CN104328301B - A kind of preparation method of particle-reinforced molybdenum-base composite material - Google Patents
A kind of preparation method of particle-reinforced molybdenum-base composite material Download PDFInfo
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Abstract
The invention discloses the preparation method of a kind of particle-reinforced molybdenum-base composite material, belong to technical field of composite preparation.The method is to add enough ammonia in molybdenum acid ammonia solution, it is allowed in alkalescence, again by soluble in water to aluminum soluble salt, zirconates or lanthanum salt, and it is slowly added in molybdenum acid ammonia solution, stirring while adding, generate flocculent deposit, reheating is evaporated, and obtains molybdenum acid ammonia/metal hydroxides composite granule, obtains molybdenum trioxide and metal-oxide composite granule through low temperature calcination, molybdenum trioxide is reduced into molybdenum powder again, after repressed, sintering, makes particle-reinforced molybdenum-base composite material.The present invention first allows the second phase be precipitated out, form nanoscale flocculent deposit, then re-evaporation crystallization, molybdenum acid ammonia is with nano level second for forming core core forming core, Second Phase Particle Dispersed precipitate is on Mo substrate, and it is metallurgical binding completely between Mo substrate, and when can effectively stop sintering, crystal grain is grown up, and has the effect of crystal grain thinning.
Description
Technical field
Present invention relates particularly to the preparation method of a kind of particle-reinforced molybdenum-base composite material, belong to composite technology of preparing neck
Territory.
Background technology
Molybdenum and molybdenum-base composite material have good elevated temperature strength and high temperature hardness, good heat conductivity and electric conductivity, low heat
The coefficient of expansion, excellent wearability and corrosion resistance, it is widely used in space flight and aviation, electricity power, microelectronics, biology
The fields such as medicine, machining, medical apparatus and instruments, illumination, glass, national defense construction.China is second-biggest-in-the-world Mo resource state
(being only second to the U.S.) and the first great Chan molybdenum state.
In the special application field such as high temperature resistance, High-temperature-resandant andant wear-resistant, molybdenum-base composite material has irreplaceable advantage, such as molybdenum top
Head, Aero-Space high temperature jet pipe material, nozzle material, distribution valve body, Gas Pipe pipeline material etc..Vacuum drying oven industry is used
High temperature molybdenum plate, falsework, molybdenum heat screen, molybdenum support member, molybdenum bolt etc. require to work long hours under hyperthermal environments also
And the change of tolerable temperature field and indeformable, say, that require have the highest high-temperature creep resistance and creep rupture strength.
Along with the development of science and technology, the high-temperature behavior of molybdenum-base composite material is required more and more higher, develops the more preferable molybdenio of high-temperature behavior multiple
Composite product is the most urgent.
The development trend of molybdenum-base composite material is mainly reflected in: (1) exploitation novel Mo based composites, introduces high hard wear-resistant matter
Point, and Hard Inclusion is well combined with Mo substrate；(2) research of NEW TYPE OF COMPOSITE technique, with ensure Hard Inclusion granule tiny and
It is evenly distributed, crisp and hard ceramic particle is even more important, if ceramic particle is excessive when forging or rolling, easily induce
Crackle；(3) complex intensifying study mechanism, the multiple strengthening of intercrystalline strengthening, solution strengthening and dispersion-strengtherning, promote strengthening effect.
Under normal circumstances, when using crystallization process to prepare particle-reinforced molybdenum-base composite material, by soluble-salt and the molybdic acid of oxide
Ammonia mixes and dissolves in distilled water, and then evaporative crystallization obtains mixed powder.But, oxygen in general molybdenum-base composite material
The addition of compound is all little, and when evaporative crystallization, first molybdenum acid ammonia reaches saturated, and gradually separates out, grows up, to the last,
The soluble-salt of the second phase just reaches saturated and separates out, and result is segregation occur, and mixing is uniform not, and the crystal grain of ammonium molybdate is relatively
For thick.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of particle-reinforced molybdenum-base composite material.
In order to realize object above, the technical solution adopted in the present invention is:
The preparation method of a kind of particle-reinforced molybdenum-base composite material, comprises the following steps:
(1) it is 9～14 standby for adding ammonia to pH value in ammonium molybdate solution；
(2) by soluble in water to aluminium salt, zirconates or billows salt, then it is added in the solution of step (1), stirring while adding,
Generating flocculent deposit, control ph is not less than 8 (can add ammonia regulation), and heating is evaporated, and obtains ammonium molybdate/metallic hydrogen oxidation
Thing (aluminium hydroxide, zirconium hydroxide or lanthanum hydroxide) composite granule；
(3) take composite granule to calcine 1～5 hour at 500～580 DEG C, obtain (the oxidation of molybdenum trioxide/metal-oxide
Aluminum, zirconium oxide or lanthana) composite granule, molybdenum trioxide is reduced to molybdenum powder, nano-oxide particles is adsorbed equably
Around molybdenum granule, re-compacted, sintering, obtain metal oxide particle and strengthen molybdenum-base composite material.
In described composite, metal-oxide is combined with arbitrary proportion with molybdenum, and the content of the two is all not zero.Preferably,
In terms of weight/mass percentage composition, 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 more
Low, granularity is the least；The granularity of molybdenum is 1～4 micron.Oxide has the effect stoping molybdenum crystal grain to be grown up, so, oxide
Content is the highest, and the crystal grain of molybdenum is the most tiny, and meanwhile, oxide itself then has, along with the increase of content, the trend grown 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, such as aluminum nitrate, aluminum sulfate, aluminum chloride etc..
Zirconates in described step (2) is solubility zirconates, such as zirconium nitrate, zirconium oxychloride etc..
Lanthanum salt in described step (2) is solubility lanthanum salt, such as Lanthanum (III) nitrate etc..
Molybdenum trioxide is reduced in described step (3) molybdenum powder is: once reduce 3～5 little at 520～580 DEG C with hydrogen
Time, with hydrogen secondary reduction 4～8 hours at 890～1000 DEG C.
In described step (3), pressing pressure is 150～300MPa, and the press time is 10～60 minutes.
Described step (3) is sintered to 1650～2000 DEG C, sinter 1～10 hour under hydrogen atmosphere.
Beneficial effects of the present invention:
The present invention adds enough ammonia in molybdenum acid ammonia solution, is allowed in alkalescence, then by aluminum soluble salt, zirconates or lanthanum salt
Soluble in water, and be slowly added in molybdenum acid ammonia solution, stirring while adding, generate flocculent deposit, reheating is evaporated, and obtains
Molybdenum acid ammonia/metal hydroxides composite granule, obtains molybdenum trioxide and metal-oxide (aluminium oxide, zirconium oxide through low temperature calcination
Or lanthana) composite granule, then molybdenum trioxide is reduced into molybdenum powder, makes particle-reinforced molybdenum-base after repressed, sintering and be combined
Material.The present invention first allows the second phase be precipitated out, formed nanoscale flocculent deposit, then re-evaporation crystallization, allow molybdenum acid ammonia with
Nano level second phase is forming core core forming core, may advantageously facilitate forming core, crystal grain thinning, reduces segregation, make uniform doping.
In composite, Second Phase Particle Dispersed precipitate is on Mo substrate, and is metallurgical binding completely between Mo substrate, and can have
When effect stops sintering, crystal grain is grown up, and has the effect of crystal grain thinning.
The preparation method of particle-reinforced molybdenum-base composite material of the present invention has the advantage that (1) mix homogeneously, and granule is tiny,
Nanoscale mixes.The precipitation first generated can promote molybdenum acid ammonia forming core and limit it and grow up, and the flocculent deposit of generation is the most several
Nanometer is thick, is about the filament of hundreds of nanometers, and in evaporation process, on the one hand nano-filaments can promote ammonium molybdate forming core, increases
Adding number of nuclei, molybdenum acid ammonia and is grown up with nano-filaments for core forming core, and on the other hand these heterogeneous nano-filaments can stop again
Growing up of molybdenum acid ammonia, ultimately forms uniform and tiny mixed powder.(2) Second Phase Particle is tiny, strong crystal grain thinning,
Up to nanoscale, produce metallurgical binding completely with Mo substrate.(3) technique uniform doping and controllability are good, in composite
Biphase can be combined with arbitrary proportion, and the method well can dock with molybdenum acid ammonia production process in plant produced, can be directly
The molybdenum acid ammonia solution prepared with factory, as raw material, adds ammonia and soluble metallic salt (such as aluminium salt, zirconates and lanthanum salt),
Increase stirring operation during evaporation and can complete doping process, there is wide application, development prospect and promotional value.
Detailed description of the invention
The present invention is only described in further detail by following embodiment, but does not constitute any limitation of the invention.
Embodiment 1
Al in the present embodiment2O3Particle-reinforced molybdenum-base composite material (Al2O3Content 1.0%) preparation method, including following
Step:
(1) according to composite 100g dispensing, wherein Al2O3It is that 1:99 carries out burdening calculation with the mass ratio of Mo, point
Another name takes 171.19g ammonium tetramolybdate, 7.35g aluminum nitrate；
(2) being dissolved in distilled water by ammonium tetramolybdate, adding ammonia stirring is 9 standby to pH value；
(3) aluminum nitrate is dissolved in distilled water, is added drop-wise in the solution of step (1), drips while stir, drip complete pH
Value (adds ammonia regulation) not less than 8, then heating evaporation crystallization while stirring, has crystallized that to obtain ammonium molybdate/aluminium hydroxide multiple
Close powder body；
(4) take composite granule to calcine 5 hours at 500 DEG C, obtain molybdenum trioxide/Al2O3Composite granule, then at 530 DEG C
Lower hydrogen once reduces 5 hours, and at 920 DEG C, hydrogen secondary reduction obtains Al in 8 hours2O3/ molybdenum composite granule；
(5) Al is taken2O3/ molybdenum composite granule is isostatic cool pressing under 180MPa pressure, and pressurize makes blank in 60 minutes；
(6) being placed in by blank in Medium frequency induction sintering furnace, the lower 1800 DEG C of sintering of hydrogen shield i.e. obtain Al in 3 hours2O3Content
It is the Al of 1.0%2O3Particle-reinforced molybdenum-base composite material.
Take the Al of above-mentioned preparation2O3/ Mo composite is rolled into the compound molybdenum plate that 1mm is thick, and molybdenum plate tensile strength is
1227.31MPa (being 762.42MPa with the tensile strength of the pure molybdenum plate of technique).
Embodiment 2
ZrO in the present embodiment2Particle-reinforced molybdenum-base composite material (ZrO2Content 2.0%) preparation method, including following step
Rapid:
(1) according to ZrO in composite2It is that 1:49 carries out burdening calculation with the mass ratio of Mo, weighs 180.34g respectively
Ammonium heptamolybdate, 5.51g zirconium nitrate；
(2) being dissolved in distilled water by ammonium heptamolybdate, adding ammonia stirring is 10 standby to pH value；
(3) zirconium nitrate is dissolved in distilled water, is added drop-wise in the solution of step (1), drips while stir, drip complete pH
Value (adds ammonia regulation) not less than 8, then heating evaporation crystallization while stirring, has crystallized that to obtain ammonium molybdate/zirconium hydroxide multiple
Close powder body；
(4) take composite granule to calcine 4 hours at 520 DEG C, obtain molybdenum trioxide/ZrO2Composite granule, then at 550 DEG C
Lower hydrogen once reduces 4 hours, and at 950 DEG C, hydrogen secondary reduction obtains ZrO in 5 hours2/ molybdenum composite granule；
(5) ZrO is taken2/ molybdenum composite granule is isostatic cool pressing under 220MPa pressure, and pressurize makes blank in 40 minutes；
(6) being placed in by blank in Medium frequency induction sintering furnace, the lower 1950 DEG C of sintering of hydrogen shield i.e. obtain ZrO in 5 hours2Content is
The ZrO of 2.0%2Particle-reinforced molybdenum-base composite material.
Take the ZrO of above-mentioned preparation2/ Mo composite is rolled into the compound molybdenum plate that 1mm is thick, and compound molybdenum plate tensile strength is
1032MPa (being 753MPa with the tensile strength of the pure molybdenum plate of technique).
Embodiment 3
La in the present embodiment2O2Particle-reinforced molybdenum-base composite material (La2O2Content 1.5%) preparation method, including following
Step:
(1) according to La in composite2O2It is that 3:197 carries out burdening calculation with the mass ratio of Mo, weighs 174.51g respectively
Ammonium dimolybdate, 2.66g Lanthanum (III) nitrate；
(2) being dissolved in distilled water by ammonium dimolybdate, adding ammonia stirring is 10 standby to pH value；
(3) Lanthanum (III) nitrate is dissolved in distilled water, is added drop-wise in the solution of step (1), drips while stir, drip complete pH
Value is not less than 8 (can add ammonia regulation), then heating evaporation crystallization while stirring, has crystallized and has obtained ammonium molybdate/lanthanum hydroxide
Composite granule；
(4) take composite granule to calcine 5 hours at 520 DEG C, obtain molybdenum trioxide/La2O2Composite granule, then at 550 DEG C
Lower hydrogen once reduces 4 hours, and at 950 DEG C, hydrogen secondary reduction obtains La in 5 hours2O2/ molybdenum composite granule；
(5) La is taken2O2/ molybdenum composite granule is isostatic cool pressing under 280MPa pressure, and pressurize makes blank in 10 minutes；
(6) being placed in by blank in Medium frequency induction sintering furnace, the lower 1850 DEG C of sintering of hydrogen shield i.e. obtain La in 6 hours2O2Content
It is the La of 1.5%2O2Particle-reinforced molybdenum-base composite material.
Take the La of above-mentioned preparation2O3/ Mo composite is rolled into the compound molybdenum plate that 1mm is thick, and compound molybdenum plate tensile strength is
953MPa (being 747MPa with the tensile strength of the pure molybdenum plate of technique).
Embodiment 4
Al in the present embodiment2O3/ Mo composite (Al2O3Content is 20.0%) preparation method, comprise the following steps:
(1) according to composite 100g, wherein Al2O3It is that 2:8 carries out burdening calculation with the mass ratio of Mo, weighs respectively
141.74g ammonium dimolybdate, 52.29g aluminum chloride；
(2) being dissolved in distilled water by ammonium dimolybdate, adding ammonia stirring is 14 standby to pH value；
(3) aluminum chloride is dissolved in distilled water, is added drop-wise in the solution of step (1), drips while stir, drip complete pH
Value (adds ammonia regulation) not less than 8, then heating evaporation crystallization while stirring, has crystallized that to obtain ammonium molybdate/aluminium hydroxide multiple
Close powder body；
(4) take composite granule to calcine 3 hours at 580 DEG C, obtain molybdenum trioxide/Al2O3Composite granule, then at 580 DEG C
Lower hydrogen once reduces 3 hours, and at 980 DEG C, hydrogen secondary reduction obtains Al in 4 hours2O3/ molybdenum composite granule；
(5) by Al2O3/ molybdenum composite granule is isostatic cool pressing under 280MPa pressure, and pressurize makes blank in 60 minutes；
(6) being placed in by blank in Medium frequency induction sintering furnace, the lower 1700 DEG C of sintering of hydrogen shield i.e. obtain Al in 8 hours2O3Content
It is the Al of 20.0%2O3Particle-reinforced molybdenum-base composite material.
It is 331.56Hv that the present embodiment prepares the microhardness of composite, and yield strength σ s=1189MPa is (with the pure molybdenum of technique
Material microhardness is 118.32Hv, yield strength σ s=627.56MPa).
Claims (6)
1. the preparation method of a particle-reinforced molybdenum-base composite material, it is characterised in that: comprise the following steps:
(1) it is 9～14 standby for adding ammonia to pH value in ammonium molybdate solution；
(2) by soluble in water to aluminium salt, zirconates or lanthanum salt, then it is added in the solution of step (1), stirring while adding, generate flocculent deposit, control ph is not less than 8, and heating is evaporated, and obtains ammonium molybdate/metal hydroxides composite granule；
(3) take composite granule to calcine 1～5 hour at 500～580 DEG C, obtain molybdenum trioxide/metal-oxide, molybdenum trioxide is reduced to molybdenum powder, re-compacted, sintering, obtains metal oxide particle and strengthen molybdenum-base composite material；
Aluminium salt in described step (2) is one or more in aluminum nitrate, aluminum sulfate, aluminum chloride；
Zirconates in described step (2) is one or more in zirconium nitrate, zirconium oxychloride；
Lanthanum salt in described step (2) is Lanthanum (III) nitrate.
The preparation method of particle-reinforced molybdenum-base composite material the most according to claim 1, it is characterised in that: in terms of weight/mass percentage composition, in described composite, the content of metal-oxide is more than 0, less than or equal to 20%.
The preparation method of particle-reinforced molybdenum-base composite material the most according to claim 1, it is characterised in that: the ammonium molybdate in described step (1) is one or more in ammonium dimolybdate, ammonium tetramolybdate, ammonium heptamolybdate.
The preparation method of particle-reinforced molybdenum-base composite material the most according to claim 1, it is characterized in that: molybdenum trioxide is reduced in described step (3) molybdenum powder is: once reduce with hydrogen 3～5 hours at 520～580 DEG C, with hydrogen secondary reduction 4～8 hours at 890～1000 DEG C.
The preparation method of particle-reinforced molybdenum-base composite material the most according to claim 1, it is characterised in that: in described step (3), compacting pressure is 150～300MPa, and the press time is 10～60 minutes.
The preparation method of particle-reinforced molybdenum-base composite material the most according to claim 1, it is characterised in that: described step (3) is sintered to 1650～2000 DEG C, sinter 1～10 hour under hydrogen atmosphere.
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| CN107686931B (en) * | 2017-08-29 | 2019-04-12 | 东莞市联洲知识产权运营管理有限公司 | A kind of zirconium boride niobium molybdenum-base composite material and preparation method thereof that yttrium ceramic whisker surface is modified |
| CN108149042B (en) * | 2017-12-22 | 2020-04-14 | 北京工业大学 | Low-temperature activation sintering preparation method of high-density molybdenum material |
| CN109097657B (en) * | 2018-10-23 | 2020-06-16 | 中南大学 | Mo nanoparticle reinforced CoCrNi intermediate entropy alloy composite material and preparation method thereof |
| CN109468483A (en) * | 2018-11-28 | 2019-03-15 | 河南科技大学 | A kind of Al2O3Enhance TZM alloy, composite granule and preparation method thereof |
| CN111041261B (en) * | 2019-12-24 | 2021-04-02 | 河南科技大学 | Pressing and sintering method of particle reinforced molybdenum/tungsten-based composite material |
| CN111547768A (en) * | 2020-04-26 | 2020-08-18 | 金堆城钼业股份有限公司 | Preparation method for preparing rare earth ammonium dimolybdate by nano doping |
| CN114230340B (en) * | 2022-01-18 | 2023-01-31 | 河南科技大学 | High-density high-temperature oxidation-resistant molybdenum-based composite target material and preparation method thereof |
| CN114351095B (en) * | 2022-01-18 | 2024-01-19 | 河南科技大学 | Nanocrystalline molybdenum alloy target and preparation method thereof |
| 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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