CN1321768C - Preparation of warm pressed diffusing particle reinforced iron-based powder metallized composite materials - Google Patents
Preparation of warm pressed diffusing particle reinforced iron-based powder metallized composite materials Download PDFInfo
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- CN1321768C CN1321768C CNB2005100327809A CN200510032780A CN1321768C CN 1321768 C CN1321768 C CN 1321768C CN B2005100327809 A CNB2005100327809 A CN B2005100327809A CN 200510032780 A CN200510032780 A CN 200510032780A CN 1321768 C CN1321768 C CN 1321768C
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- 239000002245 particle Substances 0.000 title claims abstract description 70
- 239000000843 powder Substances 0.000 title claims abstract description 63
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 238000000498 ball milling Methods 0.000 claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 6
- 239000010935 stainless steel Substances 0.000 claims abstract description 6
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 5
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 5
- 150000001247 metal acetylides Chemical class 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 8
- 230000033228 biological regulation Effects 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 239000011812 mixed powder Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 4
- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 claims description 4
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 4
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- RIRXDDRGHVUXNJ-UHFFFAOYSA-N [Cu].[P] Chemical compound [Cu].[P] RIRXDDRGHVUXNJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 11
- 238000003825 pressing Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 239000008187 granular material Substances 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 2
- 229910000997 High-speed steel Inorganic materials 0.000 abstract 1
- 238000003475 lamination Methods 0.000 abstract 1
- 238000005272 metallurgy Methods 0.000 abstract 1
- 238000003801 milling Methods 0.000 abstract 1
- 230000003014 reinforcing effect Effects 0.000 abstract 1
- 238000004663 powder metallurgy Methods 0.000 description 7
- 239000000919 ceramic Substances 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 229910000975 Carbon steel Inorganic materials 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- VSOYJNRFGMJBAV-UHFFFAOYSA-N N.[Mo+4] Chemical compound N.[Mo+4] VSOYJNRFGMJBAV-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000004523 agglutinating effect Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- Powder Metallurgy (AREA)
Abstract
The present invention relates to a powdery metallurgy technique, particularly to a preparation method of warm pressed diffusing particle reinforced iron-based powder metallized composite materials. Iron-based powder metallized composite materials are formed by preparing materials, mixing, milling balls, doping, warm pressing and sintering by a diffusing particle and a metal base body through the combined method of a ball milling technology and a warm pressing technique. The diffusing particle comprises diffusing metal carbides and metal oxide particles. The metal base body comprises an iron base, a stainless steel base, a high-speed steel base, etc. Composite material powder with reinforced particles are molded by warm pressing under 100DEG. C to 150DEG. C and 500MPa to 800MPa. The composite powder has good compressibility and molding performance. Green flans can not have lamination crack. The corresponding density is enhanced by 2% to 4%. The granules of the composite materials are diffused and distributed uniformly. The comprehensive mechanical performance is poor. The present invention has advantages of simple preparation technology and low cost, and opens up a new way for reinforcing precise molding of parts of the powder metallized composite materials by the particles.
Description
Technical field
The present invention relates to PM technique, specifically be meant a kind of preparation method of warm pressed diffusing particle reinforced iron-based powder metallized composite.
Background technology
The powder metallurgy warm-pressing technology is the new method of a kind of high density, low cost shaping machine components of succeeding in developing nineteen nineties, is mainly used on the powder metallurgy sintered steel, and it can make the green density of part improve 0.15～0.30g/m
3, the performance that improves the powder metallurgy iron based articles is had important effect.
Adopting powder metallurgy process can prepare with the iron and steel is the metal-base composites that base mixes hard ceramic particles such as carbide or oxide, but problem owing to the not plasticity of the hard ceramic particles of mixing and metal dust physicochemical properties, surface characteristics difference and ceramic particle, dispersiveness that morphotropism causes mixed-powder, compressibility, formability, agglutinating property difference, near-net forming to composite powder is unfavorable, and the iron-based powder metallized composite materials part that finally causes particle to strengthen is difficult to apply.The positive light of Zou etc. are at the China YouSe Acta Metallurgica Sinica, 2001, delivered be entitled as in " self propagating high temperature synthetic TiC compound additive strengthen iron-base powder metallurgy material " text 8-20 at 11 (3): 408 also mentions in capable and " adds the ceramic particle wild phase in iron powder or alloyed powder; can further strengthen iron, but effect is not ideal.-----therefore, the dispersiveness and the problem of formability and sintering temperature after how solving ceramic phase and adding, and can improve mechanical property significantly are to remain the content further studied.”
Technology contents
The objective of the invention is to overcome above-mentioned the deficiencies in the prior art part, proposing a kind of hard ceramic particles can be incorporated among the steel substrate to even dispersion, and improves the formability of composite powder and the preparation method of constrictive warm pressed diffusing particle reinforced iron-based powder metallized composite by warm-pressing technology.
The present invention can realize by following measure:
A kind of preparation method of warm pressed diffusing particle reinforced iron-based powder metallized composite, comprise that batching, mixing, temperature and pressure, sintering form, it is characterized in that, iron-based powder metallized composite materials is the method that is combined through ball-milling technology and temperature and pressure technology by diffusing particle and metallic matrix, form through batching, mixing, ball milling, doping, temperature and pressure, sintering, concrete steps and process conditions thereof are as follows:
Step 1: batching
Mass percent 5～20%, particle diameter by the composite total amount are diffusing particle metal carbides or the metal oxide of 1～20 μ m, 78～95%, particle diameter is that the metallic matrix iron-based of 3～147 μ m or the proportioning of stainless steel-based or high-speed steel-base are got the raw materials ready;
Step 2: mix
Cross 100 mesh sieves of GB6003 regulation after getting the raw materials ready by said ratio earlier, then dried at least mixing 20 minutes on mixed powder machine;
Step 3: ball milling
With ball mill ball milling 10～120 minutes, and under hydrogen shield in 600～800 ℃ of annealing 0～2 hour;
Step 4: doping
Metal phosphide powder and 0～1.0%, the particle diameter that adds mass percent 0～2.4%, particle diameter by the composite total amount and be 5～20 μ m in above-mentioned powder is that graphite powder and 0.6～0.8%, the particle diameter of 3-74 μ m is the EBS wax powder of 5-10 μ m, fully mixing 20～30 minutes on mixed powder machine;
Step 5: temperature and pressure
Above-mentioned powder is heated to 100～150 ℃, with the pressure forming of 500～800MPa;
Step 6: sintering
Sintering in molybdenum wire furnace or vacuum drying oven, sintering temperature are 1150～1350 ℃, temperature retention time 1～2 hour; Can obtain the iron-based powder metallized composite materials that high density high-performance diffusing particle strengthens.
Above-mentioned disperse metal carbide particles is selected from niobium carbide or titanium carbide or tungsten carbide, and the disperse metal oxide particle is meant aluminium oxide; Additive metal phosphide powder is meant ferrophosphorus or phosphor-copper powder.
The present invention compared with prior art has following outstanding advantage:
1, the present invention's method of adopting ball-milling technology and temperature and pressure technology to combine first is prepared into the iron-based powder metallized composite materials that the high performance diffusing particle of form height density strengthens, solve the problem of the dispersiveness that strengthens after particle adds the iron and steel based powders, formability, compressibility difference effectively, and can improve the mechanical property of composite significantly.Adopt the present invention can realize the near-net forming of iron-based powder metallized composite materials part, technology is simple, and practicality is good, therefore has the favorable industrial prospect of production.
2, adopt the composite powder of the warm pressed diffusing particle reinforced iron-based powder metallized composite of the present invention's preparation to have good formability and compressibility, be shaped under 500～800MPa pressure, slabbing does not appear in green compact, and the relative density of green compact improves 2～4%.
3, particle reinforced iron-based powder metallized composite materials provided by the invention, pottery strengthen uniform particles and mix, not segregation, and sintering character is good, can be used for making the constitutional detail of high-strength, high-anti-friction.
The specific embodiment
The invention will be further described by following embodiment:
Embodiment 1
Step 1: batching
By mass percent 1O%, the diffusing particle titanium carbide TiC particle of particle diameter in 15～20 mu m ranges of composite total amount, mass percent is 86%, the atomized iron powder of particle diameter≤147 μ m is got the raw materials ready;
Step 2: mix
By 100 mesh sieves of crossing the GB6003 regulation after the said ratio batching, efficiently mix the powder machine with V-type then and did mixed 20 minutes;
Step 3: ball milling
QM--ISP planetary high-energy ball mill ball milling 20 minutes;
Step 4: doping
In above-mentioned powder, add mass percent 2.4%, the ferrophosphorus Fe of particle diameter in 15～20 mu m ranges by the composite total amount
3The P powder, adding the mass percent consumption again is 1.O%, the graphite powder of particle diameter in 45～74 mu m ranges, the mass percent consumption is 0.6%, the EBS wax powder of particle diameter in 5～10 mu m ranges, efficiently mixes the powder machine in V-type and mixes 20 minutes;
Step 5: temperature and pressure
Composite powder is heated to 100 ℃, is shaped down with 700MPa pressure;
Step 6: sintering
In the cracked ammonium molybdenum wire furnace in 1150 ℃ of sintering 1 hour.
Promptly obtain the ferrous based powder metallurgical composite material that the warm pressed diffusing titanium carbide granule strengthens, the green compact relative density of this composite improves 4.0% than compacting under the room temperature, and slabbing does not appear in green compact, and hot strength is 520～580MPa, and wearability improves 250% than 60 carbon steels.
Embodiment 2
Step 1: batching
Mass percent 5%, the diffusing particle aluminium oxide Al of particle diameter in 1O～15 mu m ranges by the composite total amount
2O
3Particle, mass percent are 94.4%, the 316L stainless steel powder of particle diameter≤147 μ m is got the raw materials ready;
Step 2: mix
By 100 mesh sieves of crossing the GB6003 regulation after the said ratio batching, efficiently mix the powder machine with V-type then and did mixed 30 minutes;
Step 3: ball milling
ZMJ-20 stirring-type high energy ball mill ball milling 120 minutes, and under hydrogen shield, annealed 2 hours in 600 ℃;
Step 4: doping
In above-mentioned powder, add mass percent 0.6% by the composite total amount, particle diameter in 5～10 mu m ranges EBS wax powder, efficiently mix the powder machine in V-type and mixed 20 minutes;
Step 5: temperature and pressure
Composite powder is heated to 130 ℃, is shaped down with 800MPa pressure;
Step 6: sintering
In the cracked ammonium molybdenum wire furnace in 1300 ℃ of sintering 2 hours.
Promptly obtain the stainless steel-based composite powder metallurgy material that the warm pressed diffusing alumina particle strengthens, the green compact relative density of this composite improves 3.0% than compacting under the room temperature, slabbing does not appear in green compact, and the composite hot strength is 350～400MPa, and wearability improves 200% than 316L stainless steel.
Embodiment 3
Step 1: batching
By mass percent 20%, the diffusing particle niobium carbide NbC particle of particle diameter in 2～3 mu m ranges of composite total amount, mass percent is 79.2%, the M3 high speed comminuted steel shot of particle diameter≤74 μ m is got the raw materials ready;
Step 2: mix
By 100 mesh sieves of crossing the GB6003 regulation after the said ratio batching, efficiently mix the powder machine with V-type then and did mixed 40 minutes;
Step 3: ball milling
QM--ISP planetary high-energy ball mill ball milling 60 minutes, and under hydrogen shield in 800 ℃ of annealing 2 hours;
Step 4: doping
In above-mentioned powder, add mass percent 0.8%, the EBS wax powder of particle diameter in 5～10 mu m ranges, efficiently mix the powder machine in V-type and mixed 30 minutes by the composite total amount;
Step 5: temperature and pressure
Composite powder is heated to 150 ℃, is shaped down with 600MPa pressure;
Step 6: sintering
In the vacuum drying oven stove in 1300 ℃ of sintering 1.5 hours.
Promptly obtain the high-speed steel-base composite powder metallurgy material that the warm pressed diffusing particles of niobium carbide strengthens, the green compact relative density of this composite improves 2.5% than compacting under the room temperature, slabbing does not appear in green compact, the composite bending strength is 950～1000MPa, and wearability improves 300～350% than 12CrNi3A heat treatment state.
Embodiment 4
Step 1: batching
By mass percent 10%, the diffusing particle tungsten carbide wc particle of particle diameter in 2～5 mu m ranges of composite total amount, mass percent is 85.9%, the iron powder of particle diameter≤74 μ m is got the raw materials ready;
Step 2: mix
By 100 mesh sieves of crossing the GB6003 regulation after the said ratio batching, efficiently mix the powder machine with V-type then and did mixed 40 minutes;
Step 3: ball milling
QM--ISP planetary high-energy ball mill ball milling 60 minutes, and under hydrogen shield in 700 ℃ of annealing 2 hours;
Step 4: doping
In above-mentioned powder, add mass percent 2.4%, the phosphor-copper Cu of particle diameter in 15～20 mu m ranges by the composite total amount
3The P powder adds the mass percent consumption and is 1.0%, graphite powder and the mass percent consumption of particle diameter in 3～5 mu m ranges is 0.7%, the EBS wax powder of particle diameter in 5～10 mu m ranges again, efficiently mixes the powder machine in V-type and mixes 20 minutes;
Step 5: temperature and pressure
Composite powder is heated to 130 ℃, is shaped down with 600MPa pressure;
Step 6: sintering
In the vacuum drying oven stove in 1200 ℃ of sintering 1.5 hours.
Promptly obtain the ferrous based powder metallurgical composite material that the warm pressed diffusing tungsten carbide particle strengthens, the green compact relative density of this composite improves 2% than compacting under the room temperature, slabbing does not appear in green compact, and the composite hot strength is 450～500MPa, and wearability improves 350% than 45 carbon steels.
Claims (3)
1, a kind of preparation method of warm pressed diffusing particle reinforced iron-based powder metallized composite comprises that batching, mixing, temperature and pressure, sintering form, and concrete steps and process conditions thereof are as follows:
Step 1: batching
By the mass percent 5～20% of composite total amount, metal carbides or the metal oxide that particle diameter is 1～20 μ m, 78～95%, particle diameter is that the iron-based of 3～147 μ m or the proportioning of stainless steel-based or high-speed steel-base are got the raw materials ready;
Step 2: mix
Cross 100 mesh sieves of GB6003 regulation after getting the raw materials ready by said ratio earlier, then dried at least mixing 20 minutes on mixed powder machine;
Step 3: ball milling
With ball mill ball milling 10～120 minutes, and under hydrogen shield in 600～800 ℃ of annealing 0～2 hour;
Step 4: doping
Metal phosphide powder and 0～1.0%, the particle diameter that adds mass percent 0～2.4%, particle diameter by the composite total amount and be 5～20 μ m in above-mentioned powder is that graphite powder and 0.6～0.8%, the particle diameter of 3-74 μ m is the EBS wax powder of 5-10 μ m, fully mixing 20～30 minutes on mixed powder machine;
Step 5: temperature and pressure
Above-mentioned powder is heated to 100～150 ℃, with the pressure forming of 500～800MPa;
Step 6: sintering
Sintering in molybdenum wire furnace or vacuum drying oven, sintering temperature are 1150～1350 ℃, and temperature retention time is 1～2 hour; Can obtain the iron-based powder metallized composite materials that diffusing particle strengthens.
2, the preparation method of warm pressed diffusing particle reinforced iron-based powder metallized composite according to claim 1 is characterized in that, the disperse metal carbide particles is selected from niobium carbide or titanium carbide or tungsten carbide, and the disperse metal oxide particle is meant aluminium oxide.
3, the preparation method of warm pressed diffusing particle reinforced iron-based powder metallized composite according to claim 1 is characterized in that, additive metal phosphide powder is meant ferrophosphorus or phosphor-copper powder.
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