CN1083024A - A kind of carbon steel preparation of nanomaterials - Google Patents
A kind of carbon steel preparation of nanomaterials Download PDFInfo
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- CN1083024A CN1083024A CN 92105939 CN92105939A CN1083024A CN 1083024 A CN1083024 A CN 1083024A CN 92105939 CN92105939 CN 92105939 CN 92105939 A CN92105939 A CN 92105939A CN 1083024 A CN1083024 A CN 1083024A
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- nano level
- iron
- preparation
- nano
- iron carbide
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Abstract
A kind of iron carbide preparation of nanomaterials has overcome the defective of using explosion hazard gases in the existing synthetic Fe-C based compound method, provides a kind of simple and easy synthesis method to prepare nano level carbonization iron.
The present invention adopts the colloidal sol technology to prepare nano level brown iron oxide, nano oxidized iron powder is placed in the silica tube of sealing, feeds to heat up after liquefied gas drains air, temperature is controlled at 350 ℃-550 ℃, be incubated 1 hour, cooling again, can obtain particle diameter is 10～30nm nano level carbonization iron material.
Nano silicon carbide iron powder with present method preparation has good magnetic property, can make magnetic recording material, and burning-point is low in addition, is the good fuel that is used for smokeless cigarette.
Description
The present invention is a kind of iron carbide preparation of nanomaterials, relates to solid state chemistry and magnetics.
One of characteristics of Fe-C based compound are that high saturation magnetic moment (σ is arranged
=110～140emu/g) and high coercive force (Hc=8000 Oe); Two of characteristics be difficult for oxidized, the chemical stability height.Thereby many in recent years countries are at development Fe-C based compound.Because it is not only a kind of extremely promising magnetic recording material, also, produce CO seldom because its burning-point is low, thereby or the good combustion material of smoke-less cigarette.
The generation of Fe-C based compound is except parent material Fe
2O
3Deng outside, also need H
2+ CO, H
2+ alcohols gas or CO participate in reaction, and these gases are comparatively harmful, and be particularly explosive.This not only gives to synthesize has increased difficulty, and makes synthetic equipment also therefore and more complicated, thereby cost strengthens.And at present external synthetic iron carbide is the granularity about 1 μ m mostly, because granularity is big, has influenced the effective magnetic property of Fe-C based compound.
For example " needle-like iron carbide particle manufacture method ", synthesis gas adopts N
2+ CO mixed gas, the particle diameter 0.6 μ m of synthetic Fe-C based compound, (Japanese Patent: clear 59-231587).
For another example: " preparation process of iron carbide ultra-fine grain " (European patent: when 89101464.9) synthesizing, feed CO, obtain the iron carbide of 0.1 μ m particle diameter at last.
The objective of the invention is to overcome and use this defective of explosion hazard gases in the existing synthetic Fe-C based compound method, provide a kind of simple synthesis to prepare small particle size and have the nano level carbonization iron of high saturated carbonation intension.
Characteristic of the present invention is to adopt cheap and than H
2, CO be safety liquefied gas as carbon source, at 350 ℃ of-550 ℃ of synthetic Fe-C based compounds.
Technical essential of the present invention is the thinning processing technology of synthetic iron carbide parent material and the control techniques that adopts the iron carbide of nano level parent material synthesis nano.
The present invention at first adopts colloidal sol technology (sol-gol) to produce nano level α-Fe
2O
3At first get octyl phenol Soxylat A 25-7 and n-hexyl alcohol mixed solution 5ml, add 2% iron nitrate solution, add the 11ml hexanaphthene again after the vibration evenly, vibration again, make its microemulsion that becomes homogeneous transparent, under agitation splash into then, precipitin reaction is carried out fully by the saturated hexanaphthene of ammonia, continue stirred for several minute, isolate throw out with high speed centrifugation, repeatedly wash with dehydrated alcohol and water at last, obtain α-Fe
2O
3Nanoparticle is with the about 3-5nm of TEM (transmission electron microscope) analysis particle diameter.
α-Fe with refinement
2O
3Place in the quartz boat in the silica tube of synthesizer, feed liquefied gas behind the good seal, earlier the air in the silica tube is drained, again according to the difference of synthesizing the iron carbide kind, temperature is controlled at 350 ℃-550 ℃, be incubated after one hour, control cooling more just can obtain needed nano level carbonization iron.
Use the iron carbide of the present invention's preparation, because the preparation method is simple, cost is low, thereby synthetic iron carbide material price is also lower, is suitable for industrial extensive application, also can promote the practicability of no-smoke incense; Use the iron carbide of the inventive method preparation since in optimization process on the granularity to about the 10-30nm, thereby saturation magnetic moment and remanence ratic are all improved greatly, thereby make iron carbide become the magnetic recording material that the utmost point has application prospect.
The inventive method and existing preparation iron carbide method ratio, dangerous little, equipment is simple.
Embodiment:
1, gets the α-Fe of 2.5g refinement
2O
3, place in the silica tube logical liquefied gas half an hour, get rid of inner air tube, flow 1000 ml/min are warmed up to 550 ℃ again, 5 ℃/min of speed, flow of lpg 300 ml/min, after temperature reaches 550 ℃, be incubated 1 hour, and then 3 ℃/min of control rate of temperature fall, up to room temperature, promptly obtaining particle diameter is the nano level Fe of 10～30nm
3The C powder.
2, get the α-Fe of 2.5 gram refinements
2O
3, place in the silica tube, logical liquefied gas eliminating half an hour inner air tube, flow of lpg 1000 ml/min are warmed up to 400 ℃ again, 5 ℃/min of speed, flow of lpg 300 ml/min.When temperature reaches 400 ℃, insulation 1 hour, and then control rate of temperature fall 3 ℃/min is up to room temperature, promptly obtaining particle diameter is the nano level Fe of 10～30nm
5C
2
The iron carbide sample analysis:
1, structural performance: iron carbide is very stable calking molecules, at room temperature is good magnetic substance.Fe
5C
2Be monoclinic crystal, crystalline size is 11.56A * 4.57A * 5.06A, and the β angle is 97.8 degree, and 4 Fe are arranged in the per unit crystal
5C
2Molecule, Fe
3C is a rhombic system, and crystalline size is 4.52A * 5.09A * 6.74A.Fe
5The Curie point of C is 214 ℃, Fe
5C
2Curie point be 248 ℃.
2, the magnetic property of nano silicon carbide iron
Claims (5)
1, a kind of iron carbide preparation of nanomaterials is characterized in that, this method is by the thinning processing of synthetic iron carbide parent material and adopts nano level parent material synthetic control techniques to constitute.
2, preparation method as claimed in claim 1 is characterized in that adopting the colloidal sol technology to produce in the silica tube that nano level brown iron oxide is placed on sealing then, feeds liquefied gas, drain air, temperature is controlled at 350 ℃-550 ℃, is incubated 1 hour, control cooling again.
3, preparation method as claimed in claim 1 is characterized in that, adopts the colloidal sol technology to produce nano level brown iron oxide then, be placed in the silica tube of sealing, feed liquefied gas, drain air, be warmed up to 550 ℃, promptly obtaining particle diameter is the nano level Fe of 10～30nm
3The C powder.
4, technology of preparing as claimed in claim 1, it is characterized in that adopting the colloidal sol technology to produce nano level brown iron oxide after, be placed in the silica tube of sealing, feed liquefied gas, drain air, be warmed up to 400 ℃, promptly obtaining particle diameter is 10～30nm nano level Fe
5C
2Powder.
5, the iron carbide nano material made of preparation method as claimed in claim 1 is characterized in that, the particle diameter of synthetic iron carbide nano powder is at 10～30nm
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92105939 CN1033159C (en) | 1992-07-20 | 1992-07-20 | Process for preparing nanometer material of carburetted steel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92105939 CN1033159C (en) | 1992-07-20 | 1992-07-20 | Process for preparing nanometer material of carburetted steel |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1083024A true CN1083024A (en) | 1994-03-02 |
| CN1033159C CN1033159C (en) | 1996-10-30 |
Family
ID=4941671
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92105939 Expired - Fee Related CN1033159C (en) | 1992-07-20 | 1992-07-20 | Process for preparing nanometer material of carburetted steel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1033159C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100410170C (en) * | 2005-12-31 | 2008-08-13 | 武汉科技大学 | Method for preparing iron carbide using iron ore concentrate powder |
| CN1454851B (en) * | 2002-04-17 | 2011-11-02 | 国际商业机器公司 | Synthesizing of magnetite nano particles and method for forming iron-base nano material |
| CN103030143A (en) * | 2012-08-09 | 2013-04-10 | 北京大学 | Iron carbide particle, and fabrication method and application thereof |
| CN106395913A (en) * | 2016-08-26 | 2017-02-15 | 天津大学 | Ferromagnetic nano alpha-Fe2O3 with iron defects, and preparation method thereof |
| CN108217654A (en) * | 2018-01-31 | 2018-06-29 | 杨汉玉 | A kind of preparation method of catalyst for preparing hydrogen and catalyzing manufacturing of hydrogen method |
-
1992
- 1992-07-20 CN CN 92105939 patent/CN1033159C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1454851B (en) * | 2002-04-17 | 2011-11-02 | 国际商业机器公司 | Synthesizing of magnetite nano particles and method for forming iron-base nano material |
| CN100410170C (en) * | 2005-12-31 | 2008-08-13 | 武汉科技大学 | Method for preparing iron carbide using iron ore concentrate powder |
| CN103030143A (en) * | 2012-08-09 | 2013-04-10 | 北京大学 | Iron carbide particle, and fabrication method and application thereof |
| CN103030143B (en) * | 2012-08-09 | 2015-02-18 | 北京大学 | Iron carbide particle, and fabrication method and application thereof |
| CN106395913A (en) * | 2016-08-26 | 2017-02-15 | 天津大学 | Ferromagnetic nano alpha-Fe2O3 with iron defects, and preparation method thereof |
| CN108217654A (en) * | 2018-01-31 | 2018-06-29 | 杨汉玉 | A kind of preparation method of catalyst for preparing hydrogen and catalyzing manufacturing of hydrogen method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1033159C (en) | 1996-10-30 |
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