CN115141014A - Preparation method of 4D printing ceramic and ceramic part - Google Patents
Preparation method of 4D printing ceramic and ceramic part Download PDFInfo
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- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
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- B33Y10/00—Processes of additive manufacturing
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Abstract
The invention discloses a ceramic 4D printing method and a ceramic piece, wherein the ceramic 4D printing method comprises the following steps: respectively preparing first ceramic slurry and second ceramic slurry with different shrinkage rates under the same sintering condition by adopting raw materials comprising ceramic powder and light-cured resin, and then carrying out different slurry alternate printing on the first ceramic slurry and the second ceramic slurry through a 3D printer under the irradiation of ultraviolet light to prepare a blank; and sintering the green body. Through the mode, the 4D deformation of the whole structure can be realized by utilizing the internal stress generated by the shrinkage difference of the first ceramic slurry and the second ceramic slurry in the sintering process; the 4D printing method is simple to operate, and has a great application prospect in the aspects of self-assembly, self-repair or self-induction and the like.
Description
Technical Field
The invention relates to the technical field of ceramics, in particular to a preparation method of 4D printing ceramics and a ceramic piece.
Background
4D printing refers to manufacturing a material structure capable of automatically deforming through a 3D printing technology. The 4D printing embeds the deformation design into the three-dimensional structure, and then gives an environmental stimulus (sound, light, electricity, heat, magnetism and the like) to the printed structure, so that the three-dimensional structure can carry out structural transformation along with the time dimension, and self-assembly, repair or deformation are realized. At present, the 4D printing technology has huge application potential in the fields of life, art, aviation, aerospace, medical treatment and the like.
The 4D printing technology appeared in 2013 for the first time and is still in the beginning stage of germination today. The ceramic 4D printing technology was first reported in 2018, and the group of subjects of lujian professor of hong kong city university adopted a fine direct-writing 3D printing technology to uniformly disperse nano zirconia in a precursor material (polydimethylsiloxane-PDMS) of a silica ceramic, and the nano zirconia was compounded into a slurry with viscoelastic inversion characteristics, and further printed and molded by a fine direct-writing extrusion 3D printer, and after the PDMS was cured, the 4D structural ceramic was finally sintered by folding or stretching deformation. In general, 4D printing technology is still in an early development stage, but at present, the printing technology is generally cumbersome to operate, and 4D deformation occurs more before printing, which is not a true 4D printing technology.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a preparation method of 4D printing ceramic and a ceramic piece.
The invention provides a preparation method of 4D printing ceramic, which comprises the following steps:
s1, preparing first ceramic slurry by adopting a first mixed raw material, and preparing second ceramic slurry by adopting a second mixed raw material; the first mixed raw material comprises first ceramic powder and first light-cured resin, and the second mixed raw material comprises second ceramic powder and second light-cured resin; under the same sintering condition, the shrinkage rate of the first ceramic slurry is larger than that of the second ceramic slurry;
s2, under the irradiation of ultraviolet light, different slurries are alternately printed by the first ceramic slurry and the second ceramic slurry through a 3D printer to obtain a blank body;
and S3, sintering the blank.
In the step S1, the shrinkage rate of the ceramic slurry is specifically understood as that the ceramic slurry is made into a ceramic green body according to a certain operation, and then the percentage of the difference between the sizes of the ceramic green body before and after sintering and the size before sintering is the shrinkage rate of the ceramic slurry. And the shrinkage rates of the above first ceramic slurry and second ceramic slurry are shrinkage rates obtained under the same operation and sintering conditions.
The preparation method of the 4D printing ceramic provided by the embodiment of the invention at least has the following beneficial effects: according to the preparation method of the 4D printing ceramic, ceramic slurry with different shrinkage rates under the same sintering condition is adopted, the same structure is printed in a laminated and alternate mode through a 3D printing technology, then sintering is carried out, and the 4D deformation of the whole structure is achieved by utilizing internal stress generated by the shrinkage rate difference of different ceramic slurries in the sintering process; in addition, the photocuring resin is added into the raw materials of the ceramic slurry and can be used as a binder, ultraviolet light irradiation is adopted in the printing process to assist in curing and forming of the slurry, rapid forming can be facilitated, the blank can be sintered immediately after being formed, the strength of the blank is improved, the raw materials are simple, the operation is simple and convenient, and the cost is saved.
In some embodiments of the present invention, in step S1, in the first ceramic slurry preparation process, a first modifier is first used to perform a surface modification treatment on a first ceramic powder to improve the affinity of the first ceramic powder with a first photocurable resin, so as to prepare a first modified ceramic powder; preparing first ceramic slurry by adopting the first modified ceramic powder and first light-cured resin;
in the preparation process of the second ceramic slurry, a second modifier is adopted to carry out surface modification treatment on second ceramic powder so as to improve the affinity of the second ceramic powder and second light-cured resin and prepare second modified ceramic powder; preparing a second ceramic slurry by adopting the second modified ceramic powder and a second light-cured resin;
preferably, the first modifier and the second modifier are each independently selected from at least one of neopentyl glycol (NPG), polyethylene glycol (PEG), trimethylolpropane (TMP), trimethylolethane (TME), a silane coupling agent (e.g., KH-570), and PT-09 inorganic powder. Specifically, the organic silicon coating treatment can be carried out by KH-570 silane coupling agent and/or PT-09 inorganic powder.
In some embodiments of the present invention, the first ceramic powder and the second ceramic powder are selected from at least one of zirconium dioxide, titanium dioxide, silicon dioxide, and aluminum oxide. The first ceramic powder in the first ceramic slurry and the second ceramic powder in the second ceramic slurry may be the same in kind or different in kind. Preferably, the particle size of the first ceramic powder and the particle size of the second ceramic powder are 10nm to 100 μm.
In some embodiments of the present invention, the first and second light curable resins are each independently selected from at least one of epoxy acrylate, polyurethane acrylic, polyester acrylic, amino acrylic.
In some embodiments of the present invention, the first mixed raw material includes 0 to 99wt% of a first ceramic powder and 1 to 100wt% of a first photocurable resin; the second mixed raw material comprises 0-99 wt% of second ceramic powder and 1-100 wt% of second light-cured resin. The preparation process of the first ceramic slurry and the second ceramic slurry can mix the components of the mixed raw materials, and then the raw materials are mechanically stirred to be uniformly dispersed, wherein the rotating speed of the mechanical stirring can be controlled to be 10-4000 r/min.
In some embodiments of the present invention, before step S2, the method further includes: writing a printing code according to the target three-dimensional structure, and importing the printing code into a 3D printer; the step S2 specifically includes: under the irradiation of ultraviolet light, different slurries are alternately printed by the 3D printer according to the printing codes by adopting the first ceramic slurry and the second ceramic slurry, so that a blank body is prepared;
preferably, a 4D deformation factor is introduced in the process of writing and printing codes according to the target three-dimensional structure; the method specifically comprises the following steps:
performing simulation calculation by adopting slice software (such as curr, slic3r, skeinforge and the like) according to the target three-dimensional structure to obtain a preliminary G code; and then, performing secondary compiling on the primary G code, introducing a 4D deformation factor for trial and error printing, and gradually correcting to obtain a printing code of the target three-dimensional structure.
The alternate printing is preferably a stacked alternate printing. In some embodiments of the present invention, the 4D deformation factor includes at least one of an angle of overlap, a number of layers of overlap, a difference in shrinkage, and a print path of the first ceramic paste and the second ceramic paste during printing.
The 4D deformation factor is introduced into the writing of the printing code, so that the printing forming deviation can be eliminated to a certain extent, and the deviation of a final formed part from a preset target three-dimensional structure due to the influence of the deformation factor in the printing process is avoided.
The 3D printer that above adopted specifically can be meticulous 3D printer of directly writing to through meticulous 3D printing technique of directly writing printing shaping. In the printing process, the adopted pressurized gas can be air, nitrogen or other inert gases, and the gas pressure can be controlled to be 0.01-10 MPa. The printing mode can adopt the stacked alternate printing, and specifically can be carried out according to the following steps: printing first ceramic slurry on the first layer to form a first ceramic slurry layer I; printing a second layer on the first ceramic slurry layer by adopting second ceramic slurry to form a first ceramic slurry layer; and then, printing the first ceramic slurry on the first ceramic slurry layer to form a second ceramic slurry layer according to the requirement, and laminating and alternately printing. Of course, the first layer may be printed with the second ceramic paste first, and then the first ceramic paste may be printed thereon, and the printing may be performed alternately in a stacked manner, as desired. Further, the first ceramic paste and the second ceramic paste may be alternately printed in the same layer. The 3D printer specifically can include two at least feed cylinders, and in step S3, can pour into two different feed cylinders of 3D printer respectively with first ceramic thick liquids and second ceramic thick liquids, then start the 3D printer and carry out different thick liquids and print in turn according to predetermined printing code.
In some embodiments of the present invention, in step S2, the ultraviolet light irradiation may specifically adopt a single-point light source, a multi-point light source, a linear light source or a surface light source; the wavelength range of the ultraviolet light is 100-420 nm, and the light intensity range is 1-1000 cd.
In some embodiments of the present invention, the sintering temperature in step S3 is 700 to 2000 ℃.
In a second aspect of the present invention, a ceramic part is provided, which is manufactured by any one of the ceramic 4D printing methods provided in the first aspect of the present invention.
Drawings
The invention is further described with reference to the following figures and examples, in which:
FIG. 1 is a flow chart of the preparation of a first ceramic slurry according to example 1 of the present invention;
FIG. 2 is a schematic diagram showing deformation of a green body before and after sintering in example 1 of the present invention;
fig. 3 is a comparative illustration of 4D structural deformation of the ceramic parts obtained in comparative example 1, comparative example 2 and example 2.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Example 1
A ceramic 4D printing method specifically comprises the following steps:
s1, mixing 0.1wt% of KH-570 silane coupling agent with 99.9wt% of nano zirconium dioxide ceramic powder particles with the particle size of 500nm to perform surface modification treatment on nano zirconium dioxide, and combining the KH-570 silane coupling agent on the surface of the nano zirconium dioxide ceramic powder to improve the affinity of the nano zirconium dioxide ceramic powder and the photocuring resin; then, as shown in fig. 1 (a), mixing the ceramic powder subjected to surface modification treatment with a photocurable resin; then as shown in (b) of fig. 1, stirring with a mechanical stirrer for 30min to disperse uniformly, and preparing a first ceramic slurry containing 80wt% of ceramic powder and a second ceramic slurry containing 85wt% of ceramic powder, respectively, as shown in (c) of fig. 1;
s2, according to a target three-dimensional structure (a criss-cross double-layer wood stack structure), slice software simulation calculation is adopted, and a preliminary G code is obtained; secondly, compiling the obtained G code for the second time, then introducing 4D deformation factors (including a superposition mode, a superposition angle, a superposition layer number, a shrinkage rate difference and a printing path of first ceramic slurry and second ceramic slurry in the printing process) for trial and error printing, gradually correcting to obtain a printing code of a target three-dimensional structure, and then introducing the printing code into a fine direct-writing 3D printer;
s3, as shown in (D) in the figure 1, under the auxiliary irradiation of ultraviolet light, adopting the first ceramic slurry and the second ceramic slurry prepared in the step S1, and performing different slurry laminating alternate printing according to printing codes by using the fine direct-writing 3D printer in the step S2 to prepare a blank;
and S4, sintering the blank prepared in the step S3 at 1400 ℃ for 4h to obtain the finished ceramic part. The schematic diagram of the deformation of the green body before and after sintering is shown in fig. 2, wherein (a) is the schematic diagram of the structure of the green body before sintering, and (b) is the schematic diagram of the structure of the ceramic part obtained after sintering.
Example 2
A ceramic 4D printing method specifically comprises the following steps:
s1, mixing 1wt% of KH-570 silane coupling agent with 99wt% of nano zirconium dioxide ceramic powder particles with the particle size of 10nm to perform surface modification treatment on the nano zirconium dioxide; then mixing the ceramic powder subjected to surface modification treatment with a light-cured resin, stirring for 30min by using a mechanical stirrer to uniformly disperse, and respectively preparing a first ceramic slurry containing 80wt% of ceramic powder and a second ceramic slurry containing 85wt% of ceramic powder;
s2, adopting slice software simulation calculation according to a target double-layer wood pile structure (the same as that in the embodiment 1), obtaining a printing G code, and then introducing the printing G code into a fine direct-writing 3D printer, wherein the fine direct-writing 3D printer is provided with two material cylinders;
s3, respectively injecting the first ceramic slurry and the second ceramic slurry prepared in the step S1 into two different material cylinders of the fine direct-writing 3D printer in the step S2, then starting the fine direct-writing 3D printer, and performing different slurry laminating alternate printing under the auxiliary irradiation of ultraviolet light according to the printing G code to prepare a blank body;
and S4, sintering the blank prepared in the step S3 at 1400 ℃ for 4h to obtain a finished ceramic part, wherein the finished ceramic part is shown in (c) in figure 3.
Example 3
A ceramic 4D printing method specifically comprises the following steps:
s1, mixing 3wt% of neopentyl glycol (NPG) and 97wt% of titanium dioxide ceramic powder particles with the particle size of 100 mu m to perform surface modification treatment on titanium dioxide; then mixing the ceramic powder subjected to surface modification treatment with a light-cured resin, and stirring for 30min by using a mechanical stirrer to uniformly disperse to respectively prepare a first ceramic slurry containing 60wt% of ceramic powder and a second ceramic slurry containing 75wt% of ceramic powder;
s2, performing simulation calculation by adopting slicing software according to a target three-dimensional structure (a criss-cross double-layer wood pile structure) to obtain a preliminary G code; secondly, compiling the obtained G code for the second time, then introducing 4D deformation factors (including a superposition mode, a superposition angle, a superposition layer number, a shrinkage rate difference and a printing path of first ceramic slurry and second ceramic slurry in the printing process) for trial and error printing, gradually correcting to obtain a printing code of a target three-dimensional structure, and then introducing the printing code into a fine direct-writing 3D printer;
s3, under the auxiliary irradiation of ultraviolet light, adopting the first ceramic slurry and the second ceramic slurry prepared in the step S1, and carrying out different slurry laminating alternate printing according to printing codes through a fine direct-writing 3D printer in the step S2 to prepare a blank body;
and S4, sintering the blank prepared in the step S3 at 700 ℃ for 6h to obtain the finished ceramic part.
Example 4
A ceramic 4D printing method specifically comprises the following steps:
s1, mixing 2wt% of PT-09 inorganic powder and 98wt% of alumina ceramic powder particles with the particle size of 1 mu m to perform surface modification treatment on alumina, mixing the ceramic powder subjected to the surface modification treatment with a light-cured resin, and stirring for 30min by using a mechanical stirrer to uniformly disperse to respectively prepare first ceramic slurry containing 30wt% of ceramic powder and second ceramic slurry containing 50wt% of ceramic powder;
s2, performing simulation calculation by adopting slicing software according to a target three-dimensional structure (a criss-cross double-layer wood pile structure) to obtain a preliminary G code; secondly, compiling the obtained G code, then introducing 4D deformation factors (including a superposition mode, a superposition angle, a superposition layer number, a shrinkage rate difference and a printing path of first ceramic slurry and second ceramic slurry in the printing process) for trial and error printing, gradually correcting to obtain a printing code of a target three-dimensional structure, and then introducing the printing code into a fine direct-writing 3D printer;
s3, under the auxiliary irradiation of ultraviolet light, adopting the first ceramic slurry and the second ceramic slurry prepared in the step S1, and performing different slurry laminating alternate printing according to printing codes through the fine direct-writing 3D printer in the step S2 to prepare a blank body;
and S4, sintering the blank prepared in the step S3 at 2000 ℃ for 3 hours to obtain a finished ceramic piece.
Comparative example 1
A ceramic printing method specifically comprises the following steps:
s1, mixing 1wt% KH-570 silane coupling agent and 99wt% nano zirconium dioxide ceramic powder particles with the particle size of 10nm to perform surface modification treatment on nano zirconium dioxide, mixing the ceramic powder subjected to the surface modification treatment with photocuring resin, and stirring for 30min by using a mechanical stirrer to uniformly disperse to prepare ceramic slurry containing 80wt% of ceramic powder;
s2, adopting slice software simulation calculation according to a target double-layer wood pile structure (the same as that in the embodiment 1), obtaining a printing G code, and then introducing the printing G code into a fine direct-writing 3D printer, wherein the fine direct-writing 3D printer is provided with two material cylinders;
s3, respectively injecting the ceramic slurry prepared in the step S1 into two different material cylinders of the fine direct-writing 3D printer in the step S2, and then starting the fine direct-writing 3D printer to perform laminated printing according to the printing G code to prepare a blank body;
and S4, sintering the blank prepared in the step S3 at 1400 ℃ for 4h to obtain a finished ceramic part, wherein the finished ceramic part is shown as (a) in figure 3.
Comparative example 2
A ceramic printing method specifically comprises the following steps:
s1, carrying out surface modification treatment by adopting 1wt% KH-570 silane coupling agent and 99wt% nano zirconium dioxide ceramic powder particles with the particle size of 10nm, then mixing the ceramic powder subjected to the surface modification treatment with photocuring resin, and stirring for 30min by adopting a mechanical stirrer to disperse uniformly to prepare ceramic slurry containing 85wt% of ceramic powder;
s2, adopting slice software simulation calculation according to a target double-layer wood pile structure (the same as that in the embodiment 1), obtaining a printing G code, and then introducing the printing G code into a fine direct-writing 3D printer, wherein the fine direct-writing 3D printer is provided with two material cylinders;
s3, respectively injecting the ceramic slurry prepared in the step S1 into two different material cylinders of the fine direct-writing 3D printer in the step S2, and then starting the fine direct-writing 3D printer to perform laminated printing according to the printing G code to prepare a blank body;
and S4, sintering the blank prepared in the step S3 at 1400 ℃ for 4h to obtain a finished ceramic part, wherein the finished ceramic part is shown as (a) in figure 3.
Comparing the ceramic articles obtained in comparative example 1 and comparative example 2 shown in (a) and (b) of fig. 3, it can be seen that the shrinkage rate of the ceramic paste in comparative example 1 is significantly greater than that of the ceramic paste in comparative example 2 after the sintering treatment under the same conditions, and the structure thereof is maintained as the structure before printing, and no winding deformation occurs. And the ceramic part prepared in example 2 shown in fig. 3 (c) is subjected to lamination alternate printing by using the ceramic pastes with different shrinkage rates in comparative example 1 and comparative example 2, and the structure of the final product ceramic part has 4D structural deformation under the control of internal stress due to the different shrinkage rates of the two ceramic pastes.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (10)
1. The preparation method of the 4D printing ceramic is characterized by comprising the following steps:
s1, preparing first ceramic slurry by adopting a first mixed raw material, and preparing second ceramic slurry by adopting a second mixed raw material; the first mixed raw material comprises first ceramic powder and first light-cured resin, and the second mixed raw material comprises second ceramic powder and second light-cured resin; under the same sintering condition, the shrinkage rate of the first ceramic slurry is greater than that of the second ceramic slurry;
s2, under the irradiation of ultraviolet light, different slurries are alternately printed by the first ceramic slurry and the second ceramic slurry through a 3D printer to obtain a blank body;
and S3, sintering the blank.
2. The preparation method of the 4D printing ceramic, according to claim 1, characterized in that in the step S1, in the preparation process of the first ceramic slurry, a first modifier is firstly adopted to perform surface modification treatment on the first ceramic powder so as to improve the affinity of the first ceramic powder and the first light-cured resin, and thus first modified ceramic powder is prepared; preparing first ceramic slurry by adopting the first modified ceramic powder and first light-cured resin;
in the preparation process of the second ceramic slurry, a second modifier is adopted to carry out surface modification treatment on second ceramic powder so as to improve the affinity of the second ceramic powder and second light-cured resin and prepare second modified ceramic powder; preparing a second ceramic slurry by adopting the second modified ceramic powder and a second light-cured resin;
the first modifier and the second modifier are respectively and independently selected from at least one of neopentyl glycol, polyethylene glycol, trimethylolpropane, trimethylolethane, a silane coupling agent and PT-09 inorganic powder.
3. The method for preparing the 4D printing ceramic according to claim 2, wherein the first ceramic powder and the second ceramic powder are each independently selected from at least one of zirconium dioxide, titanium dioxide, silicon dioxide and aluminum oxide; preferably, the particle size of the first ceramic powder and the particle size of the second ceramic powder are 10nm to 100 μm.
4. The method of preparing 4D printing ceramic according to claim 1, wherein the first and second light-curable resins are each independently selected from at least one of epoxy acrylate, polyurethane acrylic, polyester acrylic, amino acrylic.
5. The method for preparing 4D printing ceramic according to claim 1, wherein the first mixed raw material comprises 0-99 wt% of first ceramic powder and 1-100 wt% of first light-cured resin; the second mixed raw material comprises 0-99 wt% of second ceramic powder and 1-100 wt% of second light-cured resin.
6. The method for preparing the 4D printing ceramic according to claim 1, wherein before the step S2, the method further comprises: writing a printing code according to the target three-dimensional structure, and importing the printing code into a 3D printer; the step S2 specifically includes: under the irradiation of ultraviolet light, different slurries are alternately printed by the 3D printer according to the printing codes by adopting the first ceramic slurry and the second ceramic slurry, so that a blank body is prepared;
preferably, a 4D deformation factor is introduced in the process of writing and printing codes according to the target three-dimensional structure; the method specifically comprises the following steps:
adopting slice software to carry out simulation calculation according to the target three-dimensional structure to obtain a preliminary G code; and then compiling the primary G code for the second time, introducing a 4D deformation factor for trial and error printing, and gradually correcting to obtain a printing code of the target three-dimensional structure.
7. The method for preparing 4D printing ceramic according to claim 6, wherein the 4D deformation factor comprises at least one of an overlapping angle, an overlapping layer number, a shrinkage rate difference and a printing path of the first ceramic slurry and the second ceramic slurry during printing.
8. The preparation method of the 4D printing ceramic according to claim 1, wherein in the step S2, the ultraviolet light irradiation specifically adopts a single-point light source, a light source with more than two points, a linear light source or a surface light source; the wavelength range of the ultraviolet light is 100-420 nm, and the light intensity range is 1-1000 cd.
9. The method for preparing a 4D printed ceramic according to any of claims 1 to 8, wherein in step S3, the sintering temperature is 700 to 2000 ℃.
10. A ceramic article produced by the method of producing a 4D printed ceramic according to any one of claims 1 to 9.
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