceramic precursor slurry capable of reducing volume shrinkage and generation of cracks and pores in a high-temperature cracking process of a precursor ceramic material, the invention aims to provide ceramic precursor slurry for additive manufacturing and an additive manufacturing process, the ceramic precursor solution takes organic photosensitive resin as a main raw material, and nano SiC powder with different mass fractions and the like are added, the precursor solution is matched with a specific additive manufacturing process, and is compounded by an ultraviolet light curing and laser selective sintering ceramic process, so that the integrated formation of a three-dimensional ceramic structure can be realized, the problems of low ceramic yield, large volume shrinkage, poor process precision and the like of the conventional ceramic material in additive manufacturing are solved, and simultaneously, the process can realize high-precision and rapid forming of ceramic parts of the aeroengine in China, promotes rapid development of the aeroengine technology in China, and makes a contribution to advanced manufacturing industry in China.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a ceramic precursor slurry for additive manufacturing is prepared by adding nano SiC powder into a precursor solution, wherein the adding amount of the nano SiC powder is 0.1-5% of the weight of the precursor solution; the precursor solution comprises the following components in parts by weight:
the particle size of the nano SiC powder is 1000 meshes.
The addition amount of the nano SiC powder is preferably 2.0-3.5% of the weight of the precursor solution.
The additive manufacturing process using the ceramic precursor slurry comprises the following steps:
(1) preparing ceramic precursor slurry: adding bifunctional acrylate silicon resin, trimethylolpropane triacrylate, gamma- (methacryloxypropyl) trimethoxysilane, a photoinitiator 819 and a dye Sudan III into a constant-temperature water bath according to a ratio, and magnetically stirring to obtain a uniform precursor solution; adding the nano SiC powder into a precursor solution according to a required proportion, and uniformly stirring to obtain the ceramic precursor slurry;
(2) ceramic additive manufacturing: the direct molding of the ceramic material is realized by utilizing a photocuring technology and an in-situ sintering ceramization technology. The method comprises the following specific steps: firstly, a layer of precursor slurry is paved, the slurry solidification is realized by adopting a photocuring technology, then the solidified slurry is ceramized by adopting an infrared light sintering mode, and the layer-by-layer solidification and the layer-by-layer sintering are sequentially carried out in this way, and finally the integrally formed ceramic structural member is realized.
In the light curing technology, an ultraviolet laser with the power of 500W and the wavelength of 355nm is selected for scanning.
In the infrared light sintering mode, a fiber laser with the power of 500W and the wavelength of 1064nm is selected as the laser.
The invention has the following advantages and beneficial effects:
1. the forming efficiency is high: the method is characterized in that a precursor material with light and thermal activity is adopted, a layer of precursor material is firstly paved in the forming process, the material solidification is realized by adopting a photocuring technology, then the material is ceramized by adopting an infrared light sintering mode, then a layer of precursor material is paved, and the direct integrated forming of the complex ceramic structure is finally realized by sequentially solidifying layer by layer and sintering layer by layer, so that the forming precision is ensured and the efficiency is maximized.
2. Economy of material: the experiment adopts bifunctional acrylate silicon resin as a main raw material of a precursor solution, and adds the cross-linking agent trimethylolpropane triacrylate, gamma-trimethoxy silane, the photoinitiator 819, the dye Sudan III and the nano SiC powder to prepare the precursor solution.
3. Small volume shrinkage, high ceramic yield: the bifunctional acrylate silicone resin material has high Si element content, the precursor ceramic is directly prepared by utilizing an ultraviolet curing and laser selective sintering ceramic composite process, the material utilization rate is high, meanwhile, in the preparation process of the precursor solution, the inert filler nano SiC powder is introduced, the chemical property is stable, the chemical change cannot occur in the cracking process, cracks and pores caused by the escape of small molecular gases can be filled, and the ceramic yield is improved to a certain extent.
4. The molding precision is high: the method adopts a galvanometer type laser scanning system with high scanning rate and hopping rate to realize laser scanning of ultraviolet (355nm) and infrared (1064nm) dual wavelengths, and adopts track numerical simulation and experiment to research a numerical compensation method of focal plane light spots under the scanning linear and nonlinear distortion conditions to realize flexible control of focused light spot size and energy. In the aspect of forming process control, the whole set of equipment is based on a self-adaptive layering algorithm of part geometric feature analysis, combines performance, precision and efficiency coupling optimization strategy analysis to form intelligent layering under multiple constraint conditions of structure, performance, precision and the like, and performs intelligent planning and parameter optimization combination of a light beam path based on deformation control, layer morphology and combination quality to ensure stability control of the whole forming process.
Drawings
Fig. 1 is a flow chart of the ceramic additive manufacturing process of the present invention.
FIG. 2 is a three-dimensional model of a precursor ceramic according to the present invention.
FIG. 3 is a three-dimensional sample of a precursor ceramic according to the present invention.
FIG. 4 is a line graph showing the variation of the volume shrinkage of the precursor ceramic according to the present invention with the mass fraction of the inert filler.
FIG. 5 is a line graph of the precursor ceramic yield of the present invention as a function of inert filler mass fraction.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
The invention provides a ceramic precursor slurry formula for laser additive manufacturing and an additive manufacturing process, as shown in figure 1, the ceramic precursor slurry takes bifunctional acrylate silicon resin with high silicon element content as a main raw material of a precursor solution, meanwhile, inert filler nano SiC powder is added into the precursor solution, then, the direct molding of ceramic materials is realized by utilizing photocuring and in-situ sintering ceramization technologies, and the polymer precursor ceramic additive manufacturing technology mainly based on the photocuring/thermocuring technology is specifically as follows: the ceramic material is prepared by chemical synthesis of polymer which can be converted into ceramic material by pyrolysis, cross-linking to thermosetting polymer in the additive manufacturing process, and then pyrolysis. The technology has the advantages of designability, machinability, capability of preparing ceramics at low temperature, high precision, high efficiency and the like.
The ceramic precursor slurry comprises the following components: bifunctional acrylate silicone resin, trimethylolpropane triacrylate (TMPTA), gamma- (methacryloxypropyl) trimethoxysilane (KH-570), a photoinitiator 819, a dye Sudan III and nano SiC powder; wherein:
bifunctional acrylate silicone resin: the material is cheap and easy to obtain, the Si element content of the material is high, the ceramic yield is greatly improved, and meanwhile, the resin contains a plurality of photosensitive groups, has obvious reaction on ultraviolet light and is suitable for photocuring reaction;
trimethylolpropane triacrylate: the material contains a certain amount of unsaturated groups, has obvious crosslinking promoting effect, and can increase the polymerization degree and shorten the curing time by adding the unsaturated groups;
γ - (methacryloxypropyl) trimethoxysilane: the ceramic not only has excellent fluidity, reduces the viscosity of the precursor solution, but also introduces important Si element into the system, and improves the yield of the ceramic;
photoinitiator 819: the curing speed is improved, and the printing efficiency is improved;
dye sudan iii: the transparency of the organic precursor solution is reduced, the absorption of ultraviolet light is reduced, and unnecessary curing is avoided;
nano SiC powder: as the inert filler, the ceramic filler has stable chemical property, does not generate chemical change in the cracking process, can fill cracks and pores caused by the escape of small molecule gas, and also can improve the yield of ceramics.
Example 1:
in this embodiment, a ceramic precursor slurry is first prepared by adding nano SiC powder into a precursor solution; the precursor solution composition (wt.%): 11.53% of difunctional acrylate silicone resin, 28.83% of trimethylolpropane triacrylate (TMPTA), 57.66% of gamma- (methacryloxypropyl) trimethoxysilane (KH-570), 1.96% of photoinitiator 819 and 0.02% of dye Sudan III.
The mass fractions of the added filler SiC powder were 0.1 wt%, 0.5 wt%, 1 wt%, 2 wt% and 3 wt% of the precursor solution, respectively, and each added amount was at least 5 samples.
Aiming at the ceramic precursor slurry, the direct molding of the ceramic material is realized by adopting ultraviolet curing and in-situ sintering ceramization technology; in the photocuring and in-situ sintering processes, a galvanometer type laser scanning system with high scanning rate and jumping rate is adopted to realize laser scanning of two wavelengths of ultraviolet (355nm) and infrared (1064nm), and a numerical compensation method of focal plane light spots under scanning linear and nonlinear distortion conditions is researched by adopting track numerical simulation and experiments to realize flexible control of focusing light spot size and energy. The required optical path system comprises a laser and an optical path transmission and scanning system, the optical path transmission and scanning system comprises an optical path lens group and a digital galvanometer, and light beams emitted by the laser are transmitted to the digital galvanometer through the optical path lens group; and the digital galvanometer outputs laser to scan the working area according to requirements.
The light curing and in-situ sintering process comprises the following specific steps: firstly, spreading a layer of ceramic precursor slurry, realizing material solidification by adopting a photocuring technology, then adopting an infrared light sintering mode to ceramic the solidified material, and sequentially solidifying layer by layer and sintering layer by layer to finally realize the direct integrated forming of a complex ceramic structure. In the process, an ultraviolet laser with the power of 500W and the wavelength of 355nm is selected for scanning in the photocuring technology, the wavelength of the ultraviolet laser is matched with the wavelength required by a photoinitiator 819 in a precursor solution, and the curing speed of the ultraviolet laser is improved; the infrared light is scanned by a laser with the power of 500W and the wavelength of 1064nm during sintering, the sintering temperature is 1000 ℃, and the time is 120 min. The three-dimensional mold of the ceramic sample is shown in fig. 2, and the ceramic sample after forming is shown in fig. 3.
Studying the influence of the filler amount with different mass fractions on the volume shrinkage of the precursor polymer after pyrolysis, randomly selecting 5 samples from products with each addition amount in the precursor ceramic subjected to pyrolysis under a specific temperature program, and calculating the average shrinkage of the precursor polymer, as shown in fig. 4, it can be found that the mass fraction of the nano SiC powder is gradually increased, the average volume shrinkage of the precursor ceramic is gradually reduced, and when the mass fraction of the inert filler is 3 wt%, the average volume shrinkage reaches 75.64% at the lowest; the ceramic yield line diagram of the precursor is shown in fig. 5, and similarly, when the mass fraction of SiC reaches 3 wt%, the yield of the precursor ceramic reaches up to 26.42%, the mass and volume of the inert filler reduce the generation of cracks and pores in the cracking process, the release of volatile small molecule gas is reduced, and in addition, the nano SiC powder is used as a component of the composite ceramic, and the ceramic yield is also improved.
Claims (7)
1. A ceramic precursor slurry for additive manufacturing, comprising: the ceramic precursor slurry is prepared by adding nano SiC powder into a precursor solution, wherein the addition amount of the nano SiC powder is 0.1-5% of the weight of the precursor solution; the precursor solution comprises the following components in parts by weight:
2. the ceramic precursor slurry for additive manufacturing of claim 1, wherein: the particle size of the nano SiC powder is 1000 meshes.
3. The ceramic precursor slurry for additive manufacturing of claim 1, wherein: the addition amount of the nano SiC powder is 2.0-3.5% of the weight of the precursor solution.
4. An additive manufacturing process using the ceramic precursor slurry of any one of claims 1 to 3, wherein: the process comprises the following steps:
(1) preparing ceramic precursor slurry: adding bifunctional acrylate silicon resin, trimethylolpropane triacrylate, gamma- (methacryloxypropyl) trimethoxysilane, a photoinitiator 819 and a dye Sudan III into a constant-temperature water bath according to a ratio, and magnetically stirring to obtain a uniform precursor solution; adding the nano SiC powder into a precursor solution according to a required proportion, and uniformly stirring to obtain the ceramic precursor slurry;
(2) ceramic additive manufacturing: the direct molding of the ceramic material is realized by utilizing a photocuring technology and an in-situ sintering ceramization technology.
5. An additive manufacturing process performed by a ceramic precursor slurry as claimed in claim 4, wherein: the ceramic additive manufacturing process in the step (2) is as follows: firstly, a layer of precursor slurry is paved, the slurry solidification is realized by adopting a photocuring technology, then the solidified slurry is ceramized by adopting an infrared light sintering mode, and the layer-by-layer solidification and the layer-by-layer sintering are sequentially carried out in this way, and finally the integrally formed ceramic structural member is realized.
6. An additive manufacturing process performed by a ceramic precursor slurry as claimed in claim 5, wherein: in the light curing technology, an ultraviolet laser with the power of 500W and the wavelength of 355nm is selected for scanning.
7. An additive manufacturing process performed by a ceramic precursor slurry as claimed in claim 5, wherein: in the infrared light sintering mode, a fiber laser with the power of 500W and the wavelength of 1064nm is selected as the laser.
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| CN115431376A (en) * | 2022-08-16 | 2022-12-06 | 华中科技大学 | High-strength large-scale complex ceramic biscuit and three-dimensional spray printing forming method and equipment thereof |
| CN115572170A (en) * | 2022-10-21 | 2023-01-06 | 江南大学 | Near-infrared thermal coupling curing non-oxide ceramic slurry and preparation method and application thereof |
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| CN115431376A (en) * | 2022-08-16 | 2022-12-06 | 华中科技大学 | High-strength large-scale complex ceramic biscuit and three-dimensional spray printing forming method and equipment thereof |
| CN115572170A (en) * | 2022-10-21 | 2023-01-06 | 江南大学 | Near-infrared thermal coupling curing non-oxide ceramic slurry and preparation method and application thereof |
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