CN104651696A - TiC dispersion-strengthened molybdenum alloy and preparation method thereof - Google Patents
TiC dispersion-strengthened molybdenum alloy and preparation method thereof Download PDFInfo
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- CN104651696A CN104651696A CN201510109535.7A CN201510109535A CN104651696A CN 104651696 A CN104651696 A CN 104651696A CN 201510109535 A CN201510109535 A CN 201510109535A CN 104651696 A CN104651696 A CN 104651696A
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Abstract
The invention discloses a TiC dispersion-strengthened molybdenum alloy and a preparation method thereof. The preparation method comprises the following steps: mixing 10kg of molybdenum powder, 40-60g of titanium white, 45-60g of molybdenum carbide powder and 5-7g of graphite powder by ball milling, drying, pressing, sintering, extruding, and drawing to obtain the required TiC dispersion-strengthened molybdenum alloy. The Mo-TiC alloy has the advantages of uniform strengthening-phase distribution, fine particles, higher tensile strength and higher elongation percentage.
Description
Technical field
The present invention relates to Material Field, be specifically related to a kind of TiC dispersion-strengthemolybdenum molybdenum alloy and preparation method thereof.
Background technology
Take molybdenum as the non-ferrous alloy that matrix adds other elements and forms, main alloy element has titanium, zirconium, hafnium, tungsten and rare earth element.Molybdenum alloy has good heat conduction, electroconductibility and the low coefficient of expansion, and at high temperature (1100 ~ 1650 DEG C) have high intensity, processing easier than tungsten.Can be used as grid and the anode of electron tube, the propping material of electric light source, and for making die casting and extrusion mould, the component etc. of spacecraft.In addition, molybdenum is stablized at normal temperatures, higher than can rapid oxidation when 600 DEG C, with carbon, hydrocarbon polymer or carbon monoxide generating molybdenum carbide higher than reacting when 800 DEG C, molybdenum carbide has higher melt and hardness, good thermal stability and the feature such as mechanical stability and fabulous erosion resistance.Industrial molybdenum alloy has molybdenum titanium zirconium system, molybdenum tungsten system and molybdenum rare earth-based alloy, and applying more is the first kind.The main strengthening approach of molybdenum alloy is solution strengthening, precipitation strength and work hardening.Molybdenum alloy sheet material, band, foil, tubing, bar, wire rod and section bar can be obtained by plastic working, its intensity can also be improved and improve cold plasticity.Because molybdenum alloy has low temperature brittleness and welding fragility, and high temperature is oxidizable, limits the further expansion of its use range; On the other hand, along with the scientific-technical progress in the fields such as semi-conductor industry, military affairs, more and more higher requirement is proposed to the performance, composition etc. of molybdenum product.Therefore its development is restricted.
What current application was maximum has TZM (Mo-0.5%Ti-0.008%Zr) and TZC (Mo-1.25%Ti-0.15%Zr-0.15%C), Mo-la alloy and Mo-TiC alloy.The recrystallization temperature that TZM alloy is suitable for is (1300-1450) DEG C, and temperature, more than 1500 DEG C, due to worked structure generation recrystallize, causes the strength of materials sharply to decline, and material fragility improves.Although Mo-la alloy has very high recrystallization temperature (1500-1700 DEG C), material under high temperature intensity reduces.Find after deliberation, TiC dispersion-strengthemolybdenum molybdenum alloy (Mo-TiC) and TZM alloy, Mo-La alloy phase ratio, have higher recrystallization temperature, higher hot strength and creep-resistant property.
Mo-TiC alloy is in the past direct to add in molybdenum powder by TiC powder, after mixing for some time, carries out compacting sintering, is prepared into sintering blank.Although under high temperature, major part TiC can dissolve and enter in Mo substrate, but there is part titanyl compound in TiC, and TiC is in heat-agglomerating process, the water vapour in part TiC and atmosphere reacts other oxide compounds generating TiO2 or Ti, and the strengthening effect of the oxide compound of Ti is well below the strengthening effect of TiC, further, due to TiC skewness in Mo substrate, dissolution process is too very long, cannot implement in actual production, can cause there is part TiC cannot dissolve.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of strengthening phase and is evenly distributed, and particle is tiny, has higher tensile strength and the TiC dispersion-strengthemolybdenum molybdenum alloy of unit elongation.
Another technical problem that the present invention will solve is to provide the preparation method of this TiC dispersion-strengthemolybdenum molybdenum alloy.
For solving above-mentioned first technical problem, the present invention forms primarily of the material of following weight part: molybdenum powder 10Kg, titanium valve 40 ~ 60g, carbonization molybdenum powder 45 ~ 60g, Graphite Powder 99 5 ~ 7g, above-mentioned material carried out ball mill mixing, then carries out drying, suppress, sinter, extrude, drawing process obtains required TiC dispersion-strengthemolybdenum molybdenum alloy.
For solving above-mentioned second technical problem, the present invention includes following steps and processing condition:
1) molybdenum powder 10Kg is taken, titanium valve 40 ~ 60g, carbonization molybdenum powder 45 ~ 60g, Graphite Powder 99 5 ~ 7g;
2) molybdenum powder, titanium valve, Graphite Powder 99, carbonization molybdenum powder are put into ball milling bucket, add 1500 ~ 2500ml dehydrated alcohol, ball milling mixing 0.5 ~ 10h;
3) ball milling being mixed the ball milling solution obtained is placed in drying baker, dry 2 ~ 10h under 30 ~ 80 DEG C of temperature condition, makes the ethanol volatilization in this solution clean, obtains a powdered alloy;
4) described powdered alloy is through the compacting of 200Mpa ~ 300MPa isostatic pressed, and in Intermediate frequency sintering furnace sintering, under 1700 ~ 1800 DEG C of temperature condition, be incubated 6 ~ 16h, furnace cooling obtains a sintered blank;
5), after described sintered blank is incubated 0.5 ~ 2h under 1550 ~ 1650 DEG C of temperature condition, is to extrude at 3.5: 1 with extrusion ratio, obtains an extruded bar stock;
6) described extruded bar stock is incubated 0.5 ~ 2h subsequently under 1200 ~ 1300 DEG C of temperature condition, then anneals;
7) bar of annealing is heated to 1350 ~ 1450 DEG C on high-temperature tensile testing machine, and insulation 0.3 ~ 0.6h, then stretches, obtain TiC dispersion-strengthemolybdenum molybdenum alloy material.
The granularity of described molybdenum powder, titanium valve, carbonization molybdenum powder, Graphite Powder 99 is at 400 ~ 800 orders; The tensile strength of described TiC dispersion-strengthemolybdenum molybdenum alloy material is 150 ~ 165MPa, unit elongation 23 ~ 25.6%.
Advantageous effect of the present invention is:
At 1700-1800 DEG C of temperature range inside holding, MoC is dissolved in described Mo substrate with the form of Mo and C atom completely, and graphite and titanium valve are also dissolved in described Mo substrate with the form of C atom and Ti atom respectively completely.By insulation for some time, utilize the concentration gradient of atom to spread, Ti and C atom is spread in described Mo substrate, reaches and be uniformly distributed.
Lower the temperature subsequently, the solubility with temperature of Ti and C in described Mo substrate reduces and declines, and Ti atom and C atom evolution reaction from described Mo substrate generates tiny TiC phase, achieves good dispersion-strengthened effect.
Compared with prior art, Mo-TiC alloy prepared by the present invention, strengthening phase is evenly distributed, and particle is tiny, has higher tensile strength and unit elongation.
Embodiment
Embodiment one
1) take granularity at 600 object molybdenum powder 10Kg, granularity is at 600 object titanium valve 50g, carbonization molybdenum powder 50g, Graphite Powder 99 6g;
2) molybdenum powder, titanium valve, Graphite Powder 99, carbonization molybdenum powder are put into ball milling bucket, add 2000ml dehydrated alcohol, ball milling mixing 2h;
3) ball milling being mixed the ball milling solution obtained is placed in drying baker, 60 DEG C of dry 5h, makes the ethanol volatilization in this solution clean, obtains a powdered alloy;
4) described powdered alloy is through the compacting of 240Mpa isostatic pressed, and in Intermediate frequency sintering furnace sintering, at 1800 DEG C of insulation 10h, furnace cooling obtains a sintered blank;
5) described sintered blank is after 1600 DEG C of insulation 1.5h, is to extrude at 3.5: 1, obtains an extruded bar stock with extrusion ratio;
6) described extruded bar stock is subsequently at 1250 DEG C of insulation 1.5h, then anneals;
7) bar of annealing is heated to 1400 DEG C on high-temperature tensile testing machine, and insulation 0.5h, then stretch, obtain TiC dispersion-strengthemolybdenum molybdenum alloy material, the tensile strength of this TiC dispersion-strengthemolybdenum molybdenum alloy material is 155MPa, unit elongation 25.4%.
Embodiment two
1) take granularity at 500 object molybdenum powder 10Kg, granularity is at 400 object titanium valve 45g, carbonization molybdenum powder 55g, Graphite Powder 99 5g;
2) molybdenum powder, titanium valve, Graphite Powder 99, carbonization molybdenum powder are put into ball milling bucket, add 2500ml dehydrated alcohol, ball milling mixing 10h;
3) ball milling being mixed the ball milling solution obtained is placed in drying baker, 50 DEG C of dry 6h, makes the ethanol volatilization in this solution clean, obtains a powdered alloy;
4) described powdered alloy is through the compacting of 230Mpa isostatic pressed, and in Intermediate frequency sintering furnace sintering, at 1750 DEG C of insulation 12h, furnace cooling obtains a sintered blank;
5) described sintered blank is after 1550 DEG C of insulation 2h, is to extrude at 3.5: 1, obtains an extruded bar stock with extrusion ratio;
6) described extruded bar stock is subsequently at 1200 DEG C of insulation 2h, then anneals;
7) bar of annealing is heated to 1350 DEG C on high-temperature tensile testing machine, and insulation 0.6h, then stretch, obtain TiC dispersion-strengthemolybdenum molybdenum alloy material, the tensile strength of this TiC dispersion-strengthemolybdenum molybdenum alloy material is 165MPa, unit elongation 24.2%.
Embodiment three
1) take granularity at 400 object molybdenum powder 10Kg, granularity is at 700 object titanium valve 60g, carbonization molybdenum powder 60g, Graphite Powder 99 7g;
2) molybdenum powder, titanium valve, Graphite Powder 99, carbonization molybdenum powder are put into ball milling bucket, add 1500ml dehydrated alcohol, ball milling mixing 6h;
3) ball milling being mixed the ball milling solution obtained is placed in drying baker, 70 DEG C of dry 7h, makes the ethanol volatilization in this solution clean, obtains a powdered alloy;
4) described powdered alloy is through the compacting of 300MPa isostatic pressed, and in Intermediate frequency sintering furnace sintering, at 1700 DEG C of insulation 15h, furnace cooling obtains a sintered blank;
5) described sintered blank is after 1650 DEG C of insulation 1h, is to extrude at 3.5: 1, obtains an extruded bar stock with extrusion ratio;
6) described extruded bar stock is subsequently at 1300 DEG C of insulation 1h, then anneals;
7) bar of annealing is heated to 1450 DEG C on high-temperature tensile testing machine, and insulation 0.4h, then stretch, obtain TiC dispersion-strengthemolybdenum molybdenum alloy material, the tensile strength of this TiC dispersion-strengthemolybdenum molybdenum alloy material is 160MPa, unit elongation 25.0%.
The present invention is at 1700-1800 DEG C of temperature range inside holding, and MoC is dissolved in described Mo substrate with the form of Mo and C atom completely, and graphite and titanium valve are also dissolved in described Mo substrate with the form of C atom and Ti atom respectively completely.By insulation for some time, utilize the concentration gradient of atom to spread, Ti and C atom is spread in described Mo substrate, reaches and be uniformly distributed.
Lower the temperature subsequently, the solubility with temperature of Ti and C in described Mo substrate reduces and declines, and Ti atom and C atom evolution reaction from described Mo substrate generates tiny TiC phase, achieves good dispersion-strengthened effect.
Preferably, described sintered blank is through 1600 DEG C of extruding, and extrusion ratio 3.5: 1, lining bar 1400 DEG C of tensile strength of preparation are 165MPa, unit elongation 25.6%.
Above-described embodiment, just in order to technical conceive of the present invention and feature are described, its objective is and is one of ordinary skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.The change of every equivalence done by the essence of content of the present invention or modification, all should be encompassed in protection scope of the present invention.
Claims (3)
1. a TiC dispersion-strengthemolybdenum molybdenum alloy, it is characterized in that the material primarily of following weight part forms: molybdenum powder 10Kg, titanium valve 40 ~ 60g, carbonization molybdenum powder 45 ~ 60g, Graphite Powder 99 5 ~ 7g, above-mentioned material carried out ball mill mixing, then carries out drying, suppress, sinter, extrude, drawing process obtains required TiC dispersion-strengthemolybdenum molybdenum alloy.
2. a preparation method for TiC dispersion-strengthemolybdenum molybdenum alloy, is characterized in that comprising the following steps and processing condition:
1) molybdenum powder 10Kg is taken, titanium valve 40 ~ 60g, carbonization molybdenum powder 45 ~ 60g, Graphite Powder 99 5 ~ 7g;
2) molybdenum powder, titanium valve, Graphite Powder 99, carbonization molybdenum powder are put into ball milling bucket, add 1500 ~ 2500ml dehydrated alcohol, ball milling mixing 0.5 ~ 10h;
3) ball milling being mixed the ball milling solution obtained is placed in drying baker, dry 2 ~ 10h under 30 ~ 80 DEG C of temperature condition, makes the ethanol volatilization in this solution clean, obtains a powdered alloy;
4) described powdered alloy is through the compacting of 200Mpa ~ 300MPa isostatic pressed, and in Intermediate frequency sintering furnace sintering, under 1700 ~ 1800 DEG C of temperature condition, be incubated 6 ~ 16h, furnace cooling obtains a sintered blank;
5), after described sintered blank is incubated 0.5 ~ 2h under 1550 ~ 1650 DEG C of temperature condition, is to extrude at 3.5: 1 with extrusion ratio, obtains an extruded bar stock;
6) described extruded bar stock is incubated 0.5 ~ 2h subsequently under 1200 ~ 1300 DEG C of temperature condition, then anneals;
7) bar of annealing is heated to 1350 ~ 1450 DEG C on high-temperature tensile testing machine, and insulation 0.3 ~ 0.6h, then stretches, obtain TiC dispersion-strengthemolybdenum molybdenum alloy material.
3. the preparation method of TiC dispersion-strengthemolybdenum molybdenum alloy according to claim 2, it is characterized in that described molybdenum powder, titanium valve, carbonization molybdenum powder, Graphite Powder 99 granularity at 400 ~ 800 orders; The tensile strength of described TiC dispersion-strengthemolybdenum molybdenum alloy material is 150 ~ 165MPa, unit elongation 23 ~ 25.6%.
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| CN108866414A (en) * | 2018-06-11 | 2018-11-23 | 西安建筑科技大学 | A kind of high tough molybdenum alloy and preparation method |
| CN113718150A (en) * | 2021-05-27 | 2021-11-30 | 有研工程技术研究院有限公司 | Alloy roller for continuous induction type quick quenching furnace and manufacturing method thereof |
| CN114959396A (en) * | 2022-04-22 | 2022-08-30 | 哈尔滨工程大学 | TiC/Mo alloy with lattice structure and selective laser melting preparation method thereof |
| CN115652161A (en) * | 2022-10-12 | 2023-01-31 | 西安建筑科技大学 | Preparation method of polymer carbonized porous coated nano carbide toughened molybdenum alloy |
| CN115927898A (en) * | 2022-12-08 | 2023-04-07 | 西安理工大学 | TiC particle reinforced high-strength TZM-based composite material and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108866414A (en) * | 2018-06-11 | 2018-11-23 | 西安建筑科技大学 | A kind of high tough molybdenum alloy and preparation method |
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| CN113718150A (en) * | 2021-05-27 | 2021-11-30 | 有研工程技术研究院有限公司 | Alloy roller for continuous induction type quick quenching furnace and manufacturing method thereof |
| CN114959396A (en) * | 2022-04-22 | 2022-08-30 | 哈尔滨工程大学 | TiC/Mo alloy with lattice structure and selective laser melting preparation method thereof |
| CN115652161A (en) * | 2022-10-12 | 2023-01-31 | 西安建筑科技大学 | Preparation method of polymer carbonized porous coated nano carbide toughened molybdenum alloy |
| CN115652161B (en) * | 2022-10-12 | 2023-08-04 | 西安建筑科技大学 | Preparation method of polymer carbonized porous coated nano carbide strengthening and toughening molybdenum alloy |
| CN115927898A (en) * | 2022-12-08 | 2023-04-07 | 西安理工大学 | TiC particle reinforced high-strength TZM-based composite material and preparation method thereof |
| CN115927898B (en) * | 2022-12-08 | 2024-03-19 | 西安理工大学 | TiC particle reinforced high-strength TZM-based composite material and preparation method thereof |
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Application publication date: 20150527 |