CN1322160C - Process for preparing block nano crystal/non-crystal alloy - Google Patents
Process for preparing block nano crystal/non-crystal alloy Download PDFInfo
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- CN1322160C CN1322160C CNB2004100568904A CN200410056890A CN1322160C CN 1322160 C CN1322160 C CN 1322160C CN B2004100568904 A CNB2004100568904 A CN B2004100568904A CN 200410056890 A CN200410056890 A CN 200410056890A CN 1322160 C CN1322160 C CN 1322160C
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- 239000000956 alloy Substances 0.000 title claims abstract description 16
- 239000013078 crystal Substances 0.000 title claims abstract description 11
- 229910045601 alloy Inorganic materials 0.000 title claims description 6
- 239000002159 nanocrystal Substances 0.000 title description 5
- 238000004519 manufacturing process Methods 0.000 title description 2
- 238000002425 crystallisation Methods 0.000 claims abstract description 27
- 230000008025 crystallization Effects 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 22
- 229910000808 amorphous metal alloy Inorganic materials 0.000 claims abstract description 12
- 239000005300 metallic glass Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 abstract description 10
- 239000002184 metal Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000003990 capacitor Substances 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- 230000008021 deposition Effects 0.000 abstract 1
- 230000008520 organization Effects 0.000 abstract 1
- 238000013021 overheating Methods 0.000 abstract 1
- 239000002707 nanocrystalline material Substances 0.000 description 5
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
The present invention discloses a method for preparing block nanometer crystalsize/amorphous alloy, which belongs to the preparation technology range of metal nanometer materials. The present invention uses a direct-current pulse power supply of the charge/discharge of a solid capacitor; aiming at the characteristic of block amorphous alloy, the present invention selects current density j is in a scope ranging from 100 to 10000 A/mm<2>, processing time is in a scope ranging from 2 seconds to 60 minutes, current pulse width mu is in a scope ranging from 10 to 200 mu s, and current pulse frequency is in a scope ranging from 2 to 5000Hz. The present invention has the standard that nanometer crystal grains can be obtained by crystallization, and the magnitude of the crystal grains is not increased because of overheating; the present invention promotes the diffusion and the transfer of atoms, and promotes the generation of crystal nucleus and nanometer phase deposition by using current and the interaction of metal atoms. Thus, the present invention not only promotes the crystal nucleus to uniformly generate, but also restrains the crystal grains to grow up, and the present invention can obtain block nanometer crystalsize/amorphous alloy materials which have the advantages of uniform nanometer phase size and uniform crystallization organization.
Description
Technical field
The invention belongs to metal nano material technology of preparing scope, particularly a kind of method for preparing the bulk nanocrystalline alloy material.
Technical background
Nano crystal metal material is a class type material of exploitation in the recent two decades.Their constitutional features is that grain-size is about 1～100nm.Nearest result of study shows that the mechanical property of this class material, electromagnetic property etc. all are better than the big grain material with chemical composition, therefore extremely scientific worker's concern in recent years.
The preparation method of metal current nanocrystalline material mainly contains the methods such as crystallization processing of chemical precipitation, vapour deposition and amorphous metal, and wherein to be equipped with nanocrystalline material be one of main method of the nano amorphous material of preparation at present to amorphous metal crystallization legal system.This method is to prepare the amorphous metal strip with rapid solidification method, is heated to the above insulation of amorphous transition temperature or crystallization temperature then; By the CONTROL PROCESS condition, obtain nanophase and separate out, prepare nano amorphous material.In recent years block amorphous alloy preparation makes a breakthrough, and the application of block materials is with more convenient, more extensive.Can adopt the isothermal annealing crystallization method to realize crystallization too to block amorphous alloy.
The principal feature of isothermal crystallization method is: technology controlling and process is had relatively high expectations.Because nanocrystal is easy to grow up in crystallization process, therefore must be to the strict control of holding temperature.Grain growth speed was slow when temperature was low, and crystallization, crystal grain are difficult to grow up, but but are difficult to crystallization.Therefore, can crystallization if can develop, grain-size is controlled again or crystallization temperature is lower method, will be very meaningful.Have not yet to see the open report that utilizes high-strength pulse-current direct crystallization block amorphous alloy to prepare bulk nano-crystalline material.
Summary of the invention
The objective of the invention is to propose a kind of method for preparing the bulk nanocrystalline alloy material.Adopt pulsed current to handle the technology that block amorphous alloy prepares the bulk nanocrystalline alloy material, it is characterized in that the described treatment process for preparing the method for bulk nanocrystalline alloy material is:
1) adopt the direct current pulse power source of solid capacitor charge and discharge, provide realize crystallization greater than 10
3A peak pulse current value;
2) at the feature of block amorphous alloy, select current density range: j=100～10000A/mm
2
3) treatment time is unlikely to the overheated grain growth that causes again and is as the criterion the treatment time scope: 2 seconds～60 minutes to guarantee and can crystallization obtain nanocrystal;
3) current pulse width scope: μ=10～200 μ s;
4) current pulse frequency scope: f=2～5000Hz.
The invention has the beneficial effects as follows the method that adopts high-strength pulse-current direct crystallization bulk amorphous alloy to obtain bulk nano-crystalline material, the nanophase size that obtains is even, the crystallization homogeneous microstructure.This method can realize nano-crystallization under relatively low temperature.And can prepare the bulk nano-crystalline-non-crystal heterogeneous material of different nanocrystalline content, to obtain the material of concrete different performance by processing parameter adjustment (reduce current density or reduce the treatment time).
Embodiment
The present invention is a kind of method for preparing the bulk nanocrystalline alloy material.The treatment process of this method is:
1) adopt the direct current pulse power source of solid capacitor charge and discharge, provide realize crystallization greater than 10
3A peak pulse current value;
2) at the feature of block amorphous alloy, select current density range: j=100～10000A/mm
2
3) treatment time is unlikely to the overheated grain growth that causes again and is as the criterion the treatment time scope: 2 seconds～60 minutes to guarantee and can crystallization obtain nanocrystal;
3) current pulse width scope: μ=10～200 μ s;
4) current pulse frequency scope: f=2～5000Hz.
Theoretical basis principle of the present invention is to utilize the interaction of electric current and atoms metal, promotes the atomic diffusion migration, promotes nucleus generation and nanophase to separate out.Simultaneously, use pulsed current can make the material temperature rise be unlikely to too high, therefore can promote that nucleus evenly generates, suppress grain growth again.Exemplifying specific embodiment is below further specified the present invention.
One .ZrTiCuNiBe non-crystaline amorphous metal
Utilize high-strength pulse-current that block ZrTiCuNiBe non-crystaline amorphous metal is carried out crystallization and prepare the bulk nanocrystalline alloy that grain-size is 4～30nm.Processing parameter is;
1) current density: j=500～5000A/mm
2
2) operating voltage: V=380V
3) current pulse width: μ=20～100 μ s
4) current pulse frequency: f=5～200Hz
5) treatment time: 5 seconds～60 minutes
The decrystallized alloy of two .ZrTiCuNiAl
Utilize high-strength pulse-current that block ZrTiCuNiAl non-crystaline amorphous metal is carried out crystallization and prepare the bulk nanocrystalline alloy that grain-size is 10～60nm.Processing parameter is;
1) current density: j=800-8000A/mm
2
2) operating voltage: V=380V
3) current pulse width: μ=40～200 μ s
4) current pulse frequency: f=10～300Hz
5) treatment time: 8 seconds～40 minutes
The processing method of preparation bulk nano-crystalline material replaces traditional isothermal crystallization process method, can obtain that crystal grain is tiny, the bulk nanocrystalline alloy material of homogeneous microstructure.
Claims (2)
1. a method for preparing the bulk nanocrystalline alloy material is utilized greater than 10
3The high-strength pulse-current of A peak value carries out crystallization to block amorphous alloy to be handled, it is characterized in that, utilize high-strength pulse-current that block ZrTiCuNiBe non-crystaline amorphous metal is carried out crystallization and handle, prepare the nanometer crystal alloy that grain-size is 4～30nm, processing parameter is;
1) current density: j=500～5000A/mm
2
2) operating voltage: V=380V
3) current pulse width: μ=20～100 μ s
4) current pulse frequency: f=5～200Hz
5) treatment time: 5 seconds～60 minutes.
2. a method for preparing the bulk nanocrystalline alloy material is utilized greater than 10
3The high-strength pulse-current of A peak value carries out crystallization to block amorphous alloy to be handled, it is characterized in that, utilize high-strength pulse-current that block ZrTiCuNiAl non-crystaline amorphous metal is carried out crystallization and handle, prepare the nanometer crystal alloy that grain-size is 10～60nm, processing parameter is;
1) current density: j=800-8000A/mm
2
2) operating voltage: V=380V
3) current pulse width: μ=40～200 μ s
4) current pulse frequency: f=10～300Hz
5) treatment time: 8 seconds～40 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100568904A CN1322160C (en) | 2004-08-30 | 2004-08-30 | Process for preparing block nano crystal/non-crystal alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100568904A CN1322160C (en) | 2004-08-30 | 2004-08-30 | Process for preparing block nano crystal/non-crystal alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1598034A CN1598034A (en) | 2005-03-23 |
| CN1322160C true CN1322160C (en) | 2007-06-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100568904A Expired - Fee Related CN1322160C (en) | 2004-08-30 | 2004-08-30 | Process for preparing block nano crystal/non-crystal alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1322160C (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1100472A (en) * | 1993-09-14 | 1995-03-22 | 东北大学 | Pulse current treatment for producing iron-base nano-meter crystal material |
-
2004
- 2004-08-30 CN CNB2004100568904A patent/CN1322160C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1100472A (en) * | 1993-09-14 | 1995-03-22 | 东北大学 | Pulse current treatment for producing iron-base nano-meter crystal material |
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| Publication number | Publication date |
|---|---|
| CN1598034A (en) | 2005-03-23 |
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Granted publication date: 20070620 Termination date: 20130830 |