CN104328301A - Preparation method of particular-reinforced molybdenum-based composite material - Google Patents
Preparation method of particular-reinforced molybdenum-based composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of a particular-reinforced molybdenum-based composite material and belongs to the technical field of preparation of composite materials. The method includes following steps: (1) adding enough ammonia water to an ammonium molybdate solution for enabling the ammonia water to be alkaline; (2) dissolving a soluble aluminum salt, a soluble zircon salt or a soluble lanthanum salt in water to obtain a solution and slowly adding the solution to the ammonium molybdate solution with stirring to generate a flocculent precipitation; (3) performing a heating and evaporatively-drying process to obtain an ammonium molybdate/metal hydroxide composite powder; (4) performing low-temperature calcination to obtain a molybdenum trioxide/metal hydroxide composite powder; (5) reducing the molybdenum trioxide into molybdenum powder; and (6) performing a pressing process and a sintering process to obtain the particulate reinforced molybdenum-based composite material. In the invention, a second phase is firstly precipitated out for forming a nano-scale flocculent precipitation, and then an evaporative crystallization process is carried out so that the ammonium molybdate forms a nucleus with the nano-scale second phase being a nucleation core, wherein the second phase is dispersed and distributed on a molybdenum substrate and is completely metallurgically bonded with the molybdenum substrate. Growth of crystal grain during sintering can be effectively stopped and a crystal grain refining effect is achieved.
Description
Technical field
The present invention is specifically related to a kind of preparation method of particle-reinforced molybdenum-base composite material, belongs to technical field of composite preparation.
Background technology
Molybdenum and molybdenum-base composite material have good hot strength and hot hardness, good thermal conductivity and electroconductibility, low thermal expansivity, excellent wear resistance and erosion resistance, be widely used in the fields such as space flight and aviation, electricity power, microelectronics, biological medicine, mechanical workout, medicine equipment, illumination, glass, national defense construction.China is second-biggest-in-the-world Mo resource state (being only second to the U.S.) and first Chan Mu state.
In the special application field such as high temperature resistance, High-temperature-resandant andant wear-resistant, molybdenum-base composite material has irreplaceable advantage, as molybdenum plug, aerospace high temperature jet pipe material, nozzle material, distribution valve body, gas line pipeline material etc.The high temperature molybdenum plate, falsework, molybdenum heat screen, molybdenum strut member, molybdenum bolt etc. of vacuum oven industry to require to work long hours under hyperthermal environments and the change of tolerable temperature field and indeformable, that is require very high high-temperature creep resistance and creep rupture strength.Along with the development of science and technology, require more and more higher to the high-temperature behavior of molybdenum-base composite material, development high-temperature behavior better molybdenum-base composite material product is increasingly urgent.
The development trend of molybdenum-base composite material is mainly reflected in: (1) development of new molybdenum-base composite material, introduce high hard wear-resistant particle, and Hard Inclusion is combined with Mo substrate well; (2) research of NEW TYPE OF COMPOSITE technique, to ensure that Hard Inclusion particle is tiny and be evenly distributed, is even more important for crisp and hard ceramic particle, if ceramic particle is excessive when forging or rolling, easily brings out crackle; (3) complex intensifying study mechanism, the multiple strengthening of grain-boundary strengthening, solution strengthening and dispersion-strengthened, promotes strengthening effect.
Under normal circumstances, when adopting crystallization process to prepare particle-reinforced molybdenum-base composite material, the soluble salt of oxide compound and molybdenum acid ammonia are mixed and dissolve in distilled water, then evaporative crystallization, obtains mixed powder.But, in general molybdenum-base composite material, the add-on of oxide compound is all little, when evaporative crystallization, first molybdenum acid ammonia reaches capacity, and separate out gradually, grow up, to the last, the soluble salt of second-phase just reaches capacity and separates out, and result occurs segregation, mixing is even not, and the crystal grain of ammonium molybdate is comparatively thick.
Summary of the invention
The object of this invention is to provide a kind of preparation method of particle-reinforced molybdenum-base composite material.
In order to realize above object, the technical solution adopted in the present invention is:
A preparation method for particle-reinforced molybdenum-base composite material, comprises the following steps:
(1) in ammonium molybdate solution, add ammoniacal liquor to pH value is 9 ~ 14 for subsequent use;
(2) by soluble in water to aluminium salt, zirconates or billows salt, added in the solution of step (1) again, limit edged stirs, generate flocks, control ph was not less than for 8 (can add ammoniacal liquor to regulate), heating evaporate to dryness, obtains ammonium molybdate/metal hydroxides (aluminium hydroxide, zirconium hydroxide or lanthanum hydroxide) composite granule;
(3) get composite granule to calcine 1 ~ 5 hour at 500 ~ 580 DEG C, obtain molybdic oxide/metal oxide (aluminum oxide, zirconium white or lanthanum trioxide) composite granule, molybdic oxide is reduced to molybdenum powder, nano-oxide particles is adsorbed on around molybdenum particle equably, suppress again, sinter, obtain metal oxide particle and strengthen molybdenum-base composite material.
In described matrix material, metal oxide and molybdenum are with arbitrary proportion compound, and the content of the two is all non-vanishing.Preferably, in mass percentage, content≤20% of 0% < metal oxide.Wherein, the granularity of metal oxide is 0.01 ~ 2 micron; The granularity of molybdenum is 1 ~ 4 micron.When oxide content is less than 10%, its granularity is 0.01 ~ 1 micron, and content is lower, and granularity is less; The granularity of molybdenum is 1 ~ 4 micron.Oxide compound has the effect stoping molybdenum grain growth, so oxide content is higher, the crystal grain of molybdenum is more tiny, and meanwhile, oxide compound itself is then along with the increase of content has the trend of growing up.
Ammonium molybdate in described step (1) is one or more in the crystal formations such as ammonium dimolybdate, ammonium tetramolybdate, Ammonium Heptamolybdate.
Aluminium salt in described step (2) is aluminum soluble salt, as aluminum nitrate, Tai-Ace S 150, aluminum chloride etc.
Zirconates in described step (2) is solubility zirconates, as zirconium nitrate, zirconium oxychloride etc.
Lanthanum salt in described step (2) is solubility lanthanum salt, as lanthanum nitrate etc.
In described step (3), molybdic oxide being reduced to molybdenum powder is: once reduce 3 ~ 5 hours with hydrogen at 520 ~ 580 DEG C, at 890 ~ 1000 DEG C, use hydrogen secondary reduction 4 ~ 8 hours.
In described step (3), pressing pressure is 150 ~ 300MPa, and the press time is 10 ~ 60 minutes.
Be sintered in described step (3) at 1650 ~ 2000 DEG C, sintering 1 ~ 10 hour under hydrogen atmosphere.
Beneficial effect of the present invention:
The present invention adds enough ammoniacal liquor in molybdenum acid ammonia solution, make it in alkalescence, again by soluble in water to aluminum soluble salt, zirconates or lanthanum salt, and slowly join in molybdenum acid ammonia solution, limit edged stirs, generate flocks, reheat evaporate to dryness, obtain molybdenum acid ammonia/metal hydroxides composite granule, molybdic oxide and metal oxide (aluminum oxide, zirconium white or lanthanum trioxide) composite granule is obtained through low temperature calcination, again molybdic oxide is reduced into molybdenum powder, repressed, sintering after make particle-reinforced molybdenum-base composite material.The present invention first allows second-phase be precipitated out, and forms nano level flocks, and then evaporative crystallization, and allow molybdenum acid ammonia with nano level second-phase for forming core core forming core, be conducive to promoting forming core, crystal grain thinning, reduction segregation, makes uniform doping.In matrix material, Second Phase Particle Dispersed precipitate is on Mo substrate, and is metallurgical binding completely between Mo substrate, and grain growth when effectively can stop sintering, there is the effect of crystal grain thinning.
The preparation method of particle-reinforced molybdenum-base composite material of the present invention has the following advantages: (1) mixes, and particle is tiny, and nano level mixes.The precipitation first generated can promote molybdenum acid ammonia forming core and limit it to grow up, it is thick that the flocks generated is generally several nanometer, be about the filament of hundreds of nanometers, in evaporative process, nano-filaments can promote ammonium molybdate forming core on the one hand, and increase number of nuclei, molybdenum acid ammonia take nano-filaments as core nucleation and growth, these heterogeneous nano-filaments can stop growing up of molybdenum acid ammonia again on the other hand, the mixed powder that final formation is uniform and tiny.(2) Second Phase Particle is tiny, strong crystal grain thinning, can reach nano level, produces metallurgical binding completely with Mo substrate.(3) technique uniform doping and controllability is good, in matrix material, two-phase can with arbitrary proportion compound, and the method well can be docked with molybdenum acid ammonia production process in plant produced, get final product the direct molybdenum acid ammonia solution prepared with factory for raw material, add ammoniacal liquor and soluble metallic salt (as aluminium salt, zirconates and lanthanum salt), increase stirring operation when evaporating and can complete doping process, there is wide application, development prospect and promotional value.
Embodiment
Following embodiment is only described in further detail the present invention, but does not form any limitation of the invention.
Embodiment 1
Al in the present embodiment
2o
3particle-reinforced molybdenum-base composite material (Al
2o
3content 1.0%) preparation method, comprise the following steps:
(1) prepare burden according to matrix material 100g, wherein Al
2o
3be that 1:99 carries out charge calculation with the mass ratio of Mo, take 171.19g ammonium tetramolybdate, 7.35g aluminum nitrate respectively;
(2) be dissolved in distilled water by ammonium tetramolybdate, adding ammoniacal liquor, to be stirred to pH value be 9 for subsequent use;
(3) aluminum nitrate is dissolved in distilled water, be added drop-wise in the solution of step (1), drip while stir, dropwise pH value and be not less than for 8 (adding ammoniacal liquor to regulate), heating evaporation crystallization while stirring again, crystallization completes and obtains ammonium molybdate/aluminium hydroxide composite granule;
(4) get composite granule to calcine 5 hours at 500 DEG C, obtain molybdic oxide/Al
2o
3composite granule, then hydrogen once reduces 5 hours at 530 DEG C, at 920 DEG C, hydrogen secondary reduction obtains Al in 8 hours
2o
3/ molybdenum composite granule;
(5) Al is got
2o
3/ molybdenum composite granule is isostatic cool pressing under 180MPa pressure, and pressurize makes blank in 60 minutes;
(6) be placed in by blank in Medium frequency induction sintering oven, namely the lower 1800 DEG C of sintering of hydrogen shield obtain Al in 3 hours
2o
3content is the Al of 1.0%
2o
3particle-reinforced molybdenum-base composite material.
Get the Al of above-mentioned preparation
2o
3/ Mo matrix material is rolled into the thick compound molybdenum plate of 1mm, and molybdenum plate tensile strength is 1227.31MPa (tensile strength with the pure molybdenum plate of technique is 762.42MPa).
Embodiment 2
ZrO in the present embodiment
2particle-reinforced molybdenum-base composite material (ZrO
2content 2.0%) preparation method, comprise the following steps:
(1) according to ZrO in matrix material
2be that 1:49 carries out charge calculation with the mass ratio of Mo, take 180.34g Ammonium Heptamolybdate, 5.51g zirconium nitrate respectively;
(2) be dissolved in distilled water by Ammonium Heptamolybdate, adding ammoniacal liquor, to be stirred to pH value be 10 for subsequent use;
(3) zirconium nitrate is dissolved in distilled water, be added drop-wise in the solution of step (1), drip while stir, dropwise pH value and be not less than for 8 (adding ammoniacal liquor to regulate), heating evaporation crystallization while stirring again, crystallization completes and obtains ammonium molybdate/zirconium hydroxide composite granule;
(4) get composite granule to calcine 4 hours at 520 DEG C, obtain molybdic oxide/ZrO
2composite granule, then hydrogen once reduces 4 hours at 550 DEG C, at 950 DEG C, hydrogen secondary reduction obtains ZrO in 5 hours
2/ molybdenum composite granule;
(5) ZrO is got
2/ molybdenum composite granule is isostatic cool pressing under 220MPa pressure, and pressurize makes blank in 40 minutes;
(6) be placed in by blank in Medium frequency induction sintering oven, namely the lower 1950 DEG C of sintering of hydrogen shield obtain ZrO in 5 hours
2content is the ZrO of 2.0%
2particle-reinforced molybdenum-base composite material.
Get the ZrO of above-mentioned preparation
2/ Mo matrix material is rolled into the thick compound molybdenum plate of 1mm, and compound molybdenum plate tensile strength is 1032MPa (tensile strength with the pure molybdenum plate of technique is 753MPa).
Embodiment 3
La in the present embodiment
2o
2particle-reinforced molybdenum-base composite material (La
2o
2content 1.5%) preparation method, comprise the following steps:
(1) according to La in matrix material
2o
2be that 3:197 carries out charge calculation with the mass ratio of Mo, take 174.51g ammonium dimolybdate, 2.66g lanthanum nitrate respectively;
(2) be dissolved in distilled water by ammonium dimolybdate, adding ammoniacal liquor, to be stirred to pH value be 10 for subsequent use;
(3) lanthanum nitrate is dissolved in distilled water, be added drop-wise in the solution of step (1), drip while stir, dropwise pH value and be not less than for 8 (ammoniacal liquor can be added regulate), heating evaporation crystallization while stirring again, crystallization completes and obtains ammonium molybdate/lanthanum hydroxide composite granule;
(4) get composite granule to calcine 5 hours at 520 DEG C, obtain molybdic oxide/La
2o
2composite granule, then hydrogen once reduces 4 hours at 550 DEG C, at 950 DEG C, hydrogen secondary reduction obtains La in 5 hours
2o
2/ molybdenum composite granule;
(5) La is got
2o
2/ molybdenum composite granule is isostatic cool pressing under 280MPa pressure, and pressurize makes blank in 10 minutes;
(6) be placed in by blank in Medium frequency induction sintering oven, namely the lower 1850 DEG C of sintering of hydrogen shield obtain La in 6 hours
2o
2content is the La of 1.5%
2o
2particle-reinforced molybdenum-base composite material.
Get the La of above-mentioned preparation
2o
3/ Mo matrix material is rolled into the thick compound molybdenum plate of 1mm, and compound molybdenum plate tensile strength is 953MPa (tensile strength with the pure molybdenum plate of technique is 747MPa).
Embodiment 4
Al in the present embodiment
2o
3/ Mo matrix material (Al
2o
3content is 20.0%) preparation method, comprise the following steps:
(1) according to matrix material 100g, wherein Al
2o
3be that 2:8 carries out charge calculation with the mass ratio of Mo, take 141.74g ammonium dimolybdate, 52.29g aluminum chloride respectively;
(2) be dissolved in distilled water by ammonium dimolybdate, adding ammoniacal liquor, to be stirred to pH value be 14 for subsequent use;
(3) aluminum chloride is dissolved in distilled water, be added drop-wise in the solution of step (1), drip while stir, dropwise pH value and be not less than for 8 (adding ammoniacal liquor to regulate), heating evaporation crystallization while stirring again, crystallization completes and obtains ammonium molybdate/aluminium hydroxide composite granule;
(4) get composite granule to calcine 3 hours at 580 DEG C, obtain molybdic oxide/Al
2o
3composite granule, then hydrogen once reduces 3 hours at 580 DEG C, at 980 DEG C, hydrogen secondary reduction obtains Al in 4 hours
2o
3/ molybdenum composite granule;
(5) by Al
2o
3/ molybdenum composite granule is isostatic cool pressing under 280MPa pressure, and pressurize makes blank in 60 minutes;
(6) be placed in by blank in Medium frequency induction sintering oven, namely the lower 1700 DEG C of sintering of hydrogen shield obtain Al in 8 hours
2o
3content is the Al of 20.0%
2o
3particle-reinforced molybdenum-base composite material.
The microhardness that the present embodiment prepares matrix material is 331.56Hv, yield strength σ s=1189MPa (be 118.32Hv, yield strength σ s=627.56MPa with the pure Mo microhardness of technique).
Claims (10)
1. a preparation method for particle-reinforced molybdenum-base composite material, is characterized in that: comprise the following steps:
(1) in ammonium molybdate solution, add ammoniacal liquor to pH value is 9 ~ 14 for subsequent use;
(2) by soluble in water to aluminium salt, zirconates or billows salt, then added in the solution of step (1), limit edged stirs, and generate flocks, control ph is not less than 8, heating evaporate to dryness, obtains ammonium molybdate/metal hydroxides and closes powder;
(3) get composite granule to calcine 1 ~ 5 hour at 500 ~ 580 DEG C, obtain molybdic oxide/metal oxide, molybdic oxide is reduced to molybdenum powder, then suppress, sinter, obtain metal oxide particle and strengthen molybdenum-base composite material.
2. the preparation method of particle-reinforced molybdenum-base composite material according to claim 1, is characterized in that: in described matrix material, metal oxide and molybdenum are with arbitrary proportion compound.
3. the preparation method of particle-reinforced molybdenum-base composite material according to claim 1, is characterized in that: in mass percentage, in described matrix material, the content of metal oxide is greater than 0, is less than or equal to 20%.
4. the preparation method of particle-reinforced molybdenum-base composite material according to claim 1, is characterized in that: the ammonium molybdate in described step (1) is one or more in ammonium dimolybdate, ammonium tetramolybdate, Ammonium Heptamolybdate.
5. the preparation method of particle-reinforced molybdenum-base composite material according to claim 1, is characterized in that: the aluminium salt in described step (2) is one or more in aluminum nitrate, Tai-Ace S 150, aluminum chloride.
6. the preparation method of particle-reinforced molybdenum-base composite material according to claim 1, is characterized in that: the zirconates in described step (2) is one or more in zirconium nitrate, zirconium oxychloride.
7. the preparation method of particle-reinforced molybdenum-base composite material according to claim 1, is characterized in that: the lanthanum salt in described step (2) is lanthanum nitrate.
8. the preparation method of particle-reinforced molybdenum-base composite material according to claim 1, it is characterized in that: in described step (3), molybdic oxide being reduced to molybdenum powder is: once reduce 3 ~ 5 hours with hydrogen at 520 ~ 580 DEG C, at 890 ~ 1000 DEG C, use hydrogen secondary reduction 4 ~ 8 hours.
9. the preparation method of particle-reinforced molybdenum-base composite material according to claim 1, is characterized in that: in described step (3), pressing pressure is 150 ~ 300MPa, and the press time is 10 ~ 60 minutes.
10. the preparation method of particle-reinforced molybdenum-base composite material according to claim 1, is characterized in that: be sintered in described step (3) at 1650 ~ 2000 DEG C, sintering 1 ~ 10 hour under hydrogen atmosphere.
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| CN108149042A (en) * | 2017-12-22 | 2018-06-12 | 北京工业大学 | A kind of cryogenic activating sintering preparation method of high-compactness molybdenum material |
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| CN114351095B (en) * | 2022-01-18 | 2024-01-19 | 河南科技大学 | Nanocrystalline molybdenum alloy target and preparation method thereof |
| CN115194173A (en) * | 2022-06-02 | 2022-10-18 | 英特派铂业股份有限公司 | Novel preparation method of nano-zirconia dispersion strengthened platinum |
| CN115194173B (en) * | 2022-06-02 | 2023-10-27 | 英特派铂业股份有限公司 | New preparation method of nano zirconia dispersion strengthening platinum |
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