CN101670440A - Material for preparing object by powder metallurgy material - Google Patents
Material for preparing object by powder metallurgy material Download PDFInfo
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- CN101670440A CN101670440A CN200910174373A CN200910174373A CN101670440A CN 101670440 A CN101670440 A CN 101670440A CN 200910174373 A CN200910174373 A CN 200910174373A CN 200910174373 A CN200910174373 A CN 200910174373A CN 101670440 A CN101670440 A CN 101670440A
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- oxide
- metal oxide
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- adhesive
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The present invention relates to a method for preparing object by powder metallurgy material, which comprises the following steps: a) mixing the powder shaped metal oxide with bonding agent; b) granulating the mixture obtained from the step a); c) removing the bonding agent in the metal oxide particles; and d) deoxygenating the metal oxide particles. In one embodiment solution, the following stepsare than performed: e) pressing the metal oxide obtained from the step d); and f) sintering the obtained pressed object. The invention also relates to a workpiece prepared by the method of the invention and the application of the workpiece in an internal combustion engine as an injection device.
Description
Technology neck city
The present invention relates to a kind of by powdered metallurgical material prepare the method for object, by the application of workpiece and this workpiece of this method gained.
Background technology
Now, powder metallurgy has increasing importance to the preparation in enormous quantities of complicated hardware.Compare with the smear metal processing method, can prepare member with big production capacity near final profile ground by powder metallurgic method such as compacting, casting or extruding.
Usually in powder metallurgy process, pressing aid agent such as adhesive or lubricant are added in the metal dust, and it is mixed and uses the specific method of forming of technology to carry out mechanical ramming, produce required shape thus.So the press body (blank) of gained through removing the pressing aid agent that adds, is a sintering through heat treatment process then at first.This porous molding is transformed into intimate closely knit final member through reducing pore volume.
The typical mean granularity of this metal dust is 10-50 μ m according to forming method.But the germination that takes place during by used granularity and sintering, the granularity part of this material structure is obviously greater than 100 μ m.Material with acinose texture of nanocrystal is desirable, because this produces favourable influence to mechanical property.Increase with its microstructure fineness, the trade mark is that the steel of Hall-Petch is almost keeping having the intensity that increases under the identical toughness.So far, the steel for preparing this nanocrystal mutually by fusion only expends (high deformation velocity), expensive and just possible to limited geometry (planar sheet) with extra-high-speed.
For preparing this grain structure, need be starkly lower than the granularity of 5 μ m by powder metallurgic method.But this metal dust can not prepare fully or only expend just and can prepare with height, and is expensive thus, is impossible so prepare corresponding member economically.
A kind of method that is replaced metal dust by metal oxide powder has been described in the prior art.For example EP 1268105 B1 disclose the method that a kind of preparation has the metallic object of the plastically deformable of specifying geometry, this method is by metal compound particles being mixed with adhesive and be pressed into moulded parts, removing adhesive afterwards and by charge into reducing gas under higher temperature metallic compound is reduced into metal.
Under the sintering temperature of the metallic compound that is lower than reduction, reduce, and use the binder combination of forming by removable as soluble component and stable component as insoluble.In addition, for example useable solvents is removed this removable component, and then in 550-950 ℃ oxidizing atmosphere this molding is pressurizeed.This stable adhesive ingredients is transformed into gaseous decomposition product thus, and by removing in the matrix.This molding through prereduction, restores with hydrogen-containing gas in carbon-containing atmosphere then.
But the shortcoming of this method is, the density contrast that produces during the metal oxide reduction can cause stress in porous member, and this stress can cause crackle and member distortion.The other method of needs when preparing object thus with powder metallurgy.
Summary of the invention
Therefore, the invention provides and a kind ofly prepare the method for object by powdered metallurgical material, it comprises the following steps:
A) the powdery metal oxide is mixed with adhesive,
B) make gained mixture granulating in the step a),
C) adhesive in the removal metal oxide particle,
D) reducing metal oxide particle.
Method of the present invention at first provides metal oxide particle, then can proceed processing to this particle.
By being mixed with adhesive, the powdery metal oxide obtains having plastic properties and the material that can process in this way.The deal of this adhesive in mixture for example can be 〉=and 40 volume % are to≤70 volume %.The adhesive that is suitable for can be wax and/or thermoplastic polymer.Wax for example is stearin or paraffin, and it simultaneously also can be at granulation step b) in the effect of super fatting agent.Thermoplastic polymer for example is polyolefin such as polyethylene or polypropylene and polyester or polyethers.
The mixture of this gained can be granulated with usual way then, for example passes through by nozzle extruding granulating, and cuts this particle by rotating blade.This particle for example can be diameter for 〉=0.01mm to≤10mm with longly be 〉=0.1mm cylindrical, circular, ellipsoid or spheroid to≤10mm.The length and/or the diameter of each coccoid also can be 〉=0.03mm-≤5mm.
Therefore adhesive is suitable for reduction thereafter for example with by the use of thermal means or by behind the removal of solvents, this metal oxide still exists with granular very much.Because the reduction of this metal oxide is not to carry out in the member of compacting, but in the powder grain, carry out, so can virtually completely avoid the crackle in the material and the problem of member distortion.Its reason particularly less the evolving path Buddhist monk in the particle is not the member profile.Therefore can realize significantly more simple operation and shorter process time.
After reduction, advantageously will avoid reoxidizing by the metallic particles of gained in step d) for this metal oxide particle.This for example can be by guaranteeing with oil this metal of spraying or by implement operation in inert environments.Inert environments can be the protection compression ring border that contains argon, nitrogen or other inert gas.
Because the metallic particles of gained for example can be up to 70% high porosity and consequent high-ductility, so this metallic particles can be easy to be pressed near final profile and then carry out sintering.
The specific embodiment
Therefore the inventive method also comprises the following steps: in one embodiment
E) suppress d set by step) metallic particles of gained,
F) rolled-up stock of sintering gained.
Different with the method for prior art, the inventive method at first preparation be similar to the molding of member, but only prepare the particle of forming by metal oxide powder, this particle is reduced into metal powder granulates in reduction step thereafter.According to the complexity of member, can adopt different drawing methods such as single shaft to compacting or wait static pressure to suppress.Single shaft is to compacting or wait the pressure of static pressure compacting for example to can be 〉=100MPa-≤1000MPa, preferably 〉=and 200MPa-≤800MPa.This compacting for example can be at 〉=0 ℃-≤50 ℃, preferred 〉=and 20 ℃-≤25 ℃ temperature carries out.
For reaching the required final densities of this rolled-up stock, this rolled-up stock needs through sintering after compacting.Should consider short sintering time, so that can interrupt germination and can obtain meticulous kernel structure.Suitable sintering time for example can be 〉=1min-≤60min, and suitable sintering temperature for example can be 〉=and 400 ℃-≤800 ℃.This sintering also can recover the defective of appearance when compacting once more.This sintering step benefits under reducing atmosphere and carries out, and this rolled-up stock can be not oxidated more thus.The most suitable to this nitrogen atmosphere.
In another embodiment of the inventive method, the particle mean size d50 of this powdery metal oxide is 〉=0.01 μ m-≤3 μ m.This granularity also can be 〉=0.05 μ m-≤2.5 μ m or 〉=0.1 μ m-≤2 μ m.The d50 value can be calculated by the size distribution of measuring by mark heap ISO 13320.Obtain desired particle size in the gained reducing metal by the big I of this raw material.
In another embodiment of the inventive method, this metal oxide is selected from the group of the mixed oxide that comprises iron (II) oxide, iron (II/III) oxide, iron (III) oxide, nickel (II) oxide, chromium (III) oxide, manganese (II) oxide, manganese (IV) oxide, cobalt (II) oxide, copper (I) oxide, copper (II) oxide, molybdenum (VI) oxide, tungsten (VI) oxide and/or described element.Can obtain steel alloy or non-steel alloy as powdered metallurgical material with the method.
In another embodiment of the inventive method, this adhesive content of wax composition and thermoplastic polymer composition, and the binder removal in step c) comprises with organic solvent stripping wax composition, then is the thermal decomposition of component of polymer.
At this wax that is suitable for for example also is stearin or paraffin, and suitable thermoplastic polymer is polyolefin such as polyethylene or polypropylene and polyester or polyethers.This organic solvent should be from metal oxide particle stripping wax composition, but not stripping becomes only few stripping component of polymer.Acetone, toluene or dimethylbenzene are particularly suitable to this.
By the stripping of wax composition, in metal oxide particle, produce hole and passage, the gas that can overflow thus and when the component of polymer thermal decomposition, produce, and can not make particle impaired promptly for example last by powdered.The thermal decomposition of this polymer for example can be carried out 〉=300 ℃-≤500 ℃ temperature.
In addition, in adhesive, also can contain the catalytic activity compound of cracking catalyst action, can quicken the decomposition of this polymer thus.Can from the metal oxide powder particle, partly remove carbon compound fully or only by thermal decomposition.
In another embodiment of the inventive method, after step c) was removed adhesive, the average carbon content in this metal oxide particle was 〉=10ppm-≤1000ppm.This carbon content also can be 〉=50ppm-≤800ppm or 〉=100ppm-≤500ppm.Owing in whole particle, evenly contain to come the carbon of the remnants of Autoadhesive, so in technology thereafter, begin to take place the even reduction of the powder surface in the particle.
In another embodiment of the inventive method, the reduction of the metal oxide particle in the step d) is carried out in the atmosphere of carbonated, hydrogen and argon.The reduction fully of this metal oxide can realize by the atmosphere of reproducibility.Compare with the member of suppressing by metal oxide powder, reduction step is more simplified owing to the little the evolving path in particle.
In addition, owing to the time also do not relate to the member geometry fully, so because slight inhomogeneous reduction and inhomogeneous contraction are at the beginning all twisted the geometry of this powder particle has no adverse effect in reduction.
By select gas composition can be in wide region the reduction intensity of the partial pressure of oxygen in the regulation system and this admixture of gas.This gas can adapt to powder size and granular size to the reduction of metal oxide.Reduction Ying Yi carries out equably and in the whole particle body, and finishes before this powder begins obvious sintering.
In another embodiment of the inventive method, this is d set by step) metallic particles of gained is then through the metal cation solution-treated.The metal cation that is suitable for is copper and/or aluminium particularly.This particle should use the concentrated solution of metal cation to soak into.
Usually this metal cation can be reduced into metal more fully or deposit with finely divided oxide particle form.Can introduce second phase at crystal boundary especially thus, thereby but also can make and to diffuse into matrix and to constitute corresponding alloy by element such as the aluminium that the direct reduction of metal oxide obtains.
Another object of the present invention provides a kind of workpiece that makes with the inventive method, goes back implementation method step e) and f when this workpiece of preparation).This class workpiece contains the nanocrystal material, and needing can be used for high strength to need the component assembly of high tenacity again simultaneously.
Therefore another purpose of the present invention is that this class workpiece is used as the purposes of injection apparatus in internal combustion engine.Wherein be preferably the particularly injection apparatus of Diesel engine of engine.It for example can be the high-pressure injection device of Diesel engine or common-rail system.
Claims (10)
1. prepared the method for object by powdered metallurgical material, it comprises the following steps:
A) the powdery metal oxide is mixed with adhesive,
B) make gained mixture granulating in the step a),
C) adhesive in the removal metal oxide particle,
D) reduce this metal oxide particle.
2. the method for claim 1, it also comprises the following steps:
E) suppress d set by step) metallic particles of gained,
F) rolled-up stock of sintering gained.
3. claim 1 or 2 method, wherein, the particle mean size d50 of described pulverous metal oxide is 〉=0.01 μ m-≤3 μ m.
4. claim 1 or 2 method, wherein, described metal oxide is selected from the group of the mixed oxide that comprises iron (II) oxide, iron (II/III) oxide, iron (III) oxide, nickel (II) oxide, chromium (III) oxide, manganese (II) oxide, manganese (IV) oxide, cobalt (II) oxide, copper (I) oxide, copper (II) oxide, molybdenum (VI) oxide, tungsten (VI) oxide and/or described element.
5. claim 1 or 2 method, wherein, described adhesive content of wax composition and thermoplastic polymer composition, and the binder removal in step c) comprises with organic solvent stripping wax composition, then is the thermal decomposition of component of polymer.
6. claim 1 or 2 method, wherein, after step c) was removed adhesive, the average carbon content in the described metal oxide particle was 〉=10ppm-≤1000ppm.
7. claim 1 or 2 method, wherein, the reduction of the metal oxide particle in the step d) is carried out in the atmosphere of carbonated, hydrogen and argon.
8. claim 1 or 2 method, wherein, described d set by step) metallic particles of gained is then through the metal cation solution-treated.
9. the workpiece that makes of the method by one of claim 2-8.
The workpiece of claim 9 in internal combustion engine as the application of injection apparatus.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102008042047.6 | 2008-09-12 | ||
| DE102008042047A DE102008042047A1 (en) | 2008-09-12 | 2008-09-12 | Producing articles made of powder-metallurgy materials, comprises mixing powdered metal oxide with binder, granulating mixture obtained in the mixing step, removing binder from metal oxide granules and then reducing metal oxide granules |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101670440A true CN101670440A (en) | 2010-03-17 |
Family
ID=41667630
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910174373A Pending CN101670440A (en) | 2008-09-12 | 2009-09-11 | Material for preparing object by powder metallurgy material |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN101670440A (en) |
| DE (1) | DE102008042047A1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104325134A (en) * | 2014-11-14 | 2015-02-04 | 武汉钢铁(集团)公司 | Nano iron powder sintering body containing nano ferrous oxide and preparation method of nano iron powder sintering body |
| CN105492148A (en) * | 2013-09-02 | 2016-04-13 | 攀时奥地利公司 | Chromium-containing powder or granulated powder |
| CN107848030A (en) * | 2015-07-24 | 2018-03-27 | 罗伯特·博世有限公司 | The method of the drip molding of coating and the drip molding for manufacturing coating |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1202846A (en) * | 1995-11-27 | 1998-12-23 | H·C·施塔克公司 | Metal powder granulates, method for their production and use of the same |
| EP0688746B1 (en) * | 1994-05-27 | 2000-01-26 | Technische Universiteit Delft | Method of manufacturing molded articles from metallic or ceramic powdered particles and binder system suitable for use therein |
| US6939509B2 (en) * | 2000-03-24 | 2005-09-06 | Manfred Endrich | Method for manufacturing metal parts |
-
2008
- 2008-09-12 DE DE102008042047A patent/DE102008042047A1/en not_active Withdrawn
-
2009
- 2009-09-11 CN CN200910174373A patent/CN101670440A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0688746B1 (en) * | 1994-05-27 | 2000-01-26 | Technische Universiteit Delft | Method of manufacturing molded articles from metallic or ceramic powdered particles and binder system suitable for use therein |
| CN1202846A (en) * | 1995-11-27 | 1998-12-23 | H·C·施塔克公司 | Metal powder granulates, method for their production and use of the same |
| US6939509B2 (en) * | 2000-03-24 | 2005-09-06 | Manfred Endrich | Method for manufacturing metal parts |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105492148A (en) * | 2013-09-02 | 2016-04-13 | 攀时奥地利公司 | Chromium-containing powder or granulated powder |
| TWI679288B (en) * | 2013-09-02 | 2019-12-11 | 奧地利商攀時歐洲公司 | Chromium-containing powder or powder granulate |
| CN105492148B (en) * | 2013-09-02 | 2020-06-19 | 攀时奥地利公司 | Chromium-containing powder or powder particles |
| CN104325134A (en) * | 2014-11-14 | 2015-02-04 | 武汉钢铁(集团)公司 | Nano iron powder sintering body containing nano ferrous oxide and preparation method of nano iron powder sintering body |
| CN104325134B (en) * | 2014-11-14 | 2016-08-24 | 武汉钢铁(集团)公司 | Nanometer iron powder sintered body containing nano ferrous iron oxide and preparation method thereof |
| CN107848030A (en) * | 2015-07-24 | 2018-03-27 | 罗伯特·博世有限公司 | The method of the drip molding of coating and the drip molding for manufacturing coating |
Also Published As
| Publication number | Publication date |
|---|---|
| DE102008042047A1 (en) | 2010-03-18 |
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Application publication date: 20100317 |