CN106424716A - Method for modifying performance of sintered Mn-Cu damping alloy with ferrous oxalate - Google Patents
Method for modifying performance of sintered Mn-Cu damping alloy with ferrous oxalate Download PDFInfo
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Abstract
The invention discloses a method for modifying the performance of a sintered Mn-Cu damping alloy with ferrous oxalate. According to the method, sintering is promoted by high-activity iron produced by pyrolysis and hydrogen reduction of the ferrous oxalate, H2O, CO2 and other gases released during pyrolysis and hydrogen reduction of the ferrous oxalate can prevent a compact sealing layer from being formed on the surface of a sintered blank, and pyrolysis, reduction and sintering are performed under the action of hydrogen. Dehydration is performed at 180-240 DEG C with the heat preservation time of 1-4 h; pyrolysis is performed at 400-500 DEG C with the heat preservation time of 1-4 h; reduction is performed at 750-850 DEG C with the heat preservation time of 1-2 h; then a sintering process is finished at 850-950 DEG C with the heat preservation time of 2-4 h; and the heating speed is 5-10 DEG C/min. The sintered Mn-Cu damping alloy prepared according to the method reaches the diameter of 100 mm, the length of 200 mm, the density of 5.10-5.75 g/cm<3>, the hardness of 52-86 HRF and the bending strength of 128-184 MPa and has high uniformity.
Description
Technical field
The present invention relates to a kind of method of atmosphere sintering loose structure copper-manganese high damping alloy.It is by with Ferrox.
As ferrum element donor, pyrolysis characteristicses and its catabolite using Ferrox. improve sintering process process, realize large scale
Gauge material Even Sintering purpose.
Technical background
Manganin, as the representative of twin type damping material, is widely used the every field producing in life.Manganese
Copper damp alloy material has the antiferromagnetic transition of the manganin of γ phase constitution, forms lattice distortion, triggers microtwinning, if point
Battle array distortion induces martensitic phase transformation, then will form martensitic twin, the movement of parent phase and thermo elastic martensite boundary and heat
The mobile consumed energy of elastic martensitic twin substructure, produces high-damping phenomenon.Copper-manganese damp alloy material have nonmagnetic,
Low temperature damping capacity is very well and intensity and the good feature of toughness.If composition heat treatment is proper, its damping capacity highest can
Reach rubber level.And manganese copper alloy material has good deformability, damping alloy support, resistance can be applied to well
On these parts such as damping alloy pad, bearing, super conducting coil, pantograph frame, damping alloy thin plate, the copper-manganese resistance of main application
The composition of damping alloy is shown in Table 1.
The composition range (mass percent) of the practical copper-manganese damping alloy of table 1
In addition to the Incramute alloy of the U.S., in remaining manganin, all contain element of Fe, its scope 1.0 ~ 4.0% it
Between.Add Fe primarily to improving the mechanical performance of alloy, excessive ferrum can have to alloy damping characteristic in manganin
Detrimental effect, so the content of Fe is not to be exceeded 4.0%.Appropriate ferrum the damping capacity impact of alloy is mainly manifested in
Lower 2 points:Perfect dislocation may be made in low temperature to resolve into extended dislocation, this dislocation can become the core of stress-induced martensite
Embryo, so that ε martensite quantity increases in alloy.Meanwhile, the presence of Fe can also promote stress-inducedεmartensite phase transformation, promotees
Enter the spinodal decomposition of Mn-Cu alloy, promote the precipitation of crystal boundary, carry heavy alloyed damping capacity.
Porous metals have the advantages that density is low, intensity is high, sound absorbing capabilities are high and gradually attract much attention, metal material
Porous it is verified that being an up one of highly effective approach of Damping Property of Metal Material.Mikio Fukuhara et al.
Have studied sintering Mn- (5,10,15,20) Cu alloy damping capacity, and with casting M2052 alloy be compared, Mn powder pure
Spend for 99%, granularity is 16 μm, the purity of Cu powder is 99%, and granularity is 7 μm, and after mixing, under hydrogen environment, the pressure of 30MPa exists
1h is sintered at a temperature of 950 DEG C.Heating and rate of cooling are respectively 0.043 and 0.028 DEG C/s, and heat treating regime is:850℃×1h
+ 450℃×6h.The damping capacity of porous Mn-Cu alloy varies with temperature(-50~200℃)Affected smaller, sintering
Mn-Cu alloy can make up the unmanageable problem of high Mn alloy.The manufacture of the Mn system noiseless alloy of special steel company of Datong District application
Process patent (JP 2005-68483) (P2005-68483A) is according to certain using Mn powder and Cu-Ni-Fe-Si powder
Sintered density 5.9g/cm of the MnCu alloy that proportioning mixed sintering obtains3, dampening factor can reach 0.4.
The basic technology that powder metallurgy process prepares porous manganin is that the mixed-powder using simple substance or alloying is
Raw material, makes after pressed compact at 870~950 DEG C in atmosphere or vacuum-sintering and then 800~950 DEG C of solution treatment and 300~500
DEG C long-time Ageing Treatment.The finite concentration solid solution that simple substance Mn element is formed with Cu Elements Diffusion is in 871 DEG C of temperatures above meetings
Transient liquid phase occurring, thus playing the effect of liquid-phase sintering, obtaining the alloy of higher-strength;But sintering temperature can more than 950 DEG C
Cause liquid phase excessive and be unfavorable for the shape stability of sintered body.Due to being all rich in the moisture of certain ingredients in the atmosphere such as hydrogen, nitrogen
Pressure, can cause the surface oxidation of manganese to hinder sintering, and vacuum-sintering is conducive to mitigating the Oxidation of manganese;Pressure sintering or argon etc.
Inert gas shielding sintering also has similar effect.The heat conductivity of simple substance manganese only has 7.82 W/m. DEG C, and fine copper is 401W/m. DEG C.
Due to the low heat conductivity of manganese powder, and more or less there is oxygen or the hydrone of absorption on its surface, and often top layer is attached for large scale pressed compact
The features such as nearly pressed density is higher than core density, causes blank center and surface during heat-agglomerating to there is larger temperature
Difference, surface layer reaches sintering temperature earlier and consistency improves, when core does not reach sintering temperature or needs the insulation grown very much
Between so that the tissue of large-sized manganin sintered body and performance are extremely uneven, formed " ripe interior life outward " state.
Content of the invention
It is an object of the invention to provide improving, with a kind of Ferrox., the method that copper-manganese damps sintered alloy performance, using grass
The ferrous catabolite of acid, as the donor of ferrum element, prepares powder metallurgy copper-manganese damping alloy, iron content can 1.0~
4.0% scope, the nano level highly active Fe acceleration of sintering being obtained using Ferrox. thermal decomposition and hydrogen reduction, discharge
CO2, vapor stop pressed compact surface from forming fine and close confining bed, improve the uniformity of sintered body so that burning under hydrogen reduction atmosphere
Knot can be obtained by large-sized copper-manganese sintered body.
Specific preparation porous copper-manganese high damping alloy processing step is as follows:
1. powder prepares and mixes
By electrolytic manganese powder(Purity:>=99.7% granularity:- 100 mesh), electrolytic copper powder(Purity:>=99.7%, granularity:- 200 mesh)、
Carbonyl nickel powder(Purity:>=99.5%, granularity:2~3.6μ m), sometimes include atomizing aluminium powder(Purity:>=99.2%, mesh number:~10
μm), atomization tin powder(Purity:>=99.5%, mesh number:~10μm), atomized zinc dust(Purity:>=99.8%, mesh number:~10μm), also
Former molybdenum powder(Purity:≥99.8%, ~1μ m)With other a small amount of simple substance carbons, silicon, chromium Mechanical Crushing powder, Ferrox. is chemistry
Crystallographic powder(Purity:>=99%, mesh number:- 80 mesh), the proportioning according to following table carries out dispensing:
Mn:41~77 | Sn:0~1.2 |
Cu:17~39 | Cr:0~0.6 |
Al:0~6 | Mo:0~0.9 |
Fe:1~4 | Zn:0~4 |
Ni:0.3~5 | C:0~0.2 |
Si:0~0.2 |
The powder preparing is placed in ball grinder and is dry grinded, Ball-milling Time is that 0.5 ~ 4h is uniform to powder.
Due to having the plasticity of more amount high Cu, Sn etc. in compound, plasticity can be produced under larger pressing pressure and become
Shape, thus having high compact strength, therefore typically does not need additionally to add plasticizer.But when pressed compact desired size is larger,
The plasticizers such as a certain amount of zinc stearate, paraffin micropowder can be added, can refer to general powder metallurgical technique.
2. compressing
Mixed powder is pressed under the pressure of 100 ~ 600MPa the pressed compact of required size.Pressure limit is according to the chi of blank
The suppression performance of very little and powder mix, and the requirement of porosity, to select, has high demands for large scale, porosity, takes off
Limit;Small size, high densification take big pressure.The cold isostatic compaction to pressure such as can take if necessary.
3. pyrolysis and sintering process
Due to needing pyrolysis, reduction and sintering under the protective effect of the dry hydrogen of flowing, concretely comprise the following steps 180~240 DEG C
Insulation 1~4 hour;400~500 DEG C are incubated 1~4 hour;750 ~ 850 DEG C of temperature retention times 1 ~ 2 hour;Then at 850 ~ 950 DEG C
Temperature retention time completes sintering process in 2 ~ 4 hours;5~10 DEG C/min of programming rate.When sintered blank size is less, temperature and
Temperature retention time can remove the limit, and programming rate can capping.When sintered blank is larger-size, temperature and temperature retention time can use
Limit, programming rate can remove the limit.When Ferrox. addition is big, thermal decomposition stage temperature retention time can capping, programming rate can
Remove the limit.
4. Technology for Heating Processing
Sintering copper-manganese, through solid solution and Ageing Treatment, obtains high damping capacity, referring in particular to the technique ginseng of founding, processing and gold
Number.Manganin due to being prepared using the present invention is porous material, and during heat treatment, heat time heating time needs slightly to extend.
Consumption in every kilogram high manganese copper-manganese damping alloy for the Ferrox. is 12~120 grams.
Ferric oxalate (Fe2(C2O4)3·5H2O) formation Ferrox. (FeC can be just dehydrated in 170 DEG C of temperature below2O4·
2H2O).In argon, FeC2O4·2H2O Thermal Decomposition Mechanism is:170~240 DEG C of generation dehydrations, FeC2O4·2H2O=
FeC2O4+2H2O;400~450 DEG C of generation pyrolytic reactions, 3FeC2O4= Fe3O4+4CO +2CO2.Fe3O4At 600~900 DEG C
Under the conditions of can by hydrogen reduction, its reduction step be Fe3O4+3H2= FeO+3H2O and FeO+H2=Fe+H2O, general more than 800 DEG C
Temperature can more completely be realized reducing.In the manganin powder metallurgical technique containing Fe for the preparation, Fe is replaced using Ferrox.
The Main Function of the donor as Fe element for the powder is:1. the fine Fe element that Ferrox. thermal decomposition, reduction produce has low
Simple substance manganese powder can be fused by fusing point in relatively low temperature, thus reducing thermal resistance interface, improves thermal conductance and the temperature of sintering blank
Degree uniformity, thus improve the uniformity of copper-manganese sintered alloy;2. the temperature range decomposed in Ferrox., pressed compact surface is also
It is not carried out sintering densification, the water that therefore Ferrox. decomposes, reduction produces and carbon dioxide constantly discharge compacting base
Surface, stops pressed compact surface from forming fine and close confining bed, makes surface be in porous state, in the low-temperature heat stage, is conducive to mixing
The discharge of the surface adsorption water of powder;In the high temperature sintering stage, be conducive to hydrogen to enter sintered body, play reduction small amounts metal
The effect of element;3. Ferrox. is fine-powder it is not easy to there is plasticity bonding, is therefore beneficial to composition mix homogeneously;④
Decomposing the fine upper state Fe powder of gained, easily with elements such as manganese, copper, nickel, aluminum, sintering diffusion occurring, thus promoting liquid phase shape
Become and sintering process.
The diameter of up to 100mm of sintered alloy of the present invention, length reach 200mm, and density is 5.10~5.75g/cm3, hardness is 52
~86HRF, bending strength is 128~184MPa, and uniformity is good.By subsequent heat treatment and processing, low-density, high resistant can be obtained
Buddhist nun's copper-manganese component.
Brief description
Fig. 1 is the bending strength curve chart of embodiment 3;
Fig. 2 is the fracture apperance figure of embodiment 7.
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Embodiment 1
By the powder such as manganese, copper, nickel, aluminum, stannum, carbon, silicon and Ferrox. according to table 2 embodiment 1 ingredient composition.Table 2 embodiment
The composition range of copper-manganese damping alloy(Mass percent)
Alloying element | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
Mn | 59.3 | 47.2 | 60 | 52 | 52 | 75 | 76.6 |
Cu | 33 | 39 | 35.9 | 35.9 | 35.7 | 18 | 17 |
Al | 3.0 | 6.0 | 2.0 | 1.0 | 4.0 | / | / |
Fe* | 2.4 | 3.2 | 1.0 | 4.0 | 3.0 | 2 | 1.8 |
Ni | 0.8 | 3.2 | 0.3 | 2.2 | 2.5 | 5 | 4.6 |
Sn | 0.18 | 1.2 | / | / | / | / | / |
Cr | / | / | / | / | 0.6 | / | / |
Mo | / | / | 0.2 | 0.9 | / | / | / |
Zn | / | / | 0.6 | 4.0 | 2.0 | / | / |
C | 0.16 | 0.10 | / | / | 0.08 | / | / |
Si | 0.18 | 0.10 | / | / | 0.12 | / | / |
* it is the content of ferrum element, the used in amounts of Ferrox. will contain Fe mass ratio according to it and calculate.
The powder preparing is placed in ball grinder and is dry grinded, it is uniform to powder that Ball-milling Time is about 2h.
Mixed powder is pressed under the pressure of 600MPa by pressed compact using compacting tool set.
Pyrolysis, reduction and sintering under the protective effect of the dry hydrogen of flowing, concretely comprise the following steps 240 DEG C and are incubated 1 hour;
500 DEG C are incubated 1 hour;850 DEG C of temperature retention times 1 hour;Then in 950 DEG C of temperature retention times 2 hours.Furnace cooling, sinters copper-manganese
Obtain product through solid solution and Ageing Treatment.
The performance of gained sintered blank is listed in table 3
The size of table 3 embodiment copper-manganese damping alloy and performance
Sintering shape | Size, mm | Density, g/cm3 | Hardness, HRF | Bending strength, MPa | |
Embodiment 1 | Square | 10*24*50 | 5.39 | 52 | 128 |
Embodiment 2 | Disk | Φ72*30 | 5.15 | 59 | 156 |
Embodiment 3 | Disk | Φ44*18 | 5.11 | 61 | 140 |
Embodiment 4 | Square | 40*50*118 | 5.33 | 75 | 178 |
Embodiment 5 | Pole | Φ100*200 | 5.28 | 86 | 184 |
Embodiment 6 | Cylindric | Φ32*60 | 5.75 | 84 | 174 |
Embodiment 7 | Square | 58*55*150 | 5.10 | 76 | 143 |
Embodiment 2
By the powder such as manganese, copper, nickel, aluminum, stannum, carbon, silicon and Ferrox. according to table 2 embodiment 2 ingredient composition.By the powder preparing
Material is placed in ball grinder is dry grinded, and it is uniform to powder that Ball-milling Time is about 3h.
Mixed powder is pressed under the pressure of 300MPa by pressed compact using circular die.
Under the protective effect of the dry hydrogen of flowing, pyrolysis, reduction and sintering, concretely comprise the following steps 180 insulation 4 hours;
400 DEG C are incubated 4 hours;750 DEG C of temperature retention times 2 hours;Then in 900 DEG C of temperature retention times 4 hours;5 DEG C/min of programming rate.
Furnace cooling, sintering copper-manganese obtains product through solid solution and Ageing Treatment.The performance of gained sintered blank is listed in Table 3 below.Fig. 1 is to produce
The bending strength curve chart of product.
Embodiment 3
By manganese, copper, nickel, aluminum, molybdenum, zinc powder and Ferrox. according to table 2 embodiment 3 ingredient composition.The powder preparing is put
Dry grinded in ball grinder, it is uniform to powder that Ball-milling Time is about 0.5h.
Mixed powder is pressed under the pressure of 500MPa by pressed compact using circular compacting tool set.
Pyrolysis, reduction and sintering under the protective effect of the dry hydrogen of flowing, concretely comprise the following steps 220 DEG C and are incubated 2 hours;
460 DEG C are incubated 2 hours;800 DEG C of temperature retention times 1 hour;Then in 950 DEG C of temperature retention times 2 hours, 8 DEG C/min of programming rate.
Furnace cooling, sintering copper-manganese obtains product through solid solution and Ageing Treatment.The performance of gained sintered blank is listed in table 3.Fig. 1 is product
Bending strength curve chart.
Embodiment 4
By the powder such as manganese, copper, nickel, aluminum, molybdenum, zinc and Ferrox. according to table 2 embodiment 4 ingredient composition.By the powder preparing
It is placed in ball grinder and is dry grinded, it is uniform to powder that Ball-milling Time is about 2h.
Mixed powder is pressed under the pressure of 400MPa by pressed compact using elongated mould.
Pyrolysis, reduction and sintering under the protective effect of the dry hydrogen of flowing, concretely comprise the following steps 230 DEG C of insulations 1.5 little
When;480 DEG C are incubated 2.5 hours;800 DEG C of temperature retention times 2 hours;Then in 900 DEG C of temperature retention times 2 hours;6 DEG C of programming rate/
Minute.Furnace cooling, sintering copper-manganese obtains product through solid solution and Ageing Treatment.The performance of gained sintered blank is listed in Table 3 below.
Embodiment 5
By the powder such as manganese, copper, nickel, aluminum, chromium, zinc, carbon, silicon and Ferrox. according to the ingredient composition of table 2 embodiment 5, and add
0.8% zinc stearate.The powder preparing is placed in ball grinder and is dry grinded, it is uniform to powder that Ball-milling Time is about 4h.
Mixed powder is loaded in circular rubber set, cold isostatic compaction under the pressure of 100MPa.
Pyrolysis, reduction and sintering under the protective effect of the dry hydrogen of flowing, concretely comprise the following steps 200 DEG C and are incubated 4 hours;
420 DEG C are incubated 4 hours;800 DEG C of temperature retention times 2 hours;Then in 5 DEG C/min of 4 hours programming rates of 850 DEG C of temperature retention times.With
Stove cools down, and sintering copper-manganese obtains product through solid solution and Ageing Treatment.The performance of gained sintered blank is listed in Table 3 below.
Embodiment 6
By the powder such as manganese, copper, nickel and Ferrox. according to table 2 embodiment 6 ingredient composition.The powder preparing is placed in ball grinder
In dry grinded, Ball-milling Time be about 2h uniform to powder.
Mixed powder is pressed under the pressure of 300MPa by pressed compact using circular compacting tool set.
Pyrolysis, reduction and sintering under the protective effect of the dry hydrogen of flowing, concretely comprise the following steps 220 DEG C and are incubated 2 hours;
450 DEG C are incubated 2 hours;800 DEG C of temperature retention times 2 hours;Then in 920 DEG C of temperature retention times 3 hours;5 DEG C/min of programming rate.
Furnace cooling, sintering copper-manganese obtains product through solid solution and Ageing Treatment.The performance of gained sintered blank is listed in table 3.
Embodiment 7
By the powder such as manganese, copper, nickel and Ferrox. according to the ingredient composition of table 2 embodiment 7, and add 0.6% paraffin micropowder.
The powder preparing is placed in ball grinder and is dry grinded, it is uniform to powder that Ball-milling Time is about 3h.
Mixed powder is loaded in square rubber case, cold isostatic compaction under the pressure of 200MPa.
Under the protective effect of the dry hydrogen of flowing, pyrolysis, reduction and sintering, concretely comprise the following steps 180 insulation 4 hours;
500 DEG C are incubated 1 hour;850 DEG C of temperature retention times 1 hour;Then in 920 DEG C of temperature retention times 2 hours;500 DEG C are incubated 2 hours;
920 DEG C of temperature retention times are 2 hours;6 DEG C/min of programming rate.Furnace cooling, sintering copper-manganese obtains through solid solution and Ageing Treatment
Product.The performance of gained sintered blank is listed in Table 3 below.The fracture apperance obtaining product is as shown in Figure 2.
Claims (2)
1. improve, with Ferrox., the method that copper-manganese damps sintered alloy performance, the weight/mass percentage composition of alloy each element is:Mn:
41~77, Cu:17~39, Al:0~6, Fe:1~4, Ni:0.3~5, Sn:0~1.2, Cr:0~0.6, Mo:0~
0.9, Zn:0~4, C:0~0.2 it is characterised in that comprise the following steps:
A powder prepares and mixes
By purity >=99.7%, granularity is less than the electrolytic manganese powder of 100 mesh, purity >=99.7%, the electrolytic copper powder that granularity is less than 200,
Purity >=98.5%, purity >=99.7%, granularity is 2 ~ 3.6 μm of carbonyl nickel powder, purity >=99.2%, and granularity is 8 ~ 12 μm
Atomizing aluminium powder, purity >=99.5%, granularity is 8 ~ 12 μm of atomization tin powders, purity >=99.8%, granularity is 8 ~ 12 μm of atomized zinc dusts,
Purity >=99.8%, granularity is 1 ~ 2 μm of reduction molybdenum powder and other a small amount of simple substance carbons, silicon, chromium Mechanical Crushing powder, purity >=
99%, granularity is that according to required mass percent dispensing, wherein Ferrox. is chemicrystallization less than the Ferrox. of 80 mesh
Crystal powder;The powder preparing is placed in ball grinder and is dry grinded, Ball-milling Time is that 0.5 ~ 4h is uniform to powder;
B is compressing
Mixed powder is pressed under the pressure of 100 ~ 600MPa the pressed compact of required size, pressure limit is according to the chi of blank
The suppression performance of very little and powder mix, and the requirement of porosity is selecting;
C pyrolysis and sintering process
Pyrolysis, reduction and sintering under the protective effect of the dry hydrogen of flowing, concretely comprise the following steps 180~240 DEG C of insulations 1~4
Hour;400~500 DEG C are incubated 1~4 hour;750 ~ 850 DEG C of temperature retention times 1 ~ 2 hour;Then in 850 ~ 950 DEG C of temperature retention times
Complete sintering process within 2 ~ 4 hours;5~10 DEG C/min of programming rate;
D Technology for Heating Processing
Sintering copper-manganese, through solid solution and Ageing Treatment, obtains the alloy of high damping properties.
2. nickelous carbonate as claimed in claim 1 be used for improve sintering copper-manganese damping alloy performance method it is characterised in that:Grass
The ferrous consumption in every kilogram high manganese copper-manganese damping alloy of acid is 12~120 grams.
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