CN110639059B - 3D printing manufacturing method of artificial skull prosthesis - Google Patents
3D printing manufacturing method of artificial skull prosthesis Download PDFInfo
- Publication number
- CN110639059B CN110639059B CN201910958514.0A CN201910958514A CN110639059B CN 110639059 B CN110639059 B CN 110639059B CN 201910958514 A CN201910958514 A CN 201910958514A CN 110639059 B CN110639059 B CN 110639059B
- Authority
- CN
- China
- Prior art keywords
- printing
- ball
- powder
- test pieces
- artificial skull
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/14—Macromolecular materials
- A61L27/18—Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/12—Phosphorus-containing materials, e.g. apatite
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/14—Macromolecular materials
- A61L27/16—Macromolecular materials obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/14—Macromolecular materials
- A61L27/20—Polysaccharides
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
Abstract
The invention provides a 3D printing manufacturing method of an artificial skull prosthesis, which comprises the following steps: s1, mixing polyether-ether-ketone powder, nano hydroxyapatite powder and beta-tricalcium phosphate powder, and performing ball milling for 2 hours to obtain mixed powder; s2, adding a silane coupling agent into the mixed powder, and continuing ball milling to obtain a ball-milled mixture; s3, adding the treatment liquid into a high-speed ball mill for grinding to prepare a suspension mixed liquid; s4, stirring and mixing the suspension mixed liquor and the ball-milling mixture to obtain printing slurry; s5, printing the obtained printing slurry by using a 3D printer to obtain a skull repairing matrix; s6, placing the obtained skull repairing matrix for 10-15 minutes at a constant temperature of 80-90 ℃, and naturally cooling to room temperature to obtain the final artificial skull repairing body. The invention effectively solves the problem of mechanical comprehensive performance of the 3D printed artificial skull prosthesis, and has good biocompatibility and strong adaptability.
Description
Technical Field
The invention relates to the technical field of artificial skull restoration, in particular to a 3D printing manufacturing method of an artificial skull restoration.
Background
The artificial skull is manufactured by physical, chemical or biological methods and is used for repairing skull defects of human bodies caused by various reasons. The artificial skull material comprises silica gel, titanium alloy, polypropylene polyester high polymer material, self bone and the like.
Patent document with publication number CN 105662656 a discloses a 3D printed artificial skull patch and a preparation method thereof, which adopts 3D printing technology, and utilizes autologous bone powder and calcium hydroxy phosphate as basic raw materials of the artificial skull patch, thereby effectively solving the problem of biocompatibility of the artificial skull patch, the 3D printed artificial skull patch has high matching degree with the external dimensions of the defect part, greatly reducing the working strength of doctors, having good biocompatibility, being beneficial to inducing the growth of bone cells and promoting the repair, having high mechanical strength, and improving the safety of the operation. However, this prior art has the following drawbacks:
1. the self-body bone is utilized, but the self-body bone is limited in material selection, so that the bone body defect at another position can be caused while the skull is repaired, and an additional operation is generated when the self-body bone is selected, so that the pain and the risk of a patient are increased. Furthermore, this prior art uses autologous bone in powder form, which increases the risk of absorption of autologous bone components after application to skull repair.
2. Although the hydroxyapatite has good biocompatibility, the hydroxyapatite has the characteristics of low strength and poor toughness, and the technical effect part of the prior art shows that the compressive property of the obtained repairing material can only reach about 30MPa, and the limit value of the natural compressive strength of the human skull can reach about 60 MPa. In addition, the difference between the tensile property, the bending resistance and the impact toughness of the skull repairing material manufactured by the prior art and the skull of a human body is large.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a 3D printing manufacturing method of an artificial skull prosthesis, and the manufactured skull prosthesis has mechanical strength superior to that of a human skull while the biocompatibility of the manufactured skull prosthesis is ensured.
The technical scheme adopted by the invention for solving the technical problems is as follows: A3D printing and manufacturing method of an artificial skull prosthesis comprises the following steps:
s1, drying the polyether-ether-ketone powder, the nano hydroxyapatite powder and the beta-tricalcium phosphate powder according to a volume ratio of 82-85: 5-8: 4-5, and putting the mixture into a ball mill for ball milling for 2 hours to obtain mixed powder;
s2, adding a certain amount of silane coupling agent into the mixed powder, and continuing ball milling for 1 hour to obtain a ball-milled mixture;
s3, adding a treatment solution consisting of sodium polyacrylate, hydroxymethyl propyl cellulose, citric acid, glycerol and ethanol into a high-speed ball mill for grinding to prepare a suspension mixed solution;
s4, adding the suspension mixed liquor and the ball-milled mixture into a constant-temperature magnetic stirrer, and stirring and mixing for 20-30 minutes at 45 ℃ to obtain printing slurry;
s5, heating the obtained printing slurry to 60-70 ℃, and then printing by using a 3D printer to obtain a skull repairing matrix;
and S6, placing the obtained skull repairing matrix for 10-15 minutes at a constant temperature of 80-90 ℃, and naturally cooling to room temperature to obtain the final artificial skull repairing matrix.
Preferably, the weight ratio of the silane coupling agent to the mixed powder in the step S2 is 5-6: 100.
Preferably, the mass ratio of the sodium polyacrylate, the hydroxymethyl propyl cellulose, the citric acid, the glycerol and the ethanol in the treatment liquid is 8-12: 5-8: 3-5: 1-2: 30-35.
Preferably, the mass ratio of the suspension mixed liquid to the ball-milled mixture in the step S4 is 2-3: 10.
Preferably, the polishing time in step S3 is 20min to 30 min.
The invention has the following positive effects: the invention uses polyether-ether-ketone powder, nano-hydroxyapatite powder and beta-tricalcium phosphate powder as basic raw materials for 3D printing of the artificial skull prosthesis, uses silane coupling agent, sodium polyacrylate, hydroxymethyl propyl cellulose, citric acid and the like as suspension adhesives, adopts a 3D printing technology, effectively solves the problem of mechanical comprehensive performance of the 3D printed artificial skull prosthesis, and has good biocompatibility and strong adaptability.
Detailed Description
The following is a detailed description of preferred embodiments of the invention.
Example 1
The preferred embodiment 1 of the invention provides a 3D printing and manufacturing method of an artificial skull prosthesis, which comprises the following steps:
s1, mixing the dried polyether-ether-ketone powder, the nano hydroxyapatite powder and the beta-tricalcium phosphate powder according to the volume ratio of 82:5:4, and putting the mixture into a ball mill for ball milling for 2 hours to obtain mixed powder;
s2, adding a certain amount of silane coupling agent into the mixed powder, and continuing ball milling for 1 hour to obtain a ball-milled mixture;
s3, adding a treatment solution consisting of sodium polyacrylate, hydroxymethyl propyl cellulose, citric acid, glycerol and ethanol into a high-speed ball mill for grinding for 20min to obtain a suspension mixed solution;
s4, adding the suspension mixed liquor and the ball-milled mixture into a constant-temperature magnetic stirrer, and stirring and mixing for 20 minutes at 45 ℃ to obtain printing slurry;
s5, heating the obtained printing slurry to 65 ℃, and then respectively printing the printing slurry into mechanical test piece matrixes (tensile test pieces, compression test pieces, bending test pieces and compression test pieces with semicircular gaps) meeting the national standard GB228-96 by using a 3D printer;
s6, placing the obtained test piece matrixes at the constant temperature of 80 ℃ for 12 minutes, and naturally cooling to room temperature to obtain dumbbell-shaped tensile test pieces, plate-shaped compression test pieces, straight beam-shaped bending test pieces and straight beam-shaped compression-resistant test pieces with the thicknesses of 5 mm.
Wherein the weight ratio of the silane coupling agent to the mixed powder in step S2 is 5: 100.
The mass ratio of the sodium polyacrylate, the hydroxymethyl propyl cellulose, the citric acid, the glycerol and the ethanol in the treatment liquid is 8:5:3.5:1.2: 32.
The mass ratio of the suspension mixed liquor to the ball-milled mixture in the step S4 is 2: 10.
Example 2
The preferred embodiment 2 of the invention provides a 3D printing and manufacturing method of an artificial skull prosthesis, which comprises the following steps:
s1, mixing the dried polyether-ether-ketone powder, the nano hydroxyapatite powder and the beta-tricalcium phosphate powder according to the volume ratio of 83:6:4, and putting the mixture into a ball mill for ball milling for 2 hours to obtain mixed powder;
s2, adding a certain amount of silane coupling agent into the mixed powder, and continuing ball milling for 1 hour to obtain a ball-milled mixture;
s3, adding a treatment solution consisting of sodium polyacrylate, hydroxymethyl propyl cellulose, citric acid, glycerol and ethanol into a high-speed ball mill for grinding for 25min to obtain a suspension mixed solution;
s4, adding the suspension mixed liquor and the ball-milled mixture into a constant-temperature magnetic stirrer, and stirring and mixing for 25 minutes at 45 ℃ to obtain printing slurry;
s5, heating the obtained printing slurry to 60 ℃, and then respectively printing the printing slurry into mechanical test piece matrixes (tensile test pieces, compression test pieces, bending test pieces and compression test pieces with semicircular notches) meeting the national standard GB228-96 by using a 3D printer;
s6, placing the obtained test piece matrixes for 15 minutes at a constant temperature of 85 ℃, and naturally cooling to room temperature to obtain dumbbell-shaped tensile test pieces, plate-shaped compression test pieces, straight beam-shaped bending test pieces and straight beam-shaped compression-resistant test pieces with semicircular gaps, wherein the thicknesses of the dumbbell-shaped tensile test pieces, the plate-shaped compression test pieces, the straight beam-shaped bending test pieces and the straight beam-shaped compression-resistant test pieces are all 5 mm.
Wherein the weight ratio of the silane coupling agent to the mixed powder in step S2 is 5.5: 100.
The mass ratio of the sodium polyacrylate, the hydroxymethyl propyl cellulose, the citric acid, the glycerol and the ethanol in the treatment liquid is 9:6:4:1.5: 33.
The mass ratio of the suspension mixed liquid to the ball-milled mixture in step S4 is 2.3: 10.
Example 3
The preferred embodiment 3 of the invention provides a 3D printing and manufacturing method of an artificial skull prosthesis, which comprises the following steps:
s1, mixing the dried polyether-ether-ketone powder, the nano hydroxyapatite powder and the beta-tricalcium phosphate powder according to the volume ratio of 84:7:4.5, and putting the mixture into a ball mill for ball milling for 2 hours to obtain mixed powder;
s2, adding a certain amount of silane coupling agent into the mixed powder, and continuing ball milling for 1 hour to obtain a ball-milled mixture;
s3, adding a treatment solution consisting of sodium polyacrylate, hydroxymethyl propyl cellulose, citric acid, glycerol and ethanol into a high-speed ball mill for grinding for 25min to obtain a suspension mixed solution;
s4, adding the suspension mixed liquor and the ball-milled mixture into a constant-temperature magnetic stirrer, and stirring and mixing for 25 minutes at 45 ℃ to obtain printing slurry;
s5, heating the obtained printing slurry to 65 ℃, and then respectively printing the printing slurry into mechanical test piece matrixes (tensile test pieces, compression test pieces, bending test pieces and compression test pieces with semicircular gaps) meeting the national standard GB228-96 by using a 3D printer;
s6, placing the obtained test piece matrixes at a constant temperature of 85 ℃ for 12 minutes, and naturally cooling to room temperature to obtain dumbbell-shaped tensile test pieces, plate-shaped compression test pieces, straight beam-shaped bending test pieces and straight beam-shaped compression-resistant test pieces with semicircular gaps, wherein the thicknesses of the dumbbell-shaped tensile test pieces, the plate-shaped compression test pieces, the straight beam-shaped bending test pieces and the straight beam-shaped compression-resistant test pieces are all 5 mm.
Wherein the weight ratio of the silane coupling agent to the mixed powder in step S2 is 5.6: 100.
The mass ratio of the sodium polyacrylate, the hydroxymethyl propyl cellulose, the citric acid, the glycerol and the ethanol in the treatment liquid is 10:6.5:4:1.5: 34.
The mass ratio of the suspension mixed liquid to the ball-milled mixture in step S4 is 2.6: 10.
Example 4
The preferred embodiment 4 of the invention provides a 3D printing and manufacturing method of an artificial skull prosthesis, which comprises the following steps:
s1, mixing the dried polyether-ether-ketone powder, the nano hydroxyapatite powder and the beta-tricalcium phosphate powder according to the volume ratio of 85:8:5, and putting the mixture into a ball mill for ball milling for 2 hours to obtain mixed powder;
s2, adding a certain amount of silane coupling agent into the mixed powder, and continuing ball milling for 1 hour to obtain a ball-milled mixture;
s3, adding a treatment solution consisting of sodium polyacrylate, hydroxymethyl propyl cellulose, citric acid, glycerol and ethanol into a high-speed ball mill for grinding for 30min to prepare a suspension mixed solution;
s4, adding the suspension mixed liquor and the ball-milled mixture into a constant-temperature magnetic stirrer, and stirring and mixing for 30 minutes at 45 ℃ to obtain printing slurry;
s5, heating the obtained printing slurry to 70 ℃, and then respectively printing the printing slurry into mechanical test piece matrixes (tensile test pieces, compression test pieces, bending test pieces and compression test pieces with semicircular notches) meeting the national standard GB228-96 by using a 3D printer;
s6, placing the obtained test piece matrixes for 15 minutes at a constant temperature of 90 ℃, and naturally cooling to room temperature to obtain dumbbell-shaped tensile test pieces, plate-shaped compression test pieces, straight beam-shaped bending test pieces and straight beam-shaped compression-resistant test pieces with semicircular gaps, wherein the thicknesses of the dumbbell-shaped tensile test pieces, the plate-shaped compression test pieces, the straight beam-shaped bending test pieces and the straight beam-shaped compression-resistant test pieces are all 5 mm.
Wherein the weight ratio of the silane coupling agent to the mixed powder in step S2 is 6: 100.
The mass ratio of the sodium polyacrylate, the hydroxymethyl propyl cellulose, the citric acid, the glycerol and the ethanol in the treatment liquid is 12:7.5:5:2: 35.
The mass ratio of the suspension mixed liquid to the ball-milled mixture in the step S4 is 3: 10.
Comparative example 1
Comparative example 1 provides a 3D printing method for manufacturing an artificial skull prosthesis, comprising the steps of:
s1, mixing the dried polyether-ether-ketone powder and the nano-hydroxyapatite powder according to the volume ratio of 84:7, and putting the mixture into a ball mill for ball milling for 2 hours to obtain mixed powder; (in contrast to example 3, the addition of beta-tricalcium phosphate powder was removed)
S2, adding a certain amount of silane coupling agent into the mixed powder, and continuing ball milling for 1 hour to obtain a ball-milled mixture;
s3, adding a treatment solution consisting of sodium polyacrylate, hydroxymethyl propyl cellulose, citric acid, glycerol and ethanol into a high-speed ball mill for grinding for 25min to obtain a suspension mixed solution;
s4, adding the suspension mixed liquor and the ball-milled mixture into a constant-temperature magnetic stirrer, and stirring and mixing for 25 minutes at 45 ℃ to obtain printing slurry;
s5, heating the obtained printing slurry to 65 ℃, and then respectively printing the printing slurry into mechanical test piece matrixes (tensile test pieces, compression test pieces, bending test pieces and compression test pieces with semicircular gaps) meeting the national standard GB228-96 by using a 3D printer;
s6, placing the obtained test piece matrixes at a constant temperature of 85 ℃ for 12 minutes, and naturally cooling to room temperature to obtain dumbbell-shaped tensile test pieces, plate-shaped compression test pieces, straight beam-shaped bending test pieces and straight beam-shaped compression-resistant test pieces with semicircular gaps, wherein the thicknesses of the dumbbell-shaped tensile test pieces, the plate-shaped compression test pieces, the straight beam-shaped bending test pieces and the straight beam-shaped compression-resistant test pieces are all 5 mm.
Wherein the weight ratio of the silane coupling agent to the mixed powder in step S2 is 5.6: 100.
The mass ratio of the sodium polyacrylate, the hydroxymethyl propyl cellulose, the citric acid, the glycerol and the ethanol in the treatment liquid is 10:6.5:4:1.5: 34.
The mass ratio of the suspension mixed liquid to the ball-milled mixture in step S4 is 2.6: 10.
Comparative example 2
The comparative example 2 provides a 3D printing and manufacturing method of the artificial skull prosthesis, which comprises the following steps:
s1, mixing the dried polyether-ether-ketone powder, the nano hydroxyapatite powder and the beta-tricalcium phosphate powder according to the volume ratio of 84:7:4.5, and putting the mixture into a ball mill for ball milling for 2 hours to obtain mixed powder;
s2, adding a certain amount of silane coupling agent into the mixed powder, and continuing ball milling for 1 hour to obtain a ball-milled mixture;
s3, adding a treatment solution consisting of hydroxymethyl propyl cellulose, citric acid, glycerol and ethanol into a high-speed ball mill for grinding for 25min to prepare a suspension mixed solution; (in contrast to example 3, the addition of sodium polyacrylate was removed)
S4, adding the suspension mixed liquor and the ball-milled mixture into a constant-temperature magnetic stirrer, and stirring and mixing for 25 minutes at 45 ℃ to obtain printing slurry;
s5, heating the obtained printing slurry to 65 ℃, and then respectively printing the printing slurry into mechanical test piece matrixes (tensile test pieces, compression test pieces, bending test pieces and compression test pieces with semicircular gaps) meeting the national standard GB228-96 by using a 3D printer;
s6, placing the obtained test piece matrixes at a constant temperature of 85 ℃ for 12 minutes, and naturally cooling to room temperature to obtain dumbbell-shaped tensile test pieces, plate-shaped compression test pieces, straight beam-shaped bending test pieces and straight beam-shaped compression-resistant test pieces with semicircular gaps, wherein the thicknesses of the dumbbell-shaped tensile test pieces, the plate-shaped compression test pieces, the straight beam-shaped bending test pieces and the straight beam-shaped compression-resistant test pieces are all 5 mm.
Wherein the weight ratio of the silane coupling agent to the mixed powder in step S2 is 5.6: 100.
The mass ratio of the hydroxymethyl propyl cellulose to the citric acid to the glycerol to the ethanol in the treatment solution is 6.5:4:1.5: 34.
The mass ratio of the suspension mixed liquid to the ball-milled mixture in step S4 is 2.6: 10.
Comparative example 3
Comparative example 3 provides a 3D printing method for manufacturing an artificial skull prosthesis, comprising the steps of:
s1, mixing the dried polyether-ether-ketone powder, the nano hydroxyapatite powder and the beta-tricalcium phosphate powder according to the volume ratio of 84:7:4.5, and putting the mixture into a ball mill for ball milling for 2 hours to obtain mixed powder;
s2, adding a certain amount of silane coupling agent into the mixed powder, and continuing ball milling for 1 hour to obtain a ball-milled mixture;
s3, adding a treatment solution consisting of sodium polyacrylate, hydroxymethyl propyl cellulose, glycerol and ethanol into a high-speed ball mill for grinding for 25min to prepare a suspension mixed solution; (in contrast to example 3, the addition of citric acid was removed)
S4, adding the suspension mixed liquor and the ball-milled mixture into a constant-temperature magnetic stirrer, and stirring and mixing for 25 minutes at 45 ℃ to obtain printing slurry;
s5, heating the obtained printing slurry to 65 ℃, and then respectively printing the printing slurry into mechanical test piece matrixes (tensile test pieces, compression test pieces, bending test pieces and compression test pieces with semicircular gaps) meeting the national standard GB228-96 by using a 3D printer;
s6, placing the obtained test piece matrixes at a constant temperature of 85 ℃ for 12 minutes, and naturally cooling to room temperature to obtain dumbbell-shaped tensile test pieces, plate-shaped compression test pieces, straight beam-shaped bending test pieces and straight beam-shaped compression-resistant test pieces with semicircular gaps, wherein the thicknesses of the dumbbell-shaped tensile test pieces, the plate-shaped compression test pieces, the straight beam-shaped bending test pieces and the straight beam-shaped compression-resistant test pieces are all 5 mm.
Wherein the weight ratio of the silane coupling agent to the mixed powder in step S2 is 5.6: 100.
The mass ratio of the sodium polyacrylate, the hydroxymethyl propyl cellulose, the glycerol and the ethanol in the treatment liquid is 10:6.5: 1.5: 34.
The mass ratio of the suspension mixed liquid to the ball-milled mixture in step S4 is 2.6: 10.
The test pieces obtained in examples 1 to 4 and comparative examples 1 to 3 were subjected to mechanical comprehensive property measurement using a biomechanical measuring apparatus, and the loading speed during the measurement was 5 mm/min.
The mechanical tensile properties results are shown in table 1 below.
TABLE 1 mechanical tensile Strength Properties of the tensile test pieces
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Human skull | |
| Ultimate strength (Mpa) | 51.73 | 52.56 | 58.79 | 48.31 | 41.34 | 34.67 | 45.12 | 61.36 |
The compression resistance results are shown in table 2 below.
TABLE 2 compressive Strength Properties of the respective compression test pieces
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Human skull | |
| Ultimate strength (Mpa) | 65 | 62 | 71 | 63 | 46 | 31 | 46 | 58 |
The flexural performance results are shown in table 3 below.
TABLE 3 flexural Strength Properties of the respective flexural test pieces
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Human skull | |
| Ultimate bending strength (Mpa) | 27.5 | 29.0 | 32.4 | 25.3 | 17.6 | 13.5 | 18.7 | 21.3 |
The impact toughness performance results are shown in table 4 below.
TABLE 4 Cluster toughness Properties of each of the compression-resistant test pieces
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Human skull | |
| Impact toughness (NM/cm)2） | 1.68 | 1.34 | 2.32 | 1.41 | 1.04 | 0.33 | 0.85 | 0.46 |
The experimental result shows that the tensile strength and the compressive strength of the artificial skull prosthesis manufactured by the invention are both close to the corresponding strength of the human skull, and the bending resistance and the impact toughness of the obtained artificial skull prosthesis are obviously superior to those of the artificial skull, namely, the artificial skull prosthesis with superior mechanical comprehensive performance is obtained by the special 3D printing slurry and the printing method, and the biocompatibility is good. Meanwhile, the comparison example shows that the addition of the beta-tricalcium phosphate powder has obvious influence on the final mechanical strength of the matrix material, and the beta-tricalcium phosphate powder not only plays a role of providing a source of the matrix material for the restoration, but also can play a role of mutual matching and combination (anti-caking, acidity adjustment and stabilizing agent) with polyether-ether-ketone and nano-hydroxyapatite through corresponding treatment liquid. In addition, the special treatment fluid (especially the addition of the sodium polyacrylate and the citric acid) in the invention can play a crucial role in the bonding strength between the matrixes of the raw materials of the final restoration.
The above embodiments are only preferred embodiments of the present invention, and it should be understood that the above embodiments are only for assisting understanding of the method and the core idea of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalents and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. A3D printing and manufacturing method of an artificial skull prosthesis is characterized by comprising the following steps:
s1, drying the polyether-ether-ketone powder, the nano hydroxyapatite powder and the beta-tricalcium phosphate powder according to a volume ratio of 82-85: 5-8: 4-5, and putting the mixture into a ball mill for ball milling for 2 hours to obtain mixed powder;
s2, adding a certain amount of silane coupling agent into the mixed powder, and continuing ball milling for 1 hour to obtain a ball-milled mixture;
s3, adding a treatment solution consisting of sodium polyacrylate, hydroxymethyl propyl cellulose, citric acid, glycerol and ethanol into a high-speed ball mill for grinding to prepare a suspension mixed solution;
s4, adding the suspension mixed liquor and the ball-milling mixture into a constant-temperature magnetic stirrer, and stirring and mixing for 20-30 minutes at 45 ℃ to obtain printing slurry;
s5, heating the obtained printing slurry to 60-70 ℃, and printing by using a 3D printer to obtain a skull repairing matrix;
s6, placing the obtained skull repairing matrix for 10-15 minutes at a constant temperature of 80-90 ℃, and naturally cooling to room temperature to obtain the final artificial skull repairing body.
2. The 3D printing production method of the artificial skull prosthesis according to claim 1, wherein: in the step S2, the weight ratio of the silane coupling agent to the mixed powder is 5-6: 100.
3. The 3D printing production method of the artificial skull prosthesis according to claim 1, wherein: the mass ratio of the sodium polyacrylate, the hydroxymethyl propyl cellulose, the citric acid, the glycerol and the ethanol in the treatment liquid is 8-12: 5-8: 3-5: 1-2: 30-35.
4. The 3D printing production method of the artificial skull prosthesis according to claim 1, wherein: in the step S4, the mass ratio of the suspension mixed liquor to the ball-milled mixture is 2-3: 10.
5. The 3D printing production method of the artificial skull prosthesis according to claim 1, wherein: the grinding time in the step S3 is 20min to 30 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910958514.0A CN110639059B (en) | 2019-10-10 | 2019-10-10 | 3D printing manufacturing method of artificial skull prosthesis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910958514.0A CN110639059B (en) | 2019-10-10 | 2019-10-10 | 3D printing manufacturing method of artificial skull prosthesis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110639059A CN110639059A (en) | 2020-01-03 |
| CN110639059B true CN110639059B (en) | 2020-12-11 |
Family
ID=69012601
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910958514.0A Active CN110639059B (en) | 2019-10-10 | 2019-10-10 | 3D printing manufacturing method of artificial skull prosthesis |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110639059B (en) |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101889128B1 (en) * | 2014-12-24 | 2018-08-17 | 주식회사 바이오알파 | Device for fabricating artificial osseous tissue and method of fabricating the same |
| ES2807873T3 (en) * | 2015-10-09 | 2021-02-24 | Particle3D ApS | Method for 3D printing using a suspension |
| DE102016107223B4 (en) * | 2016-04-19 | 2018-05-24 | Karl Leibinger Medizintechnik Gmbh & Co. Kg | Hybrid implant made of a composite material |
| CN106267363B (en) * | 2016-09-18 | 2019-06-14 | 辽宁聚高智造科技有限公司 | A kind of artifical bone |
| CN106674547A (en) * | 2016-11-28 | 2017-05-17 | 安徽省春谷3D打印智能装备产业技术研究院有限公司 | Spheroidization method of polyether-ether-ketone-hydroxyapatite (Peek-HA) 3D printing powder |
| RO132753B1 (en) * | 2017-02-23 | 2019-05-30 | Institutul Naţional De Cercetare-Dezvoltare Pentru Metale Neferoase Şi Rare - Imnr | Tridimensional structures based on hydroxyapatite and polyurethane-diol, made by 3d-printing technique |
| CN107233628B (en) * | 2017-06-30 | 2020-01-31 | 南宁越洋科技有限公司 | Method for 3D printing personalized artificial tooth by using artificial bone material fused deposition molding |
| CN108273137A (en) * | 2018-01-02 | 2018-07-13 | 山东百多安医疗器械有限公司 | A kind of porous bionical material for repairing skull and personalized production method |
| CN109133908A (en) * | 2018-09-11 | 2019-01-04 | 南通理工学院 | Biology base calcium phosphate 3D printing ceramic slurry and preparation method thereof for DIW technology |
-
2019
- 2019-10-10 CN CN201910958514.0A patent/CN110639059B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN110639059A (en) | 2020-01-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106830899B (en) | Composite ceramic material and preparation method and application thereof | |
| CN104853783B (en) | Form composition, monetite cement, implant and the method for correcting Cranial defect of cement | |
| CN107032775B (en) | Nano-hydroxyapatite and dicalcium silicate composite bioceramic and preparation method and application thereof | |
| CN105536070A (en) | Composite bone cement and preparation method thereof | |
| CN110639059B (en) | 3D printing manufacturing method of artificial skull prosthesis | |
| CN109331223B (en) | Medicine-carrying bioactive glass composite calcium phosphate bone cement and application thereof | |
| CN108553691A (en) | Artificial bone renovating material of Injectable self-curable and preparation method thereof | |
| CN107362389A (en) | A kind of calcium phosphate biological bone cement composite of CNT and graphene enhancing | |
| CN103877611A (en) | 3D printing preparation method of calcium phosphate-based medical bone tissue scaffold | |
| CN1982504A (en) | Production of titanium and titanium-alloy glass ceramic coating | |
| CN112620630A (en) | Preparation method of zinc-magnesium/hydroxyapatite porous composite material | |
| JP5976014B2 (en) | Composition containing injectable self-hardening apatite cement | |
| CN114315338B (en) | Si 3 N 4 /CPP composite ceramic material and preparation method and application thereof | |
| KR20150112349A (en) | biodegradable composites for bone fixation using polylactic acid and calcium phosphate, manufacturing method thereof | |
| CN108358658B (en) | Chitosan modified biological ceramic material and preparation method thereof | |
| Dagang et al. | Physicochemical properties of TTCP/DCPA system cement formed in physiological saline solution and its cytotoxicity | |
| CN104261815B (en) | The preparation method of a kind of fluorine silicon sodium composite mixed HA biological ceramics nano-powder | |
| CN110251722A (en) | Phosphoric acid magnesium-based bone renovating material, feedstock composition and preparation method thereof, application | |
| CN112316208A (en) | Strontium bioglass artificial bone and preparation method thereof | |
| CN109503146B (en) | Hydrothermal preparation method and application of superfine calcium silicophosphate powder | |
| CN104436297B (en) | Dusty material of a kind of manufacture of intraocular bone and preparation method thereof | |
| CN1562873A (en) | Method for preparing bioceramic in complex phase of hydroxyapatite and beta triealcium phosphate | |
| CN106668933A (en) | Multiphase calcium phosphate-based composite scaffold material and preparation method thereof | |
| CN112853143A (en) | Porous titanium copper/hydroxyapatite composite material and preparation method thereof | |
| CN101444640B (en) | Doped bone repairing material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |