CN113860886A - Method for improving density of 3D gel printing ceramic material - Google Patents
Method for improving density of 3D gel printing ceramic material Download PDFInfo
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- CN113860886A CN113860886A CN202111177188.3A CN202111177188A CN113860886A CN 113860886 A CN113860886 A CN 113860886A CN 202111177188 A CN202111177188 A CN 202111177188A CN 113860886 A CN113860886 A CN 113860886A
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- 238000007639 printing Methods 0.000 title claims abstract description 100
- 238000000034 method Methods 0.000 title claims abstract description 35
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 19
- 239000000919 ceramic Substances 0.000 claims abstract description 36
- 230000008569 process Effects 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 238000005238 degreasing Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000002002 slurry Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 14
- 238000000280 densification Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 11
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 229910000859 α-Fe Inorganic materials 0.000 claims description 9
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 6
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 9
- 239000001506 calcium phosphate Substances 0.000 description 6
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- 235000011010 calcium phosphates Nutrition 0.000 description 6
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 6
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- 238000010586 diagram Methods 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
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- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
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- 239000000696 magnetic material Substances 0.000 description 1
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- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
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Abstract
The invention provides a method for improving the density of a 3D gel printing ceramic material, and belongs to the field of additive manufacturing. The process of the present invention comprises: establishing a printing model, setting a program, preparing printing raw materials, printing and forming, drying a workpiece, degreasing, sintering and the like. According to the invention, the problem of insufficient density is solved by improving the technical process of additive manufacturing of the ceramic material, the printing wires are partially overlapped by setting the printing parameters and adjusting the diameter of the actual printing wire to be larger than the diameter of the wire set by the program, so that the gap is reduced and the density is improved, and thus huge inter-wire gaps caused by accumulation of common printing wires are solved, and the density of the 3D printed ceramic product is improved. The method improves the density of the 3D printing gel ceramic material, is simple and stable to operate, can save cost and improve production efficiency.
Description
Technical Field
The invention relates to a method for improving the density of a 3D gel printing ceramic material, and belongs to the field of additive manufacturing (3D printing).
Background
Additive Manufacturing (AM) is an advanced technology with complex shapes and personalized manufacturing, in which print data is derived from a discrete part model, and a target part is built up by adding layer by layer under the guidance of the data. AM manufacturing complex shaped products requires the construction of three dimensional models in advance, which can be constructed by Computer Aided Design (CAD) or by reverse engineering methods such as scanners and computer tomography. With diversification of application and requirements, ceramic materials with multiple functions are developed at present, and have the characteristics of high hardness, high strength, high temperature resistance, good wear resistance and the like, but the characteristics make the ceramics with complex shapes difficult to manufacture by conventional methods, including dry pressing, injection molding, roll forming, tape casting and the like, and additive manufacturing is a technology capable of manufacturing very complex geometric shapes and has the potential of thoroughly changing the traditional ceramic industry, so that the additive manufacturing is continuously and deeply applied to the field of ceramic materials at present, for example, the traditional ceramics, biological ceramics, magnetic ceramics, piezoelectric ceramics and the like are widely applied. 3D gel-Printing (3 DGP) is used as a Direct ink-jet Printing technology (DIP), and has great technical advantages in the field of 3D Printing ceramic materials.
Due to the arbitrary shape design and the free combination of material components, 3D gel printing technology is becoming an advantageous method for manufacturing complex shaped articles. The density of a general ceramic material part affects the mechanical properties of ceramics and also has a decisive influence on the functions of the ceramics, wherein various factors affecting the densification of the 3D gel printing ceramic material, such as the properties of raw materials, the interaction among powders, sintering conditions and the like, but the gap between the wires is a key factor affecting the densification of the 3D gel printing technology based on the principle of stacking and forming the printing wires, and how to further reduce the gap determines the application prospect of the printing technology. The invention aims to explore the influence of key parameters of 3D gel printing in the subsequent silk stacking process and provides a technical idea of how to obtain higher ceramic density so as to meet the requirement of a compact ceramic product in practical application.
Disclosure of Invention
The 3D gel printing technology can realize the three-dimensional shaping of the appearance and the free combination of material components, and becomes a method for manufacturing a workpiece with a complex shape, but the gap between the wires is a key factor influencing the compactness of the 3D gel printing technology based on the principle of printing wire accumulation shaping, so how to further reduce the gap is necessary to research the printing method of high-density ceramics.
The invention provides a method for improving the density of a 3D gel printing ceramic material for preparing a high-density ceramic product.
Based on the above principle, the process of the present invention includes: establishing a printing model, setting a program, preparing printing raw materials, printing and forming, drying a workpiece, degreasing, sintering and the like. The invention provides a 3D printing method suitable for wire accumulation forming to improve ceramic density, which comprises the following steps:
(1) setting of the print control program: setting the diameter of the printing wire to d and the layer height to K by a printing program2d(K20.5 to 1.0), the diameter of the output printing filament used by the printer is D, and the relation between the two is set as D-K1d(K11.12-1.30), and the printing wire of the upper layer is positioned at the middle position of two adjacent wires of the lower layer in the modeling and program setting processes, as shown in fig. 1 b;
(2) preparing a printing wire and a printing process: mixing ceramic powder with 3-8 wt% of PVA solution in a certain proportion, wherein the solid content of the powder is 40% -70%, continuously adding oleic acid with the mass of 5-10 wt% of the ceramic powder, uniformly stirring to obtain ceramic slurry, loading the ceramic slurry into a charging barrel of a printer, densely adding the ceramic slurry layer by layer in a stacking mode according to a graph 1c under the control guidance of the printing program and model data, and performing gel printing to obtain a target workpiece;
(3) and then, carrying out vacuum drying on the workpiece for 8-48 h at 30-50 ℃, degreasing the dried blank for 3-6 h at 450-660 ℃, and then sintering at the temperature of more than 1000 ℃ for 2-5 h to obtain the compact ceramic workpiece.
Further, the 3D printing parameters for improving the compactness of the ceramic in step (1) are set differently, so that the overlapping degree of the stacked printing wires is different.
Further, the printing parameters in the step (1) are suitable for a 3D gel printing method based on silk stacking molding and the printing silk has certain fluidity, and the key characteristic of densification is the staggered and overlapped stacking mode of the printing silk; in the printing process, the diameter of the printing wire is larger than that of the wire set by a program, so that the adjacent wires are partially overlapped and blended, the lower limit of the overlapping degree is to completely fill the wire gap, and the printing wire is piled and formed in such a way.
Further, the raw material powder of the printing wire in the step (2) includes ceramic materials such as strontium ferrite, zirconia, calcium phosphate and the like and materials thereof.
Further, the compact ceramic part prepared in the step (3) has higher density, and the density range of the part is 98-99.8%.
The principle of the invention is as follows: by setting printing parameters and adjusting the actual printing diameter, the gaps among the stacked wires do not exist, and the gaps are reduced, so that the density is improved. Firstly, when the 3D printing technology is used for normally printing the stacked wires, the gap defect of the gray part in the graph 1a can occur, the dislocation stacking forming shown in the graph 1b is converted into the dislocation stacking forming through the model establishment and the setting of the printing program, the gap is reduced to a certain extent, the diameter of the actually printed wires is adjusted to be larger than the diameter of the actually printed wires set by the program, the printed wires are partially overlapped, as shown in the graph 1c, the printed wires have certain fluidity, the overlapped parts can fill the gaps and are mutually blended with other adjacent wires, and therefore huge gaps in the stacking of the common printed wires are solved, and the density of the 3D printed ceramic parts is improved.
Compared with the prior art, the method of the invention has the advantages that: according to the 3D gel printing method based on the wire stacking forming principle, the printing parameters are set and the actual printing parameters are adjusted, so that gaps among stacked wires do not exist, and gaps are reduced or eliminated, so that the density is improved. The method has the advantages of stable process, high production efficiency, short production period, capability of producing ceramic parts with complex shapes, higher density of the obtained ceramic parts and great development potential in the additive manufacturing field of compact ceramic materials and the like.
Drawings
FIG. 1 is a schematic diagram showing the influence of three different stacking modes of 3D gel printing wires on the compactness of a printed product,
wherein figure 1a is a schematic diagram of a common stacking of 3D gel-printed filaments,
figure 1b is a schematic diagram of a 3D gel-printed filament staggered stack,
fig. 1c is a schematic view of the 3D gel-printed wire stacking with interleaving and overlapping.
Detailed Description
The process of the present invention comprises: establishing a printing model, setting a program, preparing printing raw materials, printing and forming, drying a workpiece, degreasing, sintering and the like.
According to the method, the gap between the stacked wires does not exist by setting the printing parameters and adjusting the actual printing diameter, so that the gap is reduced, the compactness is improved, after the raw materials are printed by preparation, the target ceramic part is printed by using the mature printing parameters, and finally, the compact ceramic part with excellent performance can be prepared by drying and sintering.
Example 1: densifying strontium ferrite magnetic material part through 3D gel printing
(1) 6g of KH550 silane coupling agent is taken and 50g of SrFe is added12O19Stirring the powder evenly, adding 6g of 5 wt% PVA solution, and stirringIn the stirring process, adding proper oleic acid until the mixture is uniformly stirred to prepare SrFe12O19And (4) slurry.
(2) Respectively loading the slurries obtained in the step (1) into a charging barrel of a 3D gel printer, introducing the shape of a product to be printed into a computer control system for printing, setting the printing diameter to be 0.48mm and the printing layer height to be 0.42mm by a program, setting the diameter of a nozzle selected for printing to be 0.56mm and the layer height to be 0.49mm, and setting the printing speed to be 6mm/s, wherein the slurries can be uniformly extruded under the action of air pressure, so that the dense accumulation of printing wires is realized.
(3) And (3) carrying out vacuum drying on the blank obtained by printing for 48h at the temperature of 30-50 ℃, degreasing the blank subjected to drying for 3h at the temperature of 660 ℃, and then sintering at the temperature of 1250 ℃ for 2h to obtain the ceramic part with the relative density of 99.10%.
Example 2: densification of calcium phosphate bioceramic articles by 3D gel printing
(1) 6g of 8 wt% PVA is taken, proper oleic acid and citric acid are added in the stirring process, and finally 6g of calcium phosphate is added, and the calcium phosphate slurry is prepared after even stirring.
(2) And (2) loading the slurry obtained in the step (1) into a charging barrel of a 3D gel printer, introducing the shape of a product to be printed into a computer control system for printing, presetting the program to be 0.37mm in diameter, 0.36m in printing layer height, 0.41mm in diameter of a nozzle selected for printing, and 10mm/s in printing speed, wherein the material can be uniformly extruded under the action of air pressure, and the accumulation molding of the densification yarn is completed.
(3) And (3) drying the printed blank body at 30-50 ℃ for 8-24 h in vacuum, degreasing the dried blank body at 660 ℃ for 2h respectively, and sintering at 1100 ℃ for 3h to obtain a finished piece with the relative density of 98.20%.
Example 3: densifying zirconia bioceramic article by 3D gel printing
(1) 7.39g of acrylamide and 0.40g of N, N-methylenebisacrylamide were added to 44.24g of deionized water to form a premix, 234.68g of zirconia powder was added, and appropriate citric acid was added while stirring to form a uniform slurry.
(2) And (2) respectively loading the slurry obtained in the step (1) into a charging barrel of a 3D gel printer, introducing the shape of a product to be printed into a computer control system for printing, setting the diameter of a printing wire to be 0.41mm, the height of a printing layer to be 0.36mm, the diameter of a nozzle selected for printing to be 0.47mm, and the printing speed to be 10mm/s, wherein the material can be uniformly extruded under the action of air pressure, and the accumulation molding of the densification wire is completed.
(3) And (3) drying the printed blank body in vacuum at 30-50 ℃ for 8-24 h, degreasing the dried blank body at 250 ℃, 420 ℃ and 660 ℃ for 3h, 9h and 3h respectively, and then respectively preserving heat at 1050 ℃, 1300 ℃ and 1400 ℃ and 1500 ℃ for 2h for sintering to obtain the zirconia ceramic product with the relative density of 98.86%.
Example 4: densifying the magnesium ferrite soft magnetic ferrite product by 3D gel printing
(1) Adding 50g of magnesium ferrite powder into 6g of 6 wt% PVA solution, adding proper oleic acid and citric acid during stirring, and uniformly stirring to obtain magnesium ferrite slurry.
(2) And (2) loading the slurry obtained in the step (1) into a charging barrel of a 3D gel printer, introducing the shape of a product to be printed into a computer control system for printing, presetting the program to be 0.37mm in diameter, 0.36mm in printing layer height, 0.41mm in diameter of a nozzle selected for printing, and 10mm/s in printing speed, wherein the material can be uniformly extruded under the action of air pressure, and the accumulation molding of the densification yarn is completed.
(3) And (3) drying the printed blank body at 30-50 ℃ for 8-24 h in vacuum, degreasing the dried blank body at 660 ℃ for 3h respectively, and sintering at 1100 ℃ for 2h to obtain a finished piece with the relative density of 98.50%.
Example 5: magnetic compact part prepared by printing strontium ferrite doped calcium phosphate through 3D gel
(1) Premixing 8g of calcium phosphate powder and 2g of strontium ferrite powder, then adding 9g of 6 wt% PVA solution, adding proper oleic acid in the stirring process, and finally uniformly stirring to obtain ceramic slurry.
(2) And (2) loading the slurry obtained in the step (1) into a charging barrel of a 3D gel printer, introducing the shape of a product to be printed into a computer control system for printing, presetting the program to be 0.37mm in diameter, 0.36m in printing layer height, 0.41mm in diameter of a nozzle selected for printing, and 9mm/s in printing speed, wherein the material can be uniformly extruded under the action of air pressure, and the accumulation molding of the densification yarn is completed.
(3) And (3) drying the printed blank body at 30-50 ℃ for 8-24 h in vacuum, degreasing the dried blank body at 660 ℃ for 2h respectively, and sintering at 1150 ℃ for 3h to obtain a finished piece with relative density of 98.12%.
Claims (5)
1. A method for improving the compactness of a 3D gel printing ceramic material is characterized by comprising the following steps:
(1) setting of the print control program: printing wire diameter program set to d, layer height set to K2d(K20.5 to 1.0), the diameter of the output printing filament used by the printer is D, and the relation between the two is set as D-K1d(K11.12-1.30), and enabling the printing wire of the upper layer to be positioned in the middle of two adjacent wires of the lower layer in the aspects of model establishment and program setting;
(2) preparing printing slurry and printing: mixing ceramic powder with 3-8 wt% of polyvinyl alcohol (PVA) solution according to a certain proportion, wherein the solid content of the powder is 40% -70%, continuously adding oleic acid with the mass of 5-10 wt% of the ceramic powder, uniformly stirring to obtain ceramic slurry, loading the ceramic slurry into a charging barrel of a printer, densely piling layer by layer under the control of the printing program and model data, and performing gel printing to obtain a target workpiece;
(3) post-treatment and sintering processes: and then, carrying out vacuum drying on the workpiece for 8-48 h at 30-50 ℃, degreasing the dried blank for 3-6 h at 450-660 ℃, and then sintering at the temperature of more than 1000 ℃ for 2-5 h to obtain the compact ceramic workpiece.
2. The method for improving the densification of a 3D gel printed ceramic material according to claim 1, wherein: the printing parameters set in step (1) are different, so that the overlapping degree of the stacked printing wires is different.
3. The method for improving the densification of a 3D gel printed ceramic material according to claim 1, wherein: the printing parameters in the step (1) are suitable for a 3D gel printing method based on silk stacking molding and the printing silk has certain fluidity, and the key characteristic of densification is the staggered and overlapped stacking mode of the printing silk; in the printing process, the diameter of the printing wire is larger than that of the wire set by a program, so that the adjacent wires are partially overlapped and blended, the lower limit of the overlapping degree is to completely fill the wire gap, and the printing wire is piled and formed in such a way.
4. The method for improving the densification of a 3D gel printed ceramic material according to claim 1, wherein: the printing slurry raw material powder in the step (2) comprises strontium ferrite, zirconia, calcium phosphate ceramic and materials thereof.
5. The method for improving the densification of a 3D gel printed ceramic material according to claim 1, wherein: the compact ceramic part prepared in the step (3) has high density, and the density range of the part is 98-99.8%.
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| CN111283844A (en) * | 2020-01-22 | 2020-06-16 | 北京科技大学 | Method for preparing strontium ferrite product by 3D gel printing |
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| US20170113409A1 (en) * | 2015-10-23 | 2017-04-27 | Makerbot Industries, Llc | Build patterns for surfaces of a three-dimensionally printed object |
| US20180297272A1 (en) * | 2017-04-14 | 2018-10-18 | Desktop Metal, Inc. | High density 3d printing |
| CN109498844A (en) * | 2018-11-22 | 2019-03-22 | 北京科技大学 | A kind of method of the high compound porosity tissue scaffold design material of low cost preparation |
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