A silicon carbide ceramic slurry for 3D printing, a preparation method, application and silicon carbide ceramic

By using digital light processing photopolymerization additive manufacturing technology, combined with suitable photosensitive resin, dispersant and initiator, silicon carbide ceramic slurry with good dispersibility and curing effect is prepared, which solves the problem of fine processing of silicon carbide materials in traditional processes and realizes 3D printing of high precision and complex structures.

CN117069498BActive Publication Date: 2025-12-16SHANGHAI INST OF TECH
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Patent Information

Application Number
CN202311036697.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-08-17
Publication Date
2025-12-16
Estimated Expiration
2043-08-17

AI Technical Summary

Technical Problem

Existing technologies and traditional processes make it difficult to refine silicon carbide materials, which affects their application in the manufacture of ultra-stable lightweight space-based telescopes and space reflectors.

Method used

By employing digital light processing photocuring additive manufacturing technology, and through the appropriate combination of photosensitive resin, dispersant and initiator, as well as the control of silicon carbide powder particle size, silicon carbide ceramic slurry with good dispersibility and curing effect is prepared. The slurry layup and curing process are precisely controlled by photomechanical means to achieve precise printing.

Benefits of technology

It improves the printing accuracy of silicon carbide ceramics and the ability to form complex structures, solves the accuracy and forming problems under traditional processing methods, and achieves efficient and precise forming.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a silicon carbide ceramic slurry for 3D printing, a preparation method and application thereof, and a silicon carbide ceramic. 50 The silicon carbide ceramic slurry is prepared from the following raw materials in parts by weight: 55-70 parts of silicon carbide powder, 22-42 parts of photosensitive resin, 2-3 parts of dispersing agent, and 1-5 parts of initiator. 50 The silicon carbide powder comprises coarse silicon carbide particles with a size of 10.5-12 microns and fine silicon carbide particles with a size of 0.85-1.5 microns. The silicon carbide slurry has small scattering in the printing process of an additive manufacturing digital light processing photocuring 3D printer, has better size precision of a printed sample, and can print more complex structures.
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Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of additive manufacturing materials, and particularly relates to a silicon carbide ceramic slurry for 3D printing, a preparation method, application and silicon carbide ceramic. BACKGROUND

[0002] The silicon carbide material has low density, high rigidity and bending strength, low thermal expansion coefficient, high thermal conductivity, wear resistance and corrosion resistance and the like. Its unique thermodynamic performance and polishing ability make the silicon carbide material an ideal material for manufacturing ultra-stable lightweight space-based telescopes, space mirrors or focal planes. In order to further reduce the weight of the space mirror and save costs, it is necessary to design it into a lightweight structure, including a reduced-thickness structure, a porous structure and a foam structure. However, the silicon carbide is a covalent compound, and the traditional processing method is difficult to carry out fine processing. SUMMARY

[0003] The present application aims to overcome the shortcomings of the prior art and provide a silicon carbide ceramic slurry for 3D printing, a preparation method, application and silicon carbide ceramic, which can solve the problem that the silicon carbide material prepared by the traditional process is difficult to carry out fine processing.

[0004] To achieve the above-mentioned purpose, the technical scheme adopted by the present application is as follows:

[0005] In one aspect of the present application, a silicon carbide ceramic slurry for 3D printing is provided, which is prepared from raw materials containing the following weight parts:

[0006] Silicon carbide powder 55-70 parts, photosensitive resin 22-42 parts, dispersing agent 2-3 parts, and initiator 1-5 parts;

[0007] The silicon carbide powder includes D 50 Coarse silicon carbide particles with a size of 10.5-12 microns and D 50 Fine silicon carbide particles with a size of 0.85-1.5 microns.

[0008] Specifically, the digital light processing photocuring additive manufacturing technology is one of the technologies to replace the traditional processing mode, but the high-purity silicon carbide powder is dark gray, dark black or dark green, has high light absorbance, affects the process flow of the digital light processing photocuring additive manufacturing technology for manufacturing silicon carbide ceramics, and brings certain difficulty to the forming and processing of the silicon carbide ceramics. The photocuring 3D printing technology is a high-efficiency and precise forming means, the pixel points in the light machine are strictly controlled through a program to control the printing precision, then the height of the slurry is scraped by a scraper to control the precision of the Z axis of the sample, the local area of the layer slurry is precisely controlled, high-power energy is generated by the light machine to make the slurry solidify and form, in the photocuring 3D printing technology process, the silicon carbide powder is wrapped by the photosensitive resin and flows under the pushing action of the scraper, is bonded with each other, then the slurry generates a solidification phenomenon under the irradiation of the ultraviolet light energy of the light machine, and the blank forming is realized by repeated and accurate layering and stacking, and the particle size distribution of the silicon carbide powder plays a key role in the technology. The silicon carbide powder in the application includes D 50 10.5-12 mu m coarse silicon carbide particles and D 50 0.85-1.5 mu m fine silicon carbide particles, so that the silicon carbide in the slurry is tightly packed, and the size precision of the printed sample is better.

[0009] As a further scheme of the application: the coarse silicon carbide particles account for 40-90% of the total mass of the silicon carbide powder, and the fine silicon carbide particles account for 10-60% of the total mass of the silicon carbide powder;

[0010] And / or, the coarse silicon carbide particles are D 50 at least one of 10.5 mu m, 11 mu m and 12 mu m;

[0011] And / or, the fine silicon carbide particles are D 50 at least one of 0.85 mu m, 1.0 mu m and 1.5 mu m.

[0012] As a further scheme of the application: the dispersant is a dispersant with a model number of CPM-D-07 produced by Jiaxing Raoli Technology Co., Ltd.;

[0013] And / or, the photosensitive resin includes a photosensitive resin A and a photosensitive resin B, the photosensitive resin A is a bifunctional resin, and is at least one selected from hydroxyethyl methacrylate, 1,6-hexanediol diacrylate and propoxylated neopentyl glycol diacrylate; the photosensitive resin B is a multifunctional resin, and is at least two selected from trimethylolpropane trimethacrylate, ethoxylated trimethylolpropane triacrylate, trimethylolpropane triacrylate and epoxy methacrylate; the volume ratio of the photosensitive resin A and the photosensitive resin B is 1-3:7-9;

[0014] And / or, the initiator is selected from at least two of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, 2-phenylbenzyl-2-dimethylamine-1-(4-morpholinobenzyl phenyl) butanone, 2-isopropylthioxanthone, bis(4-tert-butylphenyl) iodine hexafluorophosphate, p-N,N-dimethylaminobenzoic acid ethyl ester, 1-hydroxycyclohexyl phenyl ketone;

[0015] And / or, the solid content of the silicon carbide ceramic slurry for 3D printing is 55% to 70%.

[0016] In the present application, the photosensitive resin is a thermoplastic photosensitive resin. In addition, the inventors of the present application found that monofunctional resin monomers can reduce the viscosity and reaction rate of the silicon carbide slurry, increase the solid content, and the green body has lower brittleness. Multifunctional resin monomers increase the reaction rate of the resin, and the green body has higher brittleness and slower debonding. The photosensitive resin of the present application needs appropriate reactivity and debonding, and too fast or too slow is not conducive to obtaining a sample with uniform organization, resulting in uneven mechanical properties. The present application proportionally mixes bifunctional resin and multifunctional resin to obtain a slurry that can print more complex honeycomb structures.

[0017] In another aspect of the present application, a preparation method of a silicon carbide ceramic slurry for 3D printing is provided, at least comprising:

[0018] Mixing the silicon carbide powder with the photosensitive resin, the dispersant and the initiator uniformly to obtain the silicon carbide ceramic slurry for 3D printing;

[0019] The silicon carbide powder comprises D 50 Coarse silicon carbide particles with a size of 10.5 to 12 microns and D 50 Fine silicon carbide particles with a size of 0.85 to 1.5 microns.

[0020] As a further aspect of the present application, the method specifically comprises:

[0021] S1, adding the dispersant to the photosensitive resin and mixing uniformly to obtain material A;

[0022] S2, adding the silicon carbide powder to the material A and ball milling to obtain material B;

[0023] S3, adding the initiator to the material B and stirring until the initiator is completely dissolved to obtain the silicon carbide ceramic slurry for 3D printing.

[0024] In the present application, after the material A is poured into the ball mill, 2 to 3 mm ceramic balls are added for stirring.

[0025] As a further aspect of the present application, in step S2, the ball milling time is 2 to 36 hours;

[0026] And / or, the rotation direction of the ball mill is clockwise first and then counterclockwise.

[0027] Optionally, the ball milling time is independently selected from 2h, 3h, 4h, 5h, 6h, 8h, 10h, 15h, 20h, 25h, 30h, 36h.

[0028] In the application, the rotation direction of the ball mill is clockwise first and then counterclockwise, which can make the photosensitive resin, dispersant, initiator and silicon carbide powder in the slurry more uniformly dispersed.

[0029] As a further aspect of the application, before step S2, the method further comprises:

[0030] The silicon carbide powder is pretreated, and the specific method is to heat the silicon carbide powder in an oven at 0-100℃ for 1-24 days.

[0031] In a third aspect of the application, the application provides the use of the silicon carbide ceramic slurry for 3D printing in the preparation of structural devices of silicon carbide materials by photocuring digital light processing 3D printing.

[0032] As a further aspect of the application, the method specifically comprises the following steps:

[0033] The 3D printing silicon carbide ceramic slurry is placed in a 3D printer, the printing parameters are adjusted, and printing is performed according to the preset structural device;

[0034] The printing parameters include: the wavelength of the LED light source carried by the printer is 385-406nm;

[0035] And / or, the printing layer thickness is 0.02-0.1mm;

[0036] And / or, the light intensity is 10-300mW / cm 2 ;

[0037] And / or, the number of bottom exposure layers is 0-9999 layers;

[0038] And / or, the bottom exposure time is 1-400s;

[0039] And / or, the exposure time of each layer is 1-400s;

[0040] And / or, after the exposure of each layer is completed, 0-200s is waited.

[0041] In the application, the preset structural device is printed by three-dimensional modeling software. Specifically, the 3D printing silicon carbide ceramic slurry is loaded into the cylinder of the 3D printer, the printer screen and the printer doctor blade are leveled based on the slurry liquid level, the gap between the screen and the doctor blade is ensured to be reasonable, and then the printing parameters are adjusted until the printing is completed.

[0042] In a fourth aspect of the present application, a silicon carbide ceramic is provided, which is prepared using the silicon carbide ceramic slurry for 3D printing.

[0043] The present application has the following beneficial effects:

[0044] The present application has the following beneficial effects:The present application has the following beneficial effects: BRIEF DESCRIPTION OF DRAWINGS

[0045] Figure 1 is a ceramic sample printed by the silicon carbide ceramic slurry for 3D printing prepared in Example 3 of the present application;

[0046] Figure 2 is a trend chart of the curing depth of Example 3 of the present application under the exposure of light intensity of 200 mW / cm 2 DETAILED DESCRIPTION

[0047] The present application will be further described in conjunction with specific examples and comparative examples, and it should be understood that these examples are only used to illustrate the present application and not used to limit the protection scope of the present application.

[0048] The embodiments of the present application will be described in detail below with specific examples, and those skilled in the art can easily understand other advantages and effects of the present application from the disclosure. The present application can also be implemented or applied by different specific embodiments, and each detail in the specification can be modified or changed based on different views and applications without departing from the spirit of the present application. The experimental methods in the following examples are not specified, and the selection is based on the conventional methods and conditions, or the instructions of the commercial products. In addition, the reagents and raw materials used in the present application are commercially available.

[0049] In the examples of the present application, the use amount of each raw material is calculated by weight parts. The 3D printer manufacturer is Jiaxing Raoli Technology Co., Ltd., and the model is RJ-4K.

[0050] Performance test method in the present application:

[0051] I. The solid content is calculated by the following formula:

[0052]

[0053] wherein: m f is the weight of the silicon carbide powder, p f is the density of the silicon carbide powder, m1 is the weight of the photosensitive resin; m2 is the weight of the dispersant; m3 is the weight of the initiator.

[0054] II. Spline width test: a set of five samples is tested using a digital vernier caliper and the results are recorded. The process is as follows: place the sample in the caliper, then read the digital vernier caliper and record the number, then take the average.

[0055] III. Sedimentation test: place the prepared slurry in a measuring cylinder and observe whether there is a solid-liquid separation phenomenon. If there is a solid-liquid separation phenomenon, it indicates poor dispersibility. If there is no solid-liquid separation phenomenon, it indicates good dispersibility. Then record the height of the overall slurry as V0 and the height of the clarified resin as V1. Thus, the formula for calculating the sedimentation rate is: sedimentation rate = V1 / V0 x 100%.

[0056] IV. Curing depth test: under the exposure machine, expose the sample for a period of time, then remove the sample, then clean it with alcohol, then observe and measure its thickness using a scanning electron microscope.

[0057] Example 1

[0058] Step S1: weigh 42 parts of a mixed photosensitive resin in which propoxylated neopentyl glycol dipropenylate, trimethylolpropane triacrylate, and 1,6-hexanediol diacrylate are mixed in a volume ratio of 1:7:1;

[0059] Step S2: add 72 parts of dispersant CPM-D, mix and shake for 5 hours;

[0060] Step S3: pour the mixed solution into a ball mill, add 2-3mm ceramic balls for stirring, and then add 55 parts of silicon carbide powder for ball milling. The ball milling time is 12 hours. The D 50 of the coarse silicon carbide particles is 10.5μm, and the D 50 of the fine silicon carbide particles is 0.85μm. The coarse silicon carbide particles account for 60% of the total mass of the silicon carbide powder, and the fine silicon carbide particles account for 40% of the total mass of the silicon carbide powder.

[0061] Step S4: add 1 part of initiator, which is 2-phenylbenzyl-2-dimethylamine-1-(4-morpholinobenzyl phenyl) butanone, 2-isopropyl thioxanthone, p-N,N-dimethylamino benzoic acid ethyl ester, and bis(4-tert-butylphenyl) iodine hexafluorophosphate in a mass ratio of 1:1:1:1, continue to stir in the ball mill for 6 hours until the initiator is completely dissolved, to prepare a silicon carbide slurry with a solid content of 55%;

[0062] Step S5, the prepared silicon carbide slurry is put into a 3D printer with a wavelength of 385 nm, the light intensity is 240 mW / cm 2 , the layer thickness is adjusted to 0.05 mm, the exposure time is 15 s, and the complex honeycomb structure of the 3D printed silicon carbide ceramic is completed.

[0063] Example 2

[0064] Step S1, the mixed photosensitive resin of propoxylated neopentyl glycol diacrylate, ethoxylated trimethylolpropane triacrylate, trimethylolpropane triacrylate and 1,6-hexanediol diacrylate is uniformly mixed in a volume ratio of 1:5:3:1, and 22 parts of the mixed photosensitive resin are weighed;

[0065] Step S2, add dispersant CPM-D-7 3 parts, mix and shake for 5 hours;

[0066] Step S3, pour the mixed solution into a ball mill, add 2-3 mm ceramic balls for stirring, then add 70 parts of silicon carbide powder heated at 100°C for 10 hours for ball milling, the ball milling time is 12 hours, wherein the D 50 of the coarse silicon carbide particles is 12 μm, the D 50 of the fine silicon carbide particles is 1 μm, the coarse silicon carbide particles account for 60% of the total mass of the silicon carbide powder, and the fine silicon carbide particles account for 40% of the total mass of the silicon carbide powder;

[0067] Step S4, add 5 parts of initiator, and continue stirring in the ball mill for 6 hours until the initiator is completely dissolved, to prepare a silicon carbide slurry with a solid content of 70%, wherein the mass ratio of the composite initiator is 1:2:2 of 2,4,6-trimethylbenzoyl-diphenyl phosphine oxide, 2 isopropyl thioxanthone and bis(4-tert-butylphenyl) iodine hexafluorophosphate.

[0068] Step S5, the prepared silicon carbide slurry is put into a 3D printer with a wavelength of 405 nm, the light intensity is 220 mW / cm 2 , the layer thickness is adjusted to 0.02 mm, the exposure parameter is 20 s, and the complex honeycomb structure of the 3D printed silicon carbide ceramic is completed.

[0069] Example 3

[0070] Step S1, the mixed photosensitive resin of propoxylated neopentyl glycol diacrylate, ethoxylated trimethylolpropane triacrylate, trimethylolpropane triacrylate and methacrylic acid epoxy ester is uniformly mixed in a volume ratio of 3:2:2:3, and 25 parts of the mixed photosensitive resin are weighed;

[0071] Step S2, add dispersant CPM-D-7 3 parts, mix and shake for 5 hours;

[0072] Step S3, pour the mixed solution into the ball mill, add 2-3mm ceramic balls for stirring, add 69 parts of silicon carbide powder for ball milling, the ball milling rotation direction is clockwise first, then counterclockwise, the ball milling time is 12 hours, wherein the D 50 of the coarse silicon carbide particles is 10.5μm, the D 50 of the fine silicon carbide particles is 1μm, the coarse silicon carbide particles account for 70% of the total mass of the silicon carbide powder, and the fine silicon carbide particles account for 30% of the total mass of the silicon carbide powder;

[0073] Step S4, add 3 parts of initiator, the initiator is 2-phenyl benzene-2-dimethyl amine-1-(4-morpholinyl benzyl phenyl) butanone, 2 isopropyl thioxanthone, p-N,N-dimethyl amino benzoic acid ethyl ester, and bis(4-tert-butylphenyl) iodine hexafluorophosphate with a mass ratio of 1:1:1:1, continue to stir in the ball mill for 6 hours until the initiator is completely dissolved, and a silicon carbide slurry is prepared, with a solid content of 55%.

[0074] Step S5, the prepared silicon carbide slurry is put into a 3D printer with a wavelength of 406nm, the light intensity is 200mW / cm 2 , the layer thickness is adjusted to 0.03mm, and the exposure parameter is 25s, and the 3D printing of the complex structure of the silicon carbide ceramic is completed.

[0075] Example 4

[0076] Step S1, weigh 30 parts of photosensitive resin of propoxylated neopentyl glycol dipropenylate, trimethylolpropane triacrylate, and epoxy methacrylate with a volume ratio of 2:2:3;

[0077] Step S2, add 73 parts of dispersant CPM-D, and mix and shake uniformly for 5 hours;

[0078] Step S3, pour the mixed solution into the ball mill, add 2-3mm ceramic balls for stirring, add 69 parts of silicon carbide powder for ball milling, the ball milling time is 12 hours, wherein the D 50 of the coarse silicon carbide particles is 12μm, the D 50 of the fine silicon carbide particles is 1.5μm, the coarse silicon carbide particles account for 90% of the total mass of the silicon carbide powder, and the fine silicon carbide particles account for 10% of the total mass of the silicon carbide powder;

[0079] Step S4, add 3 parts of initiator, the mass ratio of the composite initiator bis(4-tert-butylphenyl) iodine hexafluorophosphate, 1-hydroxy cyclohexyl phenyl ketone, and 2-methyl-2-(4-morpholinyl)-1-[4-(methylthio) phenyl]-1-propanone is 5:1:1, continue to stir in the ball mill for 6 hours until the initiator is completely dissolved, and a silicon carbide slurry is prepared, with a solid content of 55%.

[0080] Step S5, the prepared silicon carbide slurry is put into a 3D printer with a wavelength of 406 nm, the light intensity is 200 mW / cm 2 , the layer thickness is adjusted to 0.1 mm, and the exposure parameter is 30 s, and the 3D printing of the complex honeycomb structure of silicon carbide ceramic is completed.

[0081] Example 5

[0082] The difference between this embodiment and example 3 is that the ratio of the composite initiator is 1:3:2:2.

[0083] Example 6

[0084] The difference between this embodiment and example 3 is that the exposure time is 10 seconds.

[0085] Example 7

[0086] The difference between this embodiment and example 3 is that the weight fraction of the dispersant is 2.5 parts.

[0087] Example 8

[0088] The difference between this embodiment and example 5 is that the photosensitive resin is a mixed photosensitive resin uniformly mixed by propoxylated neopentyl glycol dipropenylate, trimethylolpropane triacrylate, and epoxy methacrylate in a volume ratio of 1:8:1.

[0089] Example 9

[0090] The difference between this embodiment and example 3 is that the composite initiator is composed of 2,4,6-trimethylbenzoyl-diphenyl phosphine oxide, ethyl p-N,N-dimethylaminobenzoate, 2-phenylbenzyl-2-dimethylamine-1-(4-morpholinobenzyl) butanone, 2-isopropylthioxanthone, and bis(4-tert-butylphenyl) iodine hexafluorophosphate in a mass ratio of 4:1:1:1:1.

[0091] Comparative Example 1

[0092] The difference from example 3 is that the initiator is only 3 parts of 2-isopropylthioxanthone.

[0093] Comparative Example 2

[0094] The difference from example 3 is that the photosensitive resin is 42 parts of trimethylolpropane triacrylate.

[0095] Comparative Example 3

[0096] The difference from example 3 is that the amount of dispersant added in the silicon carbide powder is 5 parts.

[0097] The silicon carbide ceramics printed in examples 1-9 and comparative examples 1-3 are subjected to sedimentation test and curing depth test, and the results are shown in table 1.

[0098] Table 1

[0099]

[0100]

[0101] The sedimentation rate and the solidification depth in Examples 1-9 and Comparative Examples 1-3 are recorded in Table 1, and it can be seen that the solidification depth of Example 3 is the largest, reaching 95 μm, and the 3D printing effect is the best.

[0102] Figure 1 Figure is a picture of a ceramic sample printed by the silicon carbide ceramic slurry for 3D printing prepared in Example 3 of the present application, and it can be seen from the figure that the sample printed by DLP has a high integrity, and the edges and corners in the sample can be clearly seen. Figure 1

[0103] Figure is a trend chart of the solidification depth of Example 3 of the present application under the exposure of light intensity of 200 mW / cm 2 , and it can be seen from the figure that when the exposure energy is 6 mJ / cm 2 , the solidification depth is 11 μm, and according to the fitting line segment, it can be concluded that when the exposure energy is only 4 mJ / cm 2 , the solidification depth can reach 10 μm, which can meet the minimum requirement of solidification printing. Figure 2 Figure 2 Example 10

[0104] The difference from Example 3 is that the coarse silicon carbide particles account for 90% of the total mass of the silicon carbide powder, and the fine silicon carbide particles account for 10% of the total mass of the silicon carbide powder.

[0105] The difference from Example 3 is that the coarse silicon carbide particles account for 80% of the total mass of the silicon carbide powder, and the fine silicon carbide particles account for 20% of the total mass of the silicon carbide powder.

[0106] Example 11

[0107] The difference from Example 3 is that the coarse silicon carbide particles account for 60% of the total mass of the silicon carbide powder, and the fine silicon carbide particles account for 40% of the total mass of the silicon carbide powder.

[0108] Example 12

[0109] The difference from Example 3 is that the coarse silicon carbide particles account for 50% of the total mass of the silicon carbide powder, and the fine silicon carbide particles account for 50% of the total mass of the silicon carbide powder.

[0110] Example 13

[0111] The difference from Example 3 is that the coarse silicon carbide particles account for 50% of the total mass of the silicon carbide powder, and the fine silicon carbide particles account for 50% of the total mass of the silicon carbide powder.

[0112] Example 14​

[0113] The difference from Example 3 is that the coarse silicon carbide particles account for 40% of the total mass of the silicon carbide powder, and the fine silicon carbide particles account for 60% of the total mass of the silicon carbide powder.

[0114] Comparative Example 4

[0115] The difference from Example 3 is that only coarse silicon carbide particles are included in the silicon carbide powder.

[0116] The samples prepared in Example 3, Examples 10-14, and Comparative Example 4 were subjected to sample width and sedimentation tests, and the results are shown in Table 2.

[0117] Table 2

[0118] Test item Silicon carbide fine particle content (%) Width (mm) Settling rate (%) Example 10 10 4.15 2.5 Example 11 20 4.18 3.0 Example 3 30 4.01 1.0 Example 12 40 3.98 0.5 Example 13 50 3.99 0.25 Example 14 60 3.97 0.15 Comparative Example 4 0 4.3 5.0

[0119] As can be seen from Table 2, as the amount of fine silicon carbide powder is increased, the size accuracy of the 3D printed sample is closer to the designed size accuracy (4 mm), and the slurry is less likely to settle and has better dispersibility.

[0120] The present application can prepare a silicon carbide ceramic slurry with good dispersibility by selecting a suitable particle size distribution ratio of the silicon carbide powder, a dispersant, a type of photoinitiator, and a proper ratio of raw materials. In the present application, the dispersant not only reduces the viscosity of the slurry, but also makes the silicon carbide slurry more uniformly dispersed. The particle size distribution of the silicon carbide particles can change the rheological behavior of the slurry, so that the present application can prepare a slurry with a high solid content. In addition, the use of a combination of photoinitiators in the present application improves the curing depth of the slurry, thereby improving the yield of the silicon carbide ceramic green body. The silicon carbide slurry of the present application does not have problems such as difficulty in printing due to high viscosity and rapid settling of the slurry, and difficulty in forming due to low curing depth during the 3D printing process. The silicon carbide slurry of the present application has less scattering during the printing process in the digital light processing photocuring 3D printer, and has better size accuracy of the printed sample, and can print more complex structures.

[0121] The above examples are only illustrative of the principles and effects of the present application, and are not intended to limit the present application. Any person skilled in the art can modify or change the above examples without departing from the spirit and scope of the present application. Therefore, all equivalent modifications or changes made by those skilled in the art without departing from the spirit and technical ideas disclosed in the present application should be covered by the claims of the present application.

Claims

1. A method for preparing silicon carbide ceramic slurry for 3D printing, characterized in that, The method specifically includes: S1. Weigh out 25 parts of photosensitive resin in a volume ratio of 3:2:2:3, which are neopentyl glycol diacrylate, ethoxylated trimethylolpropane triacrylate, trimethylolpropane triacrylate, and epoxy methacrylate. S2. Add 3 parts of dispersant CPM-D-7, mix and shake well for 5 hours; S3. Pour the mixed solution into a ball mill, add 2-3 mm ceramic balls and stir. Add 69 parts of silicon carbide powder and then ball mill. The ball mill rotation direction is first clockwise, then counterclockwise, and the ball milling time is 12 hours. The D of the coarse silicon carbide particles is then... 50 The D of fine silicon carbide particles is 10.5 μm. 50 The particle size is 1μm, with coarse silicon carbide particles accounting for 70% of the total mass of silicon carbide powder and fine silicon carbide particles accounting for 30% of the total mass of silicon carbide powder. S4. Add 3 parts of initiator, which is 2-phenylbenzyl-2-dimethylamine-1-(4-morpholinobenzylphenyl)butanone, 2-isopropylthioxanthone, ethyl p-N,N-dimethylaminobenzoate, and bis(4-tert-butylphenyl)iodohexafluorophosphate in a mass ratio of 1:1:1:

1. Continue stirring in a ball mill for 6 hours until the initiator is completely dissolved to obtain silicon carbide slurry with a solid content of 55%.

2. The method for preparing silicon carbide ceramic slurry for 3D printing according to claim 1, characterized in that, Prior to step S3, the method further includes: The silicon carbide powder is pretreated by keeping it at 0-100°C in an oven for 1-24 days.

3. The application of a silicon carbide ceramic slurry for 3D printing prepared by the method described in any one of claims 1 to 2 in the fabrication of structural devices made of silicon carbide materials using photopolymerization digital light processing 3D printing, characterized in that... Specifically, the following steps are included: The silicon carbide ceramic slurry for 3D printing is placed into the 3D printer, the printing parameters are adjusted, and printing is performed according to the preset structural device. The printing parameters include: the LED light source equipped in the printer has a wavelength of 385-406nm; And / or, the printing layer thickness is 0.02–0.1 mm; And / or, light intensity 10–300 mW / cm 2 ; And / or, the exposure time for each layer is 1 to 400 seconds.

4. A silicon carbide ceramic, characterized in that, The silicon carbide ceramic is prepared using the silicon carbide ceramic slurry for 3D printing prepared by the method described in any one of claims 1 to 2.

Citation Information

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