CN111168807B - 3D printing device and method for biomimetic porous continuous carbon fiber reinforced ceramic bone scaffold - Google Patents
3D printing device and method for biomimetic porous continuous carbon fiber reinforced ceramic bone scaffold Download PDFInfo
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- CN111168807B CN111168807B CN202010060243.XA CN202010060243A CN111168807B CN 111168807 B CN111168807 B CN 111168807B CN 202010060243 A CN202010060243 A CN 202010060243A CN 111168807 B CN111168807 B CN 111168807B
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 90
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 90
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 210000000988 bone and bone Anatomy 0.000 title claims abstract description 52
- 239000011226 reinforced ceramic Substances 0.000 title claims abstract description 28
- 238000010146 3D printing Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 18
- 230000003592 biomimetic effect Effects 0.000 title 1
- 239000002002 slurry Substances 0.000 claims abstract description 93
- 239000000835 fiber Substances 0.000 claims abstract description 69
- 239000002131 composite material Substances 0.000 claims abstract description 39
- 239000000919 ceramic Substances 0.000 claims abstract description 32
- 238000001125 extrusion Methods 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 27
- 239000011664 nicotinic acid Substances 0.000 claims abstract description 12
- 239000007790 solid phase Substances 0.000 claims description 104
- 239000000725 suspension Substances 0.000 claims description 46
- 238000010438 heat treatment Methods 0.000 claims description 43
- 239000000843 powder Substances 0.000 claims description 22
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 21
- 238000007639 printing Methods 0.000 claims description 21
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 16
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 14
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 14
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 14
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 238000010008 shearing Methods 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 8
- 238000003860 storage Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
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- 230000004071 biological effect Effects 0.000 abstract 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 63
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 63
- 239000010410 layer Substances 0.000 description 20
- 229910010293 ceramic material Inorganic materials 0.000 description 13
- 238000005187 foaming Methods 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
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- 238000001878 scanning electron micrograph Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
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- 239000001506 calcium phosphate Substances 0.000 description 1
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- 229910052799 carbon Inorganic materials 0.000 description 1
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- 238000005336 cracking Methods 0.000 description 1
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- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 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 1
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- 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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- B33—ADDITIVE MANUFACTURING TECHNOLOGY
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- B33Y10/00—Processes of additive manufacturing
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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
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
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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
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Abstract
本发明公开了一种仿生多孔连续碳纤维增强陶瓷骨支架的3D打印装置及方法，本发明所述的装置，将连续纤维预处理装置与陶瓷浆料挤出装置结合，实现了连续纤维增强陶瓷骨支架3D打印装置的一体化设计。本发明的方法所采用的纤维预处理材料为与基体材料相同但固含量较低的陶瓷浆料，固含量较低的陶瓷浆料具有更好的浸润性，不仅可以黏附于碳纤维复丝的外部，还可以渗入碳纤维复丝内部，实现黏附，从而提高复合材料的生物性能。
The invention discloses a 3D printing device and method for a bionic porous continuous carbon fiber reinforced ceramic bone scaffold. The device of the invention combines a continuous fiber pretreatment device with a ceramic slurry extrusion device to realize the continuous fiber reinforced ceramic bone scaffold. The integrated design of the stent 3D printing device. The fiber pretreatment material used in the method of the present invention is a ceramic slurry with the same matrix material but with a lower solid content. The ceramic slurry with a lower solid content has better wettability and can not only adhere to the outside of the carbon fiber multifilament , and can also penetrate into the carbon fiber multifilament to achieve adhesion, thereby improving the biological properties of the composite material.
Description
Technical Field
The invention belongs to the technical field of 3D printing, and particularly relates to a 3D printing device and method for a bionic porous continuous carbon fiber reinforced ceramic bone scaffold.
Background
The biological ceramic material such as hydroxyapatite, calcium phosphate and the like has the advantages of good biocompatibility, good osteoconductivity, no toxic or side effect on human bodies and the like, so the biological ceramic material becomes an important artificial bone grafting material, but the inherent brittleness of the ceramic material greatly limits the wide application of the biological ceramic material in the technical field of bearing capacity and high reliability. For this reason, ceramic matrix composites with fibers as reinforcement materials have been developed to improve their mechanical properties.
The carbon fiber is a novel high-strength and high-modulus fiber material with the carbon content of more than 95 percent, has a series of advantages of small density, light weight, high strength, low expansion coefficient and the like, and can effectively control the generation and growth of cracks in a matrix and greatly improve the comprehensive mechanical property of the ceramic material by taking the carbon fiber as a reinforcement.
Compare in the shaping manufacturing of traditional carbon fiber reinforced ceramic matrix composite, utilize 3D printing technique's high efficiency and flexibility, can more quick preparation hole structure controllable and have excellent mechanical properties's bone scaffold. Due to the specific viscosity characteristic of the ceramic slurry, when the viscosity of the slurry is too low, the bone scaffold cannot be molded or the mechanical property of the molded bone scaffold is poor; the viscosity is too high, the slurry is difficult to extrude, and the support precision is low. In addition, compared with the chopped fiber reinforced ceramic material, the continuous fiber reinforced ceramic material needs to be extruded in the extruding process, and the adhesion effect of the two materials needs to be considered, so that the ceramic slurry can be uniformly coated with fibers and can be extruded from a nozzle together to complete the 3D printing process.
Disclosure of Invention
To address the above-discussed shortcomings and drawbacks of the prior art, the present invention provides an apparatus and method that may implement a continuous carbon fiber reinforced ceramic bone scaffold. Through pretreatment of the carbon fiber multifilament, continuous carbon fiber adhesive ceramic slurry is extruded out from a nozzle together, so that the mechanical property of the bracket is improved; the ceramic slurry with higher viscosity can be continuously and uniformly extruded by adopting pneumatic and screw type hybrid transmission, so that the forming precision of the bracket is ensured. The ceramic bone scaffold with high precision, high strength, controllable pore structure and excellent biological performance is obtained from two aspects of devices and processes.
In order to achieve the aim, the 3D printing device of the bionic porous continuous carbon fiber reinforced ceramic bone scaffold comprises a fiber pretreatment device and a composite material extrusion device;
the fiber pretreatment device comprises a yarn storage roller and a pretreatment groove, the upper end of the pretreatment groove is provided with a yarn inlet and a yarn inlet, the lower end of the pretreatment groove is provided with a yarn outlet, the yarn outlet is provided with a heating conduit, the heating conduit is fixed in a heating block, and a fiber feeding device is arranged below the heating block;
the composite material extruding device comprises an extruding cylinder and a screw cylinder, wherein the screw cylinder is provided with a slurry input port, one end of the extruding cylinder is connected with the pneumatic device, the other end of the extruding cylinder is provided with a discharge port, and the discharge port is connected with the slurry input port through a conveying pipe; the screw is installed in the screw barrel and driven by a power device, an extension part extends downwards from the front end of the screw barrel, a nozzle is fixed at the lower end of the extension part, and a shearing device is arranged below the outer part of the nozzle.
Further, the fiber feeding device comprises a driving wheel and a driven wheel, the driving wheel is a gear, the driven wheel is a disc, and the space between the driven wheel and the driving wheel is carbon fiber wrapping the low solid-phase ratio slurry.
Further, two rows of tensioning rollers for tensioning the fibers are arranged inside the pretreatment tank.
Furthermore, a fiber guide pipe is fixedly arranged in the extension part, the upper end of the fiber guide pipe extends out of the extension part, and the lower part of the fiber guide pipe is connected with the nozzle.
A3D printing method of the 3D printing device based on the bionic porous continuous carbon fiber reinforced ceramic bone scaffold comprises the following steps:
step 1, mixing deionized water and glycerol according to a mass ratio of 7: 3-8: 2 to prepare a solution A;
9, inputting the slurry with the high solid-phase ratio in the extruding cylinder into the screw cylinder through a material conveying pipe by using a pneumatic device;
and step 12, drying the printed porous ceramic bone scaffold blank for 12-24 h at room temperature, then drying for 1-2 h in a drying oven at 50-70 ℃, heating to 400-500 ℃ at 3 ℃/min in a muffle furnace, preserving heat for 3-4 h, and finally sintering for 3-4 h at 1100-1200 ℃ in a hot pressing furnace to obtain the porous continuous carbon fiber reinforced ceramic bone scaffold.
Further, in step 3, after preparing the HA suspension with low solid phase ratio and high solid phase ratio, the HA suspension with low solid phase ratio and the HA suspension with high solid phase ratio are ball milled respectively.
Further, in step 4, n-butanol is added into the ball-milled suspension with the low solid phase ratio and the suspension with the high solid phase ratio respectively.
Compared with the prior art, the invention has at least the following beneficial technical effects:
1) according to the device, the continuous fiber pretreatment device is combined with the ceramic slurry extrusion device, so that the integrated design of the continuous fiber reinforced ceramic bone support 3D printing device is realized.
Further, the extrusion of the ceramic slurry is realized by adopting a pneumatic and screw combined mode. The mixing structure can adapt to the characteristic of high viscosity of ceramic slurry; in addition, aiming at different contents of fiber multifilaments and sizing agents with different diameters, the feeding amount and pressure of the sizing agents can be adjusted by adjusting pneumatic pressure and screw rotation speed so as to meet the molding requirements of different supports; because the pressure of the slurry is higher or the viscosity of the slurry is lower in the extrusion process, the slurry may flow out from the nozzle after the extrusion is stopped, so-called drooling phenomenon, and the screw inversion can be adopted in the screw transmission process to reduce the drooling phenomenon.
Furthermore, the carbon fibers are cured and pretreated by the heating block, and on one hand, the fibers are softened by heating to promote the combination of the slurry and the fibers; on the other hand, the slurry adhered to the surface of the carbon fiber is solidified by heating to wrap the carbon fiber, so that the fiber multifilament can be prevented from being scattered and broken during extrusion.
2) The fiber pretreatment material adopted by the method is ceramic slurry which is the same as a base material but has lower solid content, and the method mainly has the following advantages:
(1) the ceramic slurry with lower solid content has better wettability, not only can be adhered to the outside of the carbon fiber multifilament, but also can permeate into the inside of the carbon fiber multifilament to realize adhesion, thereby improving the biological performance of the composite material.
(2) The surface of the carbon fiber after pretreatment is adhered with a layer of ceramic slurry, so that the carbon fiber is prevented from being directly combined with the slurry with high solid content for forming, and the problem of difficult adhesion of the slurry with high solid content and the carbon fiber is solved through the combination of the ceramic material and the ceramic material.
(3) The traditional resin pretreatment material is finally subjected to degreasing and sintering to remove resin, and the process can cause defects of cracking, deformation and the like of the bracket. And the ceramic material is used as a pretreatment material, and degreasing sintering is not needed after the support is formed, so that the sintered support has better mechanical property.
Further, in the step 4, n-butyl alcohol is respectively added into the suspension liquid with low solid phase ratio and high solid phase ratio after ball milling is finished, so that the foaming of HA suspension liquid is prevented, and further, the defects of holes or pits of the extruded wire are prevented.
Drawings
FIG. 1 is a schematic view of a continuous carbon fiber reinforced ceramic bone scaffold 3D printing apparatus of the present invention;
FIG. 2 is a topographical view of a continuous carbon fiber reinforced hydroxyapatite bone scaffold;
FIG. 3 is a sectional SEM image of a continuous carbon fiber reinforced hydroxyapatite bone scaffold;
fig. 4 is an SEM image of the continuous carbon fiber crack bridging mechanism during stent fracture.
In the drawings: 1-filament storage roller, 2-continuous carbon fiber, 3-filament inlet, 4-feed inlet, 5-pretreatment tank, 6-tension roller, 7-filament outlet, 8-heating conduit, 9-heating speed, 10-fiber feeding device, 11-fiber conduit, 12-nozzle, 13-three-shaft moving platform, 14-screw barrel, 15-screw rod, 16-coupler, 17-stepping motor, 18-slurry inlet, 19-material conveying pipe, 20-extrusion discharge barrel, 21-pneumatic device and 22-shearing device.
Detailed Description
In order to make the objects and technical solutions of the present invention clearer and easier to understand. The present invention will be described in further detail with reference to the following drawings and examples, wherein the specific examples are provided for illustrative purposes only and are not intended to limit the present invention.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention. Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified. In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Referring to fig. 1, a 3D printing device of a bionic porous continuous carbon fiber reinforced ceramic bone scaffold comprises a fiber pretreatment device and a composite material extrusion device.
The fiber pretreatment device comprises a fiber storage roller 1 and a pretreatment groove 5, wherein the upper end of the pretreatment groove 5 is provided with a fiber inlet 3 for feeding fibers and a feed inlet 4 for adding low solid-phase ratio slurry, two rows of tensioning rollers 6 for tensioning the fibers are arranged inside the pretreatment groove, the lower end of the pretreatment groove is provided with a fiber outlet 7, the fiber outlet 7 is connected with a heating conduit 8, the heating conduit 8 is fixed in a heating block 9, a fiber feeding device 10 is arranged below the heating block 9, the fiber feeding device 10 comprises a driven wheel and a driving wheel, the driving wheel is a gear, the driven wheel is a disc, the distance between the driven wheel and the driving wheel is carbon fiber wrapping the low solid-phase ratio slurry, and the carbon fiber is fed by the driven wheel and the driving wheel in a meshed mode.
The composite material extrusion device comprises an extrusion cylinder 20, one end of the extrusion cylinder 20 is connected with a pneumatic device 21, the other end of the extrusion cylinder is provided with a discharge hole, the discharge hole is connected with one end of a material conveying pipe 19, and the other end of the material conveying pipe 19 is connected with a slurry input port 18; the slurry inlet 18 is arranged at the upper end of the screw cylinder 14 and communicated with the screw cylinder 14, the screw rod 15 is installed in the screw cylinder 14, the stepping motor 17 is connected with the input shaft end of the screw rod 15 through the coupler 16, the front end of the screw cylinder 14 extends downwards to form an extension part, the lower end of the extension part is fixed with the nozzle 12, the fiber guide pipe 11 is arranged in the extension part and fixed, the upper end of the fiber guide pipe 11 extends out of the extension part, the lower part of the fiber guide pipe is connected with the nozzle 12, the shearing device 22 is arranged below the outer part of the nozzle 12, and the three-axis motion platform 13 is arranged under the nozzle 12. The diameter of the nozzle 12 is 500-1000 μm.
The ceramic material (matrix) adopts Hydroxyapatite (HA) powder, and the carbon fiber multifilament consists of 5-20 carbon fibers.
The preparation method of the continuous carbon fiber reinforced ceramic bone scaffold comprises the following steps:
step 1, mixing deionized water and glycerol according to a mass ratio of 7: 3-8: 2 to prepare 100ml of solution, placing the solution in a magnetic stirrer, and uniformly stirring to obtain solution A.
And 4, respectively adding hydroxypropyl methyl cellulose (HPMC) serving as a binder into the HA suspensions with two different solid phase ratios, wherein the mass of the hydroxypropyl methyl cellulose is 1-2% of the mass of the HA powder in the HA suspensions, performing ball milling for 3 hours at the frequency of 30Hz, respectively adding n-butyl alcohol into the two HA suspensions subjected to ball milling, and preventing the HA suspensions from foaming to obtain low-solid-phase-ratio slurry and high-solid-phase-ratio slurry.
And 5, leading out carbon fibers 2 from the filament storage roller 1, leading the carbon fibers 2 into a pretreatment tank 5 from a filament inlet 3, passing through a tensioning roller 6 and a fiber feeding device 10, and finally leading into a fiber guide pipe 11.
And step 6, continuing to ball-mill the obtained low solid-phase ratio slurry and the high solid-phase ratio slurry for 0.5h at the frequency of 30 Hz. Adding the ball-milled slurry with the low solid-phase ratio into a pretreatment tank 5 through a feed inlet 4, and adding the slurry with the high solid-phase ratio into an extrusion barrel 20.
And 7, the carbon fiber 2 soaked with the low solid-phase ratio slurry enters a heating conduit 8 through a filament outlet 7, and is heated by a heating block 9 at the temperature of 40-50 ℃ to finish curing.
And 9, operating the pneumatic device 21, and inputting the slurry with the high solid-phase ratio in the extrusion material cylinder 20 into the screw cylinder 18 through the material conveying pipe 19.
And step 10, operating a stepping motor 17, driving a screw rod 15 to rotate through a coupler 16, pushing the high solid-phase ratio slurry to gradually move forwards to a nozzle 12, and uniformly and completely coating the cured pretreated carbon fibers at the nozzle 12 to form the composite wire. As can be seen from FIG. 3, the continuous carbon fibers are uniformly wrapped in the center of the filament material by the slurry with a high solid-to-solid ratio.
And 11, continuously extruding the composite wires from the nozzle 12, moving an XY motion platform in a three-axis motion platform 13 according to a printing path to continuously stack the composite wires on the XY motion platform, according to a pre-designed three-dimensional model, enabling the wire spacing to be 500-1000 microns, and enabling the interlayer angle to be 45-90 degrees, after printing of one layer of the composite wires is finished, cutting the composite wires at the outlet of the nozzle 12 by a shearing device 22, then descending a Z-axis lifting table by a layer thickness distance, changing the printing direction, repeating the steps, and depositing layer by layer to realize the molding of the porous ceramic bone scaffold to obtain a porous ceramic bone scaffold blank.
And step 12, drying the printed porous ceramic bone scaffold blank at room temperature for 12-24 h, then drying in a drying oven at 50-70 ℃ for 1-2 h, heating to 400-500 ℃ at 3 ℃/min in a muffle furnace, preserving heat for 3-4 h, and finally sintering in a hot pressing furnace at 1100-1200 ℃ for 3-4 h to obtain the porous continuous carbon fiber reinforced ceramic bone scaffold.
Example 1
The following example is provided to further illustrate the preparation of the continuous carbon fiber reinforced ceramic bone scaffold.
The matrix adopts Hydroxyapatite (HA) powder, and the carbon fiber multifilament consists of 10 carbon fibers.
Step 1, mixing deionized water and glycerol according to a mass ratio of 7:3 to prepare a solution of 100, placing the solution in a magnetic stirrer, and stirring for 15min to obtain a solution A.
And 3, mixing the solution B with HA powder, and respectively preparing HA suspensions with a low solid phase ratio and a high solid phase ratio, wherein the solid phase ratio of the HA suspension with the low solid phase ratio is 7.5%, the solid phase ratio of the HA suspension with the high solid phase ratio is 25%, and the two HA suspensions are respectively subjected to ball milling for 12 hours at the frequency of 30Hz, so that the slurry is more uniform and HAs better dispersibility.
And 4, respectively adding hydroxypropyl methyl cellulose (HPMC) serving as a binder into the HA suspensions with the two different solid phase ratios, wherein the mass of the hydroxypropyl methyl cellulose is 1.5% of the mass of the HA powder in the HA suspensions, performing ball milling for 12 hours at the frequency of 30Hz, respectively adding n-butyl alcohol into the two HA suspensions subjected to ball milling, preventing the HA suspensions from foaming, and obtaining the low-solid-phase-ratio slurry and the high-solid-phase-ratio slurry.
And 5, leading out carbon fibers 2 from the filament storage roller 1, leading the carbon fibers 2 into a pretreatment tank 5 from a filament inlet 3, passing through a tensioning roller 6 and a fiber feeding device 10, and finally leading into a fiber guide pipe 11.
And step 6, continuing to ball-mill the obtained low solid-phase ratio slurry and the high solid-phase ratio slurry for 0.5h at the same frequency. Adding the ball-milled slurry with the low solid-phase ratio into a pretreatment tank 5 through a feed inlet 4, and adding the slurry with the high solid-phase ratio into an extrusion barrel 20.
And 7, the carbon fiber 2 soaked with the low solid-phase ratio slurry enters a heating conduit 8 through a filament outlet 7, and is heated by a heating block 9 at the heating temperature of 40 ℃ to finish curing.
And 9, operating the pneumatic device 21, and inputting the slurry with the high solid-phase ratio in the extrusion material cylinder 20 into the screw cylinder 18 through the material conveying pipe 19.
And step 10, operating a stepping motor 17, driving a screw rod 15 to rotate through a coupler 16, pushing the high solid-phase ratio slurry to gradually move forwards to a nozzle 12, and uniformly and completely coating the cured pretreated carbon fibers at the nozzle 12 to form the composite wire. As can be seen from FIG. 3, the continuous carbon fibers are uniformly wrapped in the center of the filament material by the slurry with a high solid-to-solid ratio.
And 11, continuously extruding the composite wires from the nozzle 12, moving an XY motion platform in a triaxial motion platform 13 with the diameter of 1000 microns of the nozzle according to a printing path, continuously stacking the composite wires on the XY motion platform, according to a pre-designed three-dimensional model, enabling the wire spacing to be 600 microns, and enabling the interlayer angle to be 90 degrees, cutting the composite wires at the outlet of the nozzle 12 by a shearing device 22 after printing of one layer of composite wires is finished, then descending a Z-axis lifting platform by a layer thickness distance, changing the printing direction, repeating the steps, and depositing layer by layer to realize the molding of the porous ceramic bone scaffold to obtain a porous ceramic bone scaffold blank.
And step 12, drying the printed porous ceramic bone scaffold blank at room temperature for 12h, then drying in a drying oven at 50 ℃ for 1h, heating to 500 ℃ at a speed of 3 ℃/min in a muffle furnace, preserving heat for 3h, and finally sintering in a hot-pressing furnace at 1200 ℃ for 3h to obtain the porous continuous carbon fiber reinforced ceramic bone scaffold. The topography of the formed continuous carbon fiber reinforced hydroxyapatite bone scaffold is shown in figure 2. As can be seen from fig. 4, the continuous carbon fibers can bridge the fractured bone scaffold, thereby improving fracture toughness of the scaffold.
Example 2
The ceramic material adopts Hydroxyapatite (HA) powder, and the carbon fiber multifilament consists of 5 carbon fibers.
Step 1, mixing deionized water and glycerol according to a mass ratio of 7.5:2.5 to prepare a solution, placing the mixture of the deionized water and the glycerol in a magnetic stirrer, and uniformly stirring to obtain a solution A.
And 3, mixing the solution B with HA powder, respectively preparing HA suspensions with a low solid phase ratio and a high solid phase ratio, wherein the low solid phase ratio range is 5%, the high solid phase ratio range is 20%, ball-milling the two HA suspensions for 12 hours at the frequency of 30Hz respectively, and the ball-milling aims to make the slurry more uniform and have better dispersibility.
And 4, respectively adding hydroxypropyl methyl cellulose (HPMC) serving as a binder into the HA suspensions with the two different solid phase ratios, wherein the mass of the hydroxypropyl methyl cellulose is 1% of that of the HA powder in the HA suspensions, performing ball milling for 3 hours at the frequency of 30Hz, respectively adding n-butyl alcohol into the two HA suspensions subjected to ball milling, preventing the HA suspensions from foaming, and obtaining the low-solid-phase-ratio slurry and the high-solid-phase-ratio slurry.
The carbon fiber 2 of the solid phase ratio sizing agent enters a heating conduit 8 through a fiber outlet 7, the carbon fiber 2 is led out from a fiber storage roller 1 in the step 5 of heating the heating block through the heating of a heating block 9, the carbon fiber 2 enters a pretreatment tank 5 from a fiber inlet 3, passes through a tensioning roller 6 and a fiber feeding device 10, and finally is led into a fiber conduit 11.
And step 6, continuing to ball-mill the obtained low solid-phase ratio slurry and the high solid-phase ratio slurry for 0.6h at the same frequency. Adding the ball-milled slurry with the low solid-phase ratio into a pretreatment tank 5 through a feed inlet 4, and adding the slurry with the high solid-phase ratio into an extrusion barrel 20.
And 7, the carbon fiber 2 soaked with the low solid-phase ratio slurry enters a heating conduit 8 through a filament outlet 7, and is heated by a heating block 9 at the heating temperature of 45 ℃ to finish curing.
And 9, operating the pneumatic device 21, and inputting the slurry with the high solid-phase ratio in the extrusion material cylinder 20 into the screw cylinder 18 through the material conveying pipe 19.
And step 10, operating a stepping motor 17, driving a screw rod 15 to rotate through a coupler 16, pushing the high solid-phase ratio slurry to gradually move forwards to a nozzle 12, and uniformly and completely coating the cured pretreated carbon fibers at the nozzle 12 to form the composite wire. As can be seen from FIG. 3, the continuous carbon fibers are uniformly wrapped in the center of the filament material by the slurry with a high solid-to-solid ratio.
And 11, continuously extruding the composite wires from the nozzle 12, moving an XY motion platform in a triaxial motion platform 13 with the diameter of 500 mu m of the nozzle according to a printing path, continuously accumulating the composite wires on the XY motion platform, according to a pre-designed three-dimensional model, keeping the wire spacing of 800 mu m and the interlayer angle of 60 degrees, cutting the composite wires at the outlet of the nozzle 12 by a shearing device 22 after the printing of one layer of the composite wires is finished, then descending a Z-axis lifting platform by a layer thickness distance, changing the printing direction, repeating the steps, and depositing layer by layer to realize the molding of the porous ceramic bone scaffold to obtain a porous ceramic bone scaffold blank.
And step 12, drying the printed porous ceramic bone support blank at room temperature for 18h, then drying in a drying oven at 60 ℃ for 1.5h, heating to 450 ℃ at a rate of 3 ℃/min in a muffle furnace, preserving heat for 3h, and finally sintering in a hot-pressing furnace at 1150 ℃ for 3.5h to obtain the porous continuous carbon fiber reinforced ceramic bone support.
Example 3
The ceramic material adopts Hydroxyapatite (HA) powder, and the carbon fiber multifilament consists of 20 carbon fibers.
Step 1, mixing deionized water and glycerol according to a mass ratio of 8:2 to prepare a solution, placing the solution in a magnetic stirrer, and uniformly stirring to obtain a solution A.
And 3, mixing the solution B with HA powder, respectively preparing HA suspensions with a low solid phase ratio and a high solid phase ratio, wherein the low solid phase ratio range is 5%, the high solid phase ratio range is 30%, ball-milling the two HA suspensions for 12 hours at the frequency of 30Hz respectively, and the ball-milling aims to make the slurry more uniform and have better dispersibility.
And 4, respectively adding hydroxypropyl methyl cellulose (HPMC) serving as a binder into the HA suspensions with the two different solid phase ratios, wherein the mass of the hydroxypropyl methyl cellulose is 2% of the mass of the HA powder in the HA suspensions, performing ball milling for 3 hours at the frequency of 30Hz, respectively adding n-butyl alcohol into the two HA suspensions subjected to ball milling, preventing the HA suspensions from foaming, and obtaining the low-solid-phase-ratio slurry and the high-solid-phase-ratio slurry.
And 5, leading out carbon fibers 2 from the filament storage roller 1, leading the carbon fibers 2 into a pretreatment tank 5 from a filament inlet 3, passing through a tensioning roller 6 and a fiber feeding device 10, and finally leading into a fiber guide pipe 11.
And step 6, continuing to ball-mill the obtained low solid-phase ratio slurry and the high solid-phase ratio slurry for 0.5h at the same frequency. Adding the ball-milled slurry with the low solid-phase ratio into a pretreatment tank 5 through a feed inlet 4, and adding the slurry with the high solid-phase ratio into an extrusion barrel 20.
And 7, the carbon fiber 2 soaked with the low solid-phase ratio slurry enters a heating conduit 8 through a filament outlet 7, and is heated by a heating block 9 at the heating temperature of 50 ℃ to finish curing.
And 9, operating the pneumatic device 21, and inputting the slurry with the high solid-phase ratio in the extrusion material cylinder 20 into the screw cylinder 18 through the material conveying pipe 19.
And step 10, operating a stepping motor 17, driving a screw rod 15 to rotate through a coupler 16, pushing the high solid-phase ratio slurry to gradually move forwards to a nozzle 12, and uniformly and completely coating the cured pretreated carbon fibers at the nozzle 12 to form the composite wire. As can be seen from FIG. 3, the continuous carbon fibers are uniformly wrapped in the center of the filament material by the slurry with a high solid-to-solid ratio.
And 11, continuously extruding the composite wires from the nozzle 12, moving an XY motion platform in a triaxial motion platform 13 with the diameter of 800 microns of the nozzle according to a printing path, continuously stacking the composite wires on the XY motion platform, according to a pre-designed three-dimensional model, keeping the wire spacing of 1000 microns and the interlayer angle of 45 degrees, cutting the composite wires at the outlet of the nozzle 12 by a shearing device 22 after printing of one layer of the composite wires is finished, then descending a Z-axis lifting platform by a layer thickness distance, changing the printing direction, repeating the steps, and depositing layer by layer to realize the molding of the porous ceramic bone scaffold to obtain a porous ceramic bone scaffold blank.
And step 12, drying the printed porous ceramic bone support blank for 24 hours at room temperature, then drying the blank for 1 hour at 70 ℃ in a drying oven, heating the blank to 400 ℃ at a speed of 3 ℃/min in a muffle furnace, preserving the heat for 3 hours, and finally sintering the blank for 3 hours at a temperature of 1100 ℃ in a hot pressing furnace to obtain the porous continuous carbon fiber reinforced ceramic bone support.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (6)
1. A3D printing device of a bionic porous continuous carbon fiber reinforced ceramic bone scaffold is characterized by comprising a fiber pretreatment device and a composite material extrusion device;
the fiber pretreatment device comprises a yarn storage roller (1) and a pretreatment tank (5), wherein the upper end of the pretreatment tank (5) is provided with a yarn inlet (3) and a yarn inlet (4), the lower end of the pretreatment tank is provided with a yarn outlet (7), the yarn outlet (7) is provided with a heating pipe (8), the heating pipe (8) is fixed in a heating block (9), and a fiber feeding device (10) is arranged below the heating block (9);
the composite material extrusion device comprises an extrusion cylinder (20) and a screw cylinder (14), wherein the screw cylinder (14) is provided with a slurry input port (18), one end of the extrusion cylinder (20) is connected with a pneumatic device (21), the other end of the extrusion cylinder is provided with a discharge port, and the discharge port is connected with the slurry input port (18) through a feed delivery pipe (19); a screw (15) is installed in the screw cylinder (14), the screw (15) is driven by a power device, the front end of the screw cylinder (14) extends downwards to form an extension part, the lower end of the extension part is fixed with a nozzle (12), and a shearing device (22) is arranged below the outer part of the nozzle (12);
the fiber feeding device (10) comprises a driving wheel and a driven wheel, wherein the driving wheel is a gear, the driven wheel is a disc, and the space between the driven wheel and the driving wheel is carbon fiber wrapping the low solid-phase ratio slurry.
2. The 3D printing device of the bionic porous continuous carbon fiber reinforced ceramic bone scaffold as claimed in claim 1, wherein two rows of tensioning rollers (6) for tensioning fibers are arranged inside the pretreatment tank (5).
3. The 3D printing device for the bionic porous continuous carbon fiber reinforced ceramic bone scaffold as claimed in claim 1, wherein a fiber guide tube (11) is fixed in the extension part, the upper end of the fiber guide tube (11) extends out of the extension part, and the lower part of the fiber guide tube is connected with the nozzle (12).
4. The 3D printing method of the bionic porous continuous carbon fiber reinforced ceramic bone scaffold based on the printing device of claim 1 is characterized by comprising the following steps of:
step 1, mixing deionized water and glycerol according to a mass ratio of 7: 3-8: 2 to prepare a solution A;
step 2, adding ammonium polyacrylate with the mass being 1% -2% of that of the HA powder into the solution A, uniformly stirring, and adjusting the pH value to be 9 to obtain a solution B;
step 3, mixing the solution B with HA powder, and respectively preparing HA suspensions with low solid phase ratio and high solid phase ratio, wherein the solid phase ratio of the HA suspension with the low solid phase ratio is 5% -10%, and the solid phase ratio of the HA suspension with the high solid phase ratio is 20% -30%;
step 4, adding hydroxypropyl methyl cellulose serving as a binder into the HA suspensions with the low solid phase ratio and the high solid phase ratio prepared in the step 3 respectively, and performing ball milling to obtain low solid phase ratio slurry and high solid phase ratio slurry;
step 5, the carbon fibers (2) enter a pretreatment tank (5) from a fiber inlet (3), pass through a fiber feeding device (10) and then are introduced into a nozzle (12);
step 6, adding the low solid-phase ratio slurry into a pretreatment tank (5) from a feed inlet (4), and adding the high solid-phase ratio slurry into an extrusion barrel (20);
step 7, under the drive of a fiber feeding device (10), the carbon fibers (2) soaked with the slurry with the low solid-phase ratio enter a heating conduit (8) through a filament outlet (7), and are heated by a heating block (9) to finish curing;
step 8, feeding the cured carbon fibers (2) into a nozzle (12) through a fiber feeding device (10);
step 9, the high solid-phase ratio slurry in the extruding cylinder (20) is input into the screw cylinder (18) through a material conveying pipe (19) by a pneumatic device (21);
step 10, driving a screw (15) to rotate by a power device, pushing the high solid-phase ratio slurry to gradually move forwards to a nozzle (12), and coating the cured carbon fiber with the high solid-phase ratio slurry at the nozzle (12) to form a composite wire material;
step 11, continuously extruding the composite wires from the nozzle (12), moving an XY motion platform in a three-axis motion platform (13) according to a printing path to continuously pile the composite wires onto the XY motion platform, cutting off the composite wires at the outlet of the nozzle (12) by a shearing device (22) after printing of one layer of the composite wires is finished, descending a Z-axis lifting table by a layer thickness distance, changing the printing direction, repeating the steps, and depositing layer by layer to realize the molding of the porous ceramic bone support to obtain a porous ceramic bone support blank;
and step 12, drying the printed porous ceramic bone scaffold blank for 12-24 h at room temperature, then drying for 1-2 h in a drying oven at 50-70 ℃, heating to 400-500 ℃ at 3 ℃/min in a muffle furnace, preserving heat for 3-4 h, and finally sintering for 3-4 h at 1100-1200 ℃ in a hot pressing furnace to obtain the porous continuous carbon fiber reinforced ceramic bone scaffold.
5. The 3D printing method of the bionic porous continuous carbon fiber reinforced ceramic bone scaffold as claimed in claim 4, wherein in the step 3, after HA suspensions with low solid phase ratio and high solid phase ratio are prepared, the HA suspensions with low solid phase ratio and high solid phase ratio are respectively ball milled.
6. The 3D printing method of the bionic porous continuous carbon fiber reinforced ceramic bone scaffold as claimed in claim 4, wherein in the step 4, n-butanol is respectively added into the ball-milled suspension with the low solid phase ratio and the high solid phase ratio.
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