CN104762541B - A kind of rare earth magnesium alloy material for 3D printing and preparation method thereof - Google Patents
A kind of rare earth magnesium alloy material for 3D printing and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of 3D printing material, discloses a kind of rare earth magnesium alloy material for 3D printing and preparation method thereof.Concretely comprise the following steps：Press element M g：Mn：The mass ratio 85～97 of RE：2～10：1～5 weighs raw material；Pure magnesium, manganese and magnesium alloy are put in the crucible of preheating, coverture, in atmospheric conditions melting is added；After changing clearly, Mg RE intermediate alloys and pure rare earth element is added, after dissolving, is stirred, is warming up to 700～750 DEG C；Refining agent, 2～25min of refine is added to stand, skimming operation is poured sand mold groove into, obtains magnesium-rare earth mother metal；Again by mother metal melting, atomization, rare earth magnesium alloy material is obtained.The alloy material has excellent fire-retardancy, and powder morphology, particle diameter are easily controllable；The material can melting under the conditions of unprotect gas, solve the problems, such as that atomization prepares magnesium alloy powder inflammable, can be used for laser 3D printing.
Description
Technical field
The invention belongs to the technical field of 3D printing material, and in particular to a kind of rare earth magnesium alloy material for 3D printing
And preparation method thereof.
Background technology
3D printing is one kind of Rapid Prototyping technique, it with powdery metal or plastics etc. can jointing material, by one
The multilamellar printing type of the another layer of layer, finally directly prints product, is formed " Digitized manufacturing ".Earliest 3D printing technique begins
In the U.S. of eighties of last century the eighties, but as material and machine are extremely expensive, 3D printer does not have large-scale business
With.Initially, 3D printing is often only used for the fields such as Making mold, industrial design, after be gradually available for Aero-Space, automobile and medical treatment etc.
Field.
Due to magnesium alloy have lightweight, high intensity, resistance to pressure, radiate good, be easy to casting and molding, therefore gradually
Replace plastic material, become the advanced material in market.Magnesium alloy and 3D printing technique are combined service metal worker
Industry, can promote manufacturing industry to develop to inexpensive, short cycle, high efficiency direction.3D printing metal dust typically requires degree of purity
High, spherical read, narrow diameter distribution, oxygen content low.Raw material metal for 3D printing is more special, it has to be possible to liquefy,
Powdered, while can be bondd again in print procedure again, and with the physics and chemical property for meeting demand.
Metal dust currently used for 3D printing mainly has titanium alloy, cochrome, rustless steel and aluminum alloy materials etc., magnesium
Because its chemical property is active and inflammability, powder prepares difficult alloy, is also in experimental stage, is not widely applied to 3D printing
In field.The conventional method for preparing magnesium alloy powder is ball-milling method at present.But ball-milling method increases impurity because power consumption is high, easily.
Content of the invention
In order to overcome the primary and foremost purpose of the shortcoming and defect of prior art, the present invention to be that offer is a kind of dilute for 3D printing
The preparation method of native magnesium alloy materials.The present invention prepares magnesium-rare earth powder, the powder burning-point height of preparation, shape using atomization
Looks, particle diameter are easily controllable, and preparation process free from admixture adds, and compensate for the deficiency of ball-milling method.
Another object of the present invention is to provide by above-mentioned preparation method prepare for 3D printing magnesium-rare earth
Material.
It is still another object of the present invention to provide the above-mentioned application for 3D printing rare earth magnesium alloy material.
A kind of preparation method for 3D printing rare earth magnesium alloy material, specifically includes following steps：
(1) dispensing
The mass ratio for pressing component is Mg：Mn：RE=85～97：2～10：1～5 weighs raw material；Described raw material bag
Include magnesium alloy, pure magnesium, manganese, Mg-RE intermediate alloys and pure rare earth element；
(2) melting
Pure magnesium, manganese and magnesium alloy that step (1) is weighed are put in the crucible of preheating, coverture is added, in atmospheric condition
Lower melting, the temperature of melting is 400～600 DEG C；After pure magnesium, manganese and magnesium alloy wholeization are clear, add Mg-RE intermediate alloys and
Pure rare earth element；After pure rare earth element and Mg-RE intermediate alloys all dissolve, stirring liquation is continuously heating to 700 to uniform
～750 DEG C；Refining agent, 2～25min of refine is added to stand 5～25min then at 700～750 DEG C, skimming operation pours sand mold into
Groove, obtains magnesium-rare earth mother metal；
(3) atomization prepares rare earth magnesium alloy material
Magnesium-rare earth mother metal is put in the crucible of preheating, under vacuum in 450～550 DEG C of meltings 15～
30min, obtains magnesium-rare earth liquid；By 100～200 DEG C of magnesium-rare earth liquid superheat, being subsequently placed in atomising device is carried out
Atomization, obtains magnesium-rare earth powder；Magnesium-rare earth powder collected, is sieved, closing batch packaging, being obtained for the dilute of 3D printing
Native magnesium alloy materials.
Magnesium alloy described in step (1) is MB1 (the domestic trade mark), MB2 (the domestic trade mark), MB3 (the domestic trade mark), MB8 (states
One or more of the interior trade mark) or ZM5 (the domestic trade mark)；It is preferred that MB1.
Described in step (1), the content of Mg-RE intermediate alloy rare earth elements is not zero；The Mg-RE intermediate alloys are
MB8 (the domestic trade mark)；The RE is that rare earth element is one or more of Y, Ce, Nd or Gd；It is preferred that Y, Ce or Nd.
Pure rare earth element described in step (1) is one or more of Y, Ce, Nd or Gd；It is preferred that Y, Ce or Nd.
The temperature of the preheating of crucible described in step (2) is 400～550 DEG C.
Coverture consumption described in step (2) is that raw material (is closed in the middle of pure magnesium, manganese, magnesium alloy, Mg-RE described in step (1)
Gold and pure rare earth element) gross weight 1～2%；Generally determined with the covering precision of molten surface, molten surface should be protected
Hold 2.5～10 millimeters of coating.
Refining agent consumption described in step (2) is that raw material (is closed in the middle of pure magnesium, manganese, magnesium alloy, Mg-RE described in step (1)
Gold and pure rare earth element) gross weight 2～3%.
Crucible described in step (3) preheating temperature be：400～500 DEG C.
Atomization argon pressure described in step (3) is 0.5～3.5MPa；The reversely charging pressure of argon is 0.1～0.5MPa.
Compared with prior art, the invention has the advantages that and beneficial effect：
(1) micron order rare earth magnesium alloy material prepared by the present invention has excellent fire-retardancy, and particle diameter is in normal distribution, group
Knit that crystal grain is tiny, contactless with air in atomization process, oxygen-containing low, can be used for laser 3D printing；And the magnesium-rare earth material
Material can pass through to adjust materialization state modulator powder morphology, particle diameter distribution；
(2) present invention is prepared for rare earth magnesium alloy material using the method for melting and atomization, and melting ensure that magnesium base alloy
Into being grouped into, atomization meets requirement of the 3D printing to metal dust；
(3) rare earth magnesium alloy material burning-point prepared by the present invention brings up to 950 DEG C, can be melted under the conditions of unprotect gas
Refining, solves the problems, such as that atomization prepares magnesium alloy powder inflammable.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
Embodiment 1
(1) raw material：Mass ratio according to element is Mg：Mn：Y=85：10：(Mn's is flat for the 5 magnesium alloy MB1 for weighing 4337g
Equal content：1.9%, Mg are surplus), the pure manganese of 413g, the common 5Kg of pure rare earth element Y of 250g；
(2) crucible is preheated to 400 DEG C in resistance furnace, the pure manganese weighed in step (1) and magnesium alloy MB1 is poured into earthenware
In crucible, while being sprinkled into 1% of raw material gross weight described in step (1) coverture RJ-2 in crucible, (circle in the air Aluminum for Xuzhou City
Company limited), in atmospheric conditions in 500 DEG C of meltings, after pure manganese and magnesium alloy MB1 wholeization are clear, add pure rare earth element
Y, after pure rare earth element Y all dissolves, stirring liquation is continuously heating to 700 DEG C to uniform, adds former described in step (1)
The 2% refining agent FX-MJ (Aluminum company limited of circling in the air) of weight in material, refine 10 minutes finally maintains the temperature at 700 DEG C, quiet
Put 15 minutes, skimming operation pours sand mold groove into, becomes magnesium-rare earth mother metal；
(3) atomization prepares rare earth magnesium alloy material
Rare earth magnesium alloy material is prepared using the conventional atomization system device of tradition, step is as follows：
Magnesium-rare earth mother metal is put in the crucible having been warmed up (preheating temperature of crucible is 400 DEG C), in vacuum bar
In 450 DEG C of meltings 25 minutes under part, the degree of superheat is then controlled for 100 DEG C, obtain magnesium-rare earth liquid；By magnesium-rare earth liquid
Body is poured in the funnel of aerochamber, is atomized, and obtains magnesium-rare earth powder；By magnesium-rare earth powder through collecting, sieving
Divide, close batch packaging process, obtain the rare earth magnesium alloy material for 3D printing；The atomization argon pressure is 0.5MPa；Argon
Reversely charging pressure be 0.1Mpa.
The rare earth magnesium alloy material for 3D printing prepared by said method, its burning-point are 850 DEG C, and particle size range exists
1～30 μm, in normal distribution, pattern is spherical, can be used for laser 3D printing.
Embodiment 2
(1) raw material：Mass ratio according to element is Mg：Mn：Nd=90：7：3 to weigh 4592g magnesium alloy MB1,258g pure
The common 5Kg of the pure Nd of manganese, 150g；
(2) crucible is preheated to 450 DEG C in resistance furnace, the pure manganese weighed in step (1) and magnesium alloy MB1 is poured into earthenware
In crucible, while being sprinkled into the coverture RJ-2 of 1.5% of raw material gross weight described in step (1) in crucible, (Aluminum that circles in the air is limited
Company), in atmospheric conditions in 550 DEG C of meltings, after pure manganese and magnesium alloy MB1 wholeization are clear, pure rare earth element Nd are added, is treated
After pure rare earth element all dissolves, stirring liquation is continuously heating to 730 DEG C to uniform, adds heavy in raw material described in step (1)
The 2.5% refining agent FX-MJ (Aluminum company limited of circling in the air) of amount, refine 10 minutes finally maintain the temperature at 730 DEG C, stand 15
Minute, skimming operation is poured sand mold groove into, becomes magnesium-rare earth mother metal；
(3) atomization prepares magnesium alloy powder
It is prepared using its conventional atomization system device of tradition, step is as follows：
Magnesium-rare earth mother metal is put in the crucible having been warmed up (preheating temperature of crucible is 450 DEG C), in vacuum bar
In 500 DEG C of meltings 20 minutes under part, the degree of superheat is then controlled for 150 DEG C, obtain magnesium-rare earth liquid；By magnesium-rare earth liquid
Body is poured in the funnel of aerochamber, is atomized, and obtains magnesium-rare earth powder；By magnesium-rare earth powder through collecting, sieving
Divide, close batch packaging process, obtain the rare earth magnesium alloy material for 3D printing；The atomization argon pressure is 1.5MPa；Argon
Reversely charging pressure be 0.3Mpa.
The rare earth magnesium alloy material for 3D printing prepared by said method, 900 DEG C of its burning-point, particle size range is 8
～50 μm, journey normal distribution, pattern are spherical, can be used for laser 3D printing.
Embodiment 3
(1) raw material：Mass ratio according to element is Mg：Mn：Ce=97：2：1 weighs 4949g magnesium alloy MB8 (Mn:
1.75%, Ce:0.25%, Mg:Surplus), the pure manganese of 13.4g and the common 5Kg of the pure Ce of 37.6g；
(2) crucible is preheated to 450 DEG C in resistance furnace, the pure manganese weighed in step (1) and magnesium alloy MB8 is poured into earthenware
In crucible, while be sprinkled into 2% of raw material gross weight described in step (1) coverture RJ-2 in crucible, in atmospheric conditions in
550 DEG C of meltings, after pure manganese and magnesium alloy MB8 wholeization are clear, add pure rare earth Elements C e, treat that pure rare earth Elements C e is all dissolved
Afterwards, stirring liquation is continuously heating to 750 DEG C to uniform, adds 3% refining agent FX-MJ of weight in raw material described in step (1)
(Aluminum company limited of circling in the air), refine 10 minutes finally maintain the temperature at 750 DEG C, stand 15 minutes, and skimming operation pours sand into
Type groove, becomes magnesium-rare earth mother metal；
(3) atomization prepares rare earth magnesium alloy material
Rare earth magnesium alloy material is prepared using the conventional atomization system device of tradition, step is as follows：
Magnesium-rare earth mother metal is put in the crucible having been warmed up (preheating temperature of crucible is 500 DEG C), in vacuum bar
In 550 DEG C of meltings 20 minutes under part, the degree of superheat is then controlled for 200 DEG C, obtain magnesium-rare earth liquid；By magnesium-rare earth liquid
Body is poured in the funnel of aerochamber, is atomized, and obtains magnesium-rare earth powder；By magnesium-rare earth powder through collecting, sieving
Divide, close batch packaging process, obtain the rare earth magnesium alloy material for 3D printing；The atomization argon pressure is 3.5MPa；Argon
Reversely charging pressure be 0.5Mpa.
The rare earth magnesium alloy material for 3D printing prepared by said method, its burning-point are 950 DEG C, and particle size range exists
30～100 μm, in normal distribution, pattern is spherical, can be used for laser 3D printing.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, other any spirit without departing from the present invention and the change, modification, replacement that is made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (9)
1. a kind of preparation method for 3D printing rare earth magnesium alloy material, it is characterised in that：Specifically include following steps：
(1) dispensing
The mass ratio for pressing component is Mg：Mn：RE=85～97：2～10：1～5 weighs raw material；Described raw material includes magnesium
Alloy, pure magnesium, manganese, Mg-RE intermediate alloys and pure rare earth element；
(2) melting
Pure magnesium, manganese and magnesium alloy that step (1) is weighed are put in the crucible having been warmed up, coverture is added, in atmospheric condition
Lower melting, the temperature of melting is 400～600 DEG C；After pure magnesium, manganese and magnesium alloy wholeization are clear, add Mg-RE intermediate alloys and
Pure rare earth element；After pure rare earth element and Mg-RE intermediate alloys all dissolve, stirring liquation is continuously heating to 700 to uniform
～750 DEG C；Refining agent, 2～25min of refine is added to stand 5～25min then at 700～750 DEG C, skimming operation pours sand mold into
Groove, obtains magnesium-rare earth mother metal；
(3) atomization prepares rare earth magnesium alloy material
Magnesium-rare earth mother metal is put in the crucible of preheating, under vacuum in 450～550 DEG C of 15～30min of melting, is obtained
Arrive magnesium-rare earth liquid；By 100～200 DEG C of magnesium-rare earth liquid superheat, it is subsequently placed in atomising device and is atomized, obtain
Magnesium-rare earth powder；Magnesium-rare earth powder collected, is sieved, closing batch packaging, obtaining the magnesium-rare earth for 3D printing
Material.
2. the preparation method of 3D printing rare earth magnesium alloy material is used for according to claim 1, it is characterised in that：Step (1)
Described in magnesium alloy be MB1, MB2, MB3, MB8 or ZM5 in one or more.
3. the preparation method of 3D printing rare earth magnesium alloy material is used for according to claim 1, it is characterised in that：Step (1)
Described in the weight/mass percentage composition of Mg-RE intermediate alloy rare earth elements be not zero, wherein RE be rare earth element for Y, Ce, Nd or
Gd.
4. the preparation method of 3D printing rare earth magnesium alloy material is used for according to claim 1, it is characterised in that：Step (1)
Described in pure rare earth element be one or more of Y, Ce, Nd or Gd.
5. the preparation method of 3D printing rare earth magnesium alloy material is used for according to claim 1, it is characterised in that：Step (2)
Described in crucible preheating temperature be 400～550 DEG C；Refining agent consumption described in step (2) is that raw material is total described in step (1)
The 2～3% of weight.
6. the preparation method of 3D printing rare earth magnesium alloy material is used for according to claim 1, it is characterised in that：Step (2)
Described in coverture consumption be step (1) described in raw material gross weight 1～2%.
7. the preparation method of 3D printing rare earth magnesium alloy material is used for according to claim 1, it is characterised in that：Step (3)
Described in crucible preheating temperature be：400～500 DEG C；
Atomization argon pressure described in step (3) is 0.5～3.5MPa；The reversely charging pressure of argon is 0.1～0.5MPa.
8. a kind of preparation method described in any one of claim 1～7 prepare for 3D printing rare earth magnesium alloy material.
9. the application of 3D printing rare earth magnesium alloy material is used for according to claim 8, it is characterised in that：The rare earth magnesium is closed
Golden material is used for the technical field of 3D printing.
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| CN105251999A (en) * | 2015-09-06 | 2016-01-20 | 航星利华(北京)科技有限公司 | Method for preparing rare earth reinforced equiaxial fine-crystal part through high-energy beam metal 3D printing |
| CN107245618B (en) * | 2017-04-28 | 2019-06-25 | 苏州轻金三维科技有限公司 | It is a kind of for the preparation method of 3D printing Medical magnesium alloy material, material and application |
| CN107096924A (en) * | 2017-05-17 | 2017-08-29 | 中国科学院重庆绿色智能技术研究院 | The preparation method and product of a kind of spherical metal base rare earth nano composite powder available for 3 D-printing |
| JP7194904B2 (en) * | 2017-09-21 | 2022-12-23 | 株式会社戸畑製作所 | magnesium alloy powder |
| CN110681869B (en) * | 2019-10-15 | 2021-08-03 | 上海交通大学 | Method for preparing high-strength and high-toughness magnesium rare earth alloy by selective laser melting additive manufacturing technology |
| CN111172442B (en) * | 2020-01-09 | 2021-05-25 | 西安建筑科技大学 | Rare earth magnesium alloy powder for 3D printing and preparation method thereof |
| CN111155015B (en) * | 2020-02-08 | 2021-06-25 | 苏州轻金三维科技有限公司 | High-plasticity light alloy for three-dimensional printing and preparation method thereof |
| CN112387978B (en) * | 2020-10-21 | 2023-03-14 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of CuFe alloy powder for brake pad |
| CN115156525B (en) * | 2022-06-22 | 2023-04-04 | 广东省科学院新材料研究所 | Active modification spherical magnesium alloy powder based on electrostatic self-assembly and preparation method and application thereof |
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