CN110394447A - The preparation method of porous magnesium-rare earth alloy implantation material based on selective laser fusing (SLM) increases material manufacturing technology - Google Patents

The preparation method of porous magnesium-rare earth alloy implantation material based on selective laser fusing (SLM) increases material manufacturing technology Download PDF

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CN110394447A
CN110394447A CN201910790994.4A CN201910790994A CN110394447A CN 110394447 A CN110394447 A CN 110394447A CN 201910790994 A CN201910790994 A CN 201910790994A CN 110394447 A CN110394447 A CN 110394447A
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rare earth
earth alloy
magnesium
porous
porous magnesium
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CN110394447B (en
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王南清
付彭怀
廖海光
陈娟
彭立明
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Shanghai Jiaotong University
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    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/11—Making porous workpieces or articles
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    • 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
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    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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Abstract

The present invention provides a kind of preparation method of porous magnesium-rare earth alloy implantation material based on selective laser fusing (SLM) increases material manufacturing technology, the component for including the following steps: step 1, selecting magnesium-rare earth alloy powder；Step 2 preheats magnesium-rare earth alloy powder；Step 3, to basal plate preheating；Step 4, the threedimensional model for drawing porous magnesium-rare earth alloy implantation material；Porous magnesium-rare earth alloy implantation material entity is saved with STL format into output format file and is transmitted in delamination software by step 5, and addition bottom surface supports and carries out slicing treatment；Step 6 prints porous magnesium-rare earth alloy implantation material entity；Step 7 separates porous magnesium-rare earth alloy implantation material molded part with substrate cut；Step 8 carries out electrochemical polishing treatment.Porous implant prepared by the present invention, pore wall thickness uniformly, flawless defect, integral strength and modulus are higher；Porous implant prepared by the present invention is more matched with the intensity and modulus of skeleton.

Description

Porous magnesium-rare earth alloy based on selective laser fusing (SLM) increases material manufacturing technology is planted Enter the preparation method of object
Technical field
The invention belongs to technical field of metal material preparation, are related to a kind of based on selective laser fusing (SLM) increasing material manufacturing The preparation method of the porous magnesium-rare earth alloy implantation material of technology, and in particular to melted to by magnesium-rare earth alloy powder by selective laser Change (SLM) increases material manufacturing technology and be prepared into porous implant, such implantation material is mainly used for the reparation after human body bone injury.
Background technique
In bio-medical metal implant material, magnesium and its alloy are by good mechanical property, biocompatibility and can Degradation characteristic causes worldwide concern and research, becomes implant for into bones of new generation, intravascular stent, gear division and whole The ideal material of shape implant is known as " revolutionary metallic biomaterial ".Porous magnesium-based implantation material with three-dimensional connection, Not only it can play the role of tissue filling in implant site, while its pore structure can also promote the length of blood vessel and surrounding tissue Enter, implantation material is made to be not susceptible to loosen and fall off.Porous structure has body fluid Transport Characteristics, allows implantation material to implant site Gradually be absorbed by the body degradation during reparation or shaping, reaches Bone Defect Repari and implantation material ira situ degradation effect.In addition, logical Crossing pore character can control mechanical strength, elasticity modulus and the degradation rate of adjustment implantation material, make itself and autologous tissue's performance And it repairs rate and matches.
Currently, most researchers prepare porous magnesium and magnesium alloy by the way of powder sintered.During the preparation process, it is Raising porosity and connectivity, are often added pore creating material, such as NH in metal powder4HCO3、CO(NH2)2, NaCl, methyl Cellulose etc..Since pore creating material granule-morphology itself is different, size is unevenly distributed, in sintering process between metal powder not Effective fusion contact point can be all established, the pass uniformity and hole connectivity of this method preparation are poor.Meanwhile in pore-creating During agent removes, it may occur that pore creating material residual.Remaining pore creating material can generate corrosion to magnesium alloy substrate.Therefore, at present There are distinct disadvantages for powder sintered preparation porous magnesium and magnesium alloy.
CN201510395799.3 discloses the preparation method of another porous mg-based material: first pass through titanium particle or Iron particle prepares POROUS TITANIUM or porous iron precast body, and magnesium alloy melt is then filled porous preform in a manner of Pressure-seepage Flow In, pickling finally is carried out with hydrofluoric acid solution, titanium or Tie Tong are crossed into chemical attack removal, obtain porous magnesium alloy.This method Although the more ingenious porous structure for obtaining three-dimensional connection, since the entity part of magnesium alloy porous structure passes through titanium particle Or the gap molding of iron particle, cause porous structure wall thickness variation larger, the integral strength and modulus of porous structure are lower than people Body bone, it is poor with skeleton matching.
Therefore, it is necessary to a kind of preparation method of new porous magnesium alloy implantation material, can obtain with skeleton intensity and Modulus is more close, the porous magnesium-rare earth alloy more adaptable based on selective laser fusing (SLM) increases material manufacturing technology is planted Enter the preparation method of object.
Summary of the invention
For the defects in the prior art, the object of the present invention is to provide one kind increases material based on selective laser fusing (SLM) The preparation method of the porous magnesium-rare earth alloy implantation material of manufacturing technology.
The one kind provided according to the present invention is based on the porous magnesium-rare earth alloy of selective laser fusing (SLM) increases material manufacturing technology The preparation method of implantation material, includes the following steps:
Step 1, the component for selecting magnesium-rare earth alloy powder；
Step 2 preheats magnesium-rare earth alloy powder in a vacuum drying oven, and preheating time range is 0.5-1.5h, Preheating temperature range is 80-120 DEG C；
Step 3 selects magnesium-rare earth alloy identical with the magnesium-rare earth alloy powdery components in step 1 as substrate, to institute Substrate is stated to be preheated；Preheating temperature >=160 DEG C that the substrate is preheated in the step 3；
Step 4, the threedimensional model for drawing porous magnesium-rare earth alloy implantation material by Three-dimensional Design Software on computers, it is raw At porous magnesium-rare earth alloy implantation material entity；
Porous magnesium-rare earth alloy implantation material entity is saved into output format file and is transmitted to point with STL format by step 5 In layer software, addition bottom surface supports and imported into selective laser fusing increasing material manufacturing equipment after carrying out slicing treatment；
Step 6 opens selective laser fusing increasing material manufacturing equipment, and print parameters are arranged, are implanted into porous magnesium-rare earth alloy Object entity is printed；
The step 6 further includes that technique is adjusted using spot diameter, and the spot diameter size is selected according to formula P/DV=C It takes, wherein C is power density, and the range of C is 1.1-2.25W/mm2, D is spot diameter, and the unit of D is mm, and P is laser function Rate, the unit of P are W, and V is laser inswept distance per second, and the unit of V is mm；
The step 6 further includes using powdering compensation technique, the compensation rate of the magnesium-rare earth alloy powder of the powdering compensation It is 10-20 μm；
The step 6 further includes adjusting the air-flow size magnesium powder that ensures that air-flow will volatilize to take away substrate；
Step 7 carries out wire cutting along substrate end-face, by porous magnesium-rare earth alloy implantation material molded part and substrate cut point From porous magnesium-rare earth alloy implantation material is made；
Porous magnesium-rare earth alloy implantation material obtained in step 7 is carried out electrochemical polishing treatment by step 8.
Further, the print parameters in the step 6 are as follows: laser power range is 80-160W, and sweep speed range is 300-1500mm/s, it is 50-120 μm that laser, which fills spacing range, and powdering Layer thickness is 30-50 μm.
Further, the angle of laser scanning direction is 67 ° between two neighboring powdering layer in the step 6.
Further, the angle of laser scanning direction is 73 ° between two neighboring powdering layer in the step 6.
Further, the angle of laser scanning direction is 90 ° between two neighboring powdering layer in the step 6.
Further, the magnesium-rare earth alloy powder be Mg-2.5~3.6Nd-0.01~0.4Zn-Zr or Mg-8.0~ 14.0Gd-0.01~0.85Zn-Zr (wt.%).
Further, the magnesium-rare earth alloy powder is spherical powder, and the particle size range of the spherical powder is 21-74 μ m。
Further, porous magnesium rare earth is closed as polishing etch solution using perchloric acid alcoholic solution in the step 8 Golden implantation material carries out electrochemical polishing treatment, and the volume ratio range of perchloric acid and alcohol is in the perchloric acid alcoholic solution 0.05-0.2。
Further, magnetic agitation being carried out to the perchloric acid alcoholic solution, the range of speeds of magnetic agitation is 500~ 1000rpm, < -10 DEG C of solution temperature of the perchloric acid alcoholic solution.
Further, in the step 8 electrochemical polishing treatment parameter are as follows: polishing voltage range be 15-20V, polishing Current range is 1.5-2.5A, and polishing time range is 5-20min.
Further, pass through the matter of the porous magnesium-rare earth alloy implantation material of monitoring in the step 8 when electrochemical polishing treatment Amount guarantees the batch consistency of porous magnesium-rare earth alloy implantation material electrochemical polish.
Compared with prior art, the present invention have it is following the utility model has the advantages that
(1) the porous magnesium-rare earth alloy implantation material of the invention based on selective laser fusing (SLM) increases material manufacturing technology Preparation method, the implantation material that provides increases material preparation method, and by selective laser smelting technology can be successfully prepared pore wall thickness equal Even, flawless defect degradable magnesium rare earth alloy porous implant, the integral strength and modulus of implantation material are higher；With existing skill Art is compared, and porous implant prepared by the present invention is more matched with the intensity and modulus of skeleton.
(2) the porous magnesium-rare earth alloy implantation material of the invention based on selective laser fusing (SLM) increases material manufacturing technology Preparation method, implantation material electrochemical polishing method simple process, the consistency provided is good, and the polishing of implantation material can be effectively controlled Amount improves the repeatability of implantation material polishing.
(3) the porous magnesium-rare earth alloy implantation material of the invention based on selective laser fusing (SLM) increases material manufacturing technology Preparation method, the implantation material provided, which increases material preparation method, may be implemented the magnesium-rare earth alloy porous implant of any aperture and shape Quick manufacture, realize functional and structural strength perfect combination.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention, Objects and advantages will become more apparent upon:
Fig. 1 is the porous implant that increasing material manufacturing is melted in selective laser (before polishing)；
Fig. 2 is the porous implant that increasing material manufacturing is melted in selective laser (after polishing).
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field For personnel, without departing from the inventive concept of the premise, several changes and improvements can also be made.These belong to the present invention Protection scope.
Embodiment 1
Please refer to Fig. 1-2.As shown in Figs. 1-2, the embodiment of the invention provides one kind is increased based on selective laser fusing (SLM) The preparation method of the porous magnesium-rare earth alloy implantation material of material manufacturing technology, includes the following steps:
Step 1, the component for selecting magnesium-rare earth alloy powder；
Step 2 preheats magnesium-rare earth alloy powder, preheating time 1.5h, preheating temperature in a vacuum drying oven It is 100 DEG C；
Step 3 selects magnesium-rare earth alloy identical with the magnesium-rare earth alloy powdery components in step 1 as substrate, to institute Substrate is stated to be preheated；
Step 4, the threedimensional model for drawing porous magnesium-rare earth alloy implantation material by Three-dimensional Design Software on computers, it is raw At porous magnesium-rare earth alloy implantation material entity, wherein porous aperture is 500 μm, and porous wall thickness is 300 μm；
Porous magnesium-rare earth alloy implantation material entity is saved into output format file and is transmitted to point with STL format by step 5 In layer software, the addition bottom surface 1mm supports and imported into selective laser fusing increasing material manufacturing equipment after carrying out slicing treatment；
Step 6 opens selective laser fusing increasing material manufacturing equipment, and print parameters are arranged, are implanted into porous magnesium-rare earth alloy Object entity is printed, and porous magnesium-rare earth alloy implantation material is made；
Step 7 carries out wire cutting along substrate end-face, by porous magnesium-rare earth alloy implantation material molded part and substrate cut point From porous magnesium-rare earth alloy implantation material is made；
Porous magnesium-rare earth alloy implantation material obtained in step 7 is carried out electrochemical polishing treatment by step 8.
Print parameters in the step 6 are as follows: laser power 80W, sweep speed 450mm/s, laser fill spacing It is 90 μm, powdering thickness is 30 μm, and the angle of laser scanning direction is 73 ° between two neighboring powdering layer.
The magnesium-rare earth alloy powder is Mg-3Nd-0.2Zn-Zr (wt.%).
The magnesium-rare earth alloy powder is spherical powder, and the average grain diameter of the spherical powder is 45 μm.
The preheating temperature preheated in the step 3 to the substrate is 160 DEG C.
The step 6 further includes that technique is adjusted using spot diameter, and the spot diameter size is selected according to formula P/DV=C It takes, wherein C is power density, and the range of C is 1.1-2.25W/mm2, D is spot diameter, and the unit of D is mm, and P is laser function Rate, the unit of P are W, and V is laser inswept distance per second, and the unit of V is mm.
Specifically, C=1.62W/mm is taken2, the spot diameter of selection is 110 μm.
The step 6 further includes using powdering compensation technique, the compensation rate of the magnesium-rare earth alloy powder of the powdering compensation It is 10 μm.
The step 6 further includes adjustment gas flow, it is ensured that the magnesium powder that air-flow will volatilize takes away substrate, guarantees the magnesium of volatilization Powder does not fall in print area.
In the step 8 using perchloric acid alcoholic solution as polishing etch solution to porous magnesium-rare earth alloy implantation material into Row electrochemical polishing treatment, the volume ratio of perchloric acid and alcohol is 0.1 in the perchloric acid alcoholic solution.
Magnetic agitation is carried out to the perchloric acid alcoholic solution, the revolving speed of magnetic agitation is 1000rpm, the perchloric acid wine The solution temperature of smart solution is -20 DEG C.
The parameter of electrochemical polishing treatment in the step 8 are as follows: polishing voltage is 15V, and polishing electric current is 2A, polishing process In, stop polishing when porous magnesium-rare earth alloy implantation material loss of weight 10%.
It is tested by experiment, the porosity of porous magnesium-rare earth alloy implantation material obtained is 75 ± 5%, elasticity modulus 1 ± 0.2GPa, compression yield strength are 15 ± 3MPa, and compressive strength is 30 ± 5MPa.
Embodiment 2
The embodiment of the invention provides a kind of porous magnesium rare earth conjunctions based on selective laser fusing (SLM) increases material manufacturing technology The preparation method of golden implantation material, includes the following steps:
Step 1, the component for selecting magnesium-rare earth alloy powder；
Step 2 preheats magnesium-rare earth alloy powder, preheating time 1.5h, preheating temperature in a vacuum drying oven It is 100 DEG C；
Step 3 selects magnesium-rare earth alloy identical with the magnesium-rare earth alloy powdery components in step 1 as substrate, to institute Substrate is stated to be preheated；
Step 4, the threedimensional model for drawing porous magnesium-rare earth alloy implantation material by Three-dimensional Design Software on computers, it is raw At porous magnesium-rare earth alloy implantation material entity, wherein porous aperture is 500 μm, and porous wall thickness is 300 μm；
Porous magnesium-rare earth alloy implantation material entity is saved into output format file and is transmitted to point with STL format by step 5 In layer software, the addition bottom surface 1mm supports and imports in selective laser fusing increasing material manufacturing equipment after carrying out slicing treatment；
Step 6 opens selective laser fusing increasing material manufacturing equipment, and print parameters are arranged, are implanted into porous magnesium-rare earth alloy Object entity is printed, and porous magnesium-rare earth alloy implantation material is made；
Porous magnesium-rare earth alloy implantation material obtained in step 6 is carried out electrochemical polishing treatment by step 7.
Print parameters in the step 6 are as follows: laser power 80W, sweep speed 450mm/s, laser fill spacing It is 90 μm, powdering thickness is 30 μm, and the angle of laser scanning direction is 73 ° between two neighboring powdering layer.
The magnesium-rare earth alloy powder is Mg-3Nd-0.2Zn-Zr (wt.%).
The magnesium-rare earth alloy powder is spherical powder, and the average grain diameter of the spherical powder is 45 μm.
The preheating temperature preheated in the step 3 to the substrate is 160 DEG C.
The step 6 further includes that technique is adjusted using spot diameter, and the spot diameter size is selected according to formula P/DV=C It takes, wherein C is power density, and the range of C is 1.1-2.25W/mm2, D is spot diameter, and the unit of D is mm, and P is laser function Rate, the unit of P are W, and V is laser inswept distance per second, and the unit of V is mm.
Specifically, C=2.22W/mm is taken2, the spot diameter of selection is 80 μm.
The step 6 further includes using powdering compensation technique, the compensation rate of the magnesium-rare earth alloy powder of the powdering compensation It is 20 μm.
The step 6 further includes adjustment gas flow, it is ensured that the magnesium powder that air-flow will volatilize takes away substrate, guarantees the magnesium of volatilization Powder does not fall in print area.
In the step 7 using perchloric acid alcoholic solution as polishing etch solution to porous magnesium-rare earth alloy implantation material into Row electrochemical polishing treatment, the volume ratio of perchloric acid and alcohol is 0.1 in the perchloric acid alcoholic solution.
Magnetic agitation is carried out to the perchloric acid alcoholic solution, the revolving speed of magnetic agitation is 1000rpm, the perchloric acid wine The solution temperature of smart solution is -20 DEG C.
The parameter of electrochemical polishing treatment in the step 7 are as follows: polishing voltage is 15V, and polishing electric current is 2A, polishing process In, stop polishing when porous magnesium-rare earth alloy implantation material loss of weight 10%.
It is tested by experiment, the porosity of porous magnesium-rare earth alloy implantation material obtained is 75 ± 5%, elasticity modulus 1 ± 0.2GPa, compression yield strength are 15 ± 3MPa, and compressive strength is 25 ± 5MPa.
Embodiment 3
The embodiment of the invention provides a kind of porous magnesium rare earth conjunctions based on selective laser fusing (SLM) increases material manufacturing technology The preparation method of golden implantation material, includes the following steps:
Step 1, the component for selecting magnesium-rare earth alloy powder；
Step 2 preheats magnesium-rare earth alloy powder, preheating time 1.5h, preheating temperature in a vacuum drying oven It is 100 DEG C；
Step 3 selects magnesium-rare earth alloy identical with the magnesium-rare earth alloy powdery components in step 1 as substrate, to institute Substrate is stated to be preheated；
Step 4, the threedimensional model for drawing porous magnesium-rare earth alloy implantation material by Three-dimensional Design Software on computers, it is raw At porous magnesium-rare earth alloy implantation material entity, wherein porous aperture is 500 μm, and porous wall thickness is 300 μm；
Porous magnesium-rare earth alloy implantation material entity is saved into output format file and is transmitted to point with STL format by step 5 In layer software, the addition bottom surface 1mm supports and imported into selective laser fusing increasing material manufacturing equipment after carrying out slicing treatment；
Step 6 opens selective laser fusing increasing material manufacturing equipment, and print parameters are arranged, are implanted into porous magnesium-rare earth alloy Object entity is printed, and porous magnesium-rare earth alloy implantation material is made；
Porous magnesium-rare earth alloy implantation material obtained in step 6 is carried out electrochemical polishing treatment by step 7.
Print parameters in the step 6 are as follows: laser power 80W, sweep speed 450mm/s, laser fill spacing It is 90 μm, powdering thickness is 30 μm, and the angle of laser scanning direction is 73 ° between two neighboring powdering layer.
The magnesium-rare earth alloy powder is Mg-3Nd-0.2Zn-Zr (wt.%).
The magnesium-rare earth alloy powder is spherical powder, and the average grain diameter of the spherical powder is 45 μm.
The preheating temperature preheated in the step 3 to the substrate is 160 DEG C.
The step 6 further includes that technique is adjusted using spot diameter, and the spot diameter size is selected according to formula P/DV=C It takes, wherein C is power density, and the range of C is 1.1-2.25W/mm2, D is spot diameter, and the unit of D is mm, and P is laser function Rate, the unit of P are W, and V is laser inswept distance per second, and the unit of V is mm.
Specifically, C=1.11W/mm is taken2, the spot diameter of selection is 160 μm.
The step 6 further includes using powdering compensation technique, the compensation rate of the magnesium-rare earth alloy powder of the powdering compensation It is 10 μm.
The step 6 further includes adjustment gas flow, it is ensured that the magnesium powder that air-flow will volatilize takes away substrate, guarantees the magnesium of volatilization Powder does not fall in print area.
In the step 7 using perchloric acid alcoholic solution as polishing etch solution to porous magnesium-rare earth alloy implantation material into Row electrochemical polishing treatment, the volume ratio of perchloric acid and alcohol is 0.1 in the perchloric acid alcoholic solution.
Magnetic agitation is carried out to the perchloric acid alcoholic solution, the revolving speed of magnetic agitation is 1000rpm, the perchloric acid wine The solution temperature of smart solution is -20 DEG C.
The parameter of electrochemical polishing treatment in the step 7 are as follows: polishing voltage is 15V, and polishing electric current is 2A, polishing process In, stop polishing when porous magnesium-rare earth alloy implantation material loss of weight 10%.
It is tested by experiment, the porosity of porous magnesium-rare earth alloy implantation material obtained is 78 ± 5%, elasticity modulus 1 ± 0.2GPa, compression yield strength are 12 ± 3MPa, and compressive strength is 20 ± 5MPa.
Embodiment 4
The embodiment of the invention provides a kind of porous magnesium rare earth conjunctions based on selective laser fusing (SLM) increases material manufacturing technology The preparation method of golden implantation material, includes the following steps:
Step 1, the component for selecting magnesium-rare earth alloy powder；
Step 2 preheats magnesium-rare earth alloy powder, preheating time 1.5h, preheating temperature in a vacuum drying oven It is 100 DEG C；
Step 3 selects magnesium-rare earth alloy identical with the magnesium-rare earth alloy powdery components in step 1 as substrate, to institute Substrate is stated to be preheated；
Step 4, the threedimensional model for drawing porous magnesium-rare earth alloy implantation material by Three-dimensional Design Software on computers, it is raw At porous magnesium-rare earth alloy implantation material entity, wherein porous aperture is 500 μm, and porous wall thickness is 300 μm；
Porous magnesium-rare earth alloy implantation material entity is saved into output format file and is transmitted to point with STL format by step 5 In layer software, the addition bottom surface 1mm supports and imported into selective laser fusing increasing material manufacturing equipment after carrying out slicing treatment；
Step 6 opens selective laser fusing increasing material manufacturing equipment, and print parameters are arranged, are implanted into porous magnesium-rare earth alloy Object entity is printed, and porous magnesium-rare earth alloy implantation material is made；
Porous magnesium-rare earth alloy implantation material obtained in step 6 is carried out electrochemical polishing treatment by step 7.
Print parameters in the step 6 are as follows: laser power 80W, sweep speed 450mm/s, laser fill spacing It is 90 μm, powdering thickness is 30 μm, and the angle of laser scanning direction is 73 ° between two neighboring powdering layer.
The magnesium-rare earth alloy powder is Mg-12Gd-0.8Zn-Zr (wt.%).
The magnesium-rare earth alloy powder is spherical powder, and the average grain diameter of the spherical powder is 45 μm.
The preheating temperature preheated in the step 3 to the substrate is 160 DEG C.
The step 6 further includes that technique is adjusted using spot diameter, and the spot diameter size is selected according to formula P/DV=C It takes, wherein C is power density, and the range of C is 1.1-2.25W/mm2, D is spot diameter, and the unit of D is mm, and P is laser function Rate, the unit of P are W, and V is laser inswept distance per second, and the unit of V is mm.
Specifically, C=1.62W/mm is taken2, the spot diameter of selection is 110 μm.
The step 6 further includes using powdering compensation technique, the compensation rate of the magnesium-rare earth alloy powder of the powdering compensation It is 10 μm.
The step 6 further includes adjustment gas flow, it is ensured that the magnesium powder that air-flow will volatilize takes away substrate, guarantees the magnesium of volatilization Powder does not fall in print area.
In the step 7 using perchloric acid alcoholic solution as polishing etch solution to porous magnesium-rare earth alloy implantation material into Row electrochemical polishing treatment, the volume ratio of perchloric acid and alcohol is 0.1 in the perchloric acid alcoholic solution.
Magnetic agitation is carried out to the perchloric acid alcoholic solution, the revolving speed of magnetic agitation is 1000rpm, the perchloric acid wine The solution temperature of smart solution is -20 DEG C.
The parameter of electrochemical polishing treatment in the step 7 are as follows: polishing voltage is 15V, and polishing electric current is 2A, polishing process In, stop polishing when porous magnesium-rare earth alloy implantation material loss of weight 10%.
It is tested by experiment, the porosity of porous magnesium-rare earth alloy implantation material obtained is 75 ± 5%, elasticity modulus 1 ± 0.3GPa, compression yield strength are 20 ± 3MPa, and compressive strength is 35 ± 5MPa.
Comparative example
The preparation side of porous magnesium-rare earth alloy implantation material of the one kind based on selective laser fusing (SLM) increases material manufacturing technology Method includes the following steps:
Step 1, the component for selecting magnesium-rare earth alloy powder；
Step 2 preheats magnesium-rare earth alloy powder, preheating time 1.5h, preheating temperature in a vacuum drying oven It is 100 DEG C；
Step 3 selects magnesium-rare earth alloy identical with the magnesium-rare earth alloy powdery components in step 1 as substrate, to institute Substrate is stated to be preheated；
Step 4, the threedimensional model for drawing porous magnesium-rare earth alloy implantation material by Three-dimensional Design Software on computers, it is raw At porous magnesium-rare earth alloy implantation material entity, wherein porous aperture is 500 μm, and porous wall thickness is 300 μm；
Porous magnesium-rare earth alloy implantation material entity is saved into output format file and is transmitted to point with STL format by step 5 In layer software, the addition bottom surface 1mm supports and imported into selective laser fusing increasing material manufacturing equipment after carrying out slicing treatment；
Step 6 opens selective laser fusing increasing material manufacturing equipment, and print parameters are arranged, are implanted into porous magnesium-rare earth alloy Object entity is printed, and porous magnesium-rare earth alloy implantation material is made；
Porous magnesium-rare earth alloy implantation material obtained in step 6 is carried out electrochemical polishing treatment by step 7.
Print parameters in the step 6 are as follows: laser power 120W, sweep speed 450mm/s, laser fill spacing It is 90 μm, powdering thickness is 30 μm, and the angle of laser scanning direction is 73 ° between two neighboring powdering layer.
The magnesium-rare earth alloy powder is Mg-3Nd-0.2Zn-Zr (wt.%).
The magnesium-rare earth alloy powder is spherical powder, and the partial size of the spherical powder is 45 μm.
The preheating temperature preheated in the step 3 to the substrate is 160 DEG C.
The step 6 further includes that technique is adjusted using spot diameter, and the spot diameter size is selected according to formula P/DV=C It takes, wherein C is power density, and the range of C is 1.1-2.25W/mm2, D is spot diameter, and the unit of D is mm, and P is laser function Rate, the unit of P are W, and V is laser inswept distance per second, and the unit of V is mm.
Specifically, C=3.33W/mm is taken2, the spot diameter of selection is 80 μm.
The step 6 further includes using powdering compensation technique, the compensation rate of the magnesium-rare earth alloy powder of the powdering compensation It is 0 μm, that is, powdering compensation technique is not used.
In the step 7 using perchloric acid alcoholic solution as polishing etch solution to porous magnesium-rare earth alloy implantation material into Row electrochemical polishing treatment, the volume ratio of perchloric acid and alcohol is 0.1 in the perchloric acid alcoholic solution.
Magnetic agitation is carried out to the perchloric acid alcoholic solution, the revolving speed of magnetic agitation is 1000rpm, the perchloric acid wine The solution temperature of smart solution is -20 DEG C.
The parameter of electrochemical polishing treatment in the step 7 are as follows: polishing voltage is 15V, and polishing electric current is 2A, polishing process In, stop polishing when porous magnesium-rare earth alloy implantation material loss of weight 10%.
Micro-CT analysis the result shows that, there is the line that fendillates inside technique porous implant obtained, it is porous The intensity and performance reproducibility of implantation material are remarkably decreased.
In conclusion the porous magnesium-rare earth alloy of the invention based on selective laser fusing (SLM) increases material manufacturing technology is planted The preparation method for entering object, the implantation material provided, which increases material preparation method, can be successfully prepared hole wall by selective laser smelting technology Thickness uniformly, the degradable magnesium rare earth alloy porous implant of flawless defect, the integral strength and modulus of implantation material be higher；With The prior art is compared, and porous implant prepared by the present invention is more matched with the intensity and modulus of skeleton；The implantation of offer Object electrochemical polishing method simple process, consistency are good, and the polished amount of implantation material can be effectively controlled, and what raising implantation material polished can Repeatability；The magnesium-rare earth alloy porous implant of any aperture and shape may be implemented in the implantation material increasing material preparation method of offer Functional and structural strength perfect combination is realized in quickly manufacture.
In the description of the present application, it is to be understood that term " on ", "front", "rear", "left", "right", " is erected at "lower" Directly ", the orientation or positional relationship of the instructions such as "horizontal", "top", "bottom", "inner", "outside" is orientation based on the figure or position Relationship is set, description the application is merely for convenience of and simplifies description, rather than the device or element of indication or suggestion meaning are necessary It with specific orientation, is constructed and operated in a specific orientation, therefore should not be understood as the limitation to the application.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned Particular implementation, those skilled in the art can make a variety of changes or modify within the scope of the claims, this not shadow Ring substantive content of the invention.In the absence of conflict, the feature in embodiments herein and embodiment can any phase Mutually combination.

Claims (11)

1. the preparation method of porous magnesium-rare earth alloy implantation material of the one kind based on selective laser fusing (SLM) increases material manufacturing technology, It is characterized by comprising the following steps:
Step 1, the component for selecting magnesium-rare earth alloy powder；
Step 2 preheats magnesium-rare earth alloy powder in a vacuum drying oven, and preheating time range is 0.5-1.5h, preheating Temperature range is 80-120 DEG C；
Step 3 selects magnesium-rare earth alloy identical with the magnesium-rare earth alloy powdery components in step 1 as substrate, to the base Plate is preheated；Preheating temperature >=160 DEG C that the substrate is preheated in the step 3；
Step 4, the threedimensional model for drawing porous magnesium-rare earth alloy implantation material by Three-dimensional Design Software on computers generate more Hole magnesium-rare earth alloy implantation material entity；
Step 5, by porous magnesium-rare earth alloy implantation material entity with STL format save at output format file and be transmitted to layering it is soft In part, addition bottom surface supports and imported into selective laser fusing increasing material manufacturing equipment after carrying out slicing treatment；
Step 6 opens selective laser fusing increasing material manufacturing equipment, and print parameters are arranged, real to porous magnesium-rare earth alloy implantation material Body is printed；
The step 6 further includes that technique is adjusted using spot diameter, and the spot diameter size is chosen according to formula P/DV=C, Wherein C is power density, and the range of C is 1.1-2.25W/mm2, D is spot diameter, and the unit of D is mm, and P is laser power, P Unit be W, V is laser inswept distance per second, and the unit of V is mm；
The step 6 further includes using powdering compensation technique, and the compensation rate of the magnesium-rare earth alloy powder of the powdering compensation is 10- 20μm；
The step 6 further includes adjusting the air-flow size magnesium powder that ensures that air-flow will volatilize to take away substrate；
Step 7 carries out wire cutting along substrate end-face, and porous magnesium-rare earth alloy implantation material molded part is separated with substrate cut, is made Obtain porous magnesium-rare earth alloy implantation material；
Porous magnesium-rare earth alloy implantation material obtained in step 7 is carried out electrochemical polishing treatment by step 8.
2. the porous magnesium-rare earth alloy according to claim 1 based on selective laser fusing (SLM) increases material manufacturing technology is planted Enter the preparation method of object, which is characterized in that the print parameters in the step 6 are as follows: laser power range is 80-160W, scanning Speed range is 300-1500mm/s, and it is 50-120 μm that laser, which fills spacing range, and powdering Layer thickness is 30-50 μm.
3. the porous magnesium-rare earth alloy according to claim 2 based on selective laser fusing (SLM) increases material manufacturing technology is planted Enter the preparation method of object, which is characterized in that the angle of laser scanning direction is between two neighboring powdering layer in the step 6 67°。
4. the porous magnesium-rare earth alloy according to claim 2 based on selective laser fusing (SLM) increases material manufacturing technology is planted Enter the preparation method of object, which is characterized in that the angle of laser scanning direction is between two neighboring powdering layer in the step 6 73°。
5. the porous magnesium-rare earth alloy according to claim 2 based on selective laser fusing (SLM) increases material manufacturing technology is planted Enter the preparation method of object, which is characterized in that the angle of laser scanning direction is between two neighboring powdering layer in the step 6 90°。
6. the porous magnesium-rare earth alloy according to claim 1 based on selective laser fusing (SLM) increases material manufacturing technology is planted Enter the preparation method of object, which is characterized in that the magnesium-rare earth alloy powder be Mg-2.5~3.6Nd-0.01~0.4Zn-Zr or Mg-8.0~14.0Gd-0.01~0.85Zn-Zr.
7. the porous magnesium-rare earth alloy according to claim 1 based on selective laser fusing (SLM) increases material manufacturing technology is planted Enter the preparation method of object, which is characterized in that the magnesium-rare earth alloy powder is spherical powder, the particle size range of the spherical powder It is 21-74 μm.
8. the porous magnesium-rare earth alloy according to claim 1 based on selective laser fusing (SLM) increases material manufacturing technology is planted Enter the preparation method of object, which is characterized in that use perchloric acid alcoholic solution as polishing etch solution to porous in the step 8 Magnesium-rare earth alloy implantation material carries out electrochemical polishing treatment, the volume ratio model of perchloric acid and alcohol in the perchloric acid alcoholic solution It encloses for 0.05-0.2.
9. the porous magnesium-rare earth alloy according to claim 8 based on selective laser fusing (SLM) increases material manufacturing technology is planted Enter the preparation method of object, which is characterized in that magnetic agitation, the range of speeds of magnetic agitation are carried out to the perchloric acid alcoholic solution For 500~1000rpm, < -10 DEG C of solution temperature of the perchloric acid alcoholic solution.
10. the porous magnesium-rare earth alloy according to claim 8 based on selective laser fusing (SLM) increases material manufacturing technology is planted Enter the preparation method of object, which is characterized in that the parameter of electrochemical polishing treatment in the step 8 are as follows: polishing voltage range is 15- 20V, polishing current range are 1.5-2.5A, and polishing time range is 5-20min.
11. the porous magnesium-rare earth alloy according to claim 8 based on selective laser fusing (SLM) increases material manufacturing technology is planted Enter the preparation method of object, which is characterized in that plant when electrochemical polishing treatment by monitoring porous magnesium-rare earth alloy in the step 8 Enter the batch consistency of the porous magnesium-rare earth alloy implantation material electrochemical polish of quality assurance of object.
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