CN111349809B - Preparation method and application of magnesium alloy additive manufacturing wire containing three-dimensional network graphene - Google Patents
Preparation method and application of magnesium alloy additive manufacturing wire containing three-dimensional network graphene Download PDFInfo
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- CN111349809B CN111349809B CN202010229848.7A CN202010229848A CN111349809B CN 111349809 B CN111349809 B CN 111349809B CN 202010229848 A CN202010229848 A CN 202010229848A CN 111349809 B CN111349809 B CN 111349809B
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 84
- 239000000654 additive Substances 0.000 title claims abstract description 61
- 230000000996 additive effect Effects 0.000 title claims abstract description 61
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 60
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000005266 casting Methods 0.000 claims abstract description 14
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 14
- 239000011777 magnesium Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001125 extrusion Methods 0.000 claims description 34
- 239000007787 solid Substances 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 10
- 238000010622 cold drawing Methods 0.000 claims description 9
- 229910045601 alloy Inorganic materials 0.000 claims description 8
- 239000000956 alloy Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000003754 machining Methods 0.000 claims description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 5
- 239000001569 carbon dioxide Substances 0.000 claims description 5
- 238000010894 electron beam technology Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 2
- 239000007769 metal material Substances 0.000 abstract description 2
- 238000004891 communication Methods 0.000 description 5
- 239000000155 melt Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000010146 3D printing Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- PGTXKIZLOWULDJ-UHFFFAOYSA-N [Mg].[Zn] Chemical compound [Mg].[Zn] PGTXKIZLOWULDJ-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
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- 238000005325 percolation Methods 0.000 description 1
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- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
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- 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
- C22C1/10—Alloys containing non-metals
- C22C1/1031—Alloys containing non-metals starting from gaseous compounds or vapours of at least one of the constituents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C23/00—Extruding metal; Impact extrusion
- B21C23/02—Making uncoated products
-
- 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
- C22C23/00—Alloys based on magnesium
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
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- Extrusion Of Metal (AREA)
Abstract
A preparation method and application of a magnesium alloy additive manufacturing wire containing three-dimensional network graphene relate to a preparation method and application of a magnesium alloy additive manufacturing wire. In order to solve the problem that the forming capability is influenced due to the fact that a molten pool is unstable due to too low viscosity of magnesium and magnesium alloy in the additive manufacturing process, the magnesium alloy is heated in a crucible, graphene with a certain content is generated in a magnesium alloy melt by an in-situ preparation process or a stirring casting method, and when the volume fraction of the graphene is high enough, the graphene forms a cross-linked three-dimensional network structure in the material. And extruding or drawing the composite material cast ingot into an additive manufacturing wire material with a required diameter. The method is a novel magnesium alloy additive manufacturing wire material which has simple process and low cost and can be applied to large-scale industrial manufacturing. The invention is applied to the field of manufacture of non-ferrous metal materials.
Description
Technical Field
The invention relates to the field of non-ferrous metal material manufacturing, in particular to a preparation method and application of a wire for magnesium alloy additive manufacturing.
Background
The magnesium alloy has the advantages of low density, high specific strength, good biocompatibility and the like, and has wide application prospect in the industries of automobiles, aerospace and medical use. When the magnesium alloy is formed in a complex shape, because of the close-packed hexagonal crystal structure of the magnesium alloy, less sliding systems which can independently start at room temperature are generated, and the plastic deformation capability of the magnesium alloy is poor. Additive manufacturing techniques can solve this problem well. However, due to the active chemical nature of magnesium and the relatively high vapor pressure, additive manufacturing using magnesium powder presents a high risk of safety accidents. Thus additive manufacturing using wire is a good choice. However, the current alloying method is difficult to change the fluidity of the magnesium alloy melt, which results in poor stability of the molten pool during additive manufacturing and rapid evaporation of magnesium element. And the problem can be effectively solved by adopting the graphene to form a three-dimensional network in the magnesium alloy. Therefore, in order to improve the forming capability in the magnesium alloy additive manufacturing process, the development of a novel magnesium alloy additive manufacturing wire material has great practical significance.
Disclosure of Invention
According to the invention, the three-dimensional network is formed in the magnesium alloy, and the existence of the three-dimensional network can change the flow characteristic of the magnesium alloy melt, so that the problem of poor stability of a molten pool in the additive manufacturing process is solved, and the formability of a complex component in the additive manufacturing process is ensured; meanwhile, the existence of the graphene can effectively limit the growth of crystal grains, and the mechanical property of the additive manufacturing material is improved. The invention provides a preparation method of a magnesium alloy additive manufacturing wire material, which can solve the problems, and the method is a novel wire material which has simple process and low cost and can be applied to large-scale industrial production and magnesium alloy additive manufacturing.
The invention discloses a preparation method of a magnesium alloy additive manufacturing wire containing three-dimensional network graphene, which comprises the following steps:
firstly, selecting a magnesium alloy system, and heating and melting the alloy at a temperature which is 30-100 ℃ higher than the melting point of the alloy;
secondly, adjusting the temperature of the magnesium melt to be within the range of 640-700 ℃, and adjusting the flow rate of CO to be 0.1-5L/min2Introducing gas into the magnesium alloy melt, keeping the temperature stable in the process, converting carbon dioxide into graphene, and ensuring that the content of the graphene in the magnesium alloy is 1-10 wt.%, so as to obtain a semi-solid composite melt;
thirdly, casting the composite melt with the semi-solid characteristic obtained in the second step to obtain a composite material ingot with three-dimensional communicated graphene;
and fourthly, machining the composite material ingot which is obtained in the third step and is in three-dimensional communication with the graphene, and obtaining the magnesium alloy wire through direct extrusion or extrusion and drawing deformation.
The magnesium alloy additive manufacturing wire containing the three-dimensional network graphene is prepared by the method and is used as a raw material for magnesium alloy additive manufacturing.
The invention has the following advantages:
according to the wire material manufactured by the additive manufacturing method, as the graphene is generated in situ in the magnesium melt, when the content of the graphene reaches a percolation threshold value in the magnesium alloy (in the colloid science, when the content of a nano phase in a solution is lower than a certain critical value, the solution shows a sol characteristic, and has fluidity, and when the content of the nano phase in the solution exceeds the critical value, the solution is converted into a semisolid gel characteristic without fluidity), the property of magnesium in a molten state can be changed, so that the magnesium in the molten state is converted into the semisolid without fluidity from a liquid in a high-fluidity state, and when the wire material is used for 3D printing, the instability of a molten pool caused by the overlarge fluidity can be avoided, and the forming in the 3D printing process is facilitated. Meanwhile, due to the existence of the graphene, the growth of crystal grains in the solidification process of a molten pool can be effectively inhibited, so that the additive manufacturing component with good mechanical property can be obtained. In addition, the wire can be produced in batch by using traditional equipment, and has great practical significance.
The key point of the preparation method is that a graphene network structure with a three-dimensional network is prepared in magnesium in situ by utilizing a magnesium thermal reaction, and a molten pool of the wire can be successfully formed due to no fluidity when the wire is subjected to additive manufacturing only when the content of graphene exceeds a certain specific value.
Drawings
FIG. 1 is a melt state with semi-solid characteristics and containing three-dimensional network graphene;
FIG. 2 is a drawing of a material object of the fine magnesium alloy additive manufactured wire;
FIG. 3 optical microstructure of magnesium alloy additive manufactured wire;
FIG. 4 SEM picture of magnesium alloy additive manufacturing wire material;
FIG. 5 is a stress-strain tensile curve of a magnesium alloy additive manufactured wire;
FIG. 6 is a schematic diagram of an additive manufacturing process of an electron beam fuse deposition process for magnesium alloy wire; wherein, the picture (a) is a graphene-free object picture, and the picture (b) is an object picture containing three-dimensional network graphene.
Detailed Description
The first embodiment is as follows: the preparation method of the magnesium alloy additive manufacturing wire containing the three-dimensional network graphene comprises the following steps:
firstly, selecting a magnesium alloy system, and heating and melting the alloy at a temperature which is 30-100 ℃ higher than the melting point of the alloy;
secondly, adjusting the temperature of the magnesium melt to be within the range of 640-700 ℃, and adjusting the flow rate of CO to be 0.1-5L/min2Introducing gas into the magnesium alloy melt, keeping the temperature stable in the process, converting carbon dioxide into graphene, and ensuring that the graphene keeps high content (1-10 wt.%) in the magnesium alloy in order to form a cross-linked three-dimensional network structure in the material, so that the magnesium alloy melt has the characteristics of liquid state, semisolid state and gel;
thirdly, casting the composite melt with the semi-solid characteristic obtained in the second step to obtain a composite material ingot with three-dimensional communicated graphene;
and fourthly, machining the composite material ingot which is obtained in the third step and is in three-dimensional communication with the graphene, and obtaining the magnesium alloy wire through direct extrusion or extrusion and drawing deformation.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the alloy elements in the magnesium alloy system are aluminum, zinc, calcium, manganese, copper or zirconium. The rest is the same as the first embodiment.
The third concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the magnesium alloy is ZK61 magnesium alloy. The rest is the same as the first embodiment.
The fourth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the pressure casting in the third step is direct stirring casting or ultrasonic auxiliary stirring casting. The rest is the same as the first embodiment.
The fifth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the extrusion temperature of the four steps is 200-500 ℃, and the extrusion ratio is 70: 1. The rest is the same as the first embodiment.
The sixth specific implementation mode: the first difference between the present embodiment and the specific embodiment is: the four steps of obtaining the magnesium alloy wire through extrusion and drawing deformation are carried out in two steps: firstly, when a cast ingot is extruded, the extrusion temperature is 400 ℃, the extrusion ratio is 10:1, and an extruded bar with the diameter of phi 15 is obtained; and secondly, carrying out 5-pass cold drawing on the extruded bar to obtain the additive manufacturing wire with the diameter phi 2. The rest is the same as the first embodiment.
The seventh embodiment: the first difference between the present embodiment and the specific embodiment is: the four steps of obtaining the magnesium alloy wire through extrusion and drawing deformation are carried out in two steps: firstly, when a cast ingot is extruded, the extrusion temperature is 400 ℃, the extrusion ratio is 10:1, and an extruded bar with the diameter of 15 is obtained; secondly, the extruded bar is subjected to 10-pass cold drawing to obtain the additive manufacturing wire with the diameter phi of 1.2. The rest is the same as the first embodiment.
The specific implementation mode is eight: the first difference between the present embodiment and the specific embodiment is: the magnesium alloy wire obtained by extrusion and drawing deformation is processed in the following way: and (3) directly processing the composite material ingot with three-dimensional communicated graphene into a phi 15 bar, and performing cold drawing on the as-cast bar for 10 times to obtain the additive manufacturing wire material with the diameter phi 1.2. The rest is the same as the first embodiment.
The specific implementation method nine: the first difference between the present embodiment and the specific embodiment is: the magnesium alloy wire obtained by extrusion and drawing deformation is processed in the following way: firstly, when the cast ingot is extruded, the extrusion temperature is 400 ℃, the extrusion ratio is 10:1, an extruded bar with the diameter of phi 10 is obtained, and the extruded bar is subjected to 5-pass cold drawing, so that the additive manufacturing wire with the diameter of phi 1.2 is obtained. The rest is the same as the first embodiment.
The specific implementation mode is ten: the application of the magnesium alloy additive manufacturing wire containing the three-dimensional network graphene is used as a raw material for magnesium alloy additive manufacturing.
The beneficial effects of the present invention are demonstrated by the following examples:
example 1
The preparation method of the magnesium alloy additive manufacturing wire containing the three-dimensional network graphene comprises the following steps:
firstly, heating and melting AZ31 magnesium alloy at 720 ℃;
secondly, cooling the melt to 680 ℃, and controlling the flow rate to be 1L/minCO2Gas is introduced into the magnesium alloy melt, carbon dioxide is converted into graphene, the graphene with the content of 1 wt.% is generated in magnesium, the graphene forms a mutually-crosslinked three-dimensional network structure in the material, and the magnesium alloy is converted into a semi-solid state from fluid.
And thirdly, performing pressure casting on the composite melt with the semi-solid characteristic obtained by the reaction in the step two to obtain the graphene three-dimensionally communicated composite material ingot.
Fourthly, machining the composite material cast ingot containing the three-dimensional communication obtained in the third step, and extruding the cast ingot into phi 3 wire materials at the temperature of 450 ℃ and the extrusion ratio of 90: 1.
And fifthly, carrying out acid washing and polishing treatment on the extruded wire to obtain the additive manufacturing wire which is clean and smooth in surface.
The melt state of the three-dimensional network graphene-containing prepared by the embodiment is shown in fig. 1. The metal nut can stably exist on the upper part of the magnesium melt in a molten state at 60 ℃ higher than the melting point, and the melt shows semi-solid characteristics.
An additive manufacturing wire material object of the fine grain magnesium alloy prepared in this example is shown in fig. 2. The surface is clean and smooth, and the state is excellent.
Example 2:
the preparation method of the magnesium alloy additive manufacturing wire containing the three-dimensional network graphene comprises the following steps:
firstly, heating and melting ZK60 magnesium alloy at 720 ℃;
and secondly, preparing the composite material with the graphene content of 2 wt.% by utilizing an ultrasonic-assisted stirring casting process, wherein the graphene forms a three-dimensional communicated structure and can also keep a semi-solid characteristic above a melting point.
And thirdly, performing pressure casting on the composite melt with the semi-solid characteristic obtained by the reaction in the step two to obtain the graphene three-dimensionally communicated composite material ingot.
Fourthly, machining the composite material cast ingot containing the three-dimensional communication obtained in the third step, and extruding the cast ingot into phi 2 wire materials at the temperature of 450 ℃ and the extrusion ratio of 90: 1.
And fifthly, carrying out acid washing and polishing treatment on the extruded wire to obtain the additive manufacturing wire which is clean and smooth in surface.
FIG. 3 is an SEM image of a magnesium alloy additive manufacturing wire prepared in the embodiment, and it can be seen that graphene is well dispersed in a magnesium alloy matrix to form a three-dimensional network structure.
Example 3:
the preparation method of the magnesium alloy additive manufacturing wire containing the three-dimensional network graphene comprises the following steps:
firstly, heating and melting ZK60 magnesium alloy at 720 ℃;
secondly, cooling the melt to 680 ℃, and controlling the flow rate to be 1L/minCO2Introducing gas into the magnesium alloy melt, converting carbon dioxide into graphene, generating graphene with the content of 1.5 wt.% in magnesium, and enabling the graphene to form a cross-linked three-dimensional network structure in the material, so that the magnesium alloy is converted into a semi-solid state from a fluid.
And thirdly, performing pressure casting on the composite melt with the semi-solid characteristic obtained by the reaction in the step two to obtain the graphene three-dimensionally communicated composite material ingot.
Fourthly, machining the composite material cast ingot containing the three-dimensional communication obtained in the third step, extruding the cast ingot into a bar material with phi 15 under the condition that the temperature is 400 ℃ and the extrusion ratio is 12:1, and drawing the bar material into a wire material with phi 1.5 through 8-pass cold-drawing crystal extrusion.
And fifthly, carrying out acid washing and polishing treatment on the extruded wire to obtain the additive manufacturing wire which is clean and smooth in surface.
And sixthly, performing electron beam fuse deposition on the extruded wire, wherein the wire feeding speed is 2500mm/min, and the beam current is 22mA, and performing single-pass layer-by-layer printing.
FIG. 4 is an optical microscopic image of the magnesium alloy additive manufacturing wire prepared in this example, which shows that the grain size of the wire is in the micrometer scale due to the existence of graphene.
FIG. 5 shows the mechanical properties of the magnesium alloy additive manufactured wire prepared in this example, it can be seen that the yield strength exceeds 200MPa, the tensile strength exceeds 300MPa, and the elongation exceeds 20% because the wire has higher mechanical properties.
FIG. 6 is a single pass additive manufacturing profile of magnesium-zinc wire, where it can be seen that the graphene-free wire of FIG. 6(a) is difficult to print and form, while the wire of FIG. 6(b) has been successfully formed after the addition of graphene.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
The present invention is not limited to the above description of the embodiments, and those skilled in the art should, in light of the present disclosure, appreciate that many changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (8)
1. A preparation method of a magnesium alloy additive manufacturing wire containing three-dimensional network graphene is characterized by comprising the following steps:
firstly, selecting a magnesium alloy system, and heating and melting the alloy at a temperature which is 30-100 ℃ higher than the melting point of the alloy;
secondly, adjusting the temperature of the magnesium melt to be within the range of 640-700 ℃, and adjusting the flow rate of CO to be 0.1-5L/min2Introducing gas into the magnesium alloy melt, keeping the temperature stable in the process, converting carbon dioxide into graphene, and ensuring that the content of the graphene in the magnesium alloy is 1-10 wt.%, so as to obtain a semi-solid composite melt;
thirdly, casting the composite melt with the semi-solid characteristic obtained in the second step to obtain a composite material ingot with three-dimensional communicated graphene;
fourthly, machining the composite material ingot with the three-dimensional communicated graphene obtained in the third step, and obtaining a magnesium alloy wire through direct extrusion or extrusion and drawing deformation; the direct extrusion temperature in the fourth step is 200-500 ℃, and the extrusion ratio is 70: 1; in the fourth step, the magnesium alloy wire obtained by extrusion and drawing deformation is carried out in two steps: firstly, when a cast ingot is extruded, the extrusion temperature is 400 ℃, the extrusion ratio is 10:1, and an extruded bar with the diameter of 15 is obtained; secondly, the extruded rod is subjected to 10-pass cold drawing to obtain the additive manufacturing wire with the diameter phi of 1.2.
2. The method for preparing the magnesium alloy additive manufacturing wire containing the three-dimensional network graphene according to claim 1, wherein alloy elements in a magnesium alloy system are aluminum, zinc, calcium, manganese, copper or zirconium.
3. The method for preparing the magnesium alloy additive manufacturing wire containing the three-dimensional network graphene according to the claim 1 or 2, wherein the magnesium alloy is ZK61 magnesium alloy.
4. The method for preparing the magnesium alloy additive manufacturing wire containing the three-dimensional network graphene according to the claim 1, wherein the casting in the step three is direct stirring casting or ultrasonic-assisted stirring casting.
5. The method for preparing the magnesium alloy additive manufacturing wire containing the three-dimensional network graphene according to claim 1, wherein the four steps of obtaining the magnesium alloy wire through extrusion and drawing deformation are carried out in two steps: firstly, when a cast ingot is extruded, the extrusion temperature is 400 ℃, the extrusion ratio is 10:1, and an extruded bar with the diameter of 15 is obtained; and secondly, carrying out 5-pass cold drawing on the extruded bar to obtain the additive manufacturing wire with the diameter phi 2.
6. The method for preparing the magnesium alloy additive manufacturing wire containing the three-dimensional network graphene according to the claim 1, wherein the four steps of obtaining the magnesium alloy wire through extrusion and drawing deformation are carried out in the following modes: and (3) directly processing the composite material ingot with three-dimensional communicated graphene into a phi 15 bar, and performing cold drawing on the as-cast bar for 10 times to obtain the additive manufacturing wire material with the diameter phi 1.2.
7. The method for preparing the magnesium alloy additive manufacturing wire containing the three-dimensional network graphene according to the claim 1, wherein the four steps of obtaining the magnesium alloy wire through extrusion and drawing deformation are carried out in the following modes: firstly, when the cast ingot is extruded, the extrusion temperature is 400 ℃, the extrusion ratio is 10:1, an extruded bar with the diameter of phi 10 is obtained, and the extruded bar is subjected to 5-pass cold drawing, so that the additive manufacturing wire with the diameter of phi 1.2 is obtained.
8. Use of a magnesium alloy additive manufacturing wire containing three-dimensional network graphene as prepared according to claim 1, which is used as a raw material for magnesium alloy electron beam fuse deposition additive manufacturing.
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CN109518028A (en) * | 2018-12-19 | 2019-03-26 | 昆明理工大学 | A kind of preparation method of graphene enhancing magnesium-based composite material |
CN110306086A (en) * | 2019-06-26 | 2019-10-08 | 哈尔滨理工大学 | A kind of corrosion resistant Mg-Zn-Ca-Sn biological medical magnesium alloy preparation method of novel multiple |
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CN102583357A (en) * | 2012-03-26 | 2012-07-18 | 方大炭素新材料科技股份有限公司 | Method for preparing graphene from limestone |
CN103184397A (en) * | 2013-04-25 | 2013-07-03 | 东南大学 | Preparation method of magnesium alloy wire based on severe plastic deformation |
CN109207787A (en) * | 2018-11-22 | 2019-01-15 | 哈尔滨工业大学 | A kind of preparation method of in-situ authigenic graphene enhancing magnesium-based composite material |
CN109518028A (en) * | 2018-12-19 | 2019-03-26 | 昆明理工大学 | A kind of preparation method of graphene enhancing magnesium-based composite material |
CN109439987A (en) * | 2018-12-29 | 2019-03-08 | 厦门十维科技有限公司 | Superelevation thermal conductivity aligns graphene magnesium base alloy, preparation method and device |
CN110306086A (en) * | 2019-06-26 | 2019-10-08 | 哈尔滨理工大学 | A kind of corrosion resistant Mg-Zn-Ca-Sn biological medical magnesium alloy preparation method of novel multiple |
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