CN103331449B - Ultra-fine Grained/micron crystal block body iron material of the two size distribution of a kind of super-high-plasticity and preparation method thereof - Google Patents
Ultra-fine Grained/micron crystal block body iron material of the two size distribution of a kind of super-high-plasticity and preparation method thereof Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 153
- 239000000463 material Substances 0.000 title claims abstract description 62
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 56
- 239000013078 crystal Substances 0.000 title claims abstract description 41
- 238000009826 distribution Methods 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 79
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 17
- 239000011159 matrix material Substances 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 32
- 229910052786 argon Inorganic materials 0.000 claims description 16
- 239000010935 stainless steel Substances 0.000 claims description 14
- 229910001220 stainless steel Inorganic materials 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims description 4
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 4
- 239000000843 powder Substances 0.000 abstract description 25
- 238000011084 recovery Methods 0.000 abstract description 2
- 230000006835 compression Effects 0.000 description 5
- 238000007906 compression Methods 0.000 description 5
- 230000003064 anti-oxidating effect Effects 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000003701 mechanical milling Methods 0.000 description 4
- 238000009707 resistance sintering Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 229910000640 Fe alloy Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
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Abstract
The invention discloses the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity, its microstructure with the brilliant α-Fe of block micron for matrix phase, with the shaft-like α-Fe such as Ultra-fine Grained and Ultra-fine Grained acicular α-Fe for wild phase, comprehensive mechanical property is excellent, plastic deformation ability is extremely strong, has a good application prospect.The invention also discloses the preparation method of the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity, first by initial high-purity iron powder through high-energy ball milling to manocrystalline powders, then discharge plasma sintering system Fast Sintering is adopted, sintering temperature Ts:1253K≤Ts≤1335K, sintering time: 14 ~ 26min, sintering pressure: 40 ~ 500MPa.The inventive method is simple, easy to operate, and its crystallite dimension is controlled, and lumber recovery is high, save material and near-net forming.
Description
Technical field
The present invention relates to Ultra-fine Grained/micron crystalline metal material, particularly Ultra-fine Grained/micron crystal block body the iron material and preparation method thereof of the two size distribution of a kind of super-high-plasticity.
Background technology
Iron and Iron Alloy has low price, aboundresources, excellent performance and the feature such as easily to accomplish scale production, and thus becomes the material be most widely used at present.But the comprehensive mechanical property of high speed development to Iron and Iron Alloy of modern industry proposes more and more higher requirement, adopt suitable preparation method to obtain important subject that high comprehensive mechanical property has become material supplier author.Refined crystalline strengthening improves the important method of intensity and plasticity, can obtain micron crystalline substance, Ultra-fine Grained and nanocrystalline, make the intensity of material compare traditional casting coarse grain material and improve exponentially by crystal grain thinning means.At present, prepare Ultra-fine Grained iron material and mainly contain following several method: (1) utilizes the method for Equal-channel Angular Pressing, the ultra-fine crystal block body iron material of low-intensity high-ductility is obtained by large plastometric set crystal grain thinning, its crystallite dimension is 200 ~ 400nm, under trus stress strained condition, compressed rupture strength is 800MPa, plastic strain reaches 30%(Gertsman V.Y., Birringer R., Valiev R.Z., et al., Scripta Metall μ rgica et Materialia, 1994,30 (2): 229-234); (2) utilize cold pressing and hot-press method low temperature (683K ~ 863K) obtain the inductile Ultra-fine Grained of high strength or bulk nanometer iron material.When sintering temperature is 863K, obtain ultra-fine crystal block body iron material, crystallite dimension is 268nm, and under trus stress strained condition, compressed rupture strength is 1600MPa, and plastic strain is 12%; When sintering temperature is 683K, obtain bulk nanometer iron material, crystallite dimension is 138nm, under trus stress strained condition, compressed rupture strength is 2500MPa, plastic strain is 6%(Jia D., Ramesh K.T., Ma E..Acta Materialia, 2003,51 (12): 3495-3509); (3) discharge plasma sintering technique is utilized, the mode adopting stepped pressure is under the condition of 993K in sintering temperature, prepared two scale nanometers brilliant α-Fe/ micron brilliant α-Fe block iron material (wherein, micron brilliant α-Fe content is little) of high strength and high-ductility, under trus stress strained condition, compressed rupture strength is up to 2249MPa, plastic strain is 40%(SrinivasaraoB., Oh-ishi K., Ohk μ bo T., et al.Scripta Mater., 2008,58:759 – 762).
But when metal grain size is refined to nanoscale, although the intensity of material improves exponentially, plasticity but significantly declines.As shown in the nano crystal iron performance that Jia D. etc. obtains in experiment, although nano crystal iron has the intensity up to 2500MPa, plastic strain only has 6%.Except the method that crystal grain thinning is toughness reinforcing, according to the classical theory of structures shape performance, the composite preparing different scale and form is expected to the plasticity improving material, obtains good comprehensive mechanical property.The iron material of the brilliant two size distribution of the nanocrystalline and micron that Srinivasarao B. etc. obtain not only has the fracture strength up to 2249MPa, and plastic strain also reaches 40%.As can be seen here, the preparation method exploring the super fine crystal material of the two yardsticks of preparation or multiple dimensioned distribution is of great significance for the comprehensive mechanical property tool improving metal material.
In sum, the most high-ductility of the Ultra-fine Grained iron material utilizing various method to prepare can reach 40%(ScriptaMater., 2008,58:759 – 762), but the experiment sintering temperatures used such as Srinivasarao B. be iron ppolymorphism transition temperature (1185K) below, and the stepped pressure mode cumbersome adopted, be not easy to the densified of finished product.
Summary of the invention
In order to overcome the above-mentioned shortcoming of prior art with not enough, the object of the present invention is to provide the preparation method of the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of a kind of super-high-plasticity, the Ultra-fine Grained/micron crystal block body iron material of preparation realize microstructure crystal grain evenly, the advantage of nearly complete fine and close, super-high-plasticity and two size distribution.
Ultra-fine Grained/micron crystal block body the iron material of the two size distribution of the high-ductility that another object of the present invention is to provide above-mentioned preparation method to obtain.
Object of the present invention is achieved through the following technical solutions:
A preparation method for the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity, comprises the following steps:
(1) high-energy ball milling prepares nanocrystalline iron powder: under argon shield condition, pure iron powder is placed in stainless steel ball grinding media and carries out high-energy ball milling, until obtain the nanocrystalline iron powder that crystallite dimension is 8 ~ 12nm;
(2) discharge plasma sintering prepares the block iron material of the two size distribution of super-high-plasticity: nanocrystalline iron powder step (1) obtained loads in mould; under argon shield condition; adopt discharge plasma sintering; obtain the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity, wherein Fast Sintering process conditions are as follows:
Agglomerating plant: discharge plasma sintering system;
Sintering current type: pulse current;
Sintering temperature Ts:1253K≤Ts≤1335K;
Sintering time: 14 ~ 26min;
Sintering pressure: 40 ~ 500MPa.
In step (2) described discharge plasma sintering, heating rate is 54 ~ 235K/min, and temperature retention time controls at 0 ~ 10min.
In step (2) described discharge plasma sintering, when adopting graphite jig, sintering pressure is 40 ~ 50MPa, and when adopting tungsten carbide die, sintering pressure is 50 ~ 500MPa.
Ultra-fine Grained/micron crystal block body the iron material of the two size distribution of the high-ductility that above-mentioned preparation method obtains, its microstructure with the brilliant α-Fe of block micron for matrix phase, with the shaft-like α-Fe such as Ultra-fine Grained and Ultra-fine Grained acicular α-Fe for wild phase.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) Ultra-fine Grained/micron crystal block body iron material of two size distributions that prepared by the present invention have microstructure crystal grain evenly, the advantage of nearly complete fine and close, super-high-plasticity, comprehensive mechanical property is excellent, its room temperature compressed rupture strength and breaking strain reach 734MPa and more than 58% respectively, in plasticity, be especially far superior to the block iron material of other structures.
(2) preparation method of the Ultra-fine Grained/micron crystal block body iron material of of the present invention pair of size distribution, process is simple, easy to operate, and lumber recovery is high, save material and near-net forming; Meanwhile, moulding material size is comparatively large, material internal interface cleanness and its crystallite dimension is controlled.
(3) preparation method of the Ultra-fine Grained/micron crystal block body iron material of of the present invention pair of size distribution, when heating rate is between 54 ~ 235K/min, and temperature retention time is when controlling in 0 ~ 10min, the change of temperature retention time and heating rate does not all have a significant effect to plasticity, and the uniformity of product is good.
(4) preparation method of the Ultra-fine Grained/micron crystal block body iron material of of the present invention pair of size distribution, the present invention can prepare large-size, diameter is greater than the material of 20mm, substantially can meet the application requirement as new structure part material, be with a wide range of applications.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity prepared by embodiment 1.
Fig. 2 is the room temperature compression true stress-strain curve of the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity prepared by embodiment 1.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
The preparation method of the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity of the present embodiment, comprises the following steps:
(1) high-energy ball milling prepares nanocrystalline iron powder: pure iron powder is placed in stainless steel ball grinding media and carries out high-energy ball milling, until obtain the nanocrystalline iron powder of crystallite dimension about 8 ~ 12nm:
Initial powder is high-purity electrolytic iron powder (99.5wt.%, granularity is 38um), initial iron powder and stainless steel abrading-ball are put into together stainless steel jar mill and (between ball grinder and lid, use " O " type seal ring seal, ball radius is respectively 15mm, 10mm and 6mm, its weight ratio is 1:3:1, and abrading-ball and powder weight ratio are 10:1).In order to anti-oxidation, be filled with high-purity argon gas in ball grinder and carry out protecting (99.99%, 0.5MPa).Finally, the ball grinder being filled with argon shield being placed on model is QM-2SP20 planetary ball mill carries out high-energy ball milling (rotating speed is 3.8s
-1).After every ball milling 5h shuts down and is cooled to room temperature in mechanical milling process, take out a certain amount of powder (about 5g), for the various characterization tests of powder, until acquisition crystallite dimension is about the nanocrystalline iron powder of 10nm.
(2) discharge plasma sintering prepares the block iron material of the two size distribution of super-high-plasticity: it is in the graphite sintering mould of Φ 10mm that the nanocrystalline iron powder of 8g step (1) obtained loads diameter, by the nanocrystalline iron powder of the first precompressed of positive and negative graphite electrode to 50MPa, be evacuated down to 10
-3pa, adopts discharge plasma sintering under the condition of argon shield, and obtain the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity, wherein Fast Sintering process conditions are as follows:
Agglomerating plant: Dr.Sintering SPS-825 discharge plasma sintering system
Sintering current type: pulse current
The dutycycle of pulse current: 12:2
Sintering temperature Ts:1253K
Sintering time: 4min is warmed up to 373K, then 9min, and to be warmed up to 1233K(heating rate be 97K/min), then 1min be heated to 1253K and be incubated 10min;
Sintering pressure: 50MPa;
Carry out Fast Sintering to powder, in resistance sintering and cooling procedure, pressure remains at 50MPa, can obtain Ultra-fine Grained/micron crystal block body iron material that diameter is the two size distribution of super-high-plasticity of Φ 10mm.Scanning electron microscope (SEM) photograph as shown in Figure 1 shows, iron material (if sintering mold diameter is large, iron material size is also just large).Scanning electron microscope (SEM) photograph as shown in Figure 1 shows, its microstructure is with A in block micron brilliant α-Fe(figure) for matrix, with B in the shaft-like α-Fe(figure such as Ultra-fine Grained) and Ultra-fine Grained acicular α-Fe(figure in C) for wild phase.Further transmission electron microscope analysis shows, the crystallite dimension of block α-Fe is 2 ~ 3 μm, is 700 ~ 900nm etc. the crystallite dimension of shaft-like α-Fe, and the width of acicular α-Fe is 150 ~ 160nm.Room temperature compression true stress-strain curve as shown in Figure 2 shows, true fracture strength and breaking strain are respectively 743MPa and 59%.
Embodiment 2
The preparation method of the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of a kind of super-high-plasticity of the present embodiment, comprises the following steps:
(1) high-energy ball milling prepares nanocrystalline iron powder: pure iron powder is placed in stainless steel ball grinding media and carries out high-energy ball milling, until obtain the nanocrystalline iron powder of crystallite dimension about 8 ~ 12nm:
Initial powder is high-purity electrolytic iron powder (99.5wt.%, granularity is 38um), initial iron powder and stainless steel abrading-ball are put into together stainless steel jar mill and (between ball grinder and lid, use " O " type seal ring seal, ball radius is respectively 15mm, 10mm and 6mm, its weight ratio is 1:3:1, and abrading-ball and powder weight ratio are 10:1).In order to anti-oxidation, be filled with high-purity argon gas in ball grinder and carry out protecting (99.99%, 0.5MPa).Finally, the ball grinder being filled with argon shield being placed on model is QM-2SP20 planetary ball mill carries out high-energy ball milling (rotating speed is 3.8s
-1).After every ball milling 5h shuts down and is cooled to room temperature in mechanical milling process, take out a certain amount of powder (about 5g), for the various characterization tests of powder, until acquisition crystallite dimension is about the nanocrystalline iron powder of 10nm.
(2) discharge plasma sintering prepares the block iron material of the two size distribution of super-high-plasticity: it is in the graphite sintering mould of Φ 10mm that the nanocrystalline iron powder of 8g step (1) obtained loads diameter, by the nanocrystalline iron powder of the first precompressed of positive and negative graphite electrode to 40MPa, be evacuated down to 10
-3pa, adopts discharge plasma sintering under the condition of argon shield, and obtain the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity, wherein Fast Sintering process conditions are as follows:
Agglomerating plant: Dr.Sintering SPS-825 discharge plasma sintering system
Sintering current type: pulse current
The dutycycle of pulse current: 12:2
Sintering temperature Ts:1283K
Sintering time: 4min is warmed up to 373K, then 9min, and to be warmed up to 1263K(heating rate be 97K/min), then 1min be heated to 1283K
Sintering pressure: 40MPa
Fast Sintering is carried out to powder, in resistance sintering and cooling procedure, pressure remains at 40MPa, Ultra-fine Grained/micron crystal block body iron material that diameter is the two size distribution of super-high-plasticity of Φ 10mm can be obtained, its microstructure with the brilliant α-Fe of block micron for matrix phase, with the shaft-like α-Fe such as Ultra-fine Grained and Ultra-fine Grained acicular α-Fe for wild phase, wherein the crystallite dimension of block α-Fe is 2 ~ 4 μm, be 500 ~ 700nm etc. the crystallite dimension of shaft-like α-Fe, the width of acicular α-Fe is 120 ~ 130nm.Corresponding room temperature compression true stress-strain curve shows, the room temperature compressed rupture strength of block iron material and breaking strain are respectively 955MPa and 58%.
Embodiment 3
(1) high-energy ball milling prepares nanocrystalline iron powder: pure iron powder is placed in stainless steel ball grinding media and carries out high-energy ball milling, until obtain the nanocrystalline iron powder of crystallite dimension about 8 ~ 12nm:
Initial powder is high-purity electrolytic iron powder (99.5wt.%, granularity is 38um), initial iron powder and stainless steel abrading-ball are put into together stainless steel jar mill and (between ball grinder and lid, use " O " type seal ring seal, ball radius is respectively 15mm, 10mm and 6mm, its weight ratio is 1:3:1, and abrading-ball and powder weight ratio are 10:1).In order to anti-oxidation, be filled with high-purity argon gas in ball grinder and carry out protecting (99.99%, 0.5MPa).Finally, the ball grinder being filled with argon shield being placed on model is QM-2SP20 planetary ball mill carries out high-energy ball milling (rotating speed is 3.8s
-1).After every ball milling 5h shuts down and is cooled to room temperature in mechanical milling process, take out a certain amount of powder (about 5g), for the various characterization tests of powder, until acquisition crystallite dimension is about the nanocrystalline iron powder of 10nm.
(2) discharge plasma sintering prepares the block iron material of the two size distribution of super-high-plasticity: it is in the tungsten carbide burning sintering mold of Φ 10mm that the nanocrystalline iron powder of 8g step (1) obtained loads diameter, by the nanocrystalline iron powder of the first precompressed of positive and negative tungsten carbide electrode to 200MPa, be evacuated down to 10
-3pa, adopts discharge plasma sintering under the condition of argon shield, and obtain the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity, wherein Fast Sintering process conditions are as follows:
Agglomerating plant: Dr.Sintering SPS-825 discharge plasma sintering system
Sintering current type: pulse current
The dutycycle of pulse current: 12:2
Sintering temperature Ts:1253K
Sintering time: 4min is warmed up to 373K, then 16min, and to be warmed up to 1233K(heating rate be 54K/min), then 1min be heated to 1253K and be incubated 5min
Sintering pressure: 200MPa
Fast Sintering is carried out to powder, in resistance sintering and cooling procedure, pressure remains at 200MPa, Ultra-fine Grained/micron crystal block body iron that diameter is the two size distribution of super-high-plasticity of Φ 10mm can be obtained, its microstructure with the brilliant α-Fe of block micron for matrix phase, with the shaft-like α-Fe such as Ultra-fine Grained and Ultra-fine Grained acicular α-Fe for wild phase, wherein the crystallite dimension of block α-Fe is 1 ~ 3 μm, be 600 ~ 800nm etc. the crystallite dimension of shaft-like α-Fe, the width of acicular α-Fe is 140 ~ 150nm.Corresponding room temperature compression true stress-strain curve shows, the room temperature compressed rupture strength of block sample and breaking strain are respectively 769MPa and 58%.
Embodiment 4
The preparation method of the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity of the present embodiment, comprises the following steps:
(1) high-energy ball milling prepares nanocrystalline iron powder: pure iron powder is placed in stainless steel ball grinding media and carries out high-energy ball milling, until obtain the nanocrystalline iron powder of crystallite dimension about 8 ~ 12nm:
Initial powder is high-purity electrolytic iron powder (99.5wt.%, granularity is 38um), initial iron powder and stainless steel abrading-ball are put into together stainless steel jar mill and (between ball grinder and lid, use " O " type seal ring seal, ball radius is respectively 15mm, 10mm and 6mm, its weight ratio is 1:3:1, and abrading-ball and powder weight ratio are 10:1).In order to anti-oxidation, be filled with high-purity argon gas in ball grinder and carry out protecting (99.99%, 0.5MPa).Finally, the ball grinder being filled with argon shield being placed on model is QM-2SP20 planetary ball mill carries out high-energy ball milling (rotating speed is 3.8s
-1).After every ball milling 5h shuts down and is cooled to room temperature in mechanical milling process, take out a certain amount of powder (about 5g), for the various characterization tests of powder, until acquisition crystallite dimension is about the nanocrystalline iron powder of 10nm.
(2) discharge plasma sintering prepares the block iron material of the two size distribution of super-high-plasticity: it is in the graphite sintering mould of Φ 20mm that the nanocrystalline iron powder of 35g step (1) obtained loads diameter, by the nanocrystalline iron powder of the first precompressed of positive and negative graphite electrode to 500MPa, be evacuated down to 10
-3pa, adopts discharge plasma sintering under the condition of argon shield, and obtain the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity, wherein Fast Sintering process conditions are as follows:
Agglomerating plant: Dr.Sintering SPS-825 discharge plasma sintering system
Sintering current type: pulse current
The dutycycle of pulse current: 12:2
Sintering temperature Ts:1335K
Sintering time: 4min is warmed up to 373K, then 4min, and to be warmed up to 1315K(heating rate be 235K/min), then 1min be heated to 1335K and be incubated 10min
Sintering pressure: 500MPa
Fast Sintering is carried out to powder, in resistance sintering and cooling procedure, pressure remains at 500MPa, Ultra-fine Grained/micron crystal block body iron that diameter is the two size distribution of super-high-plasticity of Φ 20mm can be obtained, its microstructure with the brilliant α-Fe of block micron for matrix phase, with the shaft-like α-Fe such as Ultra-fine Grained and Ultra-fine Grained acicular α-Fe for wild phase.The crystallite dimension of block α-Fe is 3 ~ 5 μm, and be 400 ~ 600nm etc. the crystallite dimension of shaft-like α-Fe, the width of acicular α-Fe is 100 ~ 120nm.Corresponding room temperature compression true stress-strain curve shows, room temperature fracture strength and breaking strain are respectively 1025MPa and 60%.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not limited by the examples; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (4)
1. a preparation method for the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity, is characterized in that, comprise the following steps:
(1) high-energy ball milling prepares nanocrystalline iron powder: under argon shield condition, pure iron powder is placed in stainless steel ball grinding media and carries out high-energy ball milling, until obtain the nanocrystalline iron powder that crystallite dimension is 8 ~ 12nm;
(2) discharge plasma sintering prepares the block iron material of the two size distribution of super-high-plasticity: nanocrystalline iron powder step (1) obtained loads in mould; under argon shield condition; adopt discharge plasma sintering; obtain the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity, wherein Fast Sintering process conditions are as follows:
Agglomerating plant: discharge plasma sintering system;
Sintering current type: pulse current;
Sintering temperature Ts:1253K≤Ts≤1335K;
Sintering time: 14 ~ 26min;
Sintering pressure: 40 ~ 500MPa.
2. the preparation method of the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity according to claim 1, it is characterized in that, in step (2) described discharge plasma sintering, heating rate is 54 ~ 235K/min, and temperature retention time controls at 0 ~ 10min.
3. the preparation method of the Ultra-fine Grained/micron crystal block body iron material of the two size distribution of super-high-plasticity according to claim 1, it is characterized in that, in step (2) described discharge plasma sintering, when adopting graphite jig, sintering pressure is 40 ~ 50MPa, and when adopting tungsten carbide die, sintering pressure is 50 ~ 500MPa.
4. Ultra-fine Grained/micron crystal block body the iron material of the two size distribution of the high-ductility that described in any one of claims 1 to 3, preparation method obtains, it is characterized in that, its microstructure with the brilliant α-Fe of block micron for matrix phase, with the shaft-like α-Fe such as Ultra-fine Grained and Ultra-fine Grained acicular α-Fe for wild phase.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310221710.2A CN103331449B (en) | 2013-06-05 | 2013-06-05 | Ultra-fine Grained/micron crystal block body iron material of the two size distribution of a kind of super-high-plasticity and preparation method thereof |
| PCT/CN2013/090063 WO2014194648A1 (en) | 2013-06-05 | 2013-12-20 | Ultrahigh-plasticity double-size-distribution superfine crystal/micrometer crystal block iron material and preparation method therefor |
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| CN201310221710.2A CN103331449B (en) | 2013-06-05 | 2013-06-05 | Ultra-fine Grained/micron crystal block body iron material of the two size distribution of a kind of super-high-plasticity and preparation method thereof |
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| CN103331449B (en) * | 2013-06-05 | 2015-09-02 | 华南理工大学 | Ultra-fine Grained/micron crystal block body iron material of the two size distribution of a kind of super-high-plasticity and preparation method thereof |
| CN104445428A (en) * | 2014-11-04 | 2015-03-25 | 华文蔚 | Synthesis method of spark plasma sintered massive alpha-ferric oxide |
| CN105238954A (en) * | 2015-10-28 | 2016-01-13 | 华南理工大学 | Multi-scale and double-state structure titanium alloy based on eutectic transformation, preparation and application |
| CN106513683A (en) * | 2016-11-04 | 2017-03-22 | 天津大学 | Method for preparing fine-grain high-density yttrium oxide dispersion strengthening tungsten-base alloy |
| CN111020347B (en) * | 2019-12-30 | 2021-08-17 | 广州航海学院 | High-density complex phase alloy material and preparation method thereof |
| CN111411248B (en) * | 2020-03-24 | 2021-07-27 | 广州铁路职业技术学院（广州铁路机械学校） | Multi-scale structure alloy material, preparation method and application thereof |
| CN111519073B (en) * | 2020-06-03 | 2021-07-09 | 上海鑫烯复合材料工程技术中心有限公司 | Nano carbon reinforced metal matrix composite material with trimodal characteristics |
| CN114075631B (en) * | 2020-08-11 | 2023-02-28 | 上海交通大学 | Preparation method of biological titanium bismuth alloy implant with double-scale grain structure |
| CN112723891B (en) * | 2021-01-27 | 2023-07-25 | 合肥工业大学 | Lanthanum-calcium composite hexaboride polycrystalline cathode material and preparation method thereof |
| CN115673327B (en) * | 2022-10-18 | 2024-04-30 | 北京工业大学 | High-strength and high-toughness tungsten alloy and preparation method thereof |
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| CN1786229A (en) * | 2005-11-04 | 2006-06-14 | 北京工业大学 | Preparation method of CoSb3 pyroelectric material having nanometer/micron composite crystal structure |
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