CN102433493B - Preparation method of ceramic particle dispersion hot pressing sintering metal-nanometer ceramic composite - Google Patents
Preparation method of ceramic particle dispersion hot pressing sintering metal-nanometer ceramic composite Download PDFInfo
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- CN102433493B CN102433493B CN 201110437671 CN201110437671A CN102433493B CN 102433493 B CN102433493 B CN 102433493B CN 201110437671 CN201110437671 CN 201110437671 CN 201110437671 A CN201110437671 A CN 201110437671A CN 102433493 B CN102433493 B CN 102433493B
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Abstract
The invention discloses a preparation method of a ceramic particle dispersion hot pressing sintering metal-nanometer ceramic composite. in the method, manual mixing is combined with mechanical mixing; and nanometer ceramic powder such as magnesium oxide and calcium oxide which can exist stably at the molten steel temperature can be fully mixed with pure iron micropowder and pure molybdenum micropowder, then hot pressing sintering is performed on the mixture under the protection of an inert gas. Therefore, on one hand, the mixture of the nanometer ceramic powder, the pure iron micropowder and the pure molybdenum micropowder is solidified, namely the nanometer ceramic powder is separated from the pure iron micropowder and the pure molybdenum micropowder. On the other hand, a sintered body of which density is less than that of molten steel can be obtained, thus after added in the molten steel, the sintered body can be molten in the molten steel and the aim of adding the nanometer ceramic powder in the molten steel can be realized.
Description
Technical field
The present invention relates to the preparation method of ceramic particle discrete distribution in hot pressed sintering metal-nano ceramics complex body.
Background technology
The tiny nonmetal inclusion of disperse distribution will be of value to microtexture and the mechanical property of improving steel in the steel.Along with the development of nanotechnology, people attempt adding nano-ceramic particle in molten steel in recent years.But the density of pottery is far below molten steel on the one hand, and simple pottery will be difficult for entering among the molten steel; Because the size of nano-ceramic particle is little, and specific surface is big, therefore its total surface free energy height very easily reunites on the other hand.With regard to solving agglomeration traits, the present existing method of improving nanoparticulate dispersed, as: thereby 1, add tensio-active agent reduce its surface energy, 2, in all kinds of solution suspended dispersed, 3, adopt mechanical force dispersion etc. all the dispersion state of nanometer powder can't be remained to enter molten steel inside.Wherein the nano-ceramic particle that suspends in all kinds of solution is unavailable because of solution can not enter molten steel.Add the nano-ceramic particle of tensio-active agent, all tensio-active agents are difficult to exist under the steel temperature of fusion on the one hand, the surface energy that molten steel self is big makes it be difficult to enter among the slit between the nano-ceramic particle of being opened by surfactant-dispersed on the other hand, thereby can't allow this dispersion state enter molten steel inside.Utilize mechanical force that nano-ceramic particle is effectively mixed with metal powder granulates, use metal powder granulates nano-ceramic particle is separately realized the dispersion of nano-ceramic particle a kind of effective means of can yet be regarded as, but this powder do not make through method such as similar sintering its become complete fine and close object before (no matter whether the density after its complete densification is higher than the density of molten steel), its density all will be lower than the density of molten steel, so in adopting simple gravity adition process, all be difficult to it is added among the molten steel.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of ceramic particle discrete distribution hot pressed sintering metal-nano ceramics complex body, make its density be not less than the density of molten steel, thereby guarantee that it can be in the fusing of the inside of molten steel after adding molten steel, be suspended in the condition of creating necessity among the molten steel for nano-ceramic particle as much as possible.
The present invention is achieved through the following technical solutions.
The preparation method of a kind of ceramic powder particle dispersive hot pressed sintering metal-nano ceramics mixture is: with average particulate diameter less than 200 nanometers, can be at the nano oxidized magnesium dust of stable existence under the molten steel temperature, with median size be that 5-1 micron, purity are molybdenum powder powder more than 99% is not less than molten steel density in the density that sinters complete DB into ratio, grind manual careful the mixing 60-120 minute in the legacy at agate, carried out again mechanically mixing 60-720 minute; This mixed powder is inserted in the graphite jig, under protection of inert gas, carried out hot pressed sintering subsequently; The pressure of hot pressed sintering is the 1-30 MPa; removal load after insulation is no less than 10 minutes under 1300-1600K; body temperature degree to be sintered is reduced to and closes protection gas below the 873K temperature, and body to be sintered can take out sintered compact stand-by from graphite jig after being cooled to room temperature.
The also available nano oxidized calcium powder of described nano oxidized magnesium dust replaces.
The present invention adopts method manual and that mechanically mixing combines; can be at the magnesium oxide of stable existence under the molten steel temperature; nano-ceramic powders such as calcium oxide; carry out thorough mixing with pure iron and pure molybdenum micro mist; under protection of inert gas, carry out hot pressed sintering subsequently again; on the one hand the admixture of nano ceramic powder and pure iron and pure molybdenum micro mist is solidified; just the micro mist of pure iron and pure molybdenum is kept apart nano ceramic powder; can obtain the sintered compact that density is not less than molten steel on the other hand; thereby guarantee that sintered compact can melt in molten steel inside after molten steel is advanced in interpolation, and then realize that nano ceramic powder adds the purpose of molten steel.
Embodiment
Embodiment 1
A kind of preparation method of hot pressed sintering metal-nano magnesia complex body of ceramic particle discrete distribution:
With average particulate diameter is that 50 nanometers, purity are 99.9% nano oxidized magnesium dust, with median size be that 3.3 microns, purity are that 99.6% iron powder powder and median size are that 3.5 microns, purity are 99.7% molybdenum powder powder, in massfraction be the ratio of 2:85.8:12.2 in agate mortar manual careful mix 60 minutes after, mechanically mixing 120 minutes on planetary mixer again.Mixed powder is inserted in the graphite jig; carry out hot pressed sintering then under argon shield atmosphere, hot pressing pressure is the axle pressure of 10 MPas, is heated to 1323K; be incubated removal load after 30 minutes, body to be sintered is cooled to the 873K temperature and closes shielding gas when following.Sintered compact takes out from graphite jig after being cooled to room temperature.The nano oxidized magnesium dust that is added is many to be distributed in less than 1 micron particle dispersion on the metallic matrix in the sintered compact.
Embodiment 2
A kind of preparation method of hot pressed sintering metal-nano calcium oxide complex body of ceramic particle discrete distribution:
With average particulate diameter is that 50 nanometers, purity are 99.9% nano oxidized calcium powder, with median size be that 3.3 microns, purity are that 99.6% iron powder powder and median size are that 3.5 microns, purity are 99.7% molybdenum powder powder, in massfraction be the ratio of 2:85.8:12.2 in agate mortar manual careful mix 60 minutes after, mechanically mixing 120 minutes on planetary mixer again.Mixed powder is inserted in the graphite jig; carry out hot pressed sintering then under argon shield atmosphere, hot pressing pressure is the axle pressure of 10 MPas, is heated to 1323K; be incubated removal load after 30 minutes, body to be sintered is cooled to the 873K temperature and closes shielding gas when following.Sintered compact takes out from graphite jig after being cooled to room temperature.The nano oxidized calcium powder that is added is many to be distributed in less than 1 micron particle dispersion on the metallic matrix in the sintered compact.
Claims (2)
1. a ceramic particle disperses the preparation method of hot pressed sintering metal-nano ceramics complex body, it is characterized in that: with average particulate diameter is that 50 nanometers, purity are 99.9% nano oxidized magnesium dust, with median size be that 3.3 microns, purity are that 99.6% iron powder powder and median size are that 3.5 microns, purity are 99.7% molybdenum powder powder, in massfraction be the ratio of 2:85.8:12.2 in agate mortar manual careful mix 60 minutes after, mechanically mixing 120 minutes on planetary mixer again; Mixed powder is inserted in the graphite jig, carry out hot pressed sintering then under argon shield atmosphere, hot pressing pressure is the axle pressure of 10 MPas, is heated to 1323K, be incubated removal load after 30 minutes, body to be sintered is cooled to the 873K temperature and closes shielding gas when following; Sintered compact takes out from graphite jig after being cooled to room temperature; The nano oxidized magnesium dust that is added is many to be distributed in less than 1 micron particle dispersion on the metallic matrix in the sintered compact.
2. a kind of ceramic particle according to claim 1 disperses the preparation method of hot pressed sintering metal-nano ceramics complex body, it is characterized in that: the also available nano oxidized calcium powder of described nano oxidized magnesium dust replaces.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110437671 CN102433493B (en) | 2011-12-23 | 2011-12-23 | Preparation method of ceramic particle dispersion hot pressing sintering metal-nanometer ceramic composite |
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| CN 201110437671 CN102433493B (en) | 2011-12-23 | 2011-12-23 | Preparation method of ceramic particle dispersion hot pressing sintering metal-nanometer ceramic composite |
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| CN102433493A CN102433493A (en) | 2012-05-02 |
| CN102433493B true CN102433493B (en) | 2013-07-31 |
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| CN103600046A (en) * | 2013-11-19 | 2014-02-26 | 沈阳大学 | Method for manufacturing fine-grained steel with pre-precipitated nanometer ceramic grains in continuously cast molten steel |
| CN105090513A (en) * | 2015-08-12 | 2015-11-25 | 李纯 | Ceramic dispersion strengthening metal abrasion resisting belt and metal stamping ring floating oil seal |
| EP3356067A4 (en) * | 2015-09-29 | 2019-07-31 | Höganäs AB (publ) | New iron-based composite powder |
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| CN100519803C (en) * | 2006-08-31 | 2009-07-29 | 宝山钢铁股份有限公司 | Nano TiO2 oxide containing ferroalloy intermediate and preparation method and uses thereof |
| WO2010024150A1 (en) * | 2008-08-28 | 2010-03-04 | 日鉱金属株式会社 | Process for producing powder mixture comprising noble-metal powder and oxide powder and powder mixture comprising noble-metal powder and oxide powder |
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