CN102071360A - Tungsten carbide particle-enhanced iron-based powder metallurgy material and preparation method thereof - Google Patents
Tungsten carbide particle-enhanced iron-based powder metallurgy material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to plastic forming technology and powder metallurgy technology, in particular to a tungsten carbide particle-enhanced iron-based powder metallurgy material and a preparation method thereof. According to a specific formula, the iron-based powder metallurgy material comprises the following components in percentage by mass: 85.0 to 90.0 percent of matrix material and 10.0 to 15.0 percent of enhanced phase tungsten carbide, wherein the matrix material comprises the following components in percentage by mass: 1.4 to 2.0 percent of copper, 1.7 to 2.0 percent of nickel, 0.9 to 1.2 percent of molybdenum, 0.7 to 1.6 percent of carbon and the balance of iron. In the invention, quick spark plasma sintering is adopted; and the obtained material has the characteristics of nearly full densification, high hardness, high indoor temperature bending strength, high high-temperature mechanical property and the like, can be used as a wear-resistant material, a tool material and the like, and can reduce the dependency of Chinese tool material production on import of precious metals such as vanadium, chromium and the like. The material has high cost performance and a good industrial production prospect.
Description
Technical field
The present invention relates to plastic forming technology and powder metallurgy technology, specifically be meant a kind of wolfram varbide (WC) particle enhanced iron-base powder metallurgy material and preparation method thereof.
Background technology
Characteristics have obtained to be extensive use of iron because of having low price, aboundresources, superior performance and easily accomplish scale production etc., but along with modern industry and science and technology development, its comprehensive mechanical property are had higher requirement.Existing a kind of Fe-Cu-Ni-Mo-C mmaterial belongs to high-strength heat-treated steel, mainly form by iron matrix and alloying element, yet its friction resistant polishing machine is relatively low, easy deformation and thermal treatment process are complicated under the high temperature, have limited the application of such material on this certain degree.
Studies confirm that with low cost, the isotropy of particles reiforced metal-base composition can improve Young's modulus, hardness, wear resistance and the high-temperature behavior of material.Thereby, be a kind of feasible method by in the iron-based body, adding the second phase enhanced granule WC with the comprehensive mechanical property that improves iron.As Ka Pate (G.Kaptay) etc., in the paper of delivering on volume part 2 " amorphism solid magazine " (Journal of Non-Crystalline Solids) in 1996 the 205th～207 " pottery strengthens the surface phenomenon of amorphous metal based composites reaction process " (Interface phenomena in processing of ceramic reinforced amorphous metal composites), studied the surface reaction that WC strengthens WC particle and matrix generation in the Fe40Ni40Si14B6 based composites.They draw Fe40Ni40Si14B6 by Theoretical Calculation with test can wetting well WC particle, thereby significantly improves the friction resistant polishing machine of this matrix material.Song Yanpei etc. have studied the influence of WC particle to the Fe-C composite materials property in the paper of delivering on volume the 10th phase " functional materials " in 2005 the 36th " WC particle strengthens the performance study of iron base composite material ".Result of study shows: the WC volume fraction is in 65%～80% WC/Fe-C matrix material, WC particle is evenly distributed on bainite and the graphite matrix with bigger particle size (100um) and higher volume fraction (about 80%), the WC particle of high rigidity can effectively stop the shear action of abrasive particle to matrix, reduce the viscous deformation of matrix and the transfer of relative flour milling, thereby can increase substantially the wear resisting property of this matrix material.Simultaneously, because the existence of WC particle, make composite material surface and inside form many tiny cracks, the part stress of transferable crack tip in the thermal crack expansion process, weaken its stress concentration effect, and dislocations strengthening effect at the interface and higher interface bond strength tend to that all thermal stresses is transferred to WC particle and get on, and the result has caused the cracking of WC particle, thereby the propagation rate of the crackle that slowed down, have improved the cold-and-heat resistent fatigue property of material.But the WC particle percent by volume too high levels of adding in should studying not only wasted valuable tungsten resource, and preparation cost is higher, is unfavorable for scale operation.Wu Chengjian etc., point out that in " Metal Material Science " of metallurgical industry press publication in 2006 tungsten is the principal element that rapid steel obtains thermohardening, the form with granular carbide in steel occurs, a large amount of undissolved carbides can hinder austenite crystal and grow up when quenching heating, improve the toughness of steel.Usually, the bending strength of molybdenum high speed steel and impelling strength are higher than tungsten system, have decarburizing tendency but molybdenum is a steel when thermal treatment.If at molybdenum is that an amount of tungsten of adding can improve its thermoplasticity in the steel, comprehensive mechanical property is improved.Though relevant research shows, high rigidity and high-intensity reinforced particulate are joined in the iron-based body, can improve its comprehensive mechanical property, but because WC and ferruginous powder are under the high-energy ball milling condition, the easy decarburization of WC, and Yi Yutie forms soluble solids, thereby has weakened the enhancement of WC particle, does not strengthen the report of Fe-Cu-Ni-Mo-C mmaterial so that see relevant WC particle so far as yet.
Summary of the invention
The objective of the invention is to overcome the weak point of the Fe-Cu-Ni-Mo-C mmaterial for preparing in the prior art, at adding wild phase tungsten carbide particle design body material system and optimizing sintering process, a kind of tungsten carbide particle enhanced iron-base powder metallurgy material and preparation method thereof is provided, thereby makes iron-base powder metallurgy material have comprehensive mechanical properties such as more excellent hot hardness, intensity and creep resistance, friction resistant wearing and tearing.
Realize the present invention by following measure.
A kind of tungsten carbide particle enhanced iron-base powder metallurgy material, it contains iron, copper, nickel, molybdenum and carbon, it is characterized in that: it also contains wild phase nano level hard granulated carbon tungsten, and by mass percentage component and content thereof are as follows:
Body material 85.0～90.0%, wild phase wolfram varbide 10.0～15.0%;
Described body material is the powder of iron, copper, nickel, molybdenum and carbon, and concrete prescription component and content thereof by mass percentage is copper 1.4～2.0%, nickel 1.7～2.0%, and molybdenum 0.9～1.2%, carbon 0.7～1.6%, surplus is an iron.
A kind of preparation method of tungsten carbide particle enhanced iron-base powder metallurgy material is characterized in that: this method comprises the steps and processing condition:
Step 1: the composition design of body material
Component and content proportioning body material thereof by following mass percent: copper 1.4～2.0%, nickel 1.7～2.0%, molybdenum 0.9～1.2%, carbon 0.7～1.6%, surplus is an iron;
Step 2: high-energy ball milling body material
Place high energy ball mill to carry out ball milling the described body material of step 1, until the ball-milled powder grain refining to nano level;
Step 3: mix powder
With body material and wild phase proportioning mixed powder by following mass percent: body material 85.0～90.0%, wild phase wolfram varbide 10.0～15.0%, all the other are inevitable trace impurity;
Above-mentioned mixed powder inserted carry out ball milling in the ball mill, ball milling speed is 85～100r/min, and the ball milling time is 2～5h, mixes until body material and wild phase tungsten carbide particle;
Step 4: discharge plasma sintering
The powder that step 3 is mixed is packed in the graphite jig, adopts the discharging plasma sintering equipment sintering, and the sintering process condition is as follows:
Sintering current type: dc pulse current
Sintering pressure: 30～50MPa
Sintering temperature: 750～1000 ℃
Temperature rise rate: 50～75 ℃/min
The sintered heat insulating time: 0～5min
Sintering vacuum tightness :≤4Pa
Can obtain organizing tiny, uniform a kind of tungsten carbide particle enhanced iron-base powder metallurgy material through Fast Sintering.
Described iron, copper, nickel, molybdenum and carbon all add with simple substance form, and wherein, iron is the water-atomized iron powder of purity 〉=99.5%, granularity 45～149 μ m; Copper is the electrolytic copper powder of purity 〉=99.9%, granularity≤75 μ m; Nickel is the carbonyl nickel powder of purity 〉=99.8%, granularity 3～5 μ m; Molybdenum is the reduction molybdenum powder of purity 〉=99.7%, granularity≤75 μ m; Carbon is the oildag of granularity 2～3 μ m.
The present invention compared with prior art has the following advantages:
1, the present invention adds nano level hard particle wild phase wolfram varbide with the form of compound in the body material system, wolfram varbide high rigidity, high character such as Young's modulus have been kept, overcome the problem of the decarburization easily under the high-energy ball milling condition of wolfram varbide and ferruginous powder, Yi Yutie formation soluble solids, and the matrix material of design can the sinter molding densification under lower sintering temperature.
2, the present invention utilizes discharge plasma sintering to be shaped and the incorporate method of Fast Sintering, the Nanometre grade tungsten carbide particle enhanced iron-base powder metallurgy material of preparation has characteristics such as component, even particle size distribution and nearly full densification, can significantly improve intensity, friction resistant polishing machine, especially hot hardness and the creep-resistant property of material.
3, the present invention has reduced the addition of wild phase wolfram varbide, has saved valuable tungsten resource, and prepared iron-base powder metallurgy material is expected to carry out industrialization production with high cost performance, and the suitability for industrialized production prospect is good.
4, the prepared iron-base powder metallurgy material of the present invention is of many uses, can be used as high-abrasive material, cutter material etc., can reduce the import that China's cutter material produces noble metals such as vanadium, chromium and rely on.
Embodiment
The invention will be further described by following embodiment, but embodiments of the present invention are not limited only to this.
Embodiment 1
A kind of preparation method of tungsten carbide particle enhanced iron-base powder metallurgy material comprises the steps:
Step 1: the composition design of body material
The powder of iron, copper, nickel, molybdenum and carbon as body material, is carried out proportioning by following mass percent consumption:
Iron 94.4%, copper 2.0%, nickel 1.7%, molybdenum 1.2%, carbon 0.7%, all the other are inevitable trace impurity;
Iron, copper, nickel, molybdenum and carbon all add with simple substance form, and wherein, iron is water-atomized iron powder, purity 〉=99.5%, granularity 45～149 μ m; Copper is electrolytic copper powder, purity 〉=99.9%, granularity≤75 μ m; Nickel is carbonyl nickel powder, purity 〉=99.8%, granularity 3～5 μ m; Molybdenum is reduction molybdenum powder, purity 〉=99.7%, granularity≤75 μ m; Carbon is oildag, granularity 2～3 μ m.
Step 2: high-energy ball milling body material
Place planetary ball mill to carry out high-energy ball milling the described body material of step 1, its ratio of grinding media to material is 10: 1, and ball milling speed is 226r/min, and adopts high-purity argon gas as protective atmosphere, and the ball milling time is 40h.
Step 3: mix powder
With body material and wild phase by following mass percent proportioning mixed powder:
Body material 90.0%
Wolfram varbide 10.0%
All the other are inevitable trace impurity;
Wolfram varbide adds purity 〉=99.9%, granularity 200～800nm with the form of compound.
Place ball mill to carry out ball milling above-mentioned mixed powder, its ratio of grinding media to material is 10: 1, and ball milling speed is 85r/min, and the ball milling time is 5h.
Step 4: discharge plasma sintering
The 20g powder that step 3 the is mixed internal diameter of packing into is in the graphite sintering mold of 20mm, carries out sintering in discharging plasma sintering equipment, and wherein sintering pressure is 50MPa, sintering temperature is 750 ℃, temperature rise rate is 50 ℃/min, soaking time 5min, and vacuum tightness is 4Pa.Obtain after the Fast Sintering to organize tiny, uniform a kind of tungsten carbide particle enhanced iron-base powder metallurgy material, the density under the gained material room temperature is 7.76g/cm
3, hardness is that 45.7HRC, cross-breaking strength are that 2335MPa, abrasion loss are 1.50 * 10
-3G (is that GCr-15 steel ball, the test load of Φ 10 is that 10N, amplitude are that 100 μ m, frequency are that 50Hz and loading time are 20min to the mill part); Through three 500 ℃ of insulation 1h, cool to room temperature with the furnace, its hardness is 44.9HRC.
Embodiment 2
A kind of preparation method of tungsten carbide particle enhanced iron-base powder metallurgy material comprises the steps:
Step 1: the composition design of body material
The powder of iron, copper, nickel, molybdenum and carbon as body material, is carried out proportioning by following mass percent consumption:
Iron 94.3%, copper 1.8%, nickel 1.7%, molybdenum 1.2%, carbon 1.0%, all the other are inevitable trace impurity;
Iron, copper, nickel, molybdenum and carbon all add with simple substance form.Wherein, iron is water-atomized iron powder, purity 〉=99.5%, granularity 45～149 μ m; Copper is electrolytic copper powder, purity 〉=99.9%, granularity≤75 μ m; Nickel is carbonyl nickel powder, purity 〉=99.8%, granularity 3～5 μ m; Molybdenum is reduction molybdenum powder, purity 〉=99.7%, granularity≤75 μ m; Carbon is oildag, granularity 2～3 μ m.
Step 2: high-energy ball milling matrix
Place planetary ball mill to carry out high-energy ball milling the described body material of step 1, its ratio of grinding media to material is 10: 1, and ball milling speed is 226r/min, and adopts high-purity argon gas as protective atmosphere, and the ball milling time is 40h.
Step 3: mix powder
With body material and wild phase component and content proportioning mixed powder thereof by following mass percent:
Body material 88.0%
Wolfram varbide 12.0%
All the other are inevitable trace impurity;
Wolfram varbide adds purity 〉=99.9%, granularity 200～800nm with the form of compound.
Place ball mill to carry out ball milling the mixed powder of mentioned component proportioning, its ratio of grinding media to material is 10: 1, and ball milling speed is 96r/min, and the ball milling time is 2h.
Step 4: discharge plasma sintering
The 20g powder that step 3 the is mixed internal diameter of packing into is in the graphite sintering mold of 20mm, carries out sintering in discharging plasma sintering equipment, and wherein sintering pressure is 30MPa, sintering temperature is 1000 ℃, temperature rise rate is 65 ℃/min, soaking time 2min, and vacuum tightness is 3Pa.Obtain after the Fast Sintering to organize tiny, uniform a kind of tungsten carbide particle enhanced iron-base powder metallurgy material, the density under the gained material room temperature is 7.91g/cm
3, hardness is that 45.9HRC, cross-breaking strength are that 2637MPa, abrasion loss are 1.29 * 10
-3G (is that GCr-15 steel ball, the test load of Φ 10 is that 10N, amplitude are that 100 μ m, frequency are that 50Hz and loading time are 20min to the mill part); Through three 500 ℃ of insulation 1h, cool to room temperature with the furnace, its hardness is 45.2HRC.
Embodiment 3
A kind of preparation method of tungsten carbide particle enhanced iron-base powder metallurgy material comprises the steps:
Step 1: the composition design of body material
The powder of iron, copper, nickel, molybdenum and carbon as matrix, is carried out proportioning by following mass percent consumption:
Iron 94.6%, copper 1.4%, nickel 2.0%, molybdenum 1.0%, carbon 1.0%, all the other are inevitable trace impurity;
Iron, copper, nickel, molybdenum and carbon all add with simple substance form.Wherein, iron is water-atomized iron powder, purity 〉=99.5%, granularity 45～149 μ m; Copper is electrolytic copper powder, purity 〉=99.9%, granularity≤75 μ m; Nickel is carbonyl nickel powder, purity 〉=99.8%, granularity 3～5 μ m; Molybdenum is reduction molybdenum powder, purity 〉=99.7%, granularity≤75 μ m; Carbon is oildag, granularity 2～3 μ m.
Step 2: high-energy ball milling matrix
Place planetary ball mill to carry out high-energy ball milling the described body material of step 1, its ratio of grinding media to material is 10: 1, and ball milling speed is 226r/min, and adopts high-purity argon gas as protective atmosphere, and the ball milling time is 40h.
Step 3: mix powder
With matrix and wild phase component and content proportioning mixed powder thereof by following mass percent:
Body material 90.0%
Wolfram varbide 10.0%
All the other are inevitable trace impurity;
Wolfram varbide adds purity 〉=99.9%, granularity 200～800nm with the form of compound.
Place ball mill to carry out ball milling the mixed powder of mentioned component proportioning, its ratio of grinding media to material is 10: 1, and ball milling speed is 96r/min, and the ball milling time is 3h.
Step 4: discharge plasma sintering
The 20g powder that step 3 the is mixed internal diameter of packing into is in the graphite sintering mold of 20mm, carries out sintering in discharging plasma sintering equipment, and wherein sintering pressure is 50MPa, sintering temperature is 850 ℃, temperature rise rate is 75 ℃/min, soaking time 0min, and vacuum tightness is 3Pa.Obtain after the Fast Sintering to organize tiny, uniform a kind of tungsten carbide particle enhanced iron-base powder metallurgy material, the density under the gained material room temperature is 8.09g/cm
3, hardness is that 49.5HRC, cross-breaking strength are that 2781MPa, abrasion loss are 0.84 * 10
-3G (is that GCr-15 steel ball, the test load of Φ 10 is that 10N, amplitude are that 100 μ m, frequency are that 50Hz and loading time are 20min to the mill part); Through three 500 ℃ of insulation 1h, cool to room temperature with the furnace, its hardness is 48.3HRC.
Embodiment 4
A kind of preparation method of tungsten carbide particle enhanced iron-base powder metallurgy material comprises the steps:
Step 1: the composition design of body material
The powder of iron, copper, nickel, molybdenum and carbon as matrix, is carried out proportioning by following mass percent consumption:
Iron 93.8%, copper 2.0%, nickel 1.7%, molybdenum 0.9%, carbon 1.6%, all the other are inevitable trace impurity;
Iron, copper, nickel, molybdenum and carbon all add with simple substance form.Wherein, iron is water-atomized iron powder, purity 〉=99.5%, granularity 45～149 μ m; Copper is electrolytic copper powder, purity 〉=99.9%, granularity≤75 μ m; Nickel is carbonyl nickel powder, purity 〉=99.8%, granularity 3～5 μ m; Molybdenum is reduction molybdenum powder, purity 〉=99.7%, granularity≤75 μ m; Carbon is oildag, granularity 2～3 μ m.
Step 2: high-energy ball milling matrix
Place planetary ball mill to carry out high-energy ball milling the described body material of step 1, its ratio of grinding media to material is 10: 1, and ball milling speed is 226r/min, and adopts high-purity argon gas as protective atmosphere, and the ball milling time is 40h.
Step 3: mix powder
With matrix and wild phase component and content proportioning mixed powder thereof by following mass percent:
Body material 85.0%
Wolfram varbide 15.0%
All the other are inevitable trace impurity;
Wolfram varbide adds purity 〉=99.9%, granularity 200～800nm with the form of compound.
Place ball mill to carry out ball milling the mixed powder of mentioned component proportioning, its ratio of grinding media to material is 10: 1, and ball milling speed is 100r/min, and the ball milling time is 2h.
Step 4: discharge plasma sintering
The 20g powder that step 3 the is mixed internal diameter of packing into is in the graphite sintering mold of 20mm, carries out sintering in discharging plasma sintering equipment, and wherein sintering pressure is 40MPa, sintering temperature is 1000 ℃, temperature rise rate is 50 ℃/min, soaking time 1min, and vacuum tightness is 1Pa.Obtain after the Fast Sintering to organize tiny, uniform a kind of tungsten carbide particle enhanced iron-base powder metallurgy material, the density under the gained material room temperature is 8.42g/cm
3, hardness is that 50.6HRC, cross-breaking strength are that 2622MPa, abrasion loss are 1.08 * 10
-3G (is that GCr-15 steel ball, the test load of Φ 10 is that 10N, amplitude are that 100 μ m, frequency are that 50Hz and loading time are 20min to the mill part); Through three 500 ℃ of insulation 1h, cool to room temperature with the furnace, its hardness is 49.3HRC.
Claims (3)
1. tungsten carbide particle enhanced iron-base powder metallurgy material, it contains iron, copper, nickel, molybdenum and carbon, it is characterized in that: it also contains wild phase nano level hard granulated carbon tungsten, and concrete prescription component and content thereof by mass percentage is as follows:
Body material 85.0～90.0%, wild phase wolfram varbide 10.0～15.0%;
Described body material is the powder of iron, copper, nickel, molybdenum and carbon, and component by mass percentage and content thereof are copper 1.4～2.0%, nickel 1.7～2.0%, and molybdenum 0.9～1.2%, carbon 0.7～1.6%, surplus is an iron.
2. the preparation method of a tungsten carbide particle enhanced iron-base powder metallurgy material, it is characterized in that: this method comprises the steps and processing condition:
Step 1: the composition design of body material
Component and content proportioning body material thereof by following mass percent: copper 1.4～2.0%, nickel 1.7～2.0%, molybdenum 0.9～1.2%, carbon 0.7～1.6%, surplus is an iron;
Step 2: high-energy ball milling body material
Place high energy ball mill to carry out ball milling the described body material of step 1, until the ball-milled powder grain refining to nano level;
Step 3: mix powder
With body material and wild phase by following mass percent proportioning mixed powder: body material 85.0～90.0%, wild phase wolfram varbide 10.0～15.0%, all the other are inevitable trace impurity;
Place ball mill to carry out ball milling above-mentioned mixed powder, ball milling speed is 85～100r/min, and the ball milling time is 2～5h, mixes until body material and wild phase tungsten carbide particle;
Step 4: discharge plasma sintering
The powder that step 3 is mixed is packed in the graphite jig, adopts the discharging plasma sintering equipment sintering, and the sintering process condition is as follows:
Sintering current type: dc pulse current
Sintering pressure: 30～50MPa
Sintering temperature: 750～1000 ℃
Temperature rise rate: 50～75 ℃/min
The sintered heat insulating time: 0～5min
Sintering vacuum tightness :≤4Pa
Can obtain organizing tiny, uniform a kind of tungsten carbide particle enhanced iron-base powder metallurgy material through Fast Sintering.
3. the preparation method of a kind of tungsten carbide particle enhanced iron-base powder metallurgy material according to claim 2, it is characterized in that: described iron, copper, nickel, molybdenum and carbon, all add with simple substance form, wherein, iron is the water-atomized iron powder of purity 〉=99.5%, granularity 45～149 μ m; Copper is the electrolytic copper powder of purity 〉=99.9%, granularity≤75 μ m; Nickel is the carbonyl nickel powder of purity 〉=99.8%, granularity 3～5 μ m; Molybdenum is the reduction molybdenum powder of purity 〉=99.7%, granularity≤75 μ m; Carbon is the oildag of granularity 2～3 μ m.
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