CN102784017A - Manufacture process of artificial bone made of composite material - Google Patents
Manufacture process of artificial bone made of composite material Download PDFInfo
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- CN102784017A CN102784017A CN2012102344137A CN201210234413A CN102784017A CN 102784017 A CN102784017 A CN 102784017A CN 2012102344137 A CN2012102344137 A CN 2012102344137A CN 201210234413 A CN201210234413 A CN 201210234413A CN 102784017 A CN102784017 A CN 102784017A
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Abstract
The invention discloses manufacture process of an artificial bone made of a composite material. The technical scheme is that the process includes the following steps: selecting metal wires and processing materials; weaving a metal framework with a space three-dimensional structure; preheating a mold; smelting metal and pouring and infiltrating; post-processing; plastic working and deforming; spray-coating a hydroxyapatite (HAP) coating; simulating body fluid dipping treatment; spray-coating the HAP coating; and storing. The manufacture process has the advantages that deformation tensile strength of the precursor artificial bone is 530-550 Mpa, the toughness is 12.5-13.2 Mpa/m2, and the hardness after heat processing is HB500-550. After HAP is generated in situ, load is larger than 540 Mpa, the toughness is not lower than 10.5Mpa/m2, and wearing resistance rate is 0.002 mg/h.
Description
Technical field
The present invention relates to the organism material technical field, especially relate to a kind of artificial bone's who processes by composite preparation technology.
Background technology
At the organism medical domain, implant into body (or animal body) need have high stretching and compressive strength, high impact resistance, wear resistence, good processing and forming property, high reliability and excellent biological compatibility with the organism medical material of repairing organ and restore funcitons.In clinical orthopaedics, the Metal Substrate biomaterial has become widely used organism load embedded material, such as rustless steel, titanium alloy, Co-Cr alloy, kirsite, magnesium alloy and other rare metals etc.But in these metal materials,, there is not a kind of performance of metal material can satisfy the needs of organism fully owing to reasons such as the rejection property and the compatibilitys.
Wherein, magnesium and magnesium alloy have aboundresources, cheap, density is low, excellent comprehensive performances such as specific strength, specific stiffness height are enjoyed the good reputation of " century green engineering material ", are with a wide range of applications in biomedical materials field.The magnesium alloy biomimetic material has following advantage aspect the organism medical material: 1, especially the proportion of Compact bone is the most approaching for the proportion of magnesium and magnesium alloy and skeleton, is unlikely to increase patient's heavy burden and sense of discomfort behind the implant into body; 2, the Young's modulus of magnesium and magnesium alloy and skeleton are suitable basically, help reducing or eliminating " stress shielding " of implant and human body or other animal body bone interface, and degradation speed is close with bone growth speed, helps promoting the growth and the healing of bone; 3, rejection does not take place in magnesium alloy biologically; 4, magnesium alloy avirulence does not cause modified reaction and unusual metabolism, to organizing nonirritant, and thrombus dissolving, antithrombotic; 5, magnesium has the promotion ossification, is fit to make artificial bone or bone inside-fixture.But also there is the following shortcoming that can't overcome in magnesium alloy as the organism embedded material time: though 1, magnesium alloy is high with specific strength, bulk strength is lower; 2, magnesium alloy is perishable in biological fluid, and persistency is poor; 3, magnesium alloy degradation speed in biological fluid is fast.These drawbacks limit its application and development on the organism substitution material.
Summary of the invention
The objective of the invention is to overcome the shortcoming that exists in the prior art; A kind of artificial bone of double metallic composite material manufacturing and preparation technology of this kind artificial bone of utilizing is provided; The technical scheme that adopts is: a kind of artificial bone's who processes by composite preparation technology, and it is characterized in that: this artificial bone's preparation technology may further comprise the steps:
1, tinsel selection and material processed:
1.1, tinsel selects medical stainless steel steel wire and/or medical titanium alloy silk and/or Co-Cr alloy silk for use;
1.2, tinsel is carried out annealing in process, pickling, ultrasonic waves for cleaning, sterilization and oven dry is handled successively;
2, braiding has the metallic framework of space three-dimensional structure:
2.1, the tinsel after step 1 handled adopts three-dimensional five to be woven into the metallic framework of space three-dimensional structure to knitting skill;
2.2, will weave good metallic framework and carry out ultrasonic waves for cleaning, sterilization and dried;
3, mould and die preheating:
Metallic framework after step 2 disposed is put into the preheating together of column type mould, and makes mould keep vacuum state, and put into the front mold inwall and need stenciling coating, 530 ℃ of preheat temperatures, programming rate is 150 ℃/h, insulation 30min;
4, Metal Melting and cast infiltration:
The negative suction effect of melted magnesium alloy soln using vacuum is poured into through in the metallic framework after step 3 processing, is incubated 30min behind the casting complete, the cooling back demoulding is processed has the enhanced magnesium alloy presoma of metalolic network skeleton artificial bone;
5, post-treatment is handled:
Magnesium alloy presoma artificial bone after step 4 processing is carried out homogenizing annealing, and cut is removed oxide skin then, and then it is carried out ultrasonic waves for cleaning and disinfects;
6, plastic processing deformation:
Artificial bone after step 5 processing is carried out the molded plastic distortion, and in the middle of blocking and terminal, arrange preheating and heat treatment, finally obtain the shape and size of needed artificial bone's presoma blank;
7, spraying HAP coating:
Preparation HAP solution adopts EFI to be coated with mode on the artificial bone's presoma blank surface after step 6 processing and sprays the HAP coating, oven dry, and spraying again, this process is carried out repeatedly, till reaching needed coating layer thickness;
8, simulated body fluid impregnation process:
Artificial bone's presoma blank after step 7 processing is put into the liquid of the simulated body fluid composition of preparation and done impregnation process; Said impregnation process is meant that magnesium is constantly degraded in this processing; The continuous original position of HAP generates; Magnesium is substituted by calcium hydroxy phosphate sclerotin composition, thereby artificial bone's blank that the enhanced generated in-situ HAP of formation metalolic network skeleton is a matrix carries out ultrasonic waves for cleaning, sterilization, dried after dipping finishes;
9, spraying HAP coating:
The HAP solution of preparation doses adopts EFI to be coated with mode on the artificial bone's blank surface after step 8 processing and sprays the HAP coating, oven dry, and spraying again, this process is carried out repeatedly, till reaching needed coating layer thickness;
10, preserve:
Artificial bone's blank after step 9 handled carries out disinfection once more and dries, and obtains the artificial bone and properly preserves, and waits for and transplants requirement.
Technical characterictic of the present invention also has: diameter wiry described in the step 1 is 0.3-0.8mm.
Technical characterictic of the present invention also has: the three-dimensional five described in the step 2 is to braiding, and its braid angle is 28.36o, and the metallic framework volume fraction that is woven into is 5-15%, and through-hole rate is 100%.
Technical characterictic of the present invention also has: coating described in the step 3 is formulated by the water of 40% white titanium pigment, 20% graphite and 40%, and said percentage ratio is weight percentage.
Technical characterictic of the present invention also has: preheating method described in the step 3 is below mould, to place 600 purpose copper mesh, and mold bottom is connected a vacuum tank, and keeping vacuum is 10
-2Pa.
Technical characterictic of the present invention also has: the said magnesium alloy of step 4 is magnesium-zinc alloy (Mg-1%Zn), and said percentage ratio is weight percentage.
Technical characterictic of the present invention also has: step 6 molding die material is Cr12MoV, and preheat temperature is 350 ℃ before the blocking, arranges the T4 Technology for Heating Processing behind the finish-forging.
Technical characterictic of the present invention also has: coating layer thickness described in the step 7 is 0.5 μ m.Its main purpose is the degradation speed of reconciling magnesium matrix through the thickness of control coating; When the speed of self degrading is close with bone growth speed; Magnesium matrix is progressively degraded, and forms the main matter of organism skeleton---and HAP will be with same speed to the artificial bone internal extended, and adheres to and the network skeleton surface; Finally can original position generate the compound skeleton of network structure enhancing HAP, become genuine " bionical " bone.
Technical characterictic of the present invention also has: the liquid formulations of the composition of simulated body fluid described in the step 8 is: NaCl8.00g, KCl 0.40g, CaCl
20.14g, CaHPO
4, H
2O 0.06g, NaHCO
30.35g, NaH
2PO
40.06g, MgSO
4.7H
2O 0.20g, phenol red 0.02g, glucose 1.00g adds water to 1L, uses CaCO
3Regulate pH value to 7.2-7.4.
Technical characterictic of the present invention also has: the said HAP coating layer thickness of step 9 is 0.3-1.5 μ m.
Beneficial effect of the present invention is: 1) the present invention utilizes magnesium alloy degradable advantage in human body; Eliminate the fast shortcoming of its degradation speed; Through control magnesium alloy degradation speed; Realize that the HAP original position generates and the magnesium alloy degraded is carried out synchronously, finally obtain a kind of composite artificial bone who utilizes the enhanced calcium hydroxy phosphate base of tinsel network structure of composite material precursor preparation.Thereby overcome the deficiency of medical magnesium alloy aspect intensity, degradation speed in the prior art; Artificial bone prosthese after the machine-shaping has good toughness and fatigue resistance; The anti-wear performance of prosthese significantly improves, thereby becomes good organism medical surgical implant.
2) because this strength of materials is high, and elastic modelling quantity and density are close with the compact substance skeleton, good impact resistance, avirulence does not cause allergy and unusual metabolism, and to organizing nonirritant, antithrombotic; The magnesium base composite material of network structure enhancing simultaneously presoma has been realized magnesium steel mesh network IPN, intersects each other, runs through each other; Interpenetrate; Each other tangle and coiling, as real skeleton, have the intensity height, advantages such as density is low, wear rate is low, technology is reasonable, moderate cost.
3) the present invention is through spraying calcium hydroxy phosphate (HAP) coating on the surface of the artificial bone behind reaction in-situ; Slow down effectively or intercepted the infiltration of heavy metal to body fluid or blood; Reduced rejection and unusual metabolism, reduced the zest of tissue and the formation of thrombosis.
4) through test, this kind presoma artificial bone's distortion tensile strength 530-550Mpa, toughness 12.5-13.2Mpa/m
2, hardness HB500-550 behind the heat treatment; After original position generated HAP, load was greater than 540Mpa, and toughness is not less than 10.5Mpa/m
2, wear-resistant loss rate reaches 0.002mg/h.
Description of drawings
Accompanying drawing 1 is the artificial thigh bone sketch map that adopts this technology to process.
The specific embodiment
Below in conjunction with the specific embodiment, the present invention will be described.
Embodiment one: a kind of artificial bone's who processes by composite preparation technology, and this kind artificial bone is a hip, this artificial bone's preparation technology may further comprise the steps:
1, tinsel selection and material processed:
1.1, tinsel selects medical stainless steel steel wire and/or medical titanium alloy silk and/or Co-Cr alloy silk for use, diameter wiry is 0.3-0.8mm;
1.2, tinsel is carried out annealing in process, pickling, ultrasonic waves for cleaning, sterilization and oven dry is handled successively;
2, braiding has the metallic framework of space three-dimensional structure:
2.1, the tinsel after step 1 handled adopts three-dimensional five to be woven into the metallic framework of space three-dimensional structure to knitting skill, three-dimensional five in braiding braid angle be 28.36o, the metallic framework volume fraction that is woven into is 5-15%, through-hole rate is 100%;
2.2, will weave good metallic framework and carry out ultrasonic waves for cleaning, sterilization and dried;
3, mould and die preheating:
Metallic framework after step 2 disposed is put into the preheating together of column type mould, and makes mould keep vacuum state, puts into the front mold inwall and needs stenciling coating; 530 ℃ of preheat temperatures, programming rate are 150 ℃/h, insulation 30min; Coating is formulated by the water of 40% white titanium pigment, 20% graphite and 40%, and percentage ratio is weight percentage, and preheating method is below the column type mould, to place 600 purpose copper mesh; And with vacuum tank of mold bottom connection, keeping vacuum is 10
-2Pa;
4, Metal Melting and cast infiltration:
The negative suction effect of melted magnesium alloy soln using vacuum is poured into through in the metallic framework after step 3 processing; Be incubated 30min behind the casting complete; The cooling back demoulding is processed has the enhanced magnesium alloy presoma of metalolic network skeleton artificial bone; Magnesium alloy is magnesium-zinc alloy (Mg-1%Zn), and this percentage ratio is weight percentage;
5, post-treatment is handled:
Magnesium alloy presoma artificial bone after step 4 processing is carried out homogenizing annealing, and cut is removed oxide skin then, and then it is carried out ultrasonic waves for cleaning and disinfects;
6, plastic processing deformation:
Artificial bone after step 5 processing is carried out the molded plastic distortion; And at middle preheating and the heat treatment arranged of blocking and terminal; The final shape and size that obtain needed artificial bone's presoma blank; The molding die material is Cr12MoV, and preheat temperature is 350 ℃ before the blocking, arranges the T4 Technology for Heating Processing behind the finish-forging;
7, spraying HAP coating:
Preparation HAP solution adopts EFI to be coated with mode on the artificial bone's presoma blank surface after step 6 processing and sprays the HAP coating, oven dry; Spraying again, this process is carried out repeatedly, till reaching needed coating layer thickness; Coating layer thickness is typically chosen in 0.5 μ m; Its main purpose is the degradation speed of reconciling magnesium matrix through the thickness of control coating, and when the speed of self degrading was close with bone growth speed, magnesium matrix was progressively degraded; And form the organism skeleton main matter---HAP will be with same speed to the artificial bone internal extended; And adhere to and the network skeleton surface, finally understand original position and generate the compound skeleton of network structure enhancing HAP, become genuine " bionical " bone;
8, simulated body fluid impregnation process:
Artificial bone's presoma blank after step 7 processing is put into the liquid of the simulated body fluid composition of preparation and done impregnation process; Said impregnation process is meant that magnesium is constantly degraded in this processing; The continuous original position of HAP generates, and magnesium is substituted by calcium hydroxy phosphate sclerotin composition, thus artificial bone's blank that the enhanced generated in-situ HAP of formation metalolic network skeleton is a matrix; After finishing, dipping carries out ultrasonic waves for cleaning, sterilization, dried; The liquid formulations of simulated body fluid composition is: NaCl8.00g, KCl 0.40g, CaCl
20.14g, CaHPO
4, H
2O 0.06g, NaHCO
30.35g, NaH
2PO
40.06g, MgSO
4.7H
2O 0.20g, phenol red 0.02g, glucose 1.00g adds water to 1L, uses CaCO
3Regulate pH value to 7.2-7.4;
9, spraying HAP coating:
The HAP solution of preparation doses adopts EFI to be coated with mode on the artificial bone's blank surface after step 8 processing and sprays the HAP coating, oven dry; Spraying again; This process is carried out repeatedly, and till reaching needed coating layer thickness, the HAP coating layer thickness is 0.3-1.5 μ m; The application scope is all sprayings on the artificial thigh bone blank surface that generates in position; The HAP coating layer thickness is 0.3-1.5 μ m, its objective is isolated or slows down the infiltration of heavy metal to human body, eliminates modified reaction and unusual metabolism;
10, preserve:
Artificial bone's blank after step 9 handled carries out disinfection once more and dries, and obtains the artificial bone and properly preserves, and waits for and transplants requirement.
Embodiment two: be with embodiment one difference: adopt rolling deformation in the step 6, operating temperature is 250-350 ℃, and pressure is 150-250MPa, strain rate 0.1-0.5s
-1, the 2-5 passage.
Embodiment three: be with embodiment one difference: magnesium alloy is AZ31B; Adopt rolling deformation in the step 6, operating temperature is 250-350 ℃, and pressure is 150-250MPa, strain rate 0.1-0.5s
-1, the 2-5 passage.
Embodiment four: be with embodiment one difference: magnesium alloy is AM60B; Adopt crimp in the step 6, operating temperature is 250-350 ℃, and pressure is 150-270MPa, extrusion ratio 10-32.
Among above-mentioned four embodiment corresponding extruding or rolling after the composite diphase material performance parameter see following table for details.
Certainly, above-mentioned explanation is not a limitation of the present invention, and the present invention also is not limited only to above-mentioned giving an example, and variation, remodeling, interpolation or replacement that those skilled in the art are made in essential scope of the present invention also belong to protection scope of the present invention.
Claims (10)
1. an artificial bone who processes by composite preparation technology, it is characterized in that: this artificial bone's preparation technology may further comprise the steps:
1, tinsel selection and material processed:
1.1, tinsel selects medical stainless steel steel wire and/or medical titanium alloy silk and/or Co-Cr alloy silk for use;
1.2, tinsel is carried out annealing in process, pickling, ultrasonic waves for cleaning, sterilization and oven dry is handled successively;
2, braiding has the metallic framework of space three-dimensional structure:
2.1, the tinsel after step 1 handled adopts three-dimensional five to be woven into the metallic framework of space three-dimensional structure to knitting skill;
2.2, will weave good metallic framework and carry out ultrasonic waves for cleaning, sterilization and dried;
3, mould and die preheating:
Metallic framework after step 2 disposed is put into the preheating together of column type mould, and makes mould keep vacuum state, and put into the front mold inwall and need stenciling coating, 530 ℃ of preheat temperatures, programming rate is 150 ℃/h, insulation 30min;
4, Metal Melting and cast infiltration:
The negative suction effect of melted magnesium alloy soln using vacuum is poured into through in the metallic framework after step 3 processing, is incubated 30min behind the casting complete, the cooling back demoulding is processed has the enhanced magnesium alloy presoma of metalolic network skeleton artificial bone;
5, post-treatment is handled:
Magnesium alloy presoma artificial bone after step 4 processing is carried out homogenizing annealing, and cut is removed oxide skin then, and then it is carried out ultrasonic waves for cleaning and disinfects;
6, plastic processing deformation:
Artificial bone after step 5 processing is carried out the molded plastic distortion, and in the middle of blocking and terminal, arrange preheating and heat treatment, finally obtain the shape and size of needed artificial bone's presoma blank;
7, spraying HAP coating:
Preparation HAP solution adopts EFI to be coated with mode on the artificial bone's presoma blank surface after step 6 processing and sprays the HAP coating, oven dry, and spraying again, this process is carried out repeatedly, till reaching needed coating layer thickness;
8, simulated body fluid impregnation process:
Artificial bone's presoma blank after step 7 processing is put into the liquid of the simulated body fluid composition of preparation and done impregnation process; Said impregnation process is meant that magnesium is constantly degraded in this processing; The continuous original position of HAP generates; Magnesium is substituted by calcium hydroxy phosphate sclerotin composition, thereby artificial bone's blank that the enhanced generated in-situ HAP of formation metalolic network skeleton is a matrix carries out ultrasonic waves for cleaning, sterilization, dried after dipping finishes;
9, spraying HAP coating:
The HAP solution of preparation doses adopts EFI to be coated with mode on the artificial bone's blank surface after step 8 processing and sprays the HAP coating, oven dry, and spraying again, this process is carried out repeatedly, till reaching needed coating layer thickness;
10, preserve:
Artificial bone's blank after step 9 handled carries out disinfection once more and dries, and obtains the artificial bone and properly preserves, and waits for and transplants requirement.
2. according to the described artificial bone's who processes by composite of claim 1 preparation technology, it is characterized in that:
Diameter wiry described in the step 1 is 0.3-0.8mm.
3. according to the described artificial bone's who processes by composite of claim 1 preparation technology, it is characterized in that:
Three-dimensional five described in the step 2 is to braiding, and its braid angle is 28.36o, and the metallic framework volume fraction that is woven into is 5-15%, and through-hole rate is 100%.
4. according to the described artificial bone's who is processed by composite of claim 1 preparation technology, it is characterized in that: coating described in the step 3 is formulated by the water of 40% white titanium pigment, 20% graphite and 40%, and said percentage ratio is weight percentage.
5. according to the described artificial bone's who is processed by composite of claim 1 preparation technology, it is characterized in that: preheating method described in the step 3 is below mould, to place 600 purpose copper mesh, and mold bottom is connected a vacuum tank, and keeping vacuum is 10
-2Pa.
6. according to the described artificial bone's who is processed by composite of claim 1 preparation technology, it is characterized in that: the said magnesium alloy of step 4 is magnesium-zinc alloy (Mg-1%Zn), and said percentage ratio is weight percentage.
7. according to the described artificial bone's who is processed by composite of claim 1 preparation technology, it is characterized in that: step 6 molding die material is Cr12MoV, and preheat temperature is 350 ℃ before the blocking, arranges the T4 Technology for Heating Processing behind the finish-forging.
8. according to the described artificial bone's who is processed by composite of claim 1 preparation technology, it is characterized in that: coating layer thickness described in the step 7 is 0.5 μ m.
9. according to the described artificial bone's who is processed by composite of claim 1 preparation technology, it is characterized in that: the liquid formulations of the composition of simulated body fluid described in the step 8 is: NaCl8.00g, KCl 0.40g, CaCl
20.14g, CaHPO
4, H
2O 0.06g, NaHCO
30.35g, NaH
2PO
40.06g, MgSO
4.7H
2O 0.20g, phenol red 0.02g, glucose 1.00g adds water to 1L, uses CaCO
3Regulate pH value to 7.2-7.4.
10. according to the described artificial bone's who is processed by composite of claim 1 preparation technology, it is characterized in that: the said HAP coating layer thickness of step 9 is 0.3-1.5 μ m.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103120604A (en) * | 2012-12-14 | 2013-05-29 | 山东省文登市整骨科技开发有限公司 | Implant artificial hip joint stem |
| CN104096267A (en) * | 2014-07-09 | 2014-10-15 | 上海交通大学 | Medical gradient composite material |
| CN109022843A (en) * | 2018-08-01 | 2018-12-18 | 郑州大学第附属医院 | Medical embedded degradable composite bar of one kind and preparation method thereof |
| WO2019037659A1 (en) * | 2017-08-23 | 2019-02-28 | 湖南碳康生物科技有限公司 | Integrated carbon fiber composite artificial bone and preparation method thereof |
| CN111842851A (en) * | 2020-07-31 | 2020-10-30 | 湖南华耀百奥医疗科技有限公司 | Preparation method and application of medical degradable zinc-based composite board |
| CN114042898A (en) * | 2021-11-10 | 2022-02-15 | 温州医科大学附属口腔医院 | Preparation method of biomedical degradable metal skeleton reinforced Zn-based composite material with large-area galvanic corrosion structure |
Families Citing this family (1)
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| CN105239009A (en) * | 2015-09-06 | 2016-01-13 | 苏州市宝玛数控设备有限公司 | Cutting bridge of cutting machine |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103120604A (en) * | 2012-12-14 | 2013-05-29 | 山东省文登市整骨科技开发有限公司 | Implant artificial hip joint stem |
| CN104096267A (en) * | 2014-07-09 | 2014-10-15 | 上海交通大学 | Medical gradient composite material |
| WO2019037659A1 (en) * | 2017-08-23 | 2019-02-28 | 湖南碳康生物科技有限公司 | Integrated carbon fiber composite artificial bone and preparation method thereof |
| CN109022843A (en) * | 2018-08-01 | 2018-12-18 | 郑州大学第附属医院 | Medical embedded degradable composite bar of one kind and preparation method thereof |
| CN111842851A (en) * | 2020-07-31 | 2020-10-30 | 湖南华耀百奥医疗科技有限公司 | Preparation method and application of medical degradable zinc-based composite board |
| CN111842851B (en) * | 2020-07-31 | 2021-11-09 | 湖南华耀百奥医疗科技有限公司 | Preparation method and application of medical degradable zinc-based composite board |
| CN114042898A (en) * | 2021-11-10 | 2022-02-15 | 温州医科大学附属口腔医院 | Preparation method of biomedical degradable metal skeleton reinforced Zn-based composite material with large-area galvanic corrosion structure |
| CN114042898B (en) * | 2021-11-10 | 2023-02-28 | 温州医科大学附属口腔医院 | Preparation method of biomedical degradable metal skeleton reinforced Zn-based composite material with large-area galvanic corrosion structure |
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|---|---|
| CN102784017B (en) | 2014-10-22 |
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