CN114770695A - Method for photocuring 3D printing ceramic - Google Patents
Method for photocuring 3D printing ceramic Download PDFInfo
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- CN114770695A CN114770695A CN202210386838.3A CN202210386838A CN114770695A CN 114770695 A CN114770695 A CN 114770695A CN 202210386838 A CN202210386838 A CN 202210386838A CN 114770695 A CN114770695 A CN 114770695A
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- photocuring
- curing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/001—Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- 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
Abstract
The invention provides a preparation method of photocuring 3D printing ceramic, which realizes single-layer one-time curing by reasonably controlling printing parameters such as interlayer thickness, illumination time and the like; in subsequent printing, ultraviolet light can penetrate through the current curing layer to perform secondary curing on the front curing layer, so that the chemical combination between the reinforcing layers becomes tighter; after printing is finished, the prefabricated part is integrally cured for three times by adopting an ultraviolet lamp, interlayer stress caused in the printing process is effectively eliminated, and interlayer binding force is obviously improved. Through the three-time curing process, the possibility of cracks and delamination after degreasing and sintering can be effectively avoided, and the performance of the ceramic component is expected to be improved. The method disclosed by the invention is simple and efficient in process and easy to control in operation, and can be used for preparing the photocuring 3D printing ceramic without delamination and cracks.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a method for photocuring 3D printing ceramic.
Background
The ceramic photocuring 3D printing technology is characterized in that a 3D model is divided into a plurality of equal-thickness exposure surfaces, printing parameters such as illumination time and interlayer thickness are set, the movement of a printing platform is matched by means of optical mask projection, and the photocuring slurry is irradiated by ultraviolet rays to realize layer-by-layer curing forming, so that a prefabricated part with a certain shape and size is finally obtained. And degreasing and sintering the prefabricated member, and removing organic matters such as photosensitive resin, a dispersing agent, a defoaming agent and the like to obtain the photocuring 3D printing ceramic piece.
However, due to the layer-by-layer stacking 3D printing mode, interlayer bonding is weak, interlayer stress is easily generated in the curing and shrinking process of subsequent printing layers, and cracks and even delamination easily occur after degreasing and sintering of a ceramic printing piece. This not only reduces the performance of the material, but also loses the significance of ceramic additive manufacturing. Therefore, the development of a preparation technology of the photocuring 3D printing ceramic without delamination and cracks can eliminate interlayer stress caused in the printing process and enhance interlayer bonding force in the prefabricated member, and the preparation technology is the key for obtaining the photocuring 3D printing ceramic without delamination and cracks.
Disclosure of Invention
In view of the problems in the prior art, it is an object of the present disclosure to provide a method of photocuring 3D printed ceramics.
To achieve the above object, the present disclosure provides a method of photocuring 3D printed ceramics, comprising the steps of: step one, stirring the photocuring ceramic slurry at normal temperature for 0.5-15 h, transferring the mixture into a vacuum drying oven, removing bubbles in vacuum for 1 n-90min to obtain bubble-free photocuring ceramic slurry, and placing the photocuring ceramic slurry in a material tank of a 3D printer; setting the thickness and the exposure time of the printing layer to realize one-time curing of the printing surface; step three, repeating the step two, wherein when a second layer is printed, the new layer is cured while light is irradiated, and the previous primary cured layer can be penetrated to carry out a secondary curing process; step four, repeating the step three until the required component size is printed, so as to obtain a prefabricated member; step five, putting the prefabricated part prepared in the step four into a photosensitive resin cleaning agent, performing ultrasonic oscillation, and then putting into deionized water for ultrasonic cleaning; step six, wiping the surface of the prefabricated part cleaned in the step five, placing the prefabricated part under an ultraviolet curing UV lamp, setting a curing sequence, illuminating, carrying out third complete curing, and uniformly releasing the residual stress in the printing process; step seven, putting the prefabricated member solidified for three times in the step six into a vacuum drying oven to be dried for 6-72 hours; and step eight, putting the prefabricated member obtained in the step seven into a high-temperature furnace, degreasing and preserving heat for 6-60 h at the temperature of 0-650 ℃ at the heating rate of 0.01-10 ℃/min, and then sintering at high temperature to obtain the photocuring 3D printing ceramic piece.
In some embodiments, in step one, the vacuum debubbling temperature is from 30 ℃ to 90 ℃.
In some embodiments, in step two, the print layer thickness is in the range of 1 μm to 200 μm.
In some embodiments, in step two, the exposure time ranges from 0.25s to 95 s.
In some embodiments, in step five, the ultrasonic oscillation time in the photosensitive resin cleaning agent is 1min to 90min, and the ultrasonic cleaning time in the deionized water is 5min to 120 min.
In some embodiments, in step six, the ultraviolet curing UV lamp wavelength is 300nm to 450 nm.
In some embodiments, in step six, the three-time curing sequence of the preform is a monolithic, face-to-face symmetric curing.
In some embodiments, in step six, each side of the preform is exposed to an ultraviolet curing UV lamp for a period of time in the range of 5s to 200 s.
In some embodiments, in step seven, the drying temperature is from 30 ℃ to 90 ℃.
The beneficial effects of this disclosure are as follows:
according to the method, the printing parameters such as the thickness and the illumination time between layers are reasonably controlled, the three times of curing processes are realized through operation, the main bonding mode between layers is changed from physical bonding into chemical bonding through the three times of controllable curing processes, the bonding force between layers is obviously improved, and the internal stress between layers caused by the curing processes is effectively eliminated. After degreasing and sintering, the photocuring 3D printing ceramic without delamination and cracks can be obtained. The method disclosed by the invention is simple and efficient in process and easy to control in operation.
Drawings
FIG. 1 is a scanning electron microscope test chart of examples 1 to 3.
FIG. 2 is a scanning electron microscope test chart of examples 4 to 5.
FIG. 3 is a scanning electron microscope test chart of comparative examples 1 to 2.
Detailed Description
A method of photocuring 3D printed ceramics according to the present disclosure is explained in detail below.
The application discloses a method for photocuring 3D printing of ceramic, which comprises the following steps: stirring the photocuring ceramic slurry at normal temperature for 0.5-15 h, transferring the mixture into a vacuum drying oven, removing bubbles in vacuum for 1-90 min to obtain bubble-free photocuring ceramic slurry, and placing the photocuring ceramic slurry into a material tank of a 3D printer; setting the thickness and the exposure time of the printing layer to realize one-time curing of the printing surface; step three, repeating the step two, wherein when a second layer is printed, the new layer is cured while light is irradiated, and the previous primary cured layer can be penetrated to carry out a secondary curing process; step four, repeating the step three until the required component size is printed, so as to obtain a prefabricated member; step five, putting the prefabricated part prepared in the step four into a photosensitive resin cleaning agent, performing ultrasonic oscillation, and then putting into deionized water for ultrasonic cleaning; step six, wiping the surface of the prefabricated part cleaned in the step five, placing the prefabricated part under an ultraviolet curing UV lamp, setting a curing sequence, illuminating, carrying out third complete curing, and uniformly releasing the residual stress in the printing process; step seven, putting the prefabricated member solidified for three times in the step six into a vacuum drying oven to be dried for 6-72 hours; and step eight, putting the prefabricated member obtained in the step seven into a high-temperature furnace, degreasing and preserving the temperature for 6-60 h at the temperature of 0-650 ℃ at the heating rate of 0.01-10 ℃/min, and then sintering at high temperature to obtain the photocuring 3D printing ceramic piece.
According to the method, the printing parameters such as the thickness between layers, the illumination time and the like are reasonably controlled, so that the ultraviolet light can penetrate through the current curing layer to realize secondary curing on the previous layer except for single-layer primary curing in the printing process; and the whole prefabricated member is cured for three times through the ultraviolet curing UV lamp, so that chemical bonding between layers is realized, the bonding force between layers is obviously improved, and meanwhile, the interlayer stress caused in the printing process is effectively eliminated, so that the interlayer bonding of the prefabricated member is more stable. After the treated prefabricated member adopts a proper degreasing and sintering system, the photocuring 3D printing ceramic without delamination and cracks can be prepared.
In the second step, the primary curing means that the curing is not complete when the light is irradiated for the first time, and the curing rate does not reach one hundred percent. The printing surface refers to the ultraviolet exposure pattern projected on the slurry, and then the slurry under the pattern is cured to form a layer, and the layer is the printing surface.
It should be noted that the secondary curing is based on the primary curing. And it should be emphasized that the secondary curing is not a one-time process, the light can act once through one layer, and can act once through two layers, and how many times it can act up to how many layers it can act, it is not an action once, and it is a repeated cumulative effect.
In the third step, in the secondary curing process, the two layers are cured simultaneously, so that the chemical bonding force between the two layers can be improved.
In some embodiments, in step one, the vacuum debubbling temperature is from 30 ℃ to 90 ℃. The viscosity of the light-cured ceramic slurry is high, bubbles in the slurry cannot overflow and burst at a low temperature, and the components of organic matters in the slurry are changed at a high temperature.
In some embodiments, in step two, the print layer thickness is in the range of 1 μm to 200 μm. The thickness of the printing layer is set to be too small, the single layer is cured too thoroughly, and the bonding force between layers is weak; the printing layer thickness is set too large to maintain the single layer shape well, losing the meaning of 3D printing.
In some embodiments, in step two, the exposure time ranges from 0.25s to 95 s. The light irradiation time is too short to form the thin slice, and the thin slice is not completely formed; when the illumination time reaches a certain value, the thickness of the slice is not changed greatly when the illumination time is continuously increased, and the slice is also twisted severely under the action of stress.
In some embodiments, in step five, the ultrasonic oscillation time in the photosensitive resin cleaning agent is 1min to 90min, and the ultrasonic cleaning time in the deionized water is 5min to 120 min. The sonication time is too short to clean all uncured resin; too long an ultrasound time can cause cracks in the preform.
In some embodiments, in step six, the ultraviolet curing UV lamp wavelength is 300nm to 450 nm. Visible light outside this wavelength range does not excite the photoinitiator used to effectively cure the photosensitive resin. The UV wavelength is not limited thereto and may be selected according to the types of the photosensitive resin and the initiator used.
In some embodiments, in step six, the three-cure sequence of the preform is a monolithic, face-to-face symmetric cure. By side is meant that each side is cured three times in sequence. The sequence is then symmetrical, after one face is illuminated, the next face is the face that is symmetrical to it. The integral type can ensure that the prefabricated body can be fully and integrally solidified, the interlayer combination degree is enhanced, and the internal stress is eliminated. The plane-by-plane symmetrical curing can balance and offset the internal stress newly generated during three times of curing.
In some embodiments, in step six, each side of the preform is exposed to an ultraviolet curing UV lamp for a period of time in the range of 5s to 200 s. The illumination time is too short, and the effect of integral three-time curing cannot be achieved; the light exposure time is too long, causing new stresses to the preform.
In some embodiments, in step seven, the drying temperature is from 30 ℃ to 90 ℃. The temperature is too high, and the cured resin can be softened and deformed for a long time; the temperature is too low to function as a drying and stress relief.
[ test procedures and test results ]
Example 1
Firstly, stirring photocuring ceramic slurry with the solid phase content of 45 vol% at normal temperature for 0.5-15 h, then moving the mixture into a vacuum drying oven, removing bubbles in vacuum at the temperature of 60 ℃ for 60min to obtain bubble-free photocuring ceramic slurry, and placing the photocuring ceramic slurry into a material tank of a 3D printer;
setting the thickness of the printing layer to be 50 mu m and the exposure time to be 5s to realize primary curing of the printing surface;
step three, repeating the step two, and when a second layer is printed, illuminating a new layer and simultaneously penetrating through the previous primary curing layer to perform a secondary curing process;
step four, repeating the step three until the required component size is printed, so as to obtain a prefabricated member;
fifthly, putting the prefabricated part prepared in the fourth step into 30ml of photosensitive resin cleaning agent, performing ultrasonic oscillation for 20min, and then putting the prefabricated part into deionized water for ultrasonic cleaning for 30 min;
step six, after the surface of the prefabricated part cleaned in the step five is wiped dry, the prefabricated part is placed under a 405nm ultraviolet curing UV lamp, the curing sequence is set, the illumination is carried out for 15s, the third time of complete curing is carried out, and the residual stress in the printing process is uniformly released;
step seven, putting the prefabricated member solidified for three times in the step six into a vacuum drying oven to be dried for 24 hours at the temperature of 60 ℃;
and step eight, placing the prefabricated member obtained in the step seven into a high-temperature furnace, heating to 650 ℃ at the temperature rise rate of 0.5 ℃/min, degreasing and preserving heat for 45 hours, and then sintering at 1650 ℃ to obtain the photocuring 3D printing ceramic piece.
The test pattern is shown in FIG. 1 (a).
Example 2
The light irradiation time was set to 5s and the interlayer thickness was set to 10 μm in the second step, as the interlayer thickness for photocuring 3D printing, and the rest was the same as in example 1. The test chart is shown in FIG. 1 (b).
Example 3
The light irradiation time was set to 5s and the interlayer thickness was set to 100 μm in the second step, as the interlayer thickness for photocuring 3D printing, and the rest was the same as in example 1. The test pattern is shown in FIG. 1 (c).
Example 4
In step six, the surfaces were illuminated under UV curing lamps for 25 seconds, as in example 1. The test pattern is shown in FIG. 2 (a).
Example 5
In step six, each side was illuminated under an ultraviolet curing UV lamp for 120 seconds, as in example 1. The test pattern is shown in FIG. 2 (b).
Comparative example 1
Setting the illumination time as 100s in the second step, which is used as the illumination time for photocuring 3D printing, the rest of the procedure is the same as that of example 1. The test pattern is shown in FIG. 3 (a).
No photocured 3D printed ceramic without delamination and cracking could be obtained.
Comparative example 2
After the surfaces of the preforms in the sixth step were wiped dry, each surface was illuminated for 0s, and the rest was the same as in example 1. The test chart is shown in FIG. 3 (b).
No photocured 3D printed ceramic without delamination and cracking could be obtained.
In the scanning electron microscope test chart of fig. 1 (parallel to the printing direction) it can be seen that:
in the embodiment 2, the illumination time is unchanged, the interlayer thickness is changed into 10 mu m, the interlayer combination on the surface of the sample is tighter than that in the embodiment 1, the number of small-size holes is obviously increased, and no delamination or crack is generated;
in the embodiment 3, the illumination time is unchanged, the interlayer thickness is changed into 100 mu m, the surface interlayer combination degree of the sample is obviously reduced compared with the sample in the embodiment 1, the 3D printing step effect is very obvious, the hole size is large, and no delamination and cracks exist.
In the sem test chart of fig. 2 (parallel to the printing direction) it can be seen that:
in the example 4, the three times of curing time of each surface of the preform is 25s, and compared with the sample in the example 1, the connection of each layer on the surface of the sample is tight, but the number of holes is increased remarkably;
in example 5, the three curing times of each side of the preform are 120s, and the layers on the surface of the sample are more tightly connected than those in example 1.
In the sem test chart of fig. 3 (parallel to the printing direction) it can be seen that:
in comparative example 1, the illumination time is 100s, the interlayer stress is too large, and the sample has obvious layering phenomenon;
in comparative example 2, three times of curing is not performed, the interlayer bonding force is small, the sample has cross-layer cracks, and the photo-curing 3D printing ceramic without cracks cannot be obtained.
The above-disclosed features are not intended to limit the scope of practice of the present disclosure, and therefore, all equivalent variations that are described in the claims of the present disclosure are intended to be included within the scope of the claims of the present disclosure.
Claims (9)
1. A method of photocuring 3D printed ceramics comprising the steps of:
step one, stirring the photocuring ceramic slurry at normal temperature for 0.5-15 h, transferring the mixture into a vacuum drying oven, removing bubbles in vacuum for 1-90 min to obtain bubble-free photocuring ceramic slurry, and placing the photocuring ceramic slurry into a material tank of a 3D printer;
setting the thickness and the exposure time of the printing layer to realize one-time curing of the printing surface;
step three, repeating the step two, and when a second layer is printed, illuminating a new layer and simultaneously penetrating through the previous primary curing layer to perform a secondary curing process;
step four, repeating the step three until the required component size is printed, so as to obtain a prefabricated member;
step five, putting the prefabricated part prepared in the step four into a photosensitive resin cleaning agent, performing ultrasonic oscillation, and then putting into deionized water for ultrasonic cleaning;
step six, wiping the surface of the prefabricated part cleaned in the step five, placing the prefabricated part under an ultraviolet curing UV lamp, setting a curing sequence, illuminating, carrying out third complete curing, and uniformly releasing the residual stress in the printing process;
seventhly, putting the prefabricated member cured for three times in the sixth step into a vacuum drying oven for drying for 6-72 hours;
and step eight, putting the prefabricated member obtained in the step seven into a high-temperature furnace, degreasing and preserving heat for 6-60 h at the temperature of 0-650 ℃ at the heating rate of 0.01-10 ℃/min, and then sintering at high temperature to obtain the photocuring 3D printing ceramic piece.
2. The method of photocuring 3D printed ceramic of claim 1,
in the first step, the vacuum defoaming temperature is 30-90 ℃.
3. The method of photocuring 3D printed ceramic of claim 1,
in step two, the thickness of the printing layer ranges from 1 μm to 200 μm.
4. The method of photocuring 3D printed ceramic of claim 1,
in step two, the exposure time ranges from 0.25s to 95 s.
5. The method of photocuring 3D printed ceramic of claim 1,
in the fifth step, the ultrasonic oscillation time in the photosensitive resin cleaning agent is 1min-90min, and the ultrasonic cleaning time in the deionized water is 5min-120 min.
6. The method of photocuring 3D printed ceramic of claim 1,
in the sixth step, the wavelength of the ultraviolet curing UV lamp is 300nm-450 nm.
7. The method of photocuring 3D printed ceramic of claim 1,
in the sixth step, the three-time curing sequence of the prefabricated part adopts an integral type plane-by-plane symmetrical curing mode.
8. The method of photocuring 3D printed ceramic of claim 1,
in the sixth step, each surface of the prefabricated body is irradiated for 5s-200s under an ultraviolet curing UV lamp.
9. The method of photocuring 3D printed ceramic of claim 1, wherein in step seven the drying temperature is from 30 ℃ to 90 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117021568A (en) * | 2023-08-17 | 2023-11-10 | 中国地质大学（武汉） | Photo-curing 3D printing preparation method and packaging method of LED lens |
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