A kind of nano la2o3 evenly doped nano molybdenum composite powder and its preparation method

Abstract

The invention discloses a nano La 2 o 3 Uniformly doped nanomolybdenum composite powder La 2 o 3 The size of the composite powder with Mo is 30~100nm, La 2 o 3 The content is 0.5~5.0wt.%. It is also disclosed that its preparation process is: preparation of solution→solution heating→adding glucose→synthesis of precursor→precursor reduction→nanometer La 2 o 3 Uniformly doped nano molybdenum composite powder. The invention not only ensures the uniform dispersion and stability of the nanoparticles, but also can effectively control the size of the powder. At the same time, the reaction synthesis temperature of the precursor is low, the reaction time is short, the efficiency is high, the energy is saved and the operation is simple.

Description

technical field

[0001] The present invention relates to nanometer La 2 o 3 The technical field of doping, specifically referring to a kind of nanometer La 2 o 3 Uniformly doped nano-molybdenum composite powder and its preparation method. Background technique

[0002] Metal molybdenum is an important refractory metal material. Due to the poor toughness of molybdenum at room temperature and the high ductile-brittle transition temperature (DBTT), the toughness is still insufficient at higher temperatures. These defects limit the use of molybdenum and molybdenum alloys in structural materials. aspects of application. Using La 2 o 3 The rare earth oxide doped molybdenum alloy prepared by rare earth oxide doping technology has good room / high temperature strength and toughness. The uniform dispersion and refinement of rare earth oxide particles is the difficulty and key point of rare earth oxide doping technology.

[0003] At present, there are three methods for preparing r...

Examples

Embodiment 1

[0027] A nano La 2 o 3 The preparation process of uniformly doped nano-molybdenum composite powder is as follows: figure 1 shown.

[0028] (1) Put 12.4g of ammonium molybdate tetrahydrate, 16g of ammonium nitrate, 8g of glycine and 0.22g of lanthanum nitrate hexahydrate into a 1000ml beaker, add 100ml of deionized water, and stir until completely dissolved to form a mixed solution.

[0029] (2) Place the beaker containing the above mixed solution on a heating furnace and heat it at 200°C.

[0030] (3) After the solution boils for 3 to 5 minutes, add 4.5g of glucose and stir fully at the same time.

[0031] (4) Continue to heat the solution after adding glucose at 200°C. When the solution forms a light blue sol, lower the temperature to 160°C. The reaction begins and a fluffy foam-like substance is formed. After 3 to 5 minutes, the reaction end, get La 2 o 3 / MoO x Precursor powder. Its TG / DSC curve is as follows figure 2 shown.

[0032] (5) The above La 2 o 3 / MoO ...

Embodiment 2

[0036] (1) Put 12.4g of ammonium molybdate tetrahydrate, 20g of ammonium nitrate, 8g of glycine and 0.55g of lanthanum nitrate hexahydrate into a 1000ml beaker, add 100ml of deionized water, and stir until completely dissolved to form a mixed solution.

[0037] (2) Place the beaker containing the above mixed solution on a heating furnace and heat it at 200°C.

[0038] (3) After the solution boils for 3 to 5 minutes, add 6.8g of glucose and stir fully at the same time.

[0039] (4) Continue to heat the solution after adding glucose at 200°C. When the solution forms a light blue sol, lower the temperature to 160°C. The reaction begins and a fluffy foam-like substance is formed. After 3 to 5 minutes, the reaction end, get La 2 o 3 / MoO x Precursor powder.

[0040] (5) The above La 2 o 3 / MoO x The precursor powder was put into the atmosphere heating furnace, and reduced at 750°C for 3 hours under the flowing hydrogen of 900ml / min. After the reduction, it was cooled with th...

Embodiment 3

[0044] (1) Put 12.4g of ammonium molybdate tetrahydrate, 24g of ammonium nitrate, 8g of glycine and 0.94g of lanthanum nitrate hexahydrate into a 1000ml beaker, add 100ml of deionized water, and stir until completely dissolved to form a mixed solution.

[0045] (2) Place the beaker containing the above mixed solution on a heating furnace and heat it at 200°C.

[0046] (3) After the solution boils for 3-5 minutes, add 9g of glucose and stir fully at the same time.

[0047] (4) Continue to heat the solution after adding glucose at 200°C. When the solution forms a light blue sol, lower the temperature to 160°C. The reaction begins and a fluffy foam-like substance is formed. After 3 to 5 minutes, the reaction end, get La 2 o 3 / MoO x Precursor powder.

[0048] (5) The above La 2 o 3 / MoO x The precursor powder was put into the atmosphere heating furnace, under the flowing hydrogen of 1000ml / min, the reduction was carried out at 700°C for 4 hours, after the reduction was com...

technical field

[0001] The present invention relates to nanometer La 2 o 3 The technical field of doping, specifically referring to a kind of nanometer La 2 o 3 Uniformly doped nano-molybdenum composite powder and its preparation method. Background technique

[0002] Metal molybdenum is an important refractory metal material. Due to the poor toughness of molybdenum at room temperature and the high ductile-brittle transition temperature (DBTT), the toughness is still insufficient at higher temperatures. These defects limit the use of molybdenum and molybdenum alloys in structural materials. aspects of application. Using La 2 o 3 The rare earth oxide doped molybdenum alloy prepared by rare earth oxide doping technology has good room / high temperature strength and toughness. The uniform dispersion and refinement of rare earth oxide particles is the difficulty and key point of rare earth oxide doping technology.

[0003] At present, there are three methods for preparing r...

Examples

Embodiment 1

[0027] A nano La 2 o 3 The preparation process of uniformly doped nano-molybdenum composite powder is as follows: figure 1 shown.

[0028] (1) Put 12.4g of ammonium molybdate tetrahydrate, 16g of ammonium nitrate, 8g of glycine and 0.22g of lanthanum nitrate hexahydrate into a 1000ml beaker, add 100ml of deionized water, and stir until completely dissolved to form a mixed solution.

[0029] (2) Place the beaker containing the above mixed solution on a heating furnace and heat it at 200°C.

[0030] (3) After the solution boils for 3 to 5 minutes, add 4.5g of glucose and stir fully at the same time.

[0031] (4) Continue to heat the solution after adding glucose at 200°C. When the solution forms a light blue sol, lower the temperature to 160°C. The reaction begins and a fluffy foam-like substance is formed. After 3 to 5 minutes, the reaction end, get La 2 o 3 / MoO x Precursor powder. Its TG / DSC curve is as follows figure 2 shown.

[0032] (5) The above La 2 o 3 / MoO ...

Embodiment 2

[0036] (1) Put 12.4g of ammonium molybdate tetrahydrate, 20g of ammonium nitrate, 8g of glycine and 0.55g of lanthanum nitrate hexahydrate into a 1000ml beaker, add 100ml of deionized water, and stir until completely dissolved to form a mixed solution.

[0037] (2) Place the beaker containing the above mixed solution on a heating furnace and heat it at 200°C.

[0038] (3) After the solution boils for 3 to 5 minutes, add 6.8g of glucose and stir fully at the same time.

[0039] (4) Continue to heat the solution after adding glucose at 200°C. When the solution forms a light blue sol, lower the temperature to 160°C. The reaction begins and a fluffy foam-like substance is formed. After 3 to 5 minutes, the reaction end, get La 2 o 3 / MoO x Precursor powder.

[0040] (5) The above La 2 o 3 / MoO x The precursor powder was put into the atmosphere heating furnace, and reduced at 750°C for 3 hours under the flowing hydrogen of 900ml / min. After the reduction, it was cooled with th...

Embodiment 3

[0044] (1) Put 12.4g of ammonium molybdate tetrahydrate, 24g of ammonium nitrate, 8g of glycine and 0.94g of lanthanum nitrate hexahydrate into a 1000ml beaker, add 100ml of deionized water, and stir until completely dissolved to form a mixed solution.

[0045] (2) Place the beaker containing the above mixed solution on a heating furnace and heat it at 200°C.

[0046] (3) After the solution boils for 3-5 minutes, add 9g of glucose and stir fully at the same time.

[0047] (4) Continue to heat the solution after adding glucose at 200°C. When the solution forms a light blue sol, lower the temperature to 160°C. The reaction begins and a fluffy foam-like substance is formed. After 3 to 5 minutes, the reaction end, get La 2 o 3 / MoO x Precursor powder.

[0048] (5) The above La 2 o 3 / MoO x The precursor powder was put into the atmosphere heating furnace, under the flowing hydrogen of 1000ml / min, the reduction was carried out at 700°C for 4 hours, after the reduction was com...

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