CN105483571B - A kind of method that ball-milling method prepares amorphous magnesium alloy - Google Patents
A kind of method that ball-milling method prepares amorphous magnesium alloy Download PDFInfo
- Publication number
- CN105483571B CN105483571B CN201610060150.0A CN201610060150A CN105483571B CN 105483571 B CN105483571 B CN 105483571B CN 201610060150 A CN201610060150 A CN 201610060150A CN 105483571 B CN105483571 B CN 105483571B
- Authority
- CN
- China
- Prior art keywords
- ball
- magnesium alloy
- milling
- alloy powder
- interlayer
- 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.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous 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
- C22C1/11—Making amorphous alloys
Abstract
The present invention relates to a kind of method that ball-milling method prepares amorphous magnesium alloy, inserted after the magnesium alloy powder mixed and ball milling ball are carried out into centrifugation batch mixing in vacuum interlayer ball grinder；Vacuumized in vacuum interlayer ball grinder, and inert gas is passed through into vacuum interlayer ball grinder and form protection, anti-oxidation, then liquid nitrogen is poured into vacuum interlayer ball grinder interlayer and cooled down；Ball milling is carried out on planetary ball mill, during which continues liquid feeding nitrogen and keeps cooling, produce amorphous magnesium alloy powder.The considered critical of the present invention process conditions of ball milling; with the extension of Ball-milling Time; cause magnesium alloy powder crystal grain refinement; and make it that magnesium alloy powder is decrystallized; inert gas shielding is used in mechanical milling process; prevent magnesium alloy powder to aoxidize, and the mixture of ball milling ball and magnesium alloy powder is carried out cold welding using liquid nitrogen interlayer.The present invention can be with better simply step, safer operation preparation amorphous magnesium alloy, so as to realize that amorphous magnesium alloy is further applied.
Description
Technical field
The present invention relates to a kind of non-crystaline amorphous metal preparation method, the side of amorphous magnesium alloy is prepared more particularly, to a kind of ball-milling method
Method.
Background technology
Magnesium and magnesium alloy are so that its density is small, specific strength is high, shock absorption good, good casting property, high dimensional stability the advantages of,
It is widely used in many fields.Can be poor yet with magnesium and corrosion resistance of magnesium alloy, limit its development.Non-crystaline amorphous metal due to
In the absence of crystal grain and crystal boundary, the defect that crystal boundary is brought is reduced, the decay resistance and mechanical performance of material is improved.
At present, the general amorphous magnesium alloy that powder morphology is made using traditional quick quenching technique of the preparation of amorphous magnesium alloy, its
Bulk can not be configured to, purposes is narrow, in addition, the processing step that quick quenching technique prepares amorphous magnesium alloy is complicated.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of step is simple, safety
The method that reliable ball-milling method prepares amorphous magnesium alloy.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of method that ball-milling method prepares amorphous magnesium alloy, comprises the following steps：
Inserted after the magnesium alloy powder mixed and ball milling ball are carried out into centrifugation batch mixing in vacuum interlayer ball grinder；
Vacuumized in vacuum interlayer ball grinder, and inert gas formation protection is passed through into vacuum interlayer ball grinder, prevented
Aoxidize, then liquid nitrogen is poured into vacuum interlayer ball grinder interlayer and cooled down；
Ball milling is carried out on planetary ball mill, during which continues liquid feeding nitrogen and keeps cooling, produce amorphous magnesium alloy powder.
The ratio of grinding media to material of ball milling ball and magnesium alloy powder is (5~30)：1, preferably 20:1.
Described magnesium alloy powder is formulated by the raw material of following components and percentage by weight：Mg 60-68%, Zn
25-32%, Si 1-4%, Ca 3-4%, Zr 0.1-0.5%.The ratio setting of above-mentioned magnesium alloy powder is suitable for realizing
The preferred proportion of ball milling formation amorphousness.
Carry out ball milling process conditions be：300~400r/min rotating speed ball milling at least 40 hours, rotating speed is preferably
380r/min。
Described vacuum interlayer ball grinder includes a cavity, is liquid nitrogen interlayer in the outside of cavity, is set above cavity
Put seal cover board, be tightly connected between described seal cover board and cavity by clamp, be provided on described cavity with very
What empty suction filtration machine was connected vacuumizes interface, and separable key valve is provided with interface is vacuumized, and described liquid nitrogen interlayer sets liquid
Nitrogen inlet screw plug and relief valve.
Described vacuum interlayer ball grinder is well mixed in use, magnesium alloy powder and ball milling ball are added into centrifugation batch mixer
Afterwards, seal cover board is opened, ball milling ball and magnesium alloy powder are poured into cavity, seal cover board is covered, tightens sealing clamp.Will
Vacuumize interface with vacuum filtration machine to be connected, lift after rotating clockwise some circles of separable key valve, open passage.Open true
Empty suction filtration machine, while being passed through inert gas.Vacuumize and finish, press separable key valve, rotate counterclockwise and closed very after some circles
Empty suction filtration machine, unloads separable key valve, and inert gas shielding state is now in cavity.From appropriate counterweight, by ball grinder
It is fixed on planetary ball mill, turns on liquid nitrogen inlet screw plug and pour into liquid nitrogen to liquid nitrogen interlayer, tighten liquid nitrogen entrance spiral shell
Line plug.350~400r/min of setting speed, opens planetary ball mill, pause adds a liquid nitrogen cooling per half an hour for operation,
The purpose of liquid nitrogen is to make the mixture of ball milling ball and magnesium alloy powder to carry out cold welding.Until more than 40 hours.Load releasing valve can be protected
Air pressure balance is demonstrate,proved, prevents nitrogen from going out valve.Sealing clamp are pulled down after end, amorphous magnesium conjunction can be obtained by opening seal cover board
Bronze end.
Described inert gas includes helium or argon gas, and the effect of inert gas is the oxidation for preventing magnesium alloy powder.
Compared with prior art, the present invention prepares amorphous magnesium alloy using the method for ball milling, considered critical of the present invention ball
The process conditions of mill, with the extension of Ball-milling Time, cause magnesium alloy powder crystal grain refinement, and inertia is used in mechanical milling process
Gas shield, it is therefore prevented that magnesium alloy powder is aoxidized, and enter the mixture of ball milling ball and magnesium alloy powder using liquid nitrogen interlayer
Row cold welding.In mechanical milling process, the abrading-ball with very big kinetic energy rolls different powder, soldering, and formation has certain atom in interlayer
The MULTILAYER COMPOSITE particle of adhesion, again by broken and cold welding repeatedly, powder crystalline structure is destroyed, and mechanical energy is inhaled by powder
Receive, make energy accumulation, and due to interatomic diffusion process, the unstable amorphous of Inner Constitution.The present invention can be with simpler
The step of, safer operation preparation amorphous magnesium alloy, so as to realize that amorphous magnesium alloy is further applied.
Brief description of the drawings
Fig. 1 is the structural representation of vacuum interlayer ball grinder.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
A kind of method that ball-milling method prepares amorphous magnesium alloy, comprises the following steps：
Inserted after the magnesium alloy powder mixed and ball milling ball are carried out into centrifugation batch mixing in vacuum interlayer ball grinder；Vacuum clip
Vacuumized in layer ball grinder, and be passed through into vacuum interlayer ball grinder helium formation protection, anti-oxidation, then to vacuum interlayer ball
Liquid nitrogen is poured into grinding jar interlayer to be cooled down；Ball milling is carried out on planetary ball mill, the process conditions of ball milling are 300r/min
Rotating speed ball milling at least 40 hours, during which continue liquid feeding nitrogen and keep cooling, produce amorphous magnesium alloy powder.
The ratio of grinding media to material of ball milling ball and magnesium alloy powder is 5:1, magnesium alloy powder is by following components and the original of percentage by weight
Material is formulated：Mg 60%, Zn32%, Si3.5%, Ca 4%, Zr 0.5%.
As shown in figure 1, vacuum interlayer ball grinder includes a cavity 8, is liquid nitrogen interlayer 7 in the outside of cavity 8, in cavity 8
Top set seal cover board 6, be tightly connected between seal cover board 6 and cavity 8 by clamp 4, be provided on cavity 8 with very
What empty suction filtration machine was connected vacuumizes interface 1, and separable key valve 2 is provided with interface 1 is vacuumized, and liquid nitrogen interlayer 7 sets liquid nitrogen
Inlet screw plug 5 and relief valve 3.
After vacuum interlayer ball grinder is in use, magnesium alloy powder and ball milling ball addition centrifugation batch mixer are well mixed, beat
Seal cover board 6 is opened, ball milling ball and magnesium alloy powder are poured into cavity 8, seal cover board 6 is covered, tightens sealing clamp 4.Will
Vacuumize interface 1 with vacuum filtration machine to be connected, lift after rotating clockwise some circles of separable key valve 2, open passage.Open
Vacuum filtration machine, while being passed through inert gas.Vacuumize and finish, press separable key valve 2, rotate counterclockwise and closed after some circles
Vacuum filtration machine, unloads separable key valve 2, and inert gas shielding state is now in cavity 8.From appropriate counterweight, by ball
Grinding jar is fixed on planetary ball mill, is turned on liquid nitrogen inlet screw plug 5 and is poured into liquid nitrogen to liquid nitrogen interlayer 7, tightens liquid nitrogen
Inlet screw plug 5.350~400r/min of setting speed, opens planetary ball mill, operation pause plus not good liquor per half an hour
Nitrogen is cooled down, and the purpose of liquid nitrogen is to make the mixture of ball milling ball and magnesium alloy powder to carry out cold welding.Until more than 40 hours.Drain charge
Valve 3 can ensure air pressure balance, prevent nitrogen from going out valve.Sealing clamp 4 are pulled down after end, opening seal cover board 6 can obtain
Amorphous magnesium alloy powder.
Embodiment 2
Difference from Example 1 is, in the present embodiment, and the process conditions of ball milling are milled to for 400r/min rotating speed
Few 40 hours, the ratio of grinding media to material of ball milling ball and magnesium alloy powder is 30:1, magnesium alloy powder is by following components and percentage by weight
Raw material is formulated：Mg 68%, Zn 25%, Si 3.9%, Ca 3%, Zr 0.1%.
Embodiment 3
Difference from Example 1 is, in the present embodiment, and the process conditions of ball milling are milled to for 380r/min rotating speed
Few 40 hours, the ratio of grinding media to material of ball milling ball and magnesium alloy powder is 20:1, magnesium alloy powder is by following components and percentage by weight
Raw material is formulated：Mg 65%, Zn 31%, Si 1%, Ca 3.7%, Zr 0.3%.
Embodiment 4
Difference from Example 1 is, in the present embodiment, and the process conditions of ball milling are milled to for 380r/min rotating speed
Few 40 hours, the ratio of grinding media to material of ball milling ball and magnesium alloy powder is 20:1, magnesium alloy powder is by following components and percentage by weight
Raw material is formulated：Mg 63%, Zn 29.6%, Si 4%, Ca 3.1%, Zr 0.3%.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using invention.
Person skilled in the art obviously can easily make various modifications to these embodiments, and described herein general
Principle is applied in other embodiment without passing through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability
Field technique personnel are according to the announcement of the present invention, and not departing from improvement and modification that scope made all should be the present invention's
Within protection domain.
Claims (6)
1. a kind of method that ball-milling method prepares amorphous magnesium alloy, it is characterised in that comprise the following steps：
Inserted after the magnesium alloy powder mixed and ball milling ball are carried out into centrifugation batch mixing in vacuum interlayer ball grinder；
Vacuumized in vacuum interlayer ball grinder, and inert gas formation is passed through into vacuum interlayer ball grinder and protected, anti-oxidation,
Liquid nitrogen is poured into vacuum interlayer ball grinder interlayer again to be cooled down；
Ball milling is carried out on planetary ball mill, during which continues liquid feeding nitrogen and keeps cooling, produce amorphous magnesium alloy powder；
Described vacuum interlayer ball grinder includes a cavity (8), is liquid nitrogen interlayer (7) in the outside of cavity (8), in cavity (8)
Top set seal cover board (6), be tightly connected between described seal cover board (6) and cavity (8) by clamp (4), it is described
Cavity (8) on be provided for being connected with vacuum filtration machine vacuumize interface (1), being provided with interface (1) is vacuumized can
Tear key valve (2) open, described liquid nitrogen interlayer (7) sets liquid nitrogen inlet screw plug (5) and relief valve (3).
2. the method that a kind of ball-milling method according to claim 1 prepares amorphous magnesium alloy, it is characterised in that ball milling ball and magnesium
The ratio of grinding media to material of alloy powder is (5~30)：1.
3. the method that a kind of ball-milling method according to claim 2 prepares amorphous magnesium alloy, it is characterised in that ball milling ball and magnesium
The ratio of grinding media to material of alloy powder is 20:1.
4. the method that a kind of ball-milling method according to claim 1 prepares amorphous magnesium alloy, it is characterised in that described magnesium is closed
Bronze end is formulated by the raw material of following components and percentage by weight：Mg 60-68%, Zn 25-32%, Si 1-4%, Ca
3-4%, Zr 0.1-0.5%.
5. the method that a kind of ball-milling method according to claim 1 prepares amorphous magnesium alloy, it is characterised in that carry out ball milling
Process conditions are：300~400r/min rotating speed ball milling at least 40 hours.
6. the method that a kind of ball-milling method according to claim 1 prepares amorphous magnesium alloy, it is characterised in that described inertia
Gas includes helium or argon gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610060150.0A CN105483571B (en) | 2016-01-28 | 2016-01-28 | A kind of method that ball-milling method prepares amorphous magnesium alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610060150.0A CN105483571B (en) | 2016-01-28 | 2016-01-28 | A kind of method that ball-milling method prepares amorphous magnesium alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105483571A CN105483571A (en) | 2016-04-13 |
| CN105483571B true CN105483571B (en) | 2017-07-25 |
Family
ID=55670834
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610060150.0A Expired - Fee Related CN105483571B (en) | 2016-01-28 | 2016-01-28 | A kind of method that ball-milling method prepares amorphous magnesium alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105483571B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107475544A (en) * | 2017-08-29 | 2017-12-15 | 天津理工大学 | A kind of method that glassy metal is prepared under the condition of high temperature |
| CN108188408B (en) * | 2018-01-04 | 2021-04-02 | 北京理工大学 | Spherical atomized magnesium-zinc amorphous alloy powder and preparation method thereof |
| CN114191616A (en) * | 2021-12-01 | 2022-03-18 | 中国地质大学(北京)郑州研究院 | Preparation method of reinforced absorbable medical implant material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1102014A (en) * | 1994-10-20 | 1995-04-26 | 浙江大学 | Magnesium base hydrogen-storing alloy electrode |
| CN1271025A (en) * | 2000-05-31 | 2000-10-25 | 南开大学 | Magnesium-base hydrogen storing alloy material |
| CN1431072A (en) * | 2003-01-23 | 2003-07-23 | 上海交通大学 | Vertical type agitation ball grinding mill of low temp |
| CN1741306A (en) * | 2005-08-30 | 2006-03-01 | 包头稀土研究院 | Amorphous magnesium-Nickel series hydron-storage electrode material and producing method thereof |
| CN103305709A (en) * | 2013-05-27 | 2013-09-18 | 河北工业大学 | Preparation method of medical magnesium-base non-crystalline material |
-
2016
- 2016-01-28 CN CN201610060150.0A patent/CN105483571B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1102014A (en) * | 1994-10-20 | 1995-04-26 | 浙江大学 | Magnesium base hydrogen-storing alloy electrode |
| CN1271025A (en) * | 2000-05-31 | 2000-10-25 | 南开大学 | Magnesium-base hydrogen storing alloy material |
| CN1431072A (en) * | 2003-01-23 | 2003-07-23 | 上海交通大学 | Vertical type agitation ball grinding mill of low temp |
| CN1741306A (en) * | 2005-08-30 | 2006-03-01 | 包头稀土研究院 | Amorphous magnesium-Nickel series hydron-storage electrode material and producing method thereof |
| CN103305709A (en) * | 2013-05-27 | 2013-09-18 | 河北工业大学 | Preparation method of medical magnesium-base non-crystalline material |
Non-Patent Citations (1)
| Title |
|---|
| 材料科学与工程学报;陈 可等;《机械合金化工艺对Ｍｇ６０Ｚｎ３０Ｔｉ５Ｓｉ５非晶合金制备的影响》;20151231;第３３卷(第６期);第810-842页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105483571A (en) | 2016-04-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105483571B (en) | A kind of method that ball-milling method prepares amorphous magnesium alloy | |
| EP3827916A1 (en) | A manufacturing method of sintered nd-fe-b permanent magnet | |
| CN104593652B (en) | Quasicrystal and alumina mixed particle reinforced magnesium-based composite material and manufacturing method thereof | |
| EP3193347A1 (en) | Production method for r-t-b sintered magnet | |
| EP4066967A1 (en) | Method for preparing aluminum-containing alloy powder, use thereof and alloy strip | |
| CN111393241A (en) | Al、Fe2O3PTFE nano composite energetic material and preparation method thereof | |
| CN105063457A (en) | Nano-graphite compounded high-capacity RE-Mg-Ni-based hydrogen storage material and preparation method thereof | |
| CN101880788B (en) | Method for enhancing SiC particle grinding of magnesium aluminum alloy | |
| CN100476002C (en) | Heat resistance casting magnesium alloy and preparation method thereof | |
| CN111689821A (en) | Activated boron powder and preparation method thereof | |
| Liu et al. | Effect of limestone ores on grain refinement of as-cast commercial AZ31 magnesium alloys | |
| CN110129624A (en) | A kind of SiC-Al3The preparation method of Ti reinforced aluminum matrix composites | |
| CN105502464B (en) | Ferro element separates except technique in a kind of titanium gypsum | |
| CN111872414B (en) | Preparation method of micro-nano pre-alloyed powder | |
| WO2011049160A1 (en) | Process for production of hydrogen-storing alloy composition | |
| JP2011214113A (en) | Method for manufacturing rare-earth-iron-nitrogen-base magnet powder and rare-earth-iron-nitrogen-base magnet obtained thereby | |
| CN105798319A (en) | Preparation method and device for silver-tungsten electrical contact material as well as electrical contact material and electrical contact | |
| CN110218926A (en) | A kind of super coarse-grain WC-Co hard alloy preparation method | |
| WO2014059772A1 (en) | High corrosion-resistant re-(fe, tm)-b magnet and preparing method thereof | |
| JP2560566B2 (en) | Method for producing hydrogen storage alloy | |
| CN202719869U (en) | Alumina crucible with slag hole for producing high purity master alloy by external furnace method | |
| JP2560567B2 (en) | Method for producing hydrogen storage alloy | |
| CN106191542B (en) | A kind of hydrogen rich water hydrogen manufacturing material and its preparation method and application | |
| CN106756355B (en) | Fuel cell stores hydrogen intermediate alloy, hydrogen storage material and preparation method with Mg-Sn-Ni ternary | |
| CN101871056A (en) | Production method of high-boron-nickel alloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170725 Termination date: 20220128 |