CN104451325B - Process for preparing Mo2FeB2-based metal ceramic - Google Patents
Process for preparing Mo2FeB2-based metal ceramic Download PDFInfo
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- CN104451325B CN104451325B CN201410772081.7A CN201410772081A CN104451325B CN 104451325 B CN104451325 B CN 104451325B CN 201410772081 A CN201410772081 A CN 201410772081A CN 104451325 B CN104451325 B CN 104451325B
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Abstract
The invention discloses a process for preparing Mo2FeB2-based metal ceramic. The process comprises the following steps: firstly selecting high-purity Fe2B powder and Mo powder as raw materials, controlling weight ratio at (0.25-0.5):(0.75-0.5), adding a small amount of absolute ethyl alcohol as a process control agent, weighing, and then carrying out vacuum ball milling for 5-25 hours; then filling mixed powder into a metal mould for compression moulding forming; and finally placing a compression moulding forming blank into a graphite mould, carrying out pressureless sintering in a vacuum sintering furnace at the sintering temperature of 1250-1350 without carrying out heat insulation treatment, and after the sintering is finished, cooling with the vacuum sintering furnace together. The process disclosed by the invention is simple in process. The Mo2FeB2-based metal ceramic prepared through the process disclosed by the invention has the advantages of higher relative density and good main mechanical property index, not only is suitable for an occasion in the filed of abrasion resistance, but also is used for the field of corrosion resistance.
Description
Technical field
The present invention relates to a kind of ceramic-metallic technology of preparing, the ceramic metal preparation method being made up of particularly to one hard phase (percentage by volume is about 60%-80%) and Binder Phase.
Background technology
Mo2FeB2Based ceramic metal is (by hard phase Mo2FeB2Forming with Binder Phase Fe, wherein hard phase percentage by volume general control is between 60%-80%) there is the combination property of excellence, it is with a wide range of applications in the field such as wear-resisting, anti-corrosion, it is also possible to utilize Mo2FeB2The binding ability that ceramic metal is good with steel, the method using the sintering of welding or combination, wearability and the corrosion resistance coating with excellence is formed on the steel matrix surface that height is tough, can be applicable to the slide carriage in high-speed line the lining collars of milling train, colliery, the protective plate of nuclear reactor, tank armor plate, coal washer scraper plate, powder concentrator guide plate etc., advantageously reduce abrasion and the etching extent on steel surface.At present, Japan and other countries is by research Mo2FeB2The composition of based ceramic metal, mutual relation between microstructure sintering mechanism and performance so that it is performance has been continuously available raising, is mainly used in mold materials, the feature that its obdurability with excellence has concurrently mutually with hardness.On the domestic scholar such as the unit such as University of Science & Technology, Beijing, Nanjing Aero-Space University Research foundation abroad, utilize Mo2FeB2Based ceramic metal and the good combination performance of steel, prepare coating in steel matrix and improve the service life of steel.
Mo is prepared in home and abroad at present2FeB2The raw material that based ceramic metal uses is mainly ferro-boron powder, hydroxy iron powder and molybdenum powder (existing lot of documents is reported), higher yet with silicon amount inherent in ferro-boron powder, substantial amounts of silicon-boron of being formed in sintering process, the compound that the fragility such as silicon-molybdenum is bigger, to Mo2FeB2The infringement of based ceramic metal mechanical property is bigger so that it is performance is unable to reach most preferably.To this end, Chinese patent CN102618769A provides is successfully prepared Mo with BN, iron carbonyl and molybdenum for raw material2FeB2Based ceramic metal, but the method needs add plasticizer (gasoline rubber), needing to carry out the binder removal stage in sintering process, and when binder removal terminates finally to sinter, also need isothermal holding, this adds manufacturing cycle undoubtedly；Further, since there are three kinds of materials in raw material, during early stage mixes powder, the mixing uniformity of powder body need to strictly control, and the hard phase otherwise having other during reaction-sintered occurs, it is impossible to reaches to prepare high-performance Mo2FeB2Based ceramic metal final purpose.
Summary of the invention
It is an object of the invention to provide that a kind of cost is relatively low, process stabilizing and be prone to preparation high-performance Mo of industrialization2FeB2The method of based ceramic metal.
For reaching object above, the present invention adopts the following technical scheme that and is achieved:
A kind of Mo2FeB2The preparation technology of based ceramic metal, it is characterised in that comprise the steps:
(1) purity is selected to be not less than the Fe of 99.9%2B powder and Mo powder are raw material, by weight Fe2B:Mo=(0.25-0.5): (0.75-0.5), adds the dehydrated alcohol of mixed powder weight 0.5%, loads in ball grinder and evacuation after weighing；
(2) ball grinder is put into ball milling 5-25 hour in ball mill, take out mixed powder and be filled in metal die, compression molding under 150MPa-300MPa；
(3) base substrate of compression molding is put into vacuum sintering furnace carries out pressureless sintering, vacuum≤10-1Pa；Sintering temperature 1250 DEG C～1350 DEG C, does not make isothermal holding, furnace cooling, obtains Mo2FeB2Based ceramic metal.
In above-mentioned technique, described Fe2Granularity≤150 μm of B powder；Granularity≤100 μm of Mo powder.
The vacuum of described vacuum ball milling is 10-1Pa.The programming rate of described pressureless sintering is: 2-10 DEG C/sec.
Compared with the prior art, present invention process is simple, it is not necessary to isothermal holding, and this is owing in sintering temperature-rise period, ceramic metal has been gradually completing alloying reaction, therefore, when temperature is raised to 1250 DEG C～1350 DEG C, and Mo2FeB2Based ceramic metal has reacted (and belonging to liquid reactive sintering), if carrying out isothermal holding, Mo again2FeB2Crystal grain can substantially be grown up thus be deteriorated ceramic metal performance.The Mo prepared2FeB2Ceramic metal relative density is higher, and Main Mechanical index is good (high-compactness reaches 99.1%, and high-flexural strength reaches 2000MPa, and maximum hardness reaches 89HRA).Not only it is suitable for wear-resisting field occasion, and can be also used for anti-corrosion field.
Accompanying drawing explanation
Fig. 1 is the Mo obtained by the embodiment of the present invention 22FeB2Based ceramic metal metallographic structure photo.
Detailed description of the invention
Embodiment 1
First, raw material selects purity 99.9%, the Fe of granularity 100 μm2B powder and purity 99.99%, the Mo powder of granularity 100 μm, weight ratio controls at 0.25:0.75, and adds the dehydrated alcohol of mixed powder weight 0.5% as process control agent, loads in stainless steel jar mill and carry out evacuation after weighing, and vacuum is 10-1Pa。
Then, ball grinder being put into start in ball mill and rotates, Ball-milling Time is cooled to room temperature to tank body after 5 hours, opens tank body by Fe2The mixed powder of B and Mo is filled in metal die, compression molding under 150MPa.
Finally, being put into by compression molding base substrate and carry out pressureless sintering in graphite jig in vacuum sintering furnace, during sintering, vacuum is 10-2Pa；Programming rate is 10 DEG C/sec；Sintering temperature is: 1250 DEG C (without carrying out isothermal holding), furnace cooling after sintering, takes out sintered body and is Mo2FeB2Based ceramic metal, carries out performance test to it, and consistency is 97.1%, and three-point bending strength is 1520MPa, and hardness is 86.3HRA.
Embodiment 2
Technical process is substantially with embodiment 1, but technological parameter is different: Fe2B Powder Particle Size is 150 μm；Mo Powder Particle Size is 50 μm, and weight ratio controls at 0.5:0.5.
Ball-milling Time 25 hours；Compression molding pressure 200MPa.
Pressureless sintering vacuum is 10-1Pa；Programming rate is 5 DEG C/sec；Sintering temperature 1350 DEG C.Mo prepared by the present embodiment2FeB2Based ceramic metal consistency is 99.1%, and three-point bending strength is 2000MPa, and hardness is 87.3HRA.Its microscopic structure light micrograph (the nitric acid spirits using 5% corrodes 5 seconds) as shown in Figure 1, it is seen that Mo2FeB2Based ceramic metal dense structure, major part Mo2FeB2In square shape block distribution, therefore, it has higher comprehensive mechanical property index.
Embodiment 3
Technical process is substantially with embodiment 1, but technological parameter is different: Fe2B Powder Particle Size is 50 μm；Mo Powder Particle Size is 100 μm, and weight ratio controls at 0.4:0.6.
Ball-milling Time 15 hours；Compression molding pressure 300MPa.
Pressureless sintering vacuum is 10-3Pa；Programming rate is 2 DEG C/sec；Sintering temperature 1300 DEG C.Mo prepared by the present embodiment2FeB2Based ceramic metal consistency is 98.4%, and three-point bending strength is 1691MPa, and hardness is 89.0HRA.
Claims (2)
1. a Mo2FeB2The preparation technology of based ceramic metal, it is characterised in that comprise the steps:
(1) purity is selected to be not less than the Fe of 99.9%2B powder and Mo powder are raw material, by weight Fe2B:
Mo=(0.25-0.5): (0.75-0.5), adds the dehydrated alcohol of mixed powder weight 0.5%, fills after weighing
Enter in ball grinder and evacuation；
(2) ball grinder is put into ball milling 5-25 hour in ball mill, take out mixed powder and be filled to metal pattern
In tool, compression molding under 150MPa-300MPa；
(3) base substrate of compression molding is put into vacuum sintering furnace carries out pressureless sintering, vacuum≤
10-1Pa；Sintering temperature 1250 DEG C～1350 DEG C, does not make isothermal holding, furnace cooling, obtains Mo2FeB2
Based ceramic metal；
Described Fe2Granularity≤150 μm of B powder；Granularity≤100 μm of Mo powder；
The programming rate of described pressureless sintering is 2-10 DEG C/sec.
2. Mo as claimed in claim 12FeB2The preparation technology of based ceramic metal, it is characterised in that
The vacuum of described vacuum ball milling is 10-1Pa。
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| CN201410772081.7A CN104451325B (en) | 2014-12-12 | 2014-12-12 | Process for preparing Mo2FeB2-based metal ceramic |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106048357B (en) * | 2016-06-13 | 2017-10-10 | 陕西理工学院 | A kind of MoSiC2 base metal-ceramic materials and preparation method thereof |
| CN106916986B (en) * | 2017-02-22 | 2018-05-08 | 三峡大学 | A kind of low cost Mo2FeB2The preparation method of based ceramic metal |
| CN111041321A (en) * | 2019-12-24 | 2020-04-21 | 浙江恒大数控装备有限公司 | Metal ceramic for machine tool guide rail and preparation process thereof |
| CN115652127B (en) * | 2022-11-01 | 2023-09-08 | 西安近代化学研究所 | Nearly equiaxial grain Mo 2 FeB 2 Preparation method of base metal ceramic |
| CN116117145A (en) * | 2022-11-25 | 2023-05-16 | 西安近代化学研究所 | TiB (titanium-boron) 2 Modified Mo 2 FeB 2 Method for producing a base composite material |
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| CN102618769B (en) * | 2012-04-05 | 2013-05-22 | 北京科技大学 | Manufacturing method of Mo2FeB2 based steel bonded hard alloy |
| CN104004953B (en) * | 2014-06-08 | 2016-03-16 | 湖南人文科技学院 | Boride-base cerment of a kind of pair of hard phase complex intensifying and preparation method thereof |
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