CN104525960A - Preparation method for Fe-Mn metal powder materials for 3D printing - Google Patents
Preparation method for Fe-Mn metal powder materials for 3D printing Download PDFInfo
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- CN104525960A CN104525960A CN201410825661.8A CN201410825661A CN104525960A CN 104525960 A CN104525960 A CN 104525960A CN 201410825661 A CN201410825661 A CN 201410825661A CN 104525960 A CN104525960 A CN 104525960A
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Abstract
The invention belongs to the field of medical metallic materials, and provides a production method for Fe-Mn metal powder suitable for 3D printing, the metal powder contains low oxygen and high purity, and the particle size of the metal powder ranges from 0.5 micron to 3 microns. The method is characterized in that a raw material is melted through induction melting until the raw material is boiling, and then an appropriate amount of alloy is added into melt for deoxygenation processing; casting powder with appropriate components is added to remove nonmetallic inclusion, upward floating of the nonmetallic inclusion is promoted through electromagnetic purification, and the is absorbed by the casting powder; atomization powder preparation is carried out through a supersonic pulse inert gas atomization method, the spherical micron or submicron Fe-Mn metal powder with the ultra-low oxygen is obtained, and finally 3D printing forming is achieved through a laser high-temperature melting lamination method or a selective laser high-temperature sintering method.
Description
Technical field
The invention belongs to medical science metal material field, provide a kind of hypoxemia, high cleanliness and there is excellent mechanical performances and biomedical degradation characteristic simultaneously can be used for the preparation method that medical domain 3D prints the Fe-Mn based metal powder material containing Pd.
Background technology
As the metallic support of medical application or graft materials except having good biomedical degradation characteristic, also need good mechanical property, as superhigh intensity and good plasticity and significant work hardening rate, ensure the uniform expansion of metallic support and the stimulation that reduces health.Compare the medical science metal material such as traditional titanium-aluminium alloy and 316L stainless steel, the biomedical degradation rate mechanical property of Fe-Mn-C or the Fe-Mn-C-Al system TWIP Steel material developed in recent years and the corrosion of good biological medical science and degradation characteristic can be used for medical domain.3D prints and is called as " engine of the third time industrial revolution ", and 3D prints and brought " metal age " into by laser sintered and selective laser sintering at present.Have expert to point out, the core that 3D prints is its overturning traditional manufacturing mode.Fe-Mn system metal material is used for skeletal support material, angiocarpy bracket etc., and the development of 3d technology, makes as each customization different size, and the product of different mechanical properties and biological property becomes possibility.The direct manufacturing technology of high-performance medical metal powder can produce the Components Shape that cannot obtain by classical production process, and mechanical property is also better, can also realize many Material claddings shaping, stock utilization can be significantly improved simultaneously, reduce manufacturing cost, avoid waste of material, shorten the production cycle.Printing with 3D the high-performance metal powder body material manufactured will be basis and the guarantee of this technical development.The invention provides a kind of preparation method being applicable to the Fe-Mn based metal powder material containing Pd that 3D prints.
Summary of the invention
The invention provides the metal powder preparation method of a kind of degradable biological metal alloy compositions Fe-Mn-Al-C-Pd system containing Pd.The constituent of material of the present invention is expressed as with mass fraction: carbon (C): 0.6-1.2%, manganese (Mn): 17-21%, aluminium (Al): 0.6-2%, phosphorus (P) <0.004%, sulphur (S) <0.004%, nitrogen (<0.02%), palladium (Pd) is containing 0.6-2%.
Because the fusing point of this metal material is at about 1600 DEG C, therefore adopt the method for supersonic atomization to prepare metal powder material, accompanying drawing 1 is preparation flow, concrete preparation method is as follows: first pass through induction furnace alloy melting according to alloying component, ferromanganese raw material is placed in crucible, adopt vacuum induction melting to be melted to and be warming up to 1650 DEG C until boiling, in melt, add appropriate alusil alloy again carry out deoxidation treatment, add Al, the element deoxidations such as Si, oxygen in molten steel is controlled at <100ppm, melt after deoxidation treatment is poured in the tundish crucible of preheating, the covering slag that crucible top has 5-15mm thick, covering slag composition is Al2O3-CaO-MgO, for absorbing the non-metallic inclusion of the large-size of liquid metal internal, as Al
2o
3, CaS etc.Treat that liquid metal places 5 minutes, between resting period at tundish crucible, tundish crucible is placed in intermediate frequency electromagnetic purifier, and the frequency of electromagnetic purification is at 5-20Hz, and electromagnetic purification promotes that inclusion floating is absorbed by covering slag.The centrifugal force produced in electromagnetic purification process, field trash and bits are concentrated to pivot district and floats, Stirring promotes the collision and coalescence of field trash and bits and maximizes, and thus easily floats and gets rid of.In addition, electromagnetic purification hinders the flowing of original gravity direction, suppresses the generation of flowing short circuit, and improve the holdup time distribution of molten steel in separation chamber, total oxygen clearance can reach more than 70%, and more than 10 microns field trashes are removed substantially.
After electromagnetic purification process terminates, supersonic speed pulse inert gas atomising device is adopted to carry out powder by atomization, open atomization source of the gas, regulate bleed pressure, by atomizer, the airflow rate of atomizer is accelerated to more than supersonic speed Mach, and forming frequency is at the air pulse of 20-200kHz, obtain the spherical micron of Ultra Low-oxygen and sub-micron Fe-Mn metal dust; After atomization terminates, the Fe-Mn metal dust of metal dust original position gathering system to preparation is utilized to collect under vacuo and classification.
Melting accumulation method of forming technology due to 3D printing heat is adopt Low Temperature Thermal to melt printing head, the printing path extruding that dynamic for melt-flow thermoplastic macromolecule material controls by the Moulds Based on Three-Dimensional Models individual-layer data of Computer Design is deposited on ad-hoc location, thermoplastic cooling curing, successively piles up shaped article.Metal dust adopts laser high-temperature fusion lamination method or selective laser high-temperature sintering process to realize 3D printing shaping.Due to metal molten or sintering temperature high, the laser generator power used by laser formation method is large, general at more than 150W, printhead is stabilized in 1500 DEG C to 2000 DEG C, and therefore Fe-Mn based metal powder utilizes selective laser sintering process to print and produces metallic element.First the Fe-Mn metal dust of average grain diameter 5-20 μm is selected, select thermoplastic molding's Binder Composition of certain proportioning, as 40% paraffin+60% polyethylene, then metal dust content and a certain proportion of molding adhesive volume content are carried out mixing, mixing temperature is at about 200 DEG C, then the threedimensional model individual-layer data of preparation will be needed to be added into printer, by select laser sintered method just printable go out the metallic article of applicable size.
Accompanying drawing explanation
Fig. 1 is flow process preparation figure of the present invention.
concrete implementation content
Specific embodiments of the present invention, printing Fe-Mn-Al-C-Pd system heart hat main support with 3D is that example is described as follows: ferromanganese raw material is placed in crucible, adopt vacuum induction melting to be melted to and be warming up to 1650 DEG C until boiling, then in melt, add appropriate alusil alloy carry out deoxidation treatment; Melt after deoxidation treatment is poured in the tundish crucible of preheating, supersonic speed pulse inert gas atomization method is adopted to carry out powder by atomization: to open atomization source of the gas, regulate bleed pressure, by atomizer, the airflow rate of atomizer is accelerated to more than 1.5 Mach, and forming frequency is at the air pulse of 20-200kHz, obtain the spherical micron of Ultra Low-oxygen and sub-micron Fe-Mn metal dust; After atomization terminates, the Fe-Mn metal dust of metal dust original position gathering system to preparation is utilized to collect under vacuo and classification.It is narrow that the metal dust prepared has size distribution interval; Mobility is better; Sphericity is high; Apparent density high.
Select the Fe-Mn metal dust of average grain diameter D50=5-30 μm and appropriate thermoplastic molding's binding agent, its composition is: 40% paraffin+60% polyethylene, 70% metal dust content+30% molding adhesive volume content, with 3 kilograms of extruders, the mixing 10kg compound of temperature less than 120 DEG C 20 hours.With power at 180W laser formation generator, printhead temperature controls to carry out 3D printing at about 1600 DEG C.
The operational effect of this programme is that 3D prints one and to have in 24 hours biomedical degradation rate more than 0.5mg/cm
2, in 48 hours, degradation rate reaches 2.5mg/cm
2, yield strength more than 700MPa, tensile strength more than 1200Mp, uniform elongation more than 30% containing the Fe-Mn system heart coronaries main support of Pt.
Compared with being preced with main support with preparation of metals Fe-Mn-Al-C-Pd system of the Fe-Mn system heart of block materials, metal dust possesses materials and economizes, and operation is simple, and formed precision is more accurate, can customize self heart arter support applicable for different patient.
Claims (8)
1. a 3D prints one and to have in 24 hours biomedical degradation rate more than 0.5mg/cm
2, in 48 hours, degradation rate reaches 2.5mg/cm
2, yield strength more than 700MPa, tensile strength more than 1200Mp, the Fe-Mn metal powder production process of uniform elongation more than 30%, this powder fine size and distributed area is narrow; Good fluidity; Sphericity is high; Apparent density is high, it is characterized in that:
In claim 1, preparation process is as follows: ferromanganese raw material is placed in crucible, adopts vacuum induction melting to be melted to and to be warming up to until seethe with excitement, then in melt, adds appropriate alusil alloy carry out deoxidation treatment; And the covering slag adding suitable component is for removing non-metallic inclusion, tundish crucible is placed in intermediate frequency electromagnetic purifier, and electromagnetic purification promotes that inclusion floating is absorbed by covering slag.
2. the melt after electromagnetic purification process is poured in the tundish crucible of preheating, supersonic speed pulse inert gas atomization method is adopted to carry out powder by atomization: to open atomization source of the gas, regulate bleed pressure, by atomizer the airflow rate of atomizer accelerated and form air pulse, obtaining the spherical micron of Ultra Low-oxygen and sub-micron Fe-Mn metal dust; After atomization terminates, the Fe-Mn metal dust of metal dust original position gathering system to preparation is utilized to collect under vacuo and classification.
3. a kind of described in claim 1 prepares the spherical a kind of described method preparing micron and sub-micron Fe-Mn metal dust of Ultra Low-oxygen, it is characterized in that, smelting temperature is between 1600 DEG C to 1700 DEG C, and the addition of described alusil alloy is mass percent 1.0-1.5%.
4. the covering slag that in claim 1, crucible top has 5-15mm thick, covering slag composition is Al203-Ca0-MgO
In claim 1, the frequency of electromagnetic purification is at 5-20Hz, and elimination time is 5-15 minute.
5. a kind of method preparing the spherical micron of Ultra Low-oxygen and sub-micron Fe-Mn metal dust described in claim 1 or 2, it is characterized in that, described bleed pressure is at 5-20MPa, by atomizer, the airflow rate of atomizer is accelerated to more than 1.5 Mach, and forming frequency is at the air pulse of 20-200kHz.
6., in claim 1, prepare the particle diameter 0.1-2 micron of metal dust, due to metal molten or sintering temperature high, metal dust adopts laser high-temperature fusion lamination method or selective laser high-temperature sintering process to realize 3D printing shaping.
7. the laser generator power used by laser formation method is large, and generally at more than 150W, printhead is stabilized between 1500 DEG C to 2000 DEG C.
8. production method as claimed in claim 1, the chemical composition that its feature is being applicable to TWIP steel is expressed as with mass fraction: carbon (C): 0.6-1.2%, manganese (Mn): 17-21%, aluminium (Al): 0.6-2%, phosphorus (P) <0.004%, sulphur (S) <0.004%, nitrogen (<0.03%), platinum (Pt) containing 0.6-2%, all the other for ferro element be Fe.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105149603A (en) * | 2015-08-26 | 2015-12-16 | 上海材料研究所 | High-sphericity Inconel 625 alloy powder and preparation method and application thereof |
| CN106270538A (en) * | 2015-05-28 | 2017-01-04 | 鞍钢股份有限公司 | A kind of preparation method of Ultra-fine Grained fe-based alloy powder |
| IT201700041618A1 (en) * | 2017-04-13 | 2018-10-13 | Tenova Spa | Method of production of metal powders by gas atomization and metal powder production plant according to this method. |
| CN111187965A (en) * | 2019-12-31 | 2020-05-22 | 中南大学湘雅二医院 | FeMn biodegradable alloy and preparation method thereof |
| CN112546291A (en) * | 2019-09-10 | 2021-03-26 | 四川大学华西医院 | Porous bone defect repair metal stent material for load bearing area and preparation method and application thereof |
| CN112658255A (en) * | 2020-11-24 | 2021-04-16 | 深圳艾利门特科技有限公司 | MIM (metal injection molding) process for Fe-Mn-Al-C series steel part |
| CN113604749A (en) * | 2021-06-29 | 2021-11-05 | 中南大学 | Low-magnetism high-strength Fe-Mn alloy and 3D printing method and application thereof |
| CN115156554A (en) * | 2021-08-27 | 2022-10-11 | 北京大学 | Preparation method of twinning induced plasticity stainless steel based on texture engineering additive manufacturing |
| CN115595510A (en) * | 2022-10-10 | 2023-01-13 | 中南大学（Cn） | Iron-manganese alloy with high work hardening capacity and preparation method and application thereof |
| CN115595462A (en) * | 2022-11-07 | 2023-01-13 | 西安建筑科技大学（Cn） | Method for manufacturing high-density Fe-Mn-Al-C light high-strength steel in additive mode |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| IT201700041618A1 (en) * | 2017-04-13 | 2018-10-13 | Tenova Spa | Method of production of metal powders by gas atomization and metal powder production plant according to this method. |
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| CN112546291A (en) * | 2019-09-10 | 2021-03-26 | 四川大学华西医院 | Porous bone defect repair metal stent material for load bearing area and preparation method and application thereof |
| CN111187965A (en) * | 2019-12-31 | 2020-05-22 | 中南大学湘雅二医院 | FeMn biodegradable alloy and preparation method thereof |
| CN112658255A (en) * | 2020-11-24 | 2021-04-16 | 深圳艾利门特科技有限公司 | MIM (metal injection molding) process for Fe-Mn-Al-C series steel part |
| CN113604749A (en) * | 2021-06-29 | 2021-11-05 | 中南大学 | Low-magnetism high-strength Fe-Mn alloy and 3D printing method and application thereof |
| CN113604749B (en) * | 2021-06-29 | 2022-07-19 | 中南大学 | Low-magnetism high-strength Fe-Mn alloy and 3D printing method and application thereof |
| CN115156554A (en) * | 2021-08-27 | 2022-10-11 | 北京大学 | Preparation method of twinning induced plasticity stainless steel based on texture engineering additive manufacturing |
| CN115595510A (en) * | 2022-10-10 | 2023-01-13 | 中南大学（Cn） | Iron-manganese alloy with high work hardening capacity and preparation method and application thereof |
| CN115595462A (en) * | 2022-11-07 | 2023-01-13 | 西安建筑科技大学（Cn） | Method for manufacturing high-density Fe-Mn-Al-C light high-strength steel in additive mode |
| CN115595462B (en) * | 2022-11-07 | 2023-11-21 | 西安建筑科技大学 | Method for manufacturing high-density Fe-Mn-Al-C light high-strength steel by additive |
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Application publication date: 20150422 |