CN102899591B - High-oxygen-content iron-based amorphous composite powder and preparation method thereof - Google Patents
High-oxygen-content iron-based amorphous composite powder and preparation method thereof Download PDFInfo
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- CN102899591B CN102899591B CN201210411503.9A CN201210411503A CN102899591B CN 102899591 B CN102899591 B CN 102899591B CN 201210411503 A CN201210411503 A CN 201210411503A CN 102899591 B CN102899591 B CN 102899591B
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Abstract
The invention discloses high-oxygen-content iron-based amorphous composite powder and a preparation method thereof. The preparation method comprises the following steps: proportioning the following materials in atom percentage: 74-78at.% of Fe, 4-6at.% of Cu, 7-9at.% of P, 5-7at.% of C, 1-3at.% of B and 4-6at.% of O; mixing; and performing high-energy ball milling to obtain the high-oxygen-content iron-based amorphous composite powder, wherein the volume fraction of an amorphous phase exceeds 90%, and the microstructure takes the amorphous phase as the base and takes alpha-Fe nanocrystal as a second phase. According to the invention, the designed composite powder has high amorphism forming capacity, a wide supercooled liquid phase region is obtained, and the adverse effect of oxygen on iron-based alloy amorphism forming is overcome, thereby being beneficial to the design of a new alloy system. The method is simple and convenient to operate, and can provide a raw material for the preparation of a high-density big amorphous composite material based on a sintering method.
Description
Technical field
The present invention relates to the preparation method of non-crystaline amorphous metal and matrix material thereof, specifically refer to Fe-based amorphous composite powder of a kind of rich oxygen content and preparation method thereof.
Background technology
Fe-based amorphous alloy has mechanical property and excellent magnetic property and the corrosion resistance nature that high strength, high rigidity, high elastic coefficient, high-wearing feature etc. are excellent, but also has lower-cost advantage, thereby causes gradually investigator's extensive concern.Along with deepening continuously of research, the size of Fe-based Bulk Metallic Glass is increasing, as functional materials and structured material, in fields such as electronic industry, petrochemical complex, magneticsubstance, war industrys, is applied.At present, Fe-based amorphous alloy and matrix material thereof mainly adopt casting and powder metallurgic method preparation.Yet because the amorphous formation ability of ferrous alloy itself is lower, and it is very high to adopt casting preparation to require for rate of cooling, thereby the acquisition of Fe-based amorphous alloy and matrix material thereof is comparatively difficult, and the maximum diameter that can reach only limits to 16 millimeters.
Powder metallurgic method can overcome the less defect of block materials size prepared by casting to a great extent, can in wider alloy system, wider composition range, prepare Fe-based amorphous alloy and the matrix material thereof that geometrical dimension is larger.So, first adopt Amorphous Phase Synthesized by Mechanical Alloying powder, then adopt the fixed amorphous powders of powder metallurgy technology such as pressure sintering, extrusion process and discharge plasma sintering, become a kind of feasible method of preparing block Fe-based amorphous alloy and matrix material thereof.
Yet, adopting casting and powder metallurgic method to prepare in the process of non-crystaline amorphous metal, can inevitably introduce impurity oxygen.At casting, prepare in non-crystaline amorphous metal, paper " the suitably enhancing impact of oxygen level on iron-base large-block amorphous alloy amorphous formation ability " (Glass-forming ability enhanced by proper additions of oxygen in a Fe-based bulk metallic glass, H.X.Li, J.E.Gao, Z.B.Jiao, Y.Wu, and Z.P.Lu, Appl.Phys.Lett., 2009,95:161905.) at Fe
73mo
3.0c
7.0si
3.3b
5.0p
8.7in alloy, introduce the oxygen of different content, result confirms to be conducive to improve when oxygen level is less than 2000appm (0.2at.%) amorphous formation ability of this alloy, surpass 2000appm and can destroy the stability of liquid phase, cause forming more stable containing oxygen crystal phase, thereby reduce the amorphous formation ability of this alloy.Yet, at mechanical alloying method, prepare in non-crystaline amorphous metal, paper " impact of oxygen on ZrAlCuNi non-crystaline amorphous metal supercooling liquid phase region viscosity " (Influence of oxygen on the viscosity of Zr – Al – Cu – Ni metallic glasses in the undercooled liquid region, A.KUbler, J.Eckert, A.Gebert, and L.Schultz, J.Appl.Phys., 1998,83:3438) confirm that working as oxygen level is 2at.%, still can obtain non-crystaline amorphous metal completely.Therefore, compare casting, the ultimate value of the oxygen level that mechanical alloying permission is introduced is larger, yet, when surpassing the oxygen of introducing after a certain ultimate value, oxygen level can increase amorphous powder in the viscosity of high temperature (or supercooling liquid phase region), reduce the width of supercooling liquid phase region, this,, by promoting to form other oxygenatedchemicals, hinders the trend that powdered alloy changes to non-crystalline state.
Therefore, whether can be by selecting suitable alloying constituent, material preparation method and processing parameter thereof, overcome the disadvantageous effect of oxygen to ferrous alloy amorphous formation, synthetic Fe-based amorphous alloy and the matrix material thereof with wider supercooling liquid phase region, elevated oxygen level, will have very important Science and engineering meaning.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art part, by the appropriate design of alloying constituent proportioning and the optimization of processing parameter thereof, provide Fe-based amorphous composite powder of a kind of rich oxygen content and preparation method thereof.
The object of the invention is achieved through the following technical solutions:
A Fe-based amorphous composite powder for rich oxygen content, is characterized in that: this composite powder contains iron, copper, phosphorus, carbon, boron, oxygen, heterogeneous microstructure is for take the composite structure that amorphous phase is second-phase as matrix, nanocrystalline α-Fe, and amorphous supercooling liquid phase region width range is 25～32K; Concrete component and be by atomic percent content: Fe74～77at.%, Cu3～6at.%, P7～9at.%, C5～7at.%, B1～3at.%, O3～6at.%, and the inevitable trace impurity of introducing.
A preparation method for the Fe-based amorphous composite powder of rich oxygen content, is characterized in that: the method comprises the steps and processing condition:
Step 1: join powder
Iron, cupric oxide, ferrophosphorus powder, carbon, boron powder starting material are joined to powder by following atomic percent consumption: Fe74～77at.%, Cu3～6at.%, P7～9at.%, C5～7at.%, B1～3at.%, O3～6at.%;
Step 2: mixed powder
The iron of proportioning in step 1, cupric oxide, ferrophosphorus powder, carbon, boron powder starting material are put into mixed powder machine and mix at least 8 hours, obtain iron content, copper, phosphorus, carbon, boron, the mixed powder of oxygen constituent element;
Step 3: high-energy ball milling
Mixed powder in step 2 is placed in to high energy ball mill and carries out high-energy ball milling, ball-milling technology condition is as follows:
Ball-grinding machine: high energy ball mill
Rotational speed of ball-mill: 180～300r/min
The high-purity argon gas protection of milling atmosphere: >99.9%
Ball-milling Time: 80～150h
Through ball milling, form amorphous volume mark and surpass 90% iron-based powder, be a kind of Fe-based amorphous composite powder of rich oxygen content.
It is that high-energy ball milling changes at solid-state lower generation non-equilibrium structure that preparation principle of the present invention is to utilize mechanical alloying, along with the increase of Ball-milling Time, and the continuous refinement of crystal grain, lattice distortion increases, and is accompanied by the increase gradually of amorphous phase.From the angle of energy, the energy sum that total free energy that the basic reason that amorphous phase forms is crystalline phase and the lattice defect producing due to ball milling increase is greater than the free energy of amorphous phase, makes crystalline phase to amorphous phase transition.And a certain amount of oxygen existing with cupric oxide form of introducing decomposes in mechanical milling process, and be evenly distributed among powder, by the control of ball-milling technology, finally obtain having the Fe-based amorphous composite powder of wider supercooling liquid phase region, elevated oxygen level.
The present invention compared with prior art, has the following advantages:
1, preparation method of the present invention, by controlling rotational speed of ball-mill, milling atmosphere and Ball-milling Time, can obtain Fe-based amorphous composite powder, and for sintering subsequently, preparing block alloy provides starting material, is conducive to prepare high fine and close iron-base large-block amorphous matrix material.
2, the present invention adopts the method for mechanical alloying (high-energy ball milling), can in wider alloy system, wider composition range, prepare Fe-based amorphous alloy or amorphous composite powder, and compare casting, the ultimate value of the oxygen level that mechanical alloying permission is introduced is larger, and high oxygen level is not destroyed the amorphous formation ability of alloy to a great extent.Therefore, the present invention has overcome the disadvantageous effect of oxygen to ferrous alloy amorphous formation, is conducive to design new alloy system, obtains Fe-based amorphous alloy and the matrix material thereof of wider supercooling liquid phase region, elevated oxygen level.
3, the high-energy ball-milling process course of processing of the present invention is simple, easy to operate, and lumber recovery is high, save material; , combine with follow-up consolidation means meanwhile, be expected to obtain larger sized matrix material, at structured material and field of magnetic material, have broad application prospects.
Accompanying drawing explanation
Fig. 1 is differential scanning calorimetric analysis (DSC) the curve comparison diagram of the Fe-based amorphous composite powder that in embodiment 4, different High Energy Ball Milling Times obtain
Embodiment
By following embodiment, the invention will be further described, but embodiments of the present invention are not limited only to this.
Embodiment 1
Step 1: join powder
Iron powder, cupric oxide powder, ferrophosphorus powder, carbon dust, boron powder are joined to powder by following atomic percent consumption: content is Fe77at.%, Cu3at.%, P9at.%, C6at.%, B1at.%, O3at.%, and the inevitable trace impurity of introducing.Iron, carbon, boron all add with simple substance form, and phosphorus adds with the form of ferrophosphorus compound, and copper and oxygen add with the form of cupric oxide compound.Wherein, the particle size of iron powder, cupric oxide powder, carbon dust, boron powder is about 48 μ m, purity >99.9%, and the particle size of ferrophosphorus powder is about 14 μ m, purity >99.9%.
Step 2: mixed powder
The iron of proportioning in step 1, cupric oxide, ferrophosphorus powder, carbon, boron powder are put into the mixed powder machine of V-type and mix 10 hours, obtaining nominal composition is Fe
77cu
4p
9c
6b
1o
3mixed powder.
Step 3: high-energy ball milling
To described in step 2, be Fe
77cu
4p
9c
6b
1o
3it is that the planetary ball mill of QM-2SP20 carries out high-energy ball milling that mixed powder is placed in model, and the ball-milling mediums such as planetary ball mill machine jar body and grinding ball material are stainless steel, and ball radius is respectively 15,10 and 6mm, and their weight ratio is 1:3:1; High-energy-milling parameter is as follows: in ball grinder, fill high-purity argon gas (99.999%, 0.5Mpa) protection, ratio of grinding media to material is 10:1, rotating speed is 180r/min.In mechanical milling process; described sampling detection time is high-energy ball milling the 2nd; 6; 10; 15 and 20h, after 20h, every 10h shuts down cooling powder to room temperature, and X-ray diffraction analysis (XRD) and differential scanning calorimetric analysis (DSC) are carried out in sampling; after sampling, continue high-energy ball milling, until form amorphous volume mark, surpass 90% iron-based powder.XRD and dsc analysis result show: the powder amorphous content of ball milling 150h is maximum, surpass the generation of 150h amorphous phase partially-crystallized, the amorphous transition temperature of 150h powder is 795K, and crystallization temperature is 827K, supercooling liquid phase region is 32K, and the area of exothermic peak is 7.058J/g.The powder transmission electron microscope picture of ball milling 150h confirms that this powder is to take the Fe-based amorphous composite powder of amorphous phase as matrix, the nanocrystalline rich oxygen content as second-phase of the α-Fe of take.
Embodiment 2
Step 1: join powder
Iron, cupric oxide, ferrophosphorus powder, carbon, boron powder are joined to powder by following atomic percent consumption: content is Fe75at.%, Cu4at.%, P7at.%, C7at.%, B3at.%, O4at.%, and the inevitable trace impurity of introducing.Iron, carbon, boron all add with simple substance form, and phosphorus adds with the form of ferrophosphorus compound, and copper and oxygen add with the form of cupric oxide compound.Wherein, the particle size of iron powder, cupric oxide powder, carbon dust, boron powder is about 48 μ m, purity >99.9%, and the particle size of ferrophosphorus powder is about 14 μ m, purity >99.9%.
Step 2: mixed powder
The iron of proportioning in step 1, cupric oxide, ferrophosphorus powder, carbon, boron powder are put into the mixed powder machine of V-type and mix 12 hours, obtaining nominal composition is Fe
75cu
4p
7c
7b
3o
4mixed powder.
Step 3: high-energy ball milling
By the Fe described in step 2
75cu
4p
7c
7b
3o
4mixed powder is placed in planetary ball mill and carries out high-energy ball milling, and the model of planetary ball mill, ball-milling medium, ratio of grinding media to material are all with embodiment 1; High-energy-milling parameter is as follows: in ball grinder, fill high-purity argon gas (99.999%, 0.5Mpa) protection, rotating speed is 300r/min.In mechanical milling process, described sampling detection time and detection means, with embodiment 1, continue high-energy ball milling after sampling, until form amorphous volume mark, surpass 90% iron-based powder.XRD and dsc analysis result show that the powder amorphous content of ball milling 80h is maximum, and its amorphous transition temperature is 805K, and crystallization temperature is 830K, and supercooling liquid phase region is 25K, and the area of exothermic peak is 5.875J/g.The powder transmission electron microscope picture of ball milling 80h confirms that this powder is to take the Fe-based amorphous composite powder of amorphous phase as matrix, the nanocrystalline rich oxygen content as second-phase of the α-Fe of take.
Embodiment 3
Step 1: join powder
Iron, cupric oxide, ferrophosphorus powder, carbon, boron powder are joined to powder by following atomic percent consumption: content is Fe76at.%, Cu5at.%, P8at.%, C5at.%, B1at.%, O5at.%, and the inevitable trace impurity of introducing.Iron, carbon, boron all add with simple substance form, and phosphorus adds with the form of ferrophosphorus compound, and copper and oxygen add with the form of cupric oxide compound.Wherein, the particle size of iron powder, cupric oxide powder, carbon dust, boron powder is about 48 μ m, purity >99.9%, and the particle size of ferrophosphorus powder is about 14 μ m, purity >99.9%.
Step 2: mixed powder
The iron of proportioning in step 1, cupric oxide, ferrophosphorus powder, carbon, boron powder are put into the mixed powder machine of V-type and mix 16 hours, obtaining nominal composition is Fe
76cu
5p
8c
5b
1o
5mixed powder.
Step 3: high-energy ball milling
By the Fe described in step 2
76cu
5p
8c
5b
1o
5mixed powder is placed in planetary ball mill and carries out high-energy ball milling, and the model of planetary ball mill, ball-milling medium, ratio of grinding media to material are all with embodiment 1; High-energy-milling parameter is as follows: in ball grinder, fill high-purity argon gas (99.999%, 0.5Mpa) protection, ratio of grinding media to material is 10:1, rotating speed is 228r/min.In mechanical milling process, in mechanical milling process, described sampling detection time and detection means, with embodiment 1, continue high-energy ball milling after sampling, until form amorphous volume mark, surpass 90% iron-based powder.XRD and dsc analysis result show: the powder amorphous content of ball milling 120h is maximum, and its amorphous transition temperature is 808K, and crystallization temperature is 835K, and supercooling liquid phase region is 27K, and the area of exothermic peak is 5.313J/g.The powder transmission electron microscope picture of ball milling 120h confirms that this powder is to take the Fe-based amorphous composite powder of amorphous phase as matrix, the nanocrystalline rich oxygen content as second-phase of the α-Fe of take.
Embodiment 4
Step 1: join powder
Iron, cupric oxide, ferrophosphorus powder, carbon, boron powder are joined to powder by following atomic percent consumption: content is Fe74at.%, Cu6at.%, P7at.%, C5at.%, B2at.%, O6at.%, and the inevitable trace impurity of introducing.Iron, carbon, boron all add with simple substance form, and phosphorus adds with the form of ferrophosphorus compound, and copper and oxygen add with the form of cupric oxide compound.Wherein, the particle size of iron powder, cupric oxide powder, carbon dust, boron powder is about 48 μ m, purity >99.9%, and the particle size of ferrophosphorus powder is about 14 μ m, purity >99.9%.
Step 2: mixed powder
The iron of proportioning in step 1, cupric oxide, ferrophosphorus powder, carbon, boron powder are put into the mixed powder machine of V-type and mix 20 hours, obtaining nominal composition is Fe
74cu
6p
7c
5b
2o
6mixed powder.
Step 3: high-energy ball milling
By the Fe described in step 2
74cu
6p
7c
5b
2o
6mixed powder is placed in planetary ball mill and carries out high-energy ball milling, and the model of planetary ball mill, ball-milling medium, ratio of grinding media to material are all with embodiment 1; High-energy-milling parameter is as follows: in ball grinder, fill high-purity argon gas (99.999%, 0.5MPa) protection, ratio of grinding media to material is 10:1, rotating speed is 228r/min.In mechanical milling process, described sampling detection time and detection means, with embodiment 1, continue high-energy ball milling after sampling, until form amorphous volume mark, surpass 90% iron-based powder.
As shown in the DSC curve of Fig. 1, in 837～865K temperature range, there is an obvious exothermic peak, this peak correspondence the crystallization of amorphous phase.When High Energy Ball Milling Time is at 60～120h, increase along with Ball-milling Time, the intensity of exothermic peak and area strengthen gradually and peak value moves to right thereupon, the amorphous phase of this explanation powder starts to form, and the volume fraction of amorphous phase increases gradually, when ball milling 120h, the intensity of exothermic peak is maximum, peak area is maximum, shows that now the volume fraction of amorphous phase reaches maximum value.Continue to be milled to 150h, exothermic peak intensity and area reduce on the contrary, and this is because part amorphous phase, under high-energy ball milling effect, crystallization has occurred.By tangent method, determined the characteristic temperature of amorphous phase, the amorphous transition temperature of the Fe-based amorphous composite powder of ball milling 120h is 810K, and crystallization change temperature is 837K, and supercooling liquid phase region width reaches 27K, and the area of exothermic peak is 6.109J/g.Transmission electron microscope picture shows that the iron-based powder of ball milling 120h is to take the Fe-based amorphous composite powder of amorphous phase as matrix, the nanocrystalline rich oxygen content as second-phase of the α-Fe of take.
Claims (2)
1. a Fe-based amorphous composite powder for rich oxygen content, is characterized in that: this composite powder contains iron, copper, phosphorus, carbon, boron, oxygen, heterogeneous microstructure is for take the composite structure that amorphous phase is second-phase as matrix, nanocrystalline α-Fe, and amorphous supercooling liquid phase region width range is 25～32K; Concrete component and be by atomic percent content: Fe74～77at.%, Cu3～6at.%, P7～9at.%, C5～7at.%, B1～3at.%, O3～6at.%, and the inevitable trace impurity of introducing.
2. a preparation method for the Fe-based amorphous composite powder of rich oxygen content, is characterized in that: the method comprises the steps and processing condition:
Step 1: join powder
Iron, cupric oxide, ferrophosphorus powder, carbon, boron powder starting material are joined to powder by following atomic percent consumption: Fe74～77at.%, Cu3～6at.%, P7～9at.%, C5～7at.%, B1～3at.%, O3～6at.%;
Step 2: mixed powder
The iron of proportioning in step 1, cupric oxide, ferrophosphorus powder, carbon, boron powder starting material are put into mixed powder machine and mix at least 8 hours, obtain iron content, copper, phosphorus, carbon, boron, the mixed powder of oxygen constituent element;
Step 3: high-energy ball milling
Mixed powder in step 2 is placed in to high energy ball mill and carries out high-energy ball milling, ball-milling technology condition is as follows:
Ball-grinding machine: high energy ball mill
Rotational speed of ball-mill: 180～300r/min
The high-purity argon gas protection of milling atmosphere: >99.9%
Ball-milling Time: 80～150h
Through ball milling, form amorphous volume mark and surpass 90% iron-based powder, be a kind of Fe-based amorphous composite powder of rich oxygen content.
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| CN105586548B (en) * | 2016-02-03 | 2017-07-18 | 北京科技大学 | Have block Fe-based amorphous alloy of high intensity and high-ductility and preparation method thereof concurrently |
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