CN107245618B - It is a kind of for the preparation method of 3D printing Medical magnesium alloy material, material and application - Google Patents
It is a kind of for the preparation method of 3D printing Medical magnesium alloy material, material and application Download PDFInfo
- Publication number
- CN107245618B CN107245618B CN201710290585.9A CN201710290585A CN107245618B CN 107245618 B CN107245618 B CN 107245618B CN 201710290585 A CN201710290585 A CN 201710290585A CN 107245618 B CN107245618 B CN 107245618B
- Authority
- CN
- China
- Prior art keywords
- magnesium alloy
- pure
- medical
- medical magnesium
- printing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/02—Inorganic materials
- A61L31/022—Metals or alloys
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L31/148—Materials at least partially resorbable by the body
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/412—Tissue-regenerating or healing or proliferative agents
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
- A61L2300/602—Type of release, e.g. controlled, sustained, slow
- A61L2300/604—Biodegradation
Abstract
The invention discloses preparation method, material and the application of a kind of Medical magnesium alloy material for 3D printing, constituent mass percentages are as follows: 10 ~ 16wt%Fe, 1 ~ 3wt%Mn, 0.2 ~ 2wt%Zn, 0.5 ~ 3wt%Ca, surplus Mg.Preparation step are as follows: compare ingredient by said components and quality；Pure magnesium, pure manganese, pure zinc and pure calcium are put into the crucible of preheating, coverture, in atmospheric conditions melting is added；After having melted, magnesium iron intermediate alloy is added, after fusing, stirs evenly, equilibrium temperature is to 700 DEG C ~ 740 DEG C；Refining agent is added, refining 5-30min skims surface scum, pour into metal type dies, obtain medical magnesium alloy base material in 700 DEG C ~ 740 DEG C standing 10-30min；Again by base material melting, atomization, Medical magnesium alloy material is obtained.The present invention is a kind of polynary degradable alloy material being made of completely the human nutrition element of biological safety, and there is excellent fire-retardancy, powder morphology, partial size are easily controllable, important application potential is all had in medical degradable inner implantation material and 3D printing field, with good application prospect.
Description
Technical field
The invention belongs to the technical fields of 3D printing material, specifically, being related to a kind of for 3D printing medical magnesium alloy material
Preparation method, material and the application of material.
Background technique
3D printing technique is called increasing material manufacturing according to its manufacturing process, belongs to one kind of rapid shaping technique, it uses powder
The adhesive materials such as last shape metal or plastics finally directly print product, shape by the multilayer printing type of layer upon layer
At " Digitized manufacturing ".
3D printing technique is derived from the photosculpture and landforms forming technique of the late 19th century American Studies, but is limited to work as
When technical conditions, the not progress of making a breakthrough property.The eighties in last century, with computer technology, new material technology it is fluffy
The exhibition of breaking out, 3D printing technique achieve significant progress, but it is commercialized, commercialization is slow.In the 21st century, 3D printing
Technology is grown rapidly, application field also by mold manufacture, industrial design etc. be gradually generalized to aerospace, automobile and
The fields such as medical treatment.
Currently, internal fixation material used in bone surgery is mainly made of stainless steel, titanium alloy etc..These materials exist
It cannot degrade in human body, be required to second operation and be drawn off.The density of magnesium alloy has preferable close to skeleton
Biomechanical compatibility, far below stainless steel, titanium alloy etc., it can not only be absorbed by the body discomfort after being implanted into human body,
The magnesium ion released may additionally facilitate the proliferation and differentiation of osteocyte, promotes bone growth, healing, can avoid second operation.Together
When, magnesium alloy can also be applied to the treatment of cardiovascular disease, and degradable magnesium alloy angiocarpy bracket not will lead to intravascular
Film hyperplasia, the case where avoiding stent restenosis generation.Therefore, magnesium alloy is gradually replacing plastic material, becomes medical market
In advanced material.If medical magnesium alloy and 3D printing technique are combined service medical field, medical material can be pushed
Develop to low cost, short cycle, high efficiency direction.
But, mainly there are titanium alloy, cochrome, stainless steel and aluminum alloy materials currently used for the metal powder of 3D printing
Deng, magnesium alloy because its chemical property is active and inflammability, powder preparation are difficult, it is also in experimental stage, is not widely applied to
In 3D printing field.The currently used method for preparing magnesium alloy powder is ball-milling method.But ball-milling method is because energy consumption is high, Yi Zengjia
Impurity.
Summary of the invention
Above-mentioned to solve the problems, such as, it is multiple that the purpose of the present invention is to provide a kind of high-strength high-elasticity modulus magnesium lithium bases
Condensation material, material and application, the preparation method prepare medical magnesium alloy powder using atomization, the powder burning point of preparation is high,
Pattern and partial size are easily controllable, and the addition of preparation process free from admixture compensates for the deficiency of ball-milling method.
In order to achieve the above objectives, the technical scheme is that
A kind of preparation method for 3D printing Medical magnesium alloy material, the preparation method include the following steps:
1) ingredient
Take including pure magnesium, pure manganese, pure zinc, pure calcium, magnesium iron intermediate alloy raw material, component mass percent in raw material
It is as follows: Fe:10 ~ 16wt%, Mn:1 ~ 3wt%, Zn:0.2 ~ 2wt%, Ca:0.5 ~ 3wt%, surplus Mg；
2) baking material
The weighed all raw materials of step 1) are preheated 2 ~ 4 hours at 180 ~ 240 DEG C respectively；
3) melting
Pure magnesium, pure manganese, pure zinc and pure calcium after step 2) drying is put into the container for being preheating to 200 ~ 400 DEG C, is added
Coverture, in atmospheric conditions melting, smelting temperature are 500 ~ 680 DEG C；
After the fusing of pure magnesium, pure manganese, pure zinc and pure calcium, melt temperature gos up to 720 ~ 760 DEG C, is added among magnesium iron and closes
Gold, after magnesium iron intermediate alloy all fusing, for stirring melt to uniform, refining agent, essence is added to 700 ~ 740 DEG C in equilibrium temperature
5 ~ 30min of refining skims surface scum, pours into metal type dies then at 700 ~ 740 DEG C of 10 ~ 30min of standing, obtains medical magnesium and closes
Golden base material；
4) atomization prepares Medical magnesium alloy material
Medical magnesium alloy base material obtained by step 3) is put into preheated container, in the vacuum that vacuum degree is 1 ~ 20kPa
Under the conditions of in 500 ~ 680 DEG C of 20 ~ 60min of melting, obtain medical magnesium alloy melt, by medical magnesium alloy melt overheat 50 ~ 250
DEG C, it is subsequently placed in atomising device and is atomized, obtain medical magnesium alloy powder, medical magnesium alloy powder is collected, screening, packet
Dress obtains the Medical magnesium alloy material for being used for 3D printing.
Preferably, degree of purity >=99.99% of degree of purity >=99.99%, Fe of Mg described in step 1).
Preferably, Fe accounts for 25wt% in the intermediate alloy of magnesium iron described in step 1).
Preferably, the preheating temperature of all raw materials described in step 2) is 210 DEG C.
Preferably, smelting technology described in step 3) is in SF6And CO2It is carried out under the conditions of mixed gas protected.
Preferably, the temperature of preheating described in step 4) is 350 ~ 550 DEG C.
Preferably, atomising device described in step 4) is atomized using argon gas, and argon pressure is 0.2 ~ 4MPa；Argon gas
Reversely charging pressure is 0.1 ~ 1MPa.
Preferably, step 3) and preheated container used in step 4) are crucible.
Meanwhile the present invention also provides 3D is used for obtained by a kind of preparation method for 3D printing Medical magnesium alloy material
Medical magnesium alloy material is printed, the material includes the ingredient of following weight percent: Fe:10 ~ 16wt%, Mn:1 ~ 3wt%, Zn:
0.2 ~ 2wt%, Ca:0.5 ~ 3wt%, surplus Mg.
Meanwhile the present invention also provides a kind of for 3D printing Medical magnesium alloy material in answering in terms of medical 3D printing
With.
Wherein, magnesium is that human body includes 4 metallic elements of flow control, is only second to K into the cell+The 2nd cation.It is catalyzed
Or activation 325 kinds of enzyme systems of body, participate in all energetic supersessions in vivo.To contraction of muscle, nervimotion function, physiological function and pre-
Anti- circulation system disease and ischemic heart disease play an important role.The excretion of magnesium mainly passes through urinary system, and magnesium is in human body interior suction
Receive the apparent increase that not will lead to serum magnesium content.So magnesium has good biological safety.It is closed in Mg-Fe-Mn-Zn-Ca
Jin Zhong significantly increases the dynamics of magnesium alloy electrochemical corrosion, thus significantly since the electrode potential of iron and magnesium differs larger
Improve the corrosion rate of magnesium alloy.
Iron is the maximum microelement of people's in-vivo content, is played an important role to bone.Iron deficiency make respiratory enzyme in skeletal muscle,
Mitochondrial oxidation enzyme and myoglobin concentration decline, cause muscle to decline for hypoxgia, aerobic capacity, lactic acid heap in blood
Collection.
Manganese is then effective activator as ionic stronger microelement, can catalytic metal activating enzymes.Trace manganese member
Element also takes part in the synthesis of hormone and vitamin.
Zinc is the main component of internal tens of kinds of enzymes, and related with brain development and intelligence.Zinc also promotes lymphocyte
The effect of proliferation and mobility, to maintaining, epithelium and mucosal tissue are normal, defense against bacterial, Virus entry, promote bone healing
Etc. lesions have magical effect.Each system of whole body can all be adversely affected when zinc deficiency.
Calcium is most one of the mineral element of people's in-vivo content, adjusts the normal function of the histoorgan of each system of human body
Its presence will be relied on.Calcium, which has, promotes skeleton growth and development effect, while promoting the activity of a variety of enzymes in vivo, maintains
Internal acid-base balance and other effects.
The beneficial effects of the present invention are: the invention has the advantages and beneficial effects that:
A) Mg-Fe-Mn-Zn-Ca alloy material of the present invention can natural degradation in vivo, reach after medical effect certain
Time in can disappear from internal, avoid the implants such as traditional stainless steel, titanium alloy bone plate, bone nail after bone tissue recovery from illness
Patient need to be allowed to avoid second operation bring pain and trouble by the drawbacks of taking out of performing the operation again；
B) present invention is prepared for Medical magnesium alloy material using the method for melting and atomization, and melting ensure that magnesium alloy
At being grouped as, atomization meets requirement of the 3D printing to metal powder；
C) medical Mg-Fe-Mn-Zn-Ca alloy material prepared by the present invention has excellent fire-retardancy, and burning point is increased to
970 DEG C or more, partial size in normal distribution, crystal grain is tiny for tissue, in atomization process it is contactless with air, it is oxygen-containing low, solve mist
Change method prepares the inflammable problem of magnesium alloy powder, can be used for 3D printing；And the Medical magnesium alloy material corrosion rate is higher, together
When have and promote bone tissue healing, anti-inflammation and sterilization and other effects.
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, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Embodiment 1
The present embodiment is related to a kind of Medical magnesium alloy material for 3D printing, which includes following weight percent
The each component of content: 10wt% Fe, 1wt% Mn, 0.2wt% Zn, 0.5wt% Ca, surplus Mg.
The present embodiment further relates to the preparation method of aforementioned medical Mg-Fe-Mn-Zn-Ca magnesium alloy materials, and preparation method includes
Following steps:
(1) ingredient: raw material is weighed according to the mass ratio of element: 10wt%Fe, 1wt%Mn, 0.2wt%Zn, 0.5wt%Ca, it is remaining
Amount is Mg；The raw material includes pure magnesium, pure manganese, pure zinc, pure calcium, Mg-25wt%Fe intermediate alloy；The degree of purity of the Mg >=
Degree of purity >=99.99% of 99.99%, Fe.
(2) baking material: the weighed all raw materials of step (1) are preheated 3 hours respectively at 180 DEG C；
(3) melting: pure magnesium, pure manganese, pure zinc and the pure calcium after step (2) drying are put into the crucible for being preheating to 200 DEG C,
Coverture, in atmospheric conditions melting is added, smelting temperature is 500 DEG C；After the fusing of pure magnesium, pure manganese, pure zinc and pure calcium, melt
Mg-25wt%Fe intermediate alloy is added when being extremely added 720 DEG C DEG C in temperature recovery；After Mg-25wt%Fe intermediate alloy all fusing,
Melt is stirred to uniform, refining agent is added to 700 DEG C in equilibrium temperature, refines 30min then at 700 DEG C of standing 30min and skims table
Face dross, pours into metal type dies, obtains medical magnesium alloy base material；The smelting technology is in SF6And CO2Mixed gas protected item
It is carried out under part；
(4) atomization prepares Medical magnesium alloy material: medical magnesium alloy base material is put into the crucible for being preheating to 350 DEG C,
In the case where vacuum degree is the vacuum condition of 20kPa in 500 DEG C of melting 60min, medical magnesium alloy melt is obtained；Medical magnesium alloy is melted
Liquid overheats 50 DEG C, is subsequently placed in atomising device and is atomized, obtains medical magnesium alloy powder；Medical magnesium alloy powder is collected,
Screening, packaging, obtain the Medical magnesium alloy material for 3D printing；The atomization is 0.2MPa with argon pressure；Argon gas it is anti-
Pressurising power is 0.1MPa.
The Medical magnesium alloy material for 3D printing prepared by the above method, burning point are 880 DEG C, and particle size range exists
0.5 ~ 30 μm, be in normal distribution, and pattern is spherical shape, can be used for 3D printing.
Embodiment 2
The present embodiment is related to a kind of Medical magnesium alloy material for 3D printing, which includes following weight percent
The each component of content: 16wt%Fe, 3wt%Mn, 2wt%Zn, 3wt%Ca, surplus Mg.
The present embodiment further relates to the preparation method of aforementioned medical Mg-Fe-Mn-Zn-Ca magnesium alloy materials, and preparation method includes
Following steps:
(1) ingredient: weigh raw material according to the mass ratio of element: 16wt%Fe, 3wt%Mn, 2wt%Zn, 3wt%Ca, surplus are
Mg；The raw material includes pure magnesium, pure manganese, pure zinc, pure calcium, Mg-25wt%Fe intermediate alloy；Degree of purity >=99.99% of the Mg,
Degree of purity >=99.99% of Fe.
(2) baking material: the weighed all raw materials of step (1) are preheated 3 hours respectively at 240 DEG C；
(3) melting: pure magnesium, pure manganese, pure zinc and the pure calcium after step (2) drying are put into the crucible for being preheating to 400 DEG C,
Coverture, in atmospheric conditions melting is added, smelting temperature is 680 DEG C；After the fusing of pure magnesium, pure manganese, pure zinc and pure calcium, melt
Mg-25wt%Fe intermediate alloy is added when being extremely added 760 DEG C DEG C in temperature recovery；After Mg-25wt%Fe intermediate alloy all fusing,
Melt is stirred to uniform, refining agent is added to 740 DEG C in equilibrium temperature, refines 5min then at 740 DEG C of standing 10min and skims table
Face dross, pours into metal type dies, obtains medical magnesium alloy base material；The smelting technology is in the mixed gas protected item of SF6 and CO2
It is carried out under part；
(4) atomization prepares Medical magnesium alloy material: medical magnesium alloy base material is put into the crucible for being preheating to 550 DEG C,
In the case where vacuum degree is the vacuum condition of 1kPa in 680 DEG C of melting 20min, medical magnesium alloy melt is obtained；Medical magnesium alloy is melted
Liquid overheats 250 DEG C, is subsequently placed in atomising device and is atomized, obtains medical magnesium alloy powder；Medical magnesium alloy powder is collected,
Screening, packaging, obtain the Medical magnesium alloy material for 3D printing；The atomization is 4MPa with argon pressure；The reversely charging of argon gas
Pressure is 1MPa.
The Medical magnesium alloy material for 3D printing prepared by the above method, burning point are 980 DEG C, and particle size range exists
10 ~ 60 μm, be in normal distribution, and pattern is spherical shape, can be used for 3D printing.
Embodiment 3
The present embodiment is related to a kind of Medical magnesium alloy material for 3D printing, which includes following weight percent
The each component of content: 13wt%Fe, 2wt%Mn, 1.1wt%Zn, 1.7wt%Ca, surplus Mg.
The present embodiment further relates to the preparation method of aforementioned medical Mg-Fe-Mn-Zn-Ca magnesium alloy materials, and preparation method includes
Following steps:
(1) ingredient: raw material is weighed according to the mass ratio of element: 13wt%Fe, 2wt%Mn, 1.1wt%Zn, 1.7wt%Ca, it is remaining
Amount is Mg；The raw material includes pure magnesium, pure manganese, pure zinc, pure calcium, Mg-25wt%Fe intermediate alloy；The degree of purity of the Mg >=
Degree of purity >=99.99% of 99.99%, Fe.
(2) baking material: the weighed all raw materials of step (1) are preheated 3 hours respectively at 210 DEG C；
(3) melting: pure magnesium, pure manganese, pure zinc and the pure calcium after step (2) drying are put into the crucible for being preheating to 300 DEG C,
Coverture, in atmospheric conditions melting is added, smelting temperature is 590 DEG C；After the fusing of pure magnesium, pure manganese, pure zinc and pure calcium, melt
Mg-25wt%Fe intermediate alloy is added when being extremely added 740 DEG C DEG C in temperature recovery；After Mg-25wt%Fe intermediate alloy all fusing,
Melt is stirred to uniform, refining agent is added to 720 DEG C in equilibrium temperature, refines 17min then at 720 DEG C of standing 20min and skims table
Face dross, pours into metal type dies, obtains medical magnesium alloy base material；The smelting technology is in the mixed gas protected item of SF6 and CO2
It is carried out under part；
(4) atomization prepares Medical magnesium alloy material: medical magnesium alloy base material is put into the crucible for being preheating to 450 DEG C,
In the case where vacuum degree is the vacuum condition of 10.5kPa in 590 DEG C of melting 40min, medical magnesium alloy melt is obtained；By medical magnesium alloy
Melt overheats 150 DEG C, is subsequently placed in atomising device and is atomized, obtains medical magnesium alloy powder；Medical magnesium alloy powder is received
Collection, screening, packaging, obtain the Medical magnesium alloy material for 3D printing；The atomization is 2.1MPa with argon pressure；Argon gas
Reversely charging pressure is 0.5MPa.
The Medical magnesium alloy material for 3D printing prepared by the above method, burning point are 940 DEG C, and particle size range exists
40 ~ 110 μm, be in normal distribution, and pattern is spherical shape, can be used for 3D printing.
It should be noted that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting.Although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to the technology of invention
Scheme is modified or replaced equivalently, and without departing from the range of technical solution of the present invention, should all be covered in power of the invention
In sharp claimed range.
Claims (2)
1. a kind of preparation method for 3D printing Medical magnesium alloy material, which is characterized in that the preparation method includes as follows
Step:
1) ingredient
Take including pure magnesium, pure manganese, pure zinc, pure calcium, Mg-25wt%Fe intermediate alloy raw material, component quality percentage in raw material
Than as follows: 16wt%Fe, 3wt%Mn, 2wt%Zn, 3wt%Ca, surplus Mg；Degree of purity >=99.99%, Fe of the Mg it is pure
Degree >=99.99%；
2) baking material
The weighed all raw materials of step 1) are preheated 3 hours respectively at 240 DEG C；
3) melting
Pure magnesium, pure manganese, pure zinc and pure calcium after step 2) drying is put into the crucible for being preheating to 400 DEG C, coverture is added,
Melting under atmospheric conditions, smelting temperature are 680 DEG C；
After pure magnesium, pure manganese, pure zinc and pure calcium fusing after, melt temperature go up to be added 760 DEG C when be added Mg-25wt%Fe among
Alloy；
After Mg-25wt%Fe intermediate alloy all fusing, for stirring melt to uniform, refining agent is added to 740 DEG C in equilibrium temperature,
Refining 5min skims surface scum, pours into metal type dies, obtain medical magnesium alloy base material then at 740 DEG C of standing 10min；
The smelting technology is in SF6And CO2It is carried out under the conditions of mixed gas protected；
4) atomization prepares Medical magnesium alloy material
Medical magnesium alloy base material is put into the crucible for being preheating to 550 DEG C, in the case where vacuum degree is the vacuum condition of 1kPa in 680 DEG C
Melting 20min obtains medical magnesium alloy melt；
Medical magnesium alloy melt is overheated 250 DEG C, atomising device is subsequently placed in and is atomized, obtain medical magnesium alloy powder；
Medical magnesium alloy powder is collected, screening, packaging, obtains the Medical magnesium alloy material for 3D printing；
The atomization is 4MPa with argon pressure；The reversely charging pressure of argon gas is 1MPa.
2. a kind of doctor for 3D printing made from the preparation method of 3D printing Medical magnesium alloy material as described in claim 1
With application of the magnesium alloy materials in terms of medical 3D printing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710290585.9A CN107245618B (en) | 2017-04-28 | 2017-04-28 | It is a kind of for the preparation method of 3D printing Medical magnesium alloy material, material and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710290585.9A CN107245618B (en) | 2017-04-28 | 2017-04-28 | It is a kind of for the preparation method of 3D printing Medical magnesium alloy material, material and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107245618A CN107245618A (en) | 2017-10-13 |
| CN107245618B true CN107245618B (en) | 2019-06-25 |
Family
ID=60016900
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710290585.9A Active CN107245618B (en) | 2017-04-28 | 2017-04-28 | It is a kind of for the preparation method of 3D printing Medical magnesium alloy material, material and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107245618B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110669971A (en) * | 2019-07-23 | 2020-01-10 | 东莞理工学院 | Medical 3D printing magnesium alloy material and preparation method thereof |
| CN111155013B (en) * | 2020-02-08 | 2021-06-04 | 苏州轻金三维科技有限公司 | Medical three-dimensional printing alloy material and preparation method thereof |
| CN111250721A (en) * | 2020-03-09 | 2020-06-09 | 深圳市晶莱新材料科技有限公司 | Method for producing Fe-Mn-Pt-based medical 3D printing metal material |
| CN113388792B (en) * | 2021-06-29 | 2022-05-17 | 江西理工大学 | Biomedical amorphous magnesium alloy powder, composite material and preparation process |
| CN113564439A (en) * | 2021-07-07 | 2021-10-29 | 广东省人民医院 | Magnesium alloy powder for additive manufacturing and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392344A (en) * | 2008-11-06 | 2009-03-25 | 上海交通大学 | Degradable Mg-Mn-Zn-Ca mulit-element magnesium alloy material in organism |
| CN101575682A (en) * | 2009-06-04 | 2009-11-11 | 重庆大学 | Degradable biomedical complex magnesium alloy |
| CN101629260A (en) * | 2008-07-18 | 2010-01-20 | 中国科学院金属研究所 | Medical absorbable Mg-Zn-Mn-Ca magnesium alloy |
| CN104762541A (en) * | 2015-03-17 | 2015-07-08 | 华南协同创新研究院 | Rare earth magnesium-alloy material for 3D printing and preparation method of same |
-
2017
- 2017-04-28 CN CN201710290585.9A patent/CN107245618B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101629260A (en) * | 2008-07-18 | 2010-01-20 | 中国科学院金属研究所 | Medical absorbable Mg-Zn-Mn-Ca magnesium alloy |
| CN101392344A (en) * | 2008-11-06 | 2009-03-25 | 上海交通大学 | Degradable Mg-Mn-Zn-Ca mulit-element magnesium alloy material in organism |
| CN101575682A (en) * | 2009-06-04 | 2009-11-11 | 重庆大学 | Degradable biomedical complex magnesium alloy |
| CN104762541A (en) * | 2015-03-17 | 2015-07-08 | 华南协同创新研究院 | Rare earth magnesium-alloy material for 3D printing and preparation method of same |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107245618A (en) | 2017-10-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107245618B (en) | It is a kind of for the preparation method of 3D printing Medical magnesium alloy material, material and application | |
| Kargozar et al. | Chemistry of biomaterials: Future prospects | |
| WO2017084363A1 (en) | Medical degradable zn-cu-x alloy material and preparation method thereof | |
| CN103028149B (en) | Medical degradable Fe-Mg binary alloy material and preparation method thereof | |
| CN101015711B (en) | Medical implantation material capable of by degraded by body fluid and its preparing process | |
| WO2017028646A1 (en) | Biodegradable medical zinc-copper alloy and preparation method and use thereof | |
| CN106890356A (en) | A kind of degradable zinc-containing alloy implantation material and preparation method and application | |
| CN109022843B (en) | Medical implantable degradable composite bar and preparation method thereof | |
| CN104911427B (en) | A kind of Mg Ca Sr Zn systems magnesium alloy and preparation method and application | |
| CN111155013B (en) | Medical three-dimensional printing alloy material and preparation method thereof | |
| CN107190191B (en) | A kind of biological medical magnesium alloy and preparation method thereof | |
| CN1792383A (en) | Bio-absorbable Mg-Zn-Ca three-elements magnesium alloy material | |
| CN104762542B (en) | Biomedical degradable absorption Mg-Sr-Cu alloy material, preparation method and application | |
| CN107456601A (en) | A kind of Zn-Cu systems kirsite and preparation method and application | |
| CN107653410A (en) | Magnesium alloy that biological medical degradable absorbs and its preparation method and application | |
| WO2020042745A1 (en) | Mg-zn-sn series magnesium alloy with controllable degradation rate, preparation method and application thereof | |
| CN108057133A (en) | A kind of preparation method of the compound bone material of renewable magnesium-based | |
| CN103028148B (en) | Medical degradable Fe-Mg-X alloy material and preparation method thereof | |
| CN112870222A (en) | Vitamin C zinc-added sustained and controlled release tablet and preparation method thereof | |
| CN106606806B (en) | A kind of Zn-Mg1Ca system kirsite and the preparation method and application thereof | |
| CN102429927B (en) | Method for preparing ox gal stone | |
| CN103800290B (en) | Aminoglucose hydrochloride pellet preparations and preparation method thereof | |
| CN108641367A (en) | A kind of preparation method of antibacterial medical silicon rubber | |
| CN112410615A (en) | Biodegradable medical zinc-tin alloy, preparation method and application thereof | |
| CN103071158A (en) | Bone capsule shell with functions of supplying calcium and building strong bones and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |