CN114099079A - 3D prints individualized alveolar bone defect and rebuilds with degradable magnesium net - Google Patents
3D prints individualized alveolar bone defect and rebuilds with degradable magnesium net Download PDFInfo
- Publication number
- CN114099079A CN114099079A CN202010883019.0A CN202010883019A CN114099079A CN 114099079 A CN114099079 A CN 114099079A CN 202010883019 A CN202010883019 A CN 202010883019A CN 114099079 A CN114099079 A CN 114099079A
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- CN
- China
- Prior art keywords
- magnesium
- mesh
- net
- coating
- alveolar bone
- 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.)
- Pending
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 223
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 212
- 239000011777 magnesium Substances 0.000 title claims abstract description 212
- 210000000988 bone and bone Anatomy 0.000 title claims abstract description 79
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
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- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 3
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- 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 claims description 3
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- 238000001816 cooling Methods 0.000 claims description 2
- 229920006237 degradable polymer Polymers 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 15
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- XAAHAAMILDNBPS-UHFFFAOYSA-L calcium hydrogenphosphate dihydrate Chemical compound O.O.[Ca+2].OP([O-])([O-])=O XAAHAAMILDNBPS-UHFFFAOYSA-L 0.000 description 12
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
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- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 1
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- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- MWKXCSMICWVRGW-UHFFFAOYSA-N calcium;phosphane Chemical compound P.[Ca] MWKXCSMICWVRGW-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
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- 150000002680 magnesium Chemical class 0.000 description 1
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
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- 210000000963 osteoblast Anatomy 0.000 description 1
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Images
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- Materials For Medical Uses (AREA)
Abstract
The invention discloses a 3D printing degradable magnesium mesh for reconstructing personalized alveolar bone defects; the magnesium mesh designs an individualized model structure according to CT data, and realizes high-precision preparation of the magnesium mesh by using a 3D printing technology, so that the magnesium mesh is tightly attached to the anatomical shape of the alveolar bone; overcomes the defects that the traditional titanium mesh needs bending in the operation and has high exposure rate after the operation, reduces the operation difficulty and time, and improves the operation success rate. The surface of the magnesium net is of a complete-opening regular hexagon structure, and the mesh structure has the advantages of self-supporting, easiness in forming, high printing precision, good mechanical property and the like. Meanwhile, the advantages of degradability of magnesium materials and bone induction and promotion of magnesium ions are combined, and the problems that titanium meshes are shielded by stress and cannot be degraded, and the dental implants need to be taken out through a secondary operation are solved. The preparation method has the advantages of simple preparation process, short preparation period, small loss of raw materials, high repeatability and no pollution, and the prepared magnesium mesh has the characteristics of controllable appearance and high precision and can be used as a new generation of large-area bone defect repair bracket for the alveolar bone.
Description
Technical Field
The invention belongs to the technical field of biomedical material preparation, and relates to a degradable magnesium mesh for reconstructing personalized alveolar bone defect by 3D printing; in particular to a degradable magnesium mesh for reconstruction of individualized alveolar bone defect, which is prepared by applying a 3D printing technology and has the advantages of self-support, easy molding, high printing precision, good mechanical property and the like.
Background
For oral clinics, the treatment of large-area jaw defects has been a difficult problem for oral implanters. The insufficiency of the bone mass at the implant implantation site affects the indications of the implant treatment, the quality of the implant, the functional load, the implant aesthetics and the effective survival time of the implant in the oral cavity. Therefore, it is necessary to increase the bone height and bone width of a bone defect portion by means of bone regeneration. Common bone augmentation techniques include autologous bone grafting, distraction osteogenesis and guided bone regeneration, in which Guided Bone Regeneration (GBR) for isolating a bone defect site from soft tissue by a biofilm layer to promote bone growth has a significant effect, and have been widely used in clinical applications. However, since the mechanical strength of the biofilm layer is low, a stable three-dimensional space at the defect site cannot be maintained for a large bone defect, and thus, it is not desirable to simply apply the GBR technique for bone augmentation. At present, the titanium mesh is increasingly accepted to provide stable three-dimensional space at the defect position by utilizing the excellent mechanical property of the titanium mesh, but the traditional forming titanium mesh which is commonly used in clinic has the defects of non-fit with the anatomical form of the alveolar bone, time and labor waste during bending in the operation, high exposure rate of the titanium mesh after the operation and the like.
With the continuous development of the additive manufacturing technology, the personalized titanium mesh prepared by combining the digital modeling technology with the 3D printing additive manufacturing technology becomes the best choice at present. The personalized titanium mesh can be designed in situ according to the defect part of a reconstructed jaw bone model, can be tightly attached to the anatomical shape of alveolar bone, provides sufficient osteogenic space for guiding and controlling the contour shape of regenerated bone, can be applied to horizontal bone defect, vertical bone defect and horizontal-vertical combined bone defect, and is particularly suitable for repairing large-area bone defect. Meanwhile, a surgery scheme can be made in advance by utilizing the personalized titanium net, manual shaping in surgery is omitted, surgery time is greatly shortened, and the method has the characteristics of good appearance, high precision, simplicity, convenience and the like; such as CN108992211A and CN 109662807A.
However, since the titanium mesh cannot be degraded, the titanium mesh needs to be taken out by a secondary operation when the tooth is implanted at the later stage, which increases the pain and economic burden of a patient, and therefore, the material needs to be optimized and improved. The magnesium alloy material is well paid attention to as a new-generation degradable medical metal material, has excellent mechanical property, can provide a stable osteogenesis space for a defect part, can accurately prepare an individualized structure by 3D printing, and can be well attached to the outline and the shape of the defect part. In particular, it has been widely used in the field of bone defects due to its good biocompatibility and mechanical properties as well as its degradable properties. The mechanical property of the magnesium material is similar to that of human bones, so that the stress shielding effect caused by too large difference of the elastic modulus of the implant and the bones can be avoided; due to the degradability of the magnesium alloy, the magnesium alloy can be gradually degraded in vivo until the magnesium alloy finally disappears, so that a secondary operation can be avoided; meanwhile, the magnesium alloy also has excellent biocompatibility, and magnesium ions released during degradation of the magnesium alloy also have the effects of promoting the adhesion and proliferation of osteoblasts and the growth of osteoid, further promoting the regeneration of bone tissues and having an obvious osteogenesis induction effect. Therefore, a new degradable structure for alveolar bone defect can be obtained by combining the 3D printing technology, and the titanium mesh which is commonly used in clinic at present can be optimized.
However, due to the characteristics of flammability and easy oxidation of magnesium alloy, the magnesium alloy has a great safety risk during 3D printing, and meanwhile, the magnesium alloy also has the characteristics of low boiling point and high vapor pressure, so that serious powder splashing can occur in the 3D printing process, and the preparation precision of 3D printing is limited, so that meshes on the surface of the prepared magnesium mesh are often distorted or blocked, and the defects seriously damage the mechanical property of the magnesium mesh and easily cause local corrosion to further influence the degradation property of the magnesium mesh, so that the application of the 3D printed magnesium mesh in alveolar bone defect reconstruction is severely restricted.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a degradable magnesium mesh for 3D printing personalized alveolar bone defect reconstruction.
The purpose of the invention is realized by the following technical scheme:
in a first aspect, the invention relates to a degradable magnesium mesh for reconstruction of an individualized alveolar bone defect, which is prepared by applying a 3D printing technology, wherein the magnesium mesh generates a three-dimensional structure model which completely covers the alveolar bone defect in situ according to an alveolar bone model reconstructed by scanning, and the three-dimensional structure model is tightly attached to the alveolar bone defect; the magnesium net is of a complete open pore structure, the surface of the magnesium net is provided with meshes, and the meshes are uniformly distributed on the whole; the edge of the magnesium net is provided with a plurality of fixing holes, and the magnesium net is fixed at the alveolar bone defect part through the fixing holes on the surface of the magnesium net and the fixing nails.
Preferably, the cross section of the magnesium mesh is U-shaped, and the edges of the magnesium mesh are in smooth transition. The height of the magnesium mesh reaches the enamel cementum boundary height of adjacent teeth or the alveolar ridge top height of the adjacent teeth, and the near-far middle-direction width is 2-3 mm from the boundary of the top of the magnesium mesh to the boundary of the adjacent teeth.
Preferably, the length of the overall size of the magnesium net is 10-100 mm, the height of the magnesium net is 5-15 mm, and the thickness of the magnesium net is 0.1-0.5 mm.
Preferably, the surface meshes are regular hexagons, and the aperture (the diameter of a hexagon circumcircle) is 100-2000 mu m.
In the system, the regular hexagonal meshes have excellent self-supporting effect, and the meshes do not collapse in the printing process; the included angle of each connecting rod of the mesh is an obtuse angle (120 degrees), so that 3D printing forming is facilitated, and mesh blockage cannot occur; the rod-shaped structure is easy to form and small in printing error. Meanwhile, on the premise of the same mesh size and thickness, the regular hexagonal meshes have the best mechanical support performance. By adopting the regular hexagonal meshes, the magnesium mesh for alveolar bone reconstruction which is more suitable for clinical needs can be prepared.
Preferably, both sides of the magnesium net are provided with fixing holes; the fixed orifices are located at the edge of the bottom of the magnesium mesh, at least two fixed orifices are arranged on each side, and the distance between every two adjacent fixed orifices is equal. Preferably, the hole shape of the fixing hole is circular, and the hole diameter is 1-3 mm.
Preferably, the magnesium net and the fixing nail are made of any one of pure magnesium or magnesium alloy; the pure magnesium is: high-purity magnesium with the purity of more than or equal to 99.99 percent; the magnesium alloy is JDBM: 95.2-97.5 wt.% of magnesium, 2-4 wt.% of neodymium, 0.2-0.3 wt.% of zinc and 0.3-0.5 wt.% of zirconium.
The high-purity magnesium has low impurity content, a microstructure is a uniform single-phase structure, the high-purity magnesium has good corrosion resistance, the corrosion rate is lower than that of magnesium alloys (AZ31, WE43 and the like), and the degradation mode is uniform degradation; according to the Mg-Nd-Zn-Zr alloy, a small amount of light rare earth element Nd with slight cytotoxicity (clinically acceptable) is added as a low-alloying element, the addition of Nd can ensure that the magnesium alloy has good aging precipitation strengthening and solid solution strengthening effects, the electrode potential of a magnesium alloy matrix can be greatly improved, and the galvanic corrosion potential difference between the matrix and a second phase is reduced, so that the uniform corrosion resistance of the magnesium alloy is improved, the corrosion rate in simulated body fluid is similar to that of high-purity magnesium and is lower than that of common magnesium alloy materials such as AZ31 and WE43, and meanwhile, the Mg-Nd-Zn-Zr alloy can be uniformly degraded, and the local corrosion phenomenon shown by the alloy can not occur. By adopting the magnesium material, the magnesium net with uniform degradation can be printed to obtain the effect required by clinic.
The surface of the magnesium mesh is also provided with a biocompatible coating; the thickness of the coating is 5-100 mu m.
Preferably, the coating is at least one of a degradable calcium phosphate coating, a degradable high polymer coating and a micro-arc oxidation coating. Specifically, the main component of the degradable calcium-phosphorus coating is brushite or hydroxyapatite; the main component of the degradable high polymer coating is polylactic acid; the main component of the micro-arc oxidation coating is magnesium oxide.
In a second aspect, the invention also relates to a preparation method of the degradable magnesium mesh for reconstructing the personalized alveolar bone defect, which comprises the following steps:
and 4, cooling the magnesium net to room temperature, taking out the magnesium net from the equipment, removing the support, carrying out surface treatment on the magnesium net, and removing the unmelted particles adhered to the surface to obtain the magnesium net.
Preferably, in step 1, the three-dimensional CT scanning mode is Cone Beam CT (CBCT) scanning, and the CBCT scanning uses cone-shaped X-rays and can rotate around the scanning position by one circle. Compared with the traditional CT scanning technology, the method can obtain more comprehensive image information, and meanwhile, the CBCT scanning has the characteristics of small radiation dose and high spatial resolution.
Preferably, in the step 2, the magnesium net is generated in situ in software, so that the magnesium net can be ensured to cover the defect part comprehensively; the fixing hole is specially made according to the implantation position and the magnesium net structure, so that the magnesium net can be tightly attached to the defect position, and the operation difficulty and time are reduced.
Preferably, in the step 3, the magnesium net is placed in an inclined manner of 30-60 degrees during printing, and if the inclined angle is smaller than 30 degrees, the magnesium net is not easy to form; if the inclination angle is more than 60 degrees, the magnesium mesh is not easy to support and raw material waste is generated.
Preferably, the magnesium powder needs to be preheated before being printed, and the preheating temperature is 150 ℃. If the powder bed is not preheated, the powder bed has a large temperature gradient in the printing process due to poor thermal conductivity of the powder bed, and the magnesium material has high thermal cracking tendency, so that the magnesium mesh is easy to generate thermal cracking.
Preferably, the magnesium powder is regular spherical, and the particle size is 20-80 μm; the 3D printing preparation parameters are that laser power is 50-100 w, scanning speed is 300-600 mm/s, scanning line width is 60-100 mu m, scanning layer thickness is 20-50 mu m, and adjacent layers rotate 73 degrees for scanning. If the roundness of the magnesium powder is low, the fluidity of the magnesium powder is poor during powder paving, so that the uniformity of the powder paving cannot be ensured, and the defect is easy to generate in the printing process; meanwhile, if the size of the magnesium powder is less than 20 microns, the preparation cost is increased, the magnesium powder is easy to splash in the printing process, and if the size of the magnesium powder is more than 80 microns, the powder is not easy to melt, and the gaps between adjacent powder are large, and pores are easy to generate after melting. In addition, when the laser power is less than 50w or the scanning speed is more than 600mm/s or the scanning line width is more than 100 μm or the scanning layer thickness is more than 50 μm, the magnesium powder can not be completely melted, so that the increase of unfused defects is caused; when the laser power is more than 100w or the scanning speed is less than 300mm/s or the scanning line width is less than 60 mu m or the scanning layer thickness is less than 20 mu m, the magnesium alloy molten pool is overheated, so that hot cracks are easily formed, and the microstructure is coarse due to the increase of the temperature gradient; when printing, the adjacent layers are scanned in a rotating mode of 73 degrees, so that the accumulation effect formed by stacking multiple layers can be avoided, and the influence of residual stress is reduced.
Preferably, in step 4, the magnesium mesh obtained by 3D printing is further subjected to surface treatment, specifically including shot blasting and chemical polishing. The reason is that the surface treatment can remove the unmelted powder adhered on the surface of the magnesium mesh, obviously improve the flatness of the surface, well realize the structural integrity similar to that of a model, and simultaneously, the smooth surface is beneficial to the subsequent coating.
Preferably, the magnesium net after polishing further comprises the step of coating at least one of a degradable calcium-phosphorus coating, a degradable polymer coating and a micro-arc oxidation coating on the surface. If the surface of the magnesium mesh is not coated with the coating, the magnesium alloy material is degraded at a high speed in a physiological environment and is accompanied with the formation of hydrogen bubbles, and the hydrogen bubbles are accumulated around an implantation part to trigger inflammation.
In the invention, the preparation method for coating the degradable calcium-phosphorus coating is any one of a chemical conversion method and a hydrothermal conversion method;
the chemical conversion method is that the magnesium net is firstly soaked in hydrofluoric acid for 8-24h, and MgF is generated on the surface of a sample through chemical reaction2Coating, wherein the thickness of the obtained coating is 1-2 mu m; then coating MgF2The coated magnesium mesh is placed in supersaturated calcium phosphorus treatment solution, and is kept stand for different times to form a uniform brushite coating on the surface of the sample. The calcium phosphorus treatment solution is Ca (H)2PO4)2·H2O、NaNO3And 30% H2O2Standing the mixed solution for 12-72 hours; the thickness of the obtained coating is 5-20 mu m;
the hydrothermal conversion method is characterized in that the magnesium mesh with the prepared brushite coating is placed in a solution containing calcium ions and hydrogen phosphate ions with certain concentration, the pH value and the reaction temperature of the solution are adjusted, and the brushite coating of a sample can be converted into the hydroxyapatite coating after standing for different time. The pH value of the solution is 7-10, the chemical reaction temperature is 60-100 ℃, the standing time is 6-24 hours, and the thickness of the obtained coating is 5-20 mu m;
the preparation method of the polylactic acid coating for coating the degradable high polymer coating is a pulling method; the pulling method is to dissolve polylactic acid in ethyl acetate to obtain a polylactic acid solution, and then prepare a polylactic acid coating on the surface of the magnesium mesh by using a dip-dip drawing instrument; the thickness of the obtained coating is 5-10 mu m;
the preparation method for coating the micro-arc oxidation coating is that the magnesium net is immersed into electrolyte with silicate or phosphate as a basic component, a current control mode is adopted, the selected current is direct current or alternating current or pulse current, the frequency range is 100-500Hz, after treatment for 5-30min, hole sealing post-treatment is carried out, and the selected hole sealing mode is silicate hole sealing or phosphate hole sealing or sol-gel hole sealing; the thickness of the obtained coating is 5-75 μm.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention determines the model structure of the individualized supporting net for alveolar bone reconstruction according to CT data, can realize size control, simultaneously realize optimal positioning of fixing nails, and realize high-precision preparation of the supporting net by utilizing a 3D printing technology, so that the supporting net can be closely attached to the anatomical shapes of alveolar bones of different patients, thereby providing enough mechanical support for the three-dimensional space of the defect part and protecting the shape of bone fillers; the defects that the traditional titanium mesh needs bending in the operation and has high exposure rate after the operation are overcome, the operation difficulty and time are reduced, and the operation success rate is improved;
(2) the preparation method adopts the 3D printing technology to prepare the magnesium mesh, can directly form the implant with a complex structure, has short preparation period, small loss of raw materials and high repeatability, and has no pollution to the magnesium mesh in the preparation process;
(3) the invention adopts the magnesium net with regular hexagonal meshes, the mesh structure has excellent self-supporting effect, and the collapse of the meshes can not occur in the printing process; the included angle of each connecting rod of the mesh is an obtuse angle (120 degrees), so that 3D printing forming is facilitated, and mesh blockage cannot occur; the rod-shaped structure is easy to form and small in printing error. Meanwhile, on the premise of the same mesh size and thickness, the regular hexagonal meshes have the best mechanical support performance;
(4) the invention fully utilizes the advantages of mechanical property, full degradation and bone induction osteogenesis promotion similar to human bones of the magnesium alloy material, and solves the problems that the traditional alveolar bone titanium mesh material has stress shielding, is not degradable, has small bone increment, needs a secondary operation to take out the titanium mesh when implanting teeth, and the like;
(5) compared with the problems that the conventional common magnesium alloy materials such as AZ31 and WE43 have local corrosion (pitting corrosion) with too high degradation speed and serious corrosion mode, and the early loss of mechanical support effect caused by too high degradation in the early stage is caused, the invention provides high-purity magnesium (the purity is more than or equal to 99.99%) and a magnesium alloy: 95-97.8 wt.% of magnesium, 2-4 wt.% of neodymium, 0.2-0.3 wt.% of zinc and 0.3-0.5 wt.% of zirconium, so that a magnesium net with uniform degradation performance can be printed to obtain an effect required by clinic;
(6) the smooth surface of the polished magnesium mesh is coated with the biocompatible coating, so that the coating can be ensured to uniformly and flatly cover a sample, and the coating can not only effectively regulate and control the corrosion degradation behavior of the magnesium mesh, but also promote the adhesion and proliferation of bone cells, and further promote the bone healing.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a three-dimensional model of a magnesium mesh sample and a corresponding printed physical map: (a) a magnesium net with triangular meshes, (b) a magnesium net with quadrangular meshes, (c) a magnesium net with hexagonal meshes, (d) a magnesium net with circular meshes, (e) a magnesium net with honeycomb circular meshes;
FIG. 2 is a schematic diagram of the overall structure and pore structure of the present invention: (a) the overall structure is schematic, wherein 1 alveolar bone, 2 magnesium meshes, 3 surface meshes, 4 fixing holes and 5 fixing screws are arranged in the alveolar bone; (b) a schematic diagram of a regular hexagonal mesh structure;
FIG. 3 is a schematic diagram of a three-dimensional structure model of a magnesium mesh and a schematic diagram of a real object after polishing of the magnesium mesh; wherein, (a) is a schematic diagram of a three-dimensional structure model of a magnesium net; (b) a physical diagram after the magnesium net is polished;
FIG. 4 is a schematic representation of a magnesium mesh coated with a brushite coating and a microstructure topography; wherein, (a) is a magnesium net object graph coated with a brushite coating; (b) is a microstructure topography of the magnesium mesh coated with the brushite coating.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
In the research and development process, the magnesium alloy is found to have serious powder splashing in the 3D printing process, and the mesh on the surface of the prepared magnesium mesh is often distorted or blocked due to the limitation of the preparation precision of the 3D printing. The defects are further overcome by optimally designing the mesh structure of the magnesium net. Meanwhile, the mechanical strength of the degradable magnesium mesh for alveolar bone defect reconstruction is closely related to the mesh structure, and the mesh structure is also important for preventing the exposure of the magnesium mesh and the growth of soft tissues. The invention finally realizes the preparation of the degradable magnesium mesh for 3D printing personalized alveolar bone defect reconstruction. See in particular the following examples:
example 1 design and preparation of magnesium nets of different mesh structures
Five kinds of supporting nets with different pore structures are designed by using 3-matic12.0 software (Materialise, Belgium), wherein the pore structures are respectively triangular, quadrangular, hexagonal, circular and honeycomb circular, and the maximum value of the pore size is 2 mm. Because the personalized magnesium net has a specific structure and is not easy to measure the mechanical property subsequently, the planar net plate is adopted for equivalent replacement, the length and the width of a standard sample of the planar net plate are respectively designed to be 40mm and 20mm, the thickness is designed to be 0.4mm according to the specification of a national standard GB/T232-2010 metal material bending test method, the standard sample is prepared by using a laser powder bed melting technology, and the used material is Mg-3 wt.% Nd-0.2 wt.% Zn-0.5 wt.% Zr magnesium alloy material.
The three-dimensional model of the flat screen sample and the corresponding printed physical image are shown in fig. 1: (a) a magnesium net with triangular meshes, (b) a magnesium net with quadrangular meshes, (c) a magnesium net with hexagonal meshes, (d) a magnesium net with circular meshes, and (e) a magnesium net with honeycomb circular meshes. As can be seen from the printed object diagram in FIG. 1, the sides of the triangular and quadrilateral magnesium mesh samples are discontinuous, and the sides have a plurality of bulges to partially block the edge meshes, because a plurality of acute angles exist in the triangular and quadrilateral meshes, and the sharp positions of the acute angles cannot be formed due to the limitation of 3D printing precision during preparation. Small holes in round and honeycomb round magnesium net samples are completely blocked by magnesium alloy powder adhered to the surfaces, and part of round meshes have obvious precision deviation and non-connection defects, which shows that printing objects of the two kinds of hole-structure magnesium nets and a design model have large printing errors, because the self-supporting performance of the round meshes is poor, the round holes can collapse during printing, so that the round holes can not be completely formed; meanwhile, due to the limitation of printing precision, the roundness in the design model cannot be completely duplicated, so that the prepared circular hole is distorted into an ellipse. The hexagonal meshes have good forming precision, the phenomenon of discontinuity or blockage of the meshes does not occur, and the repeatability with a design model is very high.
Example 2 mechanical Property test of magnesium nets of different mesh structures
The flat magnesium mesh with different pore structures prepared in the embodiment 1 is subjected to a mechanical bending experiment by using a universal testing machine according to GB/T232-2010 bending standard, and a load is applied to the flat mesh perpendicular to the plane mesh plate at a speed of 1mm/min until a magnesium mesh sample is damaged.
The load (N) and the real-time beam displacement (mm) of the magnesium mesh sample are recorded to obtain a load-displacement curve, the bending strength and the bending rigidity of the magnesium mesh sample are calculated by using a formula, and the data result is shown in Table 1. It can be seen that the hexagonal mesh and the circular mesh have the maximum bending strength and bending rigidity; and the magnesium net with triangular and honeycomb round meshes has the worst bending mechanical property. The printing errors and the mechanical properties of the magnesium nets with different pore structures are comprehensively considered, and the hexagonal mesh structure is the optimal configuration.
TABLE 1
Example 3 design and preparation of pure magnesium mesh with regular hexagonal mesh
The embodiment relates to a degradable magnesium net for alveolar bone defect is rebuild and is used, fig. 2(a) is the overall structure schematic diagram of this embodiment, including alveolar bone 1 and magnesium net 2, there is bone defect position on the surface of alveolar bone 1, magnesium net 2 covers bone defect position completely, evenly distributed's mesh 3 is seted up on magnesium net 2 surface, magnesium net 2 is connected fixedly through fixed orifices 4 and set screw 5 that the bottom was seted up and alveolar bone 1. FIG. 2(b) is a schematic view showing the mesh structure of a magnesium mesh.
The length of the magnesium net is 100mm, the height of the magnesium net is 15mm, the thickness of the magnesium net is 0.5mm, the meshes are regular hexagons, the aperture of the meshes is 1000 micrometers, the fixing holes are circular, the aperture of the fixing holes is 3mm, and the magnesium net and the fixing screws are made of high-purity magnesium (the purity is more than or equal to 99.99%).
The embodiment relates to a preparation method of the degradable magnesium mesh for reconstructing alveolar bone defects, which comprises the following steps:
And 3, importing the magnesium mesh three-dimensional structure model into 3D printing equipment, placing the magnesium mesh model and the substrate at an inclination angle of 45 degrees to generate a rod-shaped support structure, wherein the support structure is in point contact with the magnesium mesh and is convenient to remove. The method comprises the steps of utilizing an EP-M250 metal 3D printer of Beijing Yijia three-dimensional technology Limited company to print layer by layer, wherein powder is medical high-purity magnesium powder with the degradable purity of 99.99%, the shape of the powder is regular sphere, and the particle size of the magnesium powder is 50-80 mu M. Before printing, inert gas filling is carried out on a 3D printer cabin until the oxygen content of the cabin is reduced to be below 100ppm, the 3D printing preparation parameters are laser power 90w, the scanning speed is 500mm/s, the scanning line width is 90 mu m, after scanning of each layer is finished, the thickness of a substrate descending layer is 30 mu m, the manufacturing process of the previous layer is repeated until printing is finished, and the laser scanning direction of the adjacent layer rotates 73 degrees in sequence during preparation for scanning.
Example 4 design and preparation of regular hexagonal mesh magnesium alloy mesh
The embodiment relates to a degradable magnesium mesh for reconstructing the defect of an alveolar bone 1, and the overall structural schematic diagram is shown in fig. 2. The magnesium net 2 and the fixing screws 5 are made of Mg-3 wt.% Nd-0.2 wt.% Zn-0.5 wt.% Zr magnesium alloy materials, the magnesium net 2 is 20mm in length, 10mm in height and 0.3mm in thickness, 3 holes of surface meshes are regular hexagons, the hole diameter is 500 micrometers, 3 fixing holes 4 are formed in the bottom of the outer side of the magnesium net 2, the intervals between the adjacent fixing holes 4 are equal, 2 fixing holes 4 are formed in the bottom of the inner side of the magnesium net 2, and the holes of the fixing holes 4 are circular and 2mm in hole diameter. Fig. 3(a) is a schematic diagram of a three-dimensional structure model of a magnesium mesh, which accurately reflects the structural features described in the present invention, such as hexagonal hole shapes and their distribution features, the number of fixing holes and their arrangement, and so on.
The embodiment relates to a preparation method of the degradable magnesium mesh for reconstructing alveolar bone defects, which comprises the following steps:
And 3, importing the magnesium mesh three-dimensional structure model into 3D printing equipment, placing the magnesium mesh model and the substrate at an inclination angle of 30 degrees to generate a rod-shaped support structure, wherein the support structure is in point contact with the magnesium mesh, and is convenient to remove. The method comprises the steps of utilizing an EP-M250 metal 3D printer of Beijing Yijia three-dimensional science and technology limited company to print layer by layer, wherein powder is medical degradable magnesium alloy Mg-3 wt.% Nd-0.2 wt.% Zn-0.5 wt.% Zr, the powder is regular spherical, and the particle size of magnesium alloy powder is 20-50 mu M. Before printing, inert gas filling is carried out on a 3D printer cabin until the oxygen content of the cabin is reduced to be below 100ppm, the 3D printing preparation parameters are laser power 80w, the scanning speed is 400mm/s, the scanning line width is 80 microns, after scanning of each layer is finished, the thickness of a substrate descending layer is 30 microns, the manufacturing process of the previous layer is repeated until printing is finished, and the laser scanning direction of the adjacent layer rotates 73 degrees in sequence during preparation for scanning.
Fig. 3(b) is a physical diagram of the polished magnesium mesh, and it can be seen from the physical diagram that the surface of the magnesium mesh presents metallic luster, the mesh sizes on the surface are consistent and uniformly distributed, and the phenomena of mesh blockage or collapse and the like do not occur, and the overall structure is consistent with the design model in fig. 3(a), which shows the feasibility of the 3D printing technology for preparing the personalized magnesium mesh structure, and shows that the regular hexagonal mesh is suitable for the forming of the magnesium mesh, and simultaneously, the surface treatment can effectively remove surface adhesion powder, and can realize the high-precision preparation of the magnesium mesh.
Example 5 application of calcium-phosphorus coating to surface of magnesium mesh
Firstly, a magnesium net is prepared according to the method in the embodiment 3 of the invention, the magnesium net is placed in 40% hydrofluoric acid for soaking for 12 hours, and shaking table is used for shaking the hydrofluoric acid, so that a layer of uniform MgF is formed on the surface of a sample2And (4) coating. Then ultrasonic cleaning is respectively carried out for 5min by using deionized water and absolute ethyl alcohol, and drying is carried out. Placing the fluoridated magnesium net in supersaturated calcium-phosphorus treatment solution, wherein the calcium-phosphorus treatment solution is 5g/L Ca (H)2PO4)2·H2O、60g/L NaNO3And 20ml of 30% H2O2Standing for 12h, respectively ultrasonically cleaning for 5min by using deionized water and absolute ethyl alcohol, drying to form a uniform brushite coating on the surface of the sample, and observing the appearance of the coating by using an electron microscope.
FIG. 4(a) is a physical diagram of a magnesium mesh coated with a brushite coating, it can be seen that the brushite coating is uniformly distributed over the surface of the magnesium mesh, the structure of the magnesium mesh is consistent with that of the magnesium mesh in FIG. 3(b) without the surface coating treatment, and the coating is dark gray; fig. 4(b) is an electron micrograph of the brushite coating on the surface of the magnesium mesh, and it can be seen that the microstructure morphology of the coating is petal-shaped, and the coating components are O, Ca and P. The brushite coating can be uniformly formed on the surface of the magnesium alloy, and can completely cover and protect the magnesium alloy matrix.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. A degradable magnesium mesh for reconstruction of individualized alveolar bone defect prepared by applying 3D printing technology is characterized in that the magnesium mesh generates a three-dimensional structure model which completely covers the alveolar bone defect in situ according to an alveolar bone model reconstructed by scanning, and the three-dimensional structure model is tightly attached to the alveolar bone defect; the magnesium net is of a complete open pore structure, the surface of the magnesium net is provided with meshes, and the meshes are uniformly distributed on the whole; the edge of the magnesium net is provided with a plurality of fixing holes, and the magnesium net is fixed at the alveolar bone defect part through the fixing holes on the surface of the magnesium net and the fixing nails.
2. The magnesium mesh of claim 1, wherein said magnesium mesh has a U-shaped cross-sectional shape with rounded edges; the overall size length of the magnesium net is 10-100 mm, the height is 5-15 mm, and the thickness is 0.1-0.5 mm.
3. The magnesium mesh of claim 1, wherein the surface meshes are regular hexagons and have a pore size of 100 to 2000 μm.
4. The magnesium mesh of claim 1, wherein said magnesium mesh has fixing holes on both sides; the fixing holes are positioned at the edge of the bottom of the magnesium mesh, at least two fixing holes are arranged on each side, and the distance between every two adjacent fixing holes is equal; the hole shape of the fixing hole is circular, and the aperture is 1-3 mm.
5. The magnesium mesh of claim 1, wherein the magnesium mesh and the staple material are any of pure magnesium or magnesium alloy material; the pure magnesium is: high-purity magnesium with the purity of more than or equal to 99.99 percent; the magnesium alloy is as follows: 95.2-97.5 wt.% of magnesium, 2-4 wt.% of neodymium, 0.2-0.3 wt.% of zinc and 0.3-0.5 wt.% of zirconium.
6. The magnesium mesh of claims 1-5, wherein the surface of said magnesium mesh further comprises a biocompatible coating; the thickness of the coating is 5-100 mu m; the coating is at least one of a degradable calcium phosphate coating, a degradable high polymer coating and a micro-arc oxidation coating.
7. A method of producing a magnesium mesh according to any one of claims 1 to 6, characterized in that it comprises the steps of:
step 1, carrying out CT scanning on an oral cavity, acquiring tooth and jaw data, and importing the acquired data into software to reconstruct to form an alveolar bone three-dimensional model;
step 2, determining a bone defect part based on the reconstructed alveolar bone three-dimensional model, simulating an implantation site and virtual bone increment in software, and generating a magnesium mesh three-dimensional structure model capable of covering the bone defect part; determining the position and the size of a fixing nail hole based on the generated three-dimensional structure model of the magnesium mesh, and generating a corresponding fixing hole;
step 3, guiding the three-dimensional structure model of the magnesium net into 3D printing equipment, placing the magnesium net in an inclined way of 30-60 degrees, determining a support structure according to the placement position of the magnesium net, and printing layer by layer on a powder bed by using a laser powder bed melting technology to generate an individualized magnesium net;
and 4, cooling the magnesium net to room temperature, taking out the magnesium net from the equipment, removing the support, carrying out surface treatment on the magnesium net, and removing the unmelted particles adhered to the surface to obtain the magnesium net.
8. The preparation method according to claim 7, wherein in the step 3, the magnesium powder is preheated before being printed, and the preheating temperature is 150 ℃; the shape of the magnesium powder is regular spherical, and the particle size is 20-80 mu m; the 3D printing preparation parameters are that the laser power is 50-100 w, the scanning speed is 300-600 mm/s, the scanning line width is 60-100 mu m, the scanning layer thickness is 20-50 mu m, and adjacent layers rotate for 73 degrees for scanning.
9. The preparation method according to claim 7, wherein in the step 4, the magnesium mesh surface treatment comprises shot blasting and chemical polishing, and after the polishing is finished, the magnesium mesh is ultrasonically cleaned in an absolute ethyl alcohol solution for 5-30 min.
10. The method of claim 9, wherein the step of polishing the magnesium mesh further comprises coating at least one of a degradable calcium phosphate coating, a degradable polymer coating and a micro-arc oxidation coating on the surface of the magnesium mesh.
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