CN103938010B - A kind of method preparing porous molybdenum silicon boron triple-phase alloys - Google Patents
A kind of method preparing porous molybdenum silicon boron triple-phase alloys Download PDFInfo
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- CN103938010B CN103938010B CN201410165581.4A CN201410165581A CN103938010B CN 103938010 B CN103938010 B CN 103938010B CN 201410165581 A CN201410165581 A CN 201410165581A CN 103938010 B CN103938010 B CN 103938010B
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Abstract
Prepare a method for porous molybdenum silicon boron triple-phase alloys, belong to refractory metal porous material preparing technical field.Use commercial Mo powder, Si powder, B powder; prepare burden by the volume percent of required three kinds of phases; add dehydrated alcohol; use omnidirectional planetary ball mill batch mixing 12 ~ 36h; paraffin gasoline binder is added in the Mo-Si-B element powders mixed; paraffin gasoline forming aid present accounts for 5 ~ 13wt.% of Mo-Si-B element powders and paraffin gasoline binder total amount, is placed on high-temperature atmosphere sintering oven normal pressure-sintered preparation porous Mo under argon gas atmosphere protection through coldmoulding
5siB
2-Mo
3si-Mo
5si
3triple-phase alloys.Its advantage is that the erosion resistance of this porous material is better than metal polyporous material, and toughness is better than ceramic porous material, and Mo
5siB
2, Mo
3si, Mo
5si
3the fabricated in situ of three-phase and the generation of hole are that a step completes, and this technical process is simple, and economy is good.
Description
Technical field
The invention belongs to refractory metal porous material preparing technical field, relate generally to the preparation method of compound molybdenum silicon boron porous material between high-melting-point, refractory metal.
Background technology
The features such as porous material is the material comprising a large amount of hole, and different from dense material, it is low that it has density, and specific surface area is large, and high and damping capacity is good than mechanical property are a kind of functional structure materials with huge applications potentiality.Current porous material has been widely used in the numerous areas such as aerospace, petrochemical complex, nuclear power, environmental protection, medical treatment, metallurgy, building and electrochemistry, play in national economy and act on day by day significantly (Liu Peisheng. porous material draws opinion [M]. Beijing: press of Tsing-Hua University, 2004.).
Be at present porous ceramics and porous metal material at filtration, purification, the most popular porous material of catalytic field, the mechanical property of porous metal material, thermal conductivity, electroconductibility and thermal shock resistance are fine, but corrosion resistance and high temperature oxidation drag not enough.The corrosion resistance of porous ceramic film material, high temperature oxidation drag, thermotolerance, excellent in abrasion resistance, but its fragility is large, toughness, poor ductility and heat-shock resistance is poor.Porous ceramics and porous metal deficiency separately limits its application as high temperature filtration, purification, catalytic material, therefore necessary exploitation can filter in conjunction with a new generation of porous ceramics and porous metal advantage, purification, catalysis porous material.
Mo-Si-B series intermetallic compound has the chemical property between metal and pottery, Mo wherein
5siB
2-Mo
3si-Mo
5si
3triple-phase alloys has that hot strength is high, creep resistance good, toughness and heat-shock resistance be better than pottery, corrosion resistance nature and antioxidant property be better than metal (with ceramic phase when) outstanding advantages (LembergJ A, Ritchie RO.Mo-Si-B Alloys for Ultrahigh-Temperature StructuralApplications [J] .AdvancedMaterials, 2012,24 (26): 3445-3480.), be the excellent selection of porous material.There is no the relevant report of preparation porous Mo-Si-B alloy at present.
Summary of the invention
The object of this invention is to provide a kind of fabricated in situ and prepare Mo
5siB
2-Mo
3si-Mo
5si
3the method of triple-phase alloys porous material.The resistance to corrosion of the Mo-Si-B porous material prepared is better than metal polyporous material, suitable with ceramic porous material, and toughness is better than pottery, is suitable for use as filtration, purification, catalysis porous material; And Mo
5siB
2, Mo
3si, Mo
5si
3the fabricated in situ of three-phase and the generation of hole are that a step completes, and this method technical process is simple, good economy performance.
Prepare a method for porous molybdenum silicon boron triple-phase alloys, adopt fabricated in situ technique, use high-temperature atmosphere sintering oven is normal pressure-sintered under argon gas atmosphere protection prepares Mo-Si-B porous material.In Mo-Si-B porous alloy, the volume percent content scope of three kinds of phases is: 0.4%-99.8%Mo
5siB
2, 0.1%-99%Mo
3si, 0.1%-99%Mo
5si
3.(volume percent range of three kinds of phases meets Mo
5siB
2+ Mo
3si+Mo
5si
3=100%).Use (2 ~ 150 μm, commercial Mo powder, >=99.9wt.%), (2 ~ 150 μm, Si powder, >=99.9wt.%), (2 ~ 150 μm, B powder, >=99.9wt.%), after the mixed powder of preparation being added dehydrated alcohol, batch mixing is also dry, adds paraffin gasoline binder, coldmoulding in powder after the drying, powder compact prepares porous material by normal pressure-sintered, and its concrete technology flow process is as follows:
(1) by required Mo
5siB
2-Mo
3si-Mo
5si
3the volume percent content of three kinds of phases, calculate the weight percent of Mo powder, Si powder, B powder, make required mixed powder, add appropriate dehydrated alcohol, be placed in omnidirectional planetary ball mill batch mixing 12 ~ 36h, then in vacuum drying oven in 30-80 DEG C of drying 4 ~ 8h.
(2) add paraffin gasoline binder (paraffinicity is 20wt.%) in powder after the drying, paraffin gasoline forming aid present accounts for 5 ~ 13wt.% of Mo-Si-B element powders and paraffin gasoline binder total amount, then coldmoulding.It is normal pressure-sintered that the green compact suppressed are placed in high-temperature atmosphere sintering oven, and sintering atmosphere is argon gas.Sintering process is: rise to 300 ~ 400 DEG C with 5 ~ 10 DEG C/min from room temperature, insulation 1 ~ 2h, then rises to 1500 ~ 1650 DEG C with 5 ~ 20 DEG C/min, and insulation 1 ~ 3h, then stove is chilled to room temperature.
Advantage of the present invention is that the resistance to corrosion of Mo-Si-B porous material is better than metal polyporous material, and toughness is better than ceramic porous material.In addition, by adjustment sintering temperature and Si Powder Particle Size, pore structure and the pore size of porous material can be controlled, due to the Mo in alloy
5siB
2, Mo
3si, Mo
5si
3three kinds is in-situ preparation mutually, thus Entropy density deviation evenly, interfacial cleanliness, associativity be good, ensure that the excellent properties of porous Mo-Si-B alloy, and the fabricated in situ of material and the generation of hole complete simultaneously, and technical process is simple, and economy is good.
Accompanying drawing explanation
Fig. 1 is 32.37vol%Mo
5siB
2-4.5vol%Mo
3si-63.13vol%Mo
5si
3the XRD spectral line of porous material (1600 DEG C, 2h);
Fig. 2 is 32.37vol%Mo
5siB
2-4.5vol%Mo
3si-63.13vol%Mo
5si
3the scanning electron microscope pattern of porous material (1600 DEG C, 2h, 6 μm of silica flours);
Fig. 3 is 32.37vol%Mo
5siB
2-4.5vol%Mo
3si-63.13vol%Mo
5si
3the graph of pore diameter distribution of porous material (1600 DEG C, 2h, 6 μm of silica flours);
Fig. 4 is 32.37vol%Mo
5siB
2-4.5vol%Mo
3si-63.13vol%Mo
5si
3the room temperature compression true stress-true strain curve of porous material (1600 DEG C, 2h, 6 μm of silica flours);
Fig. 5 is 32.37vol%Mo
5siB
2-4.5vol%Mo
3si-63.13vol%Mo
5si
3the scanning electron microscope pattern of porous material (1600 DEG C, 2h, 75 μm of silica flours);
Fig. 6 is 32.37vol%Mo
5siB
2-4.5vol%Mo
3si-63.13vol%Mo
5si
3the graph of pore diameter distribution of porous material (1600 DEG C, 2h, 75 μm of silica flours).
Embodiment
Embodiment 1:
By thing phase volume ratio 32.37vol%Mo
5siB
2-4.5vol%Mo
3si-63.13vol%Mo
5si
3make required mixed powder, use (4 μm commercial, Mo powder, 99.9wt.%), (6 μm, Si powder, 99.999wt.%), (3.96 μm, B powder, 99.99wt.%), add dehydrated alcohol as batch mixing medium, be placed in omnidirectional planetary ball mill batch mixing 24h, then in vacuum drying oven in 50 DEG C of dry 6h, paraffin gasoline binder (paraffinicity is 20wt.%) is added in dried powder, paraffin gasoline forming aid present accounts for the 9wt.% of Mo-Si-B element powders and paraffin gasoline binder total amount, take appropriate mixed powder, be cold-pressed into Φ 13mm cylinder pressed compact.Pressed compact is placed in high-temperature atmosphere sintering oven and rises to 350 DEG C with 5 DEG C/min from room temperature under an argon atmosphere, insulation 1h, then rises to 1600 DEG C with 10 DEG C/min, and insulation 2h, then stove is chilled to room temperature, obtains the cylindrical sample of Φ 13 × 7mm.As shown in Figure 1, can find out, material prepared by reaction sintering is desired triple-phase alloys to its XRD figure spectrum, does not have the diffraction peak of other thing phases.It is 44.48% that drainage records its porosity, and open porosity is 33.81%.Fig. 2 is the scanning electron microscope secondary electron pattern of sample, and can find out that pore framework is smooth, hole is communicated with completely.Fig. 3 is the pore size distribution curve that mercury injection apparatus records, and pore size distribution mainly concentrates on 1 ~ 3 μm, and most probable pore size is 2.2 μm.Utilize mercury injection apparatus also to record its specific surface area for 0.216m simultaneously
2/ g.Fig. 4 is room temperature compression true stress-true strain curve, and its compressive strength at room temperature is 330MPa.
Embodiment 2:
By thing phase volume ratio 32.37vol%Mo
5siB
2-4.5vol%Mo
3si-63.13vol%Mo
5si
3make required mixed powder, use (4 μm commercial, Mo powder, 99.9wt.%), (75 μm, Si powder, 99.999wt.%), (3.96 μm, B powder, 99.99wt.%), add dehydrated alcohol as batch mixing medium, be placed in omnidirectional planetary ball mill batch mixing 24h, then in vacuum drying oven in 50 DEG C of dry 6h, paraffin gasoline binder (paraffinicity is 20wt.%) is added in dried powder, paraffin gasoline forming aid present accounts for the 9wt.% of Mo-Si-B element powders and paraffin gasoline binder total amount, take appropriate mixed powder, be cold-pressed into Φ 13mm cylinder pressed compact.Pressed compact is placed in high-temperature atmosphere sintering oven and rises to 350 DEG C with 5 DEG C/min from room temperature under an argon atmosphere, insulation 1h, then rises to 1600 DEG C with 10 DEG C/min, and insulation 2h, then stove is chilled to room temperature, obtains the cylindrical sample of Φ 13 × 7mm.It is 48.33% that drainage records its porosity, and open porosity is 36.98%.Fig. 5 is the scanning electron microscope secondary electron pattern of sample, and its hole aperture is greater than porous material prepared by use 6 μm of silica flours.Fig. 6 is the pore size distribution curve that mercury injection apparatus records, and pore size distribution mainly concentrates on 1 ~ 7 μm, and most probable pore size is 3.5 μm.It is 0.188m that mercury injection apparatus also records its specific surface area simultaneously
2/ g.Its compressive strength at room temperature is 143MPa.
Claims (2)
1. prepare the method for porous molybdenum silicon boron triple-phase alloys for one kind, it is characterized in that adopting fabricated in situ technique, use high-temperature atmosphere sintering oven normal pressure-sintered preparation Mo-Si-B porous material under argon gas atmosphere protection, in Mo-Si-B porous alloy, the volume percent content scope of three kinds of phases is: 0.4%-99.8%Mo
5siB
2, 0.1%-99%Mo
3si, 0.1%-99%Mo
5si
3, the volume percent range of three kinds of phases meets Mo
5siB
2+ Mo
3si+Mo
5si
3=100%, its preparation technology is: raw material adopts Mo powder, Si powder, B powder, element powders weight content is calculated by the volume percent of required three kinds of phases, make required mixed powder, add dehydrated alcohol, to be placed in after omnidirectional planetary ball mill batch mixing 12 ~ 36h at vacuum drying oven in 30-80 DEG C of drying 4 ~ 8h, paraffin gasoline binder is added in dried mixed powder, paraffinicity is 20wt.%, paraffin gasoline forming aid present accounts for 5 ~ 13wt.% of Mo-Si-B element powders and paraffin gasoline binder total amount, be placed in high-temperature atmosphere sintering oven normal pressure-sintered under an argon atmosphere through coldmoulding, 300 ~ 400 DEG C are risen to from room temperature with 5 ~ 10 DEG C/min, insulation 1 ~ 2h, 1500 ~ 1650 DEG C are risen to again with 5 ~ 20 DEG C/min, insulation 1 ~ 3h, then stove is chilled to room temperature.
2. a kind of method preparing porous molybdenum silicon boron triple-phase alloys according to claim 1, is characterized in that raw material uses commercial 2 ~ 150 μm, >=99.9wt.%Mo powder, 2 ~ 150 μm, >=99.9wt.%Si powder, 2 ~ 150 μm, >=99.9wt.%B powder.
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| CN103938010B true CN103938010B (en) | 2015-10-28 |
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| CN107385367B (en) * | 2017-08-02 | 2018-10-23 | 西北有色金属研究院 | A kind of preparation method of fine grain hypoxemia type Multiphase Mo-Si-B alloys |
| CN108580882B (en) * | 2018-06-20 | 2019-12-17 | 西安琦丰光电科技有限公司 | powder ball-milling mixing method of molybdenum-silicon-boron material for additive manufacturing |
| CN114182150B (en) * | 2021-11-01 | 2022-11-01 | 台州学院 | Novel nonequilibrium Mo + Mo5SiB2+Mo5Si3Base alloy and method for producing same |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100999321A (en) * | 2007-01-04 | 2007-07-18 | 北京科技大学 | Method of preparing molybdenum silicide powder |
| CN102534279A (en) * | 2012-01-20 | 2012-07-04 | 北京科技大学 | In situ reaction hot-pressing method for manufacturing intermetallic compound T2 phase alloys |
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2014
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100999321A (en) * | 2007-01-04 | 2007-07-18 | 北京科技大学 | Method of preparing molybdenum silicide powder |
| CN102534279A (en) * | 2012-01-20 | 2012-07-04 | 北京科技大学 | In situ reaction hot-pressing method for manufacturing intermetallic compound T2 phase alloys |
Non-Patent Citations (1)
| Title |
|---|
| Mo-Si-B三元系复合材料的制备及室温断裂韧性;刘丰收等;《北京科技大学学报》;20040229;第26卷(第1期);第63-68页 * |
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