CN101397617A - Method for preparing alloy nano rare-earth oxide doping molybdenum-silicium-boron alloy - Google Patents
Method for preparing alloy nano rare-earth oxide doping molybdenum-silicium-boron alloy Download PDFInfo
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- CN101397617A CN101397617A CNA2008102319764A CN200810231976A CN101397617A CN 101397617 A CN101397617 A CN 101397617A CN A2008102319764 A CNA2008102319764 A CN A2008102319764A CN 200810231976 A CN200810231976 A CN 200810231976A CN 101397617 A CN101397617 A CN 101397617A
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Abstract
The invention discloses a method for preparing a molybdenum-silicon-boron alloy doped with a nano rare earth oxide, which comprises the steps that: rare earth ammonium dimolybdate is taken as raw material, molybdenum alloy powder containing the rare earth oxide is obtained by adopting methods of roasting and hydrogen reduction, silicon powder and boron powder are added into the molybdenum alloy powder, ball grinding processing is carried out, and then hot pressed sintering is carried out in a vacuum hot pressed sintering furnace so as to lead the densification of the powder, wherein, the sintering temperature is 1600 to 1800 DEG C, the sintering pressure is 45 to 55MPa and the sintering time is 5 to 10 hours. The preparing method is simple and practicable, the size of the rare earth oxide particles in the prepared molybdenum-silicon-boron alloy is tiny, the average particle size is smaller than 100nm, and the prepared molybdenum-silicon-boron alloy has the advantage of high strength.
Description
Technical field
The invention belongs to powder metallurgical technology, the preparation method of particularly a kind of nano rare-earth oxide doping molybdenum-silicon-boron alloy.
Background technology
In recent years, fast development along with space flight and aviation and national defense industry, high-temperature mechanics and antioxidant property to high-temperature structural material have proposed higher, harsher requirement, and superalloys such as present widely used nickel based super alloy have become the bottleneck of restriction related industries field development because of himself limitation (the highest service temperature can not above 1100 ℃).Therefore the various countries scientist has accelerated the research progress to high-temperature structural material of future generation, and present result of study shows, by Mo, Mo
3Si and Mo
5SiB
2Molybdenum-the silicon of three phase composites-boron alloy is the most potentially can replace nickel based super alloy, becomes the optimal candidate material of high-temperature structural material of future generation.
By Mo, Mo
3Si and Mo
5SiB
2Molybdenum-the silicon of three phase composites-boron alloy is because Mo
5SiB
2The existence of phase and given this alloy and have the good high-temperature resistance of oxidation, although the existence of Mo phase can guarantee this alloy and have good toughness, but because Mo is not because of changing the character that the crystallography phase transformation takes place temperature, but how therefore the intrinsic property with bcc metals institute inherent tough-brittle transition and low temperature brittleness further improve molybdenum-silicon-boron alloy toughness to improve the key that its processability becomes exploitation molybdenum-silicon-boron alloy deep processed product and enlarges its Application Areas! Simultaneously, the problem of the undercapacity of Mo metal existence itself is also restricting the expansion of the high-temperature applications of molybdenum-silicon-boron alloy to a certain extent.
According at present as can be known to the achievement in research of molybdenum alloy highly malleablized, rare earth doped oxide compound also will be an effective means of improving this alloy obdurability in molybdenum-silicon-boron alloy, and therefore obtaining equally distributed rare earth oxide particles doping molybdenum-silicon-boron alloy will be the effective ways that solve above these problems.Simultaneously, if can be implemented in molybdenum-silicon-boron alloy matrix and be doped into the nanoscale oxide particle, this nanoscale oxide particle not only can play dispersion-strengthened action, also can have each phase in the molybdenum of making-silicon-boron alloy, especially the effect of Mo phase grain refining, therefore inventing a kind of technology of preparing that can obtain nano rare-earth oxide doping molybdenum-silicon-boron alloy, then is the key point of improving molybdenum-silicon-boron alloy obdurability and further enlarging its Application Areas.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of nano rare-earth oxide doping molybdenum-silicon-boron alloy, it is raw material preparing molybdenum-silicon-boron alloy that the present invention adopts rare earth ammonium dimolybdate (national inventing patent: ZL 0410073414.3), the rare earth oxide that contains in molybdenum-silicon-boron alloy with method preparation of the present invention is a nanoscale, the size of molybdenum, molybdenum silicon compound, molybdenum silicon boron compound is also tiny and be evenly distributed, and this molybdenum-silicon-boron alloy has intensity and the toughness better than no doped with rare-earth oxide molybdenum-silicon-boron alloy.
Technical scheme of the present invention is achieved in that the preparation process of nano rare-earth oxide doping molybdenum-silicon provided by the present invention-boron alloy is as follows:
With the rare earth ammonium dimolybdate is that (preparation method of this raw material please refer to national inventing patent to raw material: ZL0410073414.3), at first take by weighing and contain the rare earth ammonium dimolybdate crystal powder that the rare earth oxide massfraction is 0.3-2.5wt%.
With rare earth ammonium dimolybdate powder calcination and reduction, calcination technology is: temperature is 550-650 ℃, time 1-2h, the pressure of logical hydrogen be 0.3-0.5Pa, flow is 0.5-1.0m
3/ h;
Powder behind the calcination is reduced processing, and technology is: temperature is 900-1050 ℃, time 2-3h, the pressure of logical hydrogen be 0.3-0.5Pa, flow is 1-1.5m
3/ h;
Take by weighing the molybdenum alloy powder quality after the reduction, and in molybdenum alloy powder, add silica flour and boron powder, add silica flour and boron powder mass percent account for the 0.5-14.4wt% and the 0.5-4.3wt% of total mass mark (quality that contains molybdenum alloy powder, silica flour and the boron powder of rare earth oxide) respectively, mix afterwards and ball-milling processing, the ball milling time is 12-24h.
Mixed powder after grinding is carried out hot pressed sintering make its densification in the vacuum heating-press sintering stove, sintering temperature is: 1600-1800 ℃, sintering pressure is: 45-55MPa, sintering time is: 5-10h.Promptly obtain nano rare-earth oxide doping molybdenum-silicon-boron alloy material.
Nano rare-earth oxide doping molybdenum-silicon provided by the present invention-boron alloy, containing volume fraction is molybdenum silicon compound and the molybdenum silicon boron compound of 10-60%, and volume fraction is less than 5% rare earth oxide particles, all the other compositions are molybdenum, wherein the size of rare earth oxide particles is tiny, average particle size particle size is less than 100nm, and the size of molybdenum, molybdenum silicon compound and molybdenum silicon boron compound is also tiny and be evenly distributed.
The prepared nano rare-earth oxide doping molybdenum-silicon of the present invention-boron alloy contains one or both combinations or the three kinds of combinations wherein of lanthanum trioxide, cerium oxide, yttrium oxide.
This alloy has high strength and high tenacity.Under the room temperature with do not have doped with rare-earth oxide molybdenum-silicon-boron alloy and compare, intensity and fracture toughness property are significantly improved.
It is raw material preparing doped with rare-earth oxide molybdenum-silicon-boron alloy that the key problem in technology that the present invention solves is to select the rare earth ammonium dimolybdate, make that prepared molybdenum-silicon-boron alloy middle-weight rare earths oxide particle is tiny and be evenly distributed, thereby guaranteed that resulting material has the high-intensity high tenacity that also has simultaneously.
In sum, advantage of the present invention and positively effect are embodied in:
(1) the nano rare-earth oxide doping molybdenum-silicon-boron alloy preparation method of the present invention's proposition is starting material with the rare earth ammonium dimolybdate, and equipment requirements is low, and preparation technology is simple and direct, and cost is low, is easy to realize industrialization production.
(2) adopt the rare earth oxide size of the prepared doped with rare-earth oxide molybdenum-silicon-boron alloy of the technology of the present invention evenly tiny, average particle size particle size is less than 100nm.
(3) the prepared nano rare-earth oxide doping molybdenum alloys of the present invention has excellent mechanical property, and its intensity and toughness do not have doped with rare-earth oxide molybdenum-silicon-boron alloy and is significantly improved.
Embodiment
Embodiment one: take by weighing rare earth ammonium dimolybdate powder 1000 gram that contains the 0.3wt% lanthanum trioxide, carry out calcination, technology is: temperature is 560 ℃, time 2.0h, the pressure of logical hydrogen be 0.3Pa, flow is 0.6m
3/ h; Powder behind the calcination is reduced processing, and technology is: temperature is 960 ℃, time 2h, the pressure of logical hydrogen be 0.3Pa, flow is 1.2m
3/ h; Take by weighing the molybdenum alloy powder quality after the reduction, and in molybdenum alloy powder, add silica flour and boron powder, add silica flour and boron powder mass percent account for total mass fractional 4.2 wt% and 3.8 wt% respectively, mix afterwards and ball-milling processing, the ball milling time is 18h.Mixed powder after grinding is carried out hot pressed sintering make its densification in the vacuum heating-press sintering stove, sintering temperature is: 1680 ℃, sintering pressure is: 47MPa, sintering time is: 8h.Promptly obtain nano rare-earth oxide doping molybdenum-silicon-boron alloy.X ray electron diffraction analysis and spectroscopy detection result show, contain Mo, Mo in this molybdenum-silicon-boron alloy
3Si and Mo
5SiB
2And La
2O
3, quantitative metallographic analysis is the result show, contains the Mo that volume fraction is 32vol% in this molybdenum-silicon-boron alloy approximately
3Si and Mo
5SiB
2, less than the La of 1.0vol%
2O
3, all the other compositions are molybdenum.The tem study result shows that lanthanum trioxide particulate mean sizes is 84nm in prepared molybdenum-silicon-boron alloy.The ultimate compression strength of testing this molybdenum-silicon-boron alloy according to standard GB/T4740-1999 is 2.15GPa, and breaking strain is 13.7%, all is higher than molybdenum-silicon-boron alloy ultimate compression strength and the breaking strain that does not add oxide nano rare earth.(ultimate compression strength and the breaking strain that do not add the molybdenum-silicon-boron alloy of oxide nano rare earth are respectively 1.92GPa and 12.1%).
Embodiment two: take by weighing rare earth ammonium dimolybdate powder 1000 gram that contains the 0.6wt% cerium oxide, carry out calcination, technology is: temperature is 580 ℃, time 2.0h, the pressure of logical hydrogen be 0.3Pa, flow is 0.6m
3/ h; Powder behind the calcination is reduced processing, and technology is: temperature is 980 ℃, time 2h, the pressure of logical hydrogen be 0.3Pa, flow is 1.2m
3/ h; Take by weighing the molybdenum alloy powder quality after the reduction, and in molybdenum alloy powder, add silica flour and boron powder, add silica flour and boron powder mass percent account for total mass fractional 5.5wt% and 3.5wt% respectively, mix afterwards and ball-milling processing, the ball milling time is 20h.Mixed powder after grinding is carried out hot pressed sintering make its densification in the vacuum heating-press sintering stove, sintering temperature is: 1700 ℃, sintering pressure is: 45MPa, sintering time is: 6h.Promptly obtain nano rare-earth oxide doping molybdenum-silicon-boron alloy.X ray electron diffraction analysis and spectroscopy detection result show, contain Mo, Mo in this molybdenum-silicon-boron alloy
3Si and Mo
5SiB
2And CeO
2, quantitative metallographic analysis is the result show, contains the Mo that volume fraction is 51vol% in this molybdenum-silicon-boron alloy approximately
3Si and Mo
5SiB
2, less than the CeO of 1.0vol%
2, all the other compositions are molybdenum.The tem study result shows that the mean sizes of cerium oxide particle in prepared molybdenum-silicon-boron alloy is 67nm.The ultimate compression strength of testing this molybdenum-silicon-boron alloy according to standard GB/T4740-1999 is 2.17GPa, and breaking strain is 13.4%, all is higher than molybdenum-silicon-boron alloy ultimate compression strength and the breaking strain that does not add oxide nano rare earth.
Embodiment three: take by weighing rare earth ammonium dimolybdate powder 1000 gram that contains the 0.9wt% yttrium oxide, carry out calcination, technology is: temperature is 600 ℃, time 1.5h, the pressure of logical hydrogen be 0.4Pa, flow is 0.8m
3/ h; Powder behind the calcination is reduced processing, and technology is: temperature is 1020 ℃, time 2h, the pressure of logical hydrogen be 0.3Pa, flow is 1.2m
3/ h; Take by weighing the molybdenum alloy powder quality after the reduction, and in molybdenum alloy powder, add silica flour and boron powder, add silica flour and boron powder mass percent account for total mass fractional 7.2wt% and 2.6wt% respectively, mix afterwards and ball-milling processing, the ball milling time is 24h.Mixed powder after grinding is carried out hot pressed sintering make its densification in the vacuum heating-press sintering stove, sintering temperature is: 1750 ℃, sintering pressure is: 46MPa, sintering time is: 7h.Promptly obtain nano rare-earth oxide doping molybdenum-silicon-boron alloy.X ray electron diffraction analysis and spectroscopy detection result show, contain Mo, Mo in this molybdenum-silicon-boron alloy
3Si and Mo
5SiB
2And Y
2O
3, quantitative metallographic analysis is the result show, contains the Mo that volume fraction is 55vol% in this molybdenum-silicon-boron alloy approximately
3Si and Mo
5SiB
2, the Y of 1.2vol%
2O
3, all the other compositions are molybdenum.The tem study result shows that the mean sizes of yttria particles in prepared molybdenum-silicon-boron alloy is 69nm.The ultimate compression strength of testing this molybdenum-silicon-boron alloy according to standard GB/T4740-1999 is 2.21GPa, and breaking strain is 12.8%, all is higher than molybdenum-silicon-boron alloy ultimate compression strength and the breaking strain that does not add oxide nano rare earth.
Embodiment four: take by weighing rare earth ammonium dimolybdate powder 1000 gram that contains 0.6wt% lanthanum trioxide and 0.6wt% cerium oxide, carry out calcination, technology is: temperature is 560 ℃, time 2.0h, the pressure of logical hydrogen be 0.5Pa, flow is 0.5m
3/ h; Powder behind the calcination is reduced processing, and technology is: temperature is 960 ℃, time 3h, the pressure of logical hydrogen be 0.4Pa, flow is 1.0m
3/ h; Take by weighing the molybdenum alloy powder quality after the reduction, and in molybdenum alloy powder, add silica flour and boron powder, add silica flour and boron powder mass percent account for total mass fractional 3.2wt% and 1.9wt% respectively, mix afterwards and ball-milling processing, the ball milling time is 24h.Mixed powder after grinding is carried out hot pressed sintering make its densification in the vacuum heating-press sintering stove, sintering temperature is: 1800 ℃, sintering pressure is: 45MPa, sintering time is: 6h.Promptly obtain nano rare-earth oxide doping molybdenum-silicon-boron alloy.X ray electron diffraction analysis and spectroscopy detection result show, contain Mo, Mo in this molybdenum-silicon-boron alloy
3Si and Mo
5SiB
2And the rare earth oxide of lanthanum trioxide and cerium oxide composition, quantitative metallographic analysis is the result show, contains the Mo that volume fraction is 18vol% in this molybdenum-silicon-boron alloy approximately
3Si and Mo
5SiB
2, the rare earth oxide of 1.8vol%, all the other compositions are molybdenum.The tem study result shows that the mean sizes of prepared molybdenum-silicon-boron alloy middle-weight rare earths oxide particle is 92nm.The ultimate compression strength of testing this molybdenum-silicon-boron alloy according to standard GB/T4740-1999 is 2.09GPa, and breaking strain is 14.2%, all is higher than molybdenum-silicon-boron alloy ultimate compression strength and the breaking strain that does not add oxide nano rare earth.
Embodiment five: take by weighing rare earth ammonium dimolybdate powder 1000 gram that contains 0.8wt% lanthanum trioxide, 0.8wt% cerium oxide and 0.8wt% yttrium oxide, carry out calcination, technology is: temperature is 650 ℃, time 1.0h, the pressure of logical hydrogen be 0.5Pa, flow is 0.8m
3/ h; Powder behind the calcination is reduced processing, and technology is: temperature is 1050 ℃, time 3h, the pressure of logical hydrogen be 0.4Pa, flow is 1.2m
3/ h; Take by weighing the molybdenum alloy powder quality after the reduction, and in molybdenum alloy powder, add silica flour and boron powder, add silica flour and boron powder mass percent account for total mass fractional 12.6wt% and 1.4wt% respectively, mix afterwards and ball-milling processing, the ball milling time is 24h.Mixed powder after grinding is carried out hot pressed sintering make its densification in the vacuum heating-press sintering stove, sintering temperature is: 1750 ℃, sintering pressure is: 44MPa, sintering time is: 10h.Promptly obtain nano rare-earth oxide doping molybdenum-silicon-boron alloy.X ray electron diffraction analysis and spectroscopy detection result show, contain Mo, Mo in this molybdenum-silicon-boron alloy
3Si and Mo
5SiB
2And the rare earth oxide of lanthanum trioxide, cerium oxide and yttrium oxide composition, quantitative metallographic analysis is the result show, contains the Mo that volume fraction is 38vol% in this molybdenum-silicon-boron alloy approximately
3Si and Mo
5SiB
2, the rare earth oxide of 3.7vol%, all the other compositions are molybdenum.The tem study result shows that the mean sizes of prepared molybdenum-silicon-boron alloy middle-weight rare earths oxide particle is 64nm.The ultimate compression strength of testing this molybdenum-silicon-boron alloy according to standard GB/T4740-1999 is 2.23GPa, and breaking strain is 12.7%, all is higher than molybdenum-silicon-boron alloy ultimate compression strength and the breaking strain that does not add oxide nano rare earth.
Claims (2)
1, the preparation method of a kind of nano rare-earth oxide doping molybdenum-silicon-boron alloy is characterized in that, its step is as follows:
With the rare earth ammonium dimolybdate is raw material, at first takes by weighing to contain the rare earth ammonium dimolybdate crystal powder that the rare earth oxide massfraction is 0.3-2.5%; With rare earth ammonium dimolybdate powder calcination and reduction, calcination technology is then: temperature is 550-650 ℃, time 1-2h, the pressure of logical hydrogen be 0.3-0.5Pa, flow is 0.5-1.0m
3/ h; Reducing process is: temperature is 900-1050 ℃, time 2-3h, the pressure of logical hydrogen be 0.3-0.5Pa, flow is 1-1.5m
3/ h;
Take by weighing the resulting molybdenum alloy powder quality in reduction back, and in molybdenum alloy powder, add silica flour and boron powder, add silica flour and boron powder mass percent account for the total mass mark respectively, the 0.5-14.4wt% and the 0.5-4.3wt% of quality that promptly contains molybdenum alloy powder, silica flour and the boron powder of rare earth oxide, mix afterwards and ball-milling processing, the ball milling time is 12-24h;
Mixed powder after grinding is carried out hot pressed sintering make its densification in the vacuum heating-press sintering stove, sintering temperature is: 1600-1800 ℃, sintering pressure is: 45-55MPa, sintering time is: 5-10h promptly obtains nano rare-earth oxide doping molybdenum-silicon-boron alloy material.
2, the preparation method of nano rare-earth oxide doping molybdenum-silicon according to claim 1-boron alloy, it is characterized in that, prepared nano rare-earth oxide doping molybdenum-silicon-boron alloy contains one or both combinations or the three kinds of combinations wherein of lanthanum trioxide, cerium oxide, yttrium oxide.
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| CN102274969A (en) * | 2011-07-07 | 2011-12-14 | 西安交通大学 | Preparation method of molybdenum alloy electrode material doped with nano rare earth oxides |
| CN102424928A (en) * | 2011-12-03 | 2012-04-25 | 西北有色金属研究院 | Mo-Si-B-W multi-phase composite material and preparation method thereof |
| CN102728838A (en) * | 2011-04-13 | 2012-10-17 | 四平市北威金属技术研发有限公司 | Molybdenum-based rare earth oxide powder metallurgical alloy wafer and preparing method thereof |
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| CN101948976A (en) * | 2010-09-19 | 2011-01-19 | 西安交通大学 | Composite strengthened molybdenum alloy material and preparation method thereof |
| CN101948976B (en) * | 2010-09-19 | 2012-07-04 | 西安交通大学 | Composite strengthened molybdenum alloy material and preparation method thereof |
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