CN101569929A - Method for preparing nano aluminum oxide coated tungsten powder - Google Patents
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Abstract
The invention relates to a method for preparing nano aluminum oxide coated tungsten powder, belonging to the field of powder metallurgical preparation. The method solves the problems of being uneven in particle size, not reaching nanoscale, being easy to pollute, agglomeration of powder and the like in the current preparation of the nano aluminum oxide coated tungsten powder. The coated power is characterized in that nano aluminum oxide is coated on the surface of micron-sized tungsten powder, and the mol content of the aluminum oxide is 10-30%. The method for preparing the coated powder is characterized in that ammonium metatungstate powder and aluminium sulphate powder are dissolved in distilled water together, and then dispersed in liquid nitrogen for pre-freezing by using a nitrogen spray gun after being clarified; the pre-frozen mixture is placed into a freeze-dryer for vacuum drying, so that freeze-dried powder can be obtained; under hydrogen atmosphere, the freeze-dried powder is calcined and deacidized in a sectional form, and composite powder of the nano aluminum oxide coated tungsten powder can be obtained. The invention has the advantages of fewer steps in the preparation process, simple operation, cheap and easily obtained raw materials and needing not to add matrix phase particles in advance.
Description
Technical field:
The present invention relates to a kind of preparation method of nano aluminum oxide coated tungsten powder body, particularly a kind of composite powder preparation method at tungsten powder surface clad nano aluminium oxide belongs to coated powder preparation field in the powder metallurgy.
Background technology:
The composite of the composite granule preparation that the even doping metals base of nano-ceramic powder particle obtains, not only have excellent in toughness, heat-conductivity conducting of metal etc., have characteristics such as ceramic high temperature resistant, wear-resistant and corrosion-resistant and high rigidity, high chemical stability again, caused widely and paid attention to.For guaranteeing the dispersing uniformity of compound particle, to improve the performance of material the most significantly, often requirement is coated on the blapharoplast surface with doping phase particle, forms clad, reaches best degree of mixing.The composite of nano alumina powder jointed coated tungsten powder preparation has single-phase oxide or the incomparable advantage of metal.At present, solid phase ball milling and liquid phase method are adopted in the preparation of nano aluminum oxide coated tungsten powder more, mostly face the problem of some general character:
(1) granularity of the aluminum oxide coated tungsten powder that obtains by ball milling is inhomogeneous, and the aluminium oxide of clad does not reach nanoscale, the coated powder vulnerable to pollution;
(2) liquid phase method is selected the raw material costliness for use, and the preparation condition harshness is difficult to control, and because the existence of liquid phase makes final coated powder have reunion.
The existence of these problems has limited the development and the application of nano aluminum oxide coated tungsten powder composite.
Summary of the invention:
At the above problem that prior art exists, the invention provides a kind of preparation method of nano aluminum oxide coated tungsten powder.
The preparation method of a kind of nano aluminum oxide coated tungsten powder provided by the present invention is characterized in that, it may further comprise the steps:
(1) respectively according to target in the composite granule mol ratio of aluminium oxide and tungsten be aluminium oxide: tungsten=1: 9～3: 7, weighing ammonium metatungstate [(NH
4)
6H
2W
12O
4014H
2O] white crystalline powder and aluminum sulfate [Al
2(SO
4)
318H
2O] crystal powder, and the two is dissolved in the distilled water altogether, wait to clarify;
(2) use general nitrogen spray gun, the mixed solution of clarifying is dispersed in pre-freeze in the general liquid nitrogen, obtain scars, spray gun pressure is 1.5～3.5 atmospheric pressure;
(3) will use the scars of liquid nitrogen pre-freeze to place freeze dryer to carry out vacuum drying, obtain the mixed-powder of freeze-drying;
(4) mixed-powder of the freeze-drying that step (3) is obtained is carried out the segmentation calcining reduction, and atmosphere is hydrogen atmosphere, and flow is 0.1～0.5m
3/ h; Obtain the composite granule of nano aluminum oxide coated tungsten powder, about the about 20nm of aluminum oxide grain size, about the about 1 μ m of tungsten powder particle-size.
Wherein, the pressure of the nitrogen spray gun described in the step (2) is 1.5～3.5 atmospheric pressure.
The performing a programme of the described freeze dryer of step (3) is: the operating pressure in 0～2400 minute is that 250～350 millitorrs, temperature are-28～-24 ℃; Operating pressure in 2400～3800 minutes is that 120～180 millitorrs, temperature are-15～-12 ℃; Operating pressure in 3800～4600 minutes is that 50～100 millitorrs, temperature are-3～2 ℃; Operating pressure in 4600～4800 minutes is that 0～20 millitorr, temperature are 15～25 ℃.
Segmentation calcining reduction described in the step (4) comprises two sections processes: first section is reduction process, and reduction temperature is 650～850 ℃, is incubated 120～240 minutes, and ammonium metatungstate becomes tungsten through thermal decomposition, hydrogen reduction; Second section is the calcining and decomposing process, and decomposition temperature is 900～1100 ℃, is incubated 120～360 minutes, and aluminum sulfate becomes aluminium oxide through thermal decomposition, is coated on tungsten powder surface.
The present invention adopts liquid nitrogen pre-freeze-freeze-drying, by the low-temp low-pressure drying, makes the amorphous state freeze-dried powder, can prevent effectively that monophased particles is poly-partially.By the segmentation calcining reduction, obtain the composite granule of nano aluminum oxide coated tungsten powder again.Advantage of the present invention is that the preparation process step is few, simple to operate, and raw material cheaply is easy to get, and need not to add in advance matrix phase particle.
Description of drawings:
The freeze-drying mixed-powder X ray diffracting spectrum of Fig. 1: embodiment 2
The nano aluminum oxide coated tungsten powder X ray diffracting spectrum of Fig. 2: embodiment 3
The nano aluminum oxide coated tungsten powder SEM picture of Fig. 3: embodiment 4
Below in conjunction with the drawings and specific embodiments the present invention is further described.
The specific embodiment:
Employed freeze dryer is the FTD Dura-stop MP type freeze dryer of FTS company among the embodiment.
Embodiment 1:
(1) mol ratio by final aluminium oxide and tungsten powder is 2: 8, and weighing 3.567 gram ammonium metatungstate white crystalline powder and 2.222 gram aluminum sulfate white crystalline powder are dissolved in 250 ml distilled waters altogether with the two respectively, wait to clarify;
(2) use the nitrogen spray gun, the mixed solution of clarifying is dispersed in obtains scars in the liquid nitrogen, spray gun pressure is 1.5 atmospheric pressure;
(3) scars are placed freeze dryer to carry out vacuum drying, the performing a programme of freeze dryer is again: the operating pressure in 0～2400 minute is that 250 millitorrs, temperature are-24 ℃; Operating pressure in 2400～3800 minutes is that 150 millitorrs, temperature are-14 ℃; Operating pressure in 3800～4600 minutes is that 80 millitorrs, temperature are-1 ℃; Operating pressure in 4600～4800 minutes is that 0 millitorr, temperature are 20 ℃;
(4) mixed-powder after the freeze drying is packed into porcelain boat pushes porcelain boat in the tube furnace, and logical hydrogen carries out the segmentation calcining reduction, and hydrogen flowing quantity is 0.1m
3/ h; First section temperature is 650 ℃, is incubated 240 minutes, and ammonium metatungstate becomes tungsten through thermal decomposition, hydrogen reduction; Second section temperature is 900 ℃, is incubated 360 minutes, and aluminum sulfate becomes aluminium oxide through thermal decomposition, is coated on tungsten powder surface, obtains the composite granule of nano aluminum oxide coated tungsten powder, and aluminum oxide grain size is 32nm, and tungsten powder particle-size is 1.17 μ m.
Embodiment 2:
(1) mol ratio by final aluminium oxide and tungsten powder is 2: 8, and weighing 4.28 gram ammonium metatungstate white crystalline powder and 2.666 gram aluminum sulfate white crystalline powder are dissolved in 300 ml distilled waters altogether with the two respectively, wait to clarify;
(2) use the nitrogen spray gun, the mixed solution of clarifying is dispersed in obtains scars in the liquid nitrogen, spray gun pressure is 2 atmospheric pressure;
(3) scars are placed freeze dryer to carry out vacuum drying, the performing a programme of freeze dryer is again: the operating pressure in 0～2400 minute is that 300 millitorrs, temperature are-26 ℃; Operating pressure in 2400～3800 minutes is that 160 millitorrs, temperature are-13 ℃; Operating pressure in 3800～4600 minutes is that 50 millitorrs, temperature are 0 ℃; Operating pressure in 4600～4800 minutes is that 0 millitorr, temperature are 25 ℃;
(4) mixed-powder after the freeze drying is packed into porcelain boat pushes porcelain boat in the tube furnace, and logical hydrogen carries out the segmentation calcining reduction, and hydrogen flowing quantity is 0.2m
3/ h, first section temperature is 700 ℃, is incubated 240 minutes, ammonium metatungstate becomes tungsten through thermal decomposition, hydrogen reduction; Second section temperature is 1000 ℃, is incubated 240 minutes, and aluminum sulfate becomes aluminium oxide through thermal decomposition, is coated on tungsten powder surface, obtains the composite granule of nano aluminum oxide coated tungsten powder, and aluminum oxide grain size is 28nm, and tungsten powder particle-size is 0.86 μ m.
Fig. 1 is the X ray diffracting spectrum of present embodiment step (3) obtained freeze-drying mixed-powder, and as can be seen from the figure, freeze-dried powder is the amorphous state powder.
Embodiment 3:
(1) mol ratio by final aluminium oxide and tungsten powder is 2: 8, and weighing 5.35 gram ammonium metatungstate white crystalline powder and 3.332 gram aluminum sulfate white crystalline powder are dissolved in 400 ml distilled waters altogether with the two respectively, wait to clarify;
(2) use the nitrogen spray gun, the mixed solution of clarifying is dispersed in obtains scars in the liquid nitrogen, spray gun pressure is 2.5 atmospheric pressure;
(3) scars are placed freeze dryer to carry out vacuum drying, the performing a programme of freeze dryer is again: the operating pressure in 0～2400 minute is that 350 millitorrs, temperature are-28 ℃; Operating pressure in 2400～3800 minutes is that 180 millitorrs, temperature are-15 ℃; Operating pressure in 3800～4600 minutes is that 100 millitorrs, temperature are-3 ℃; Operating pressure in 4600～4800 minutes is that 20 millitorrs, temperature are 15 ℃;
(4) mixed-powder after the freeze drying is packed into porcelain boat pushes porcelain boat in the tube furnace, and logical hydrogen carries out the segmentation calcining reduction, and hydrogen flowing quantity is 0.5m
3/ h, first section temperature is 800 ℃, is incubated 180 minutes, ammonium metatungstate becomes tungsten through thermal decomposition, hydrogen reduction; Second section temperature is 1100 ℃, is incubated 120 minutes, and aluminum sulfate becomes aluminium oxide through thermal decomposition, is coated on tungsten powder surface, obtains the composite granule of nano aluminum oxide coated tungsten powder, and aluminum oxide grain size is 30nm, and tungsten powder particle-size is 0.98 μ m.
The X ray diffracting spectrum of the end product nano aluminum oxide coated tungsten powder that Fig. 2 obtains for present embodiment.As can be seen from the figure, adopt the method for liquid nitrogen pre-freeze-freeze drying-segmentation calcining reduction, the final powder that obtains behind the calcining reduction is respectively tungsten and aluminium oxide, illustrates that decomposition-reduction is abundant, has obtained required thing phase composition.
Embodiment 4:
(1) mol ratio by final aluminium oxide and tungsten powder is 1: 9, and weighing 12.038 gram ammonium metatungstate white crystalline powder and 3.332 gram aluminum sulfate white crystalline powder are dissolved in 500 ml distilled waters altogether with the two respectively, wait to clarify;
(2) use the nitrogen spray gun, the mixed solution of clarifying is dispersed in obtains scars in the liquid nitrogen, spray gun pressure is 3 atmospheric pressure;
(3) scars are placed freeze dryer to carry out vacuum drying, the performing a programme of freeze dryer is again: the operating pressure in 0～2400 minute is that 250 millitorrs, temperature are-24 ℃; Operating pressure in 2400～3800 minutes is that 120 millitorrs, temperature are-12 ℃; Operating pressure in 3800～4600 minutes is that 50 millitorrs, temperature are 2 ℃; Operating pressure in 4600～4800 minutes is that 0 millitorr, temperature are 25 ℃;
(4) mixed-powder after the freeze drying is packed into porcelain boat pushes porcelain boat in the tube furnace, and logical hydrogen carries out the segmentation calcining reduction, and hydrogen flowing quantity is 0.4m
3/ h, first section temperature is 850 ℃, is incubated 120 minutes, ammonium metatungstate becomes tungsten through thermal decomposition, hydrogen reduction; Second section temperature is 1050 ℃, is incubated 300 minutes, and aluminum sulfate becomes aluminium oxide through thermal decomposition, is coated on tungsten powder surface, obtains the composite granule of nano aluminum oxide coated tungsten powder, and aluminum oxide grain size is 35nm, and tungsten powder particle-size is 1.26 μ m.
The SEM picture of the end product nano aluminum oxide coated tungsten powder that Fig. 3 obtains for present embodiment.As can be seen from the figure, the composite granule of the nano aluminum oxide coated tungsten powder that the method for employing liquid nitrogen pre-freeze-freeze drying-segmentation calcining reduction obtains, aluminium oxide particle diameter 35nm, tungsten powder particle diameter 1.26 μ m.
Embodiment 5:
(1) mol ratio by final aluminium oxide and tungsten powder is 1: 9, and weighing 8.025 gram ammonium metatungstate white crystalline powder and 2.222 gram aluminum sulfate white crystalline powder are dissolved in 500 ml distilled waters altogether with the two respectively, wait to clarify;
(2) use the nitrogen spray gun, the mixed solution of clarifying is dispersed in obtains scars in the liquid nitrogen, spray gun pressure is 3.5 atmospheric pressure;
(3) scars are placed freeze dryer to carry out vacuum drying, the performing a programme of freeze dryer is again: the operating pressure in 0～2400 minute is that 280 millitorrs, temperature are-25 ℃; Operating pressure in 2400～3800 minutes is that 140 millitorrs, temperature are-12 ℃; Operating pressure in 3800～4600 minutes is that 50 millitorrs, temperature are 1 ℃; Operating pressure in 4600～4800 minutes is that 10 millitorrs, temperature are 22 ℃;
(4) mixed-powder after the freeze drying is packed into porcelain boat pushes porcelain boat in the tube furnace, and logical hydrogen carries out the segmentation calcining reduction, and hydrogen flowing quantity is 0.3m
3/ h, first section temperature is 750 ℃, is incubated 240 minutes, ammonium metatungstate becomes tungsten through thermal decomposition, hydrogen reduction; Second section temperature is 1100 ℃, is incubated 120 minutes, and aluminum sulfate becomes aluminium oxide through thermal decomposition, is coated on tungsten powder surface, obtains the composite granule of nano aluminum oxide coated tungsten powder, and aluminum oxide grain size is 36nm, and tungsten powder particle-size is 1.13 μ m.
Embodiment 6:
(1) mol ratio by final aluminium oxide and tungsten powder is 3: 7, and weighing 3.746 gram ammonium metatungstate white crystalline powder and 3.998 gram aluminum sulfate white crystalline powder are dissolved in 250 ml distilled waters altogether with the two respectively, wait to clarify;
(2) use the nitrogen spray gun, the mixed solution of clarifying is dispersed in obtains scars in the liquid nitrogen, spray gun pressure is 1.8 atmospheric pressure;
(3) scars are placed freeze dryer to carry out vacuum drying, the performing a programme of freeze dryer is again: the operating pressure in 0～2400 minute is that 320 millitorrs, temperature are-26 ℃; Operating pressure in 2400～3800 minutes is that 160 millitorrs, temperature are-13 ℃; Operating pressure in 3800～4600 minutes is that 80 millitorrs, temperature are 0 ℃; Operating pressure in 4600～4800 minutes is that 0 millitorr, temperature are 20 ℃;
(4) mixed-powder after the freeze drying is packed into porcelain boat pushes porcelain boat in the tube furnace, and logical hydrogen carries out the segmentation calcining reduction, and hydrogen flowing quantity is 0.1m
3/ h, first section temperature is 850 ℃, is incubated 240 minutes, ammonium metatungstate becomes tungsten through thermal decomposition, hydrogen reduction; Second section temperature is 900 ℃, is incubated 360 minutes, and aluminum sulfate becomes aluminium oxide through thermal decomposition, is coated on tungsten powder surface, obtains the composite granule of nano aluminum oxide coated tungsten powder, and aluminum oxide grain size is 32nm, and tungsten powder particle-size is 1.21 μ m.
Embodiment 7:
(1) mol ratio by final aluminium oxide and tungsten powder is 3: 7, and weighing 5.619 gram ammonium metatungstate white crystalline powder and 5.998 gram aluminum sulfate white crystalline powder are dissolved in the xx ml distilled water altogether with the two respectively, wait to clarify;
(2) use the nitrogen spray gun, the mixed solution of clarifying is dispersed in obtains scars in the liquid nitrogen, spray gun pressure is 2.8 atmospheric pressure;
(3) scars are placed freeze dryer to carry out vacuum drying, the performing a programme of freeze dryer is again: the operating pressure in 0～2400 minute is that 300 millitorrs, temperature are-26 ℃; Operating pressure in 2400～3800 minutes is that 150 millitorrs, temperature are-13 ℃; Operating pressure in 3800～4600 minutes is that 60 millitorrs, temperature are 0 ℃; Operating pressure in 4600～4800 minutes is that 0 millitorr, temperature are 20 ℃;
(4) mixed-powder after the freeze drying is packed into porcelain boat pushes porcelain boat in the tube furnace, and logical hydrogen carries out the segmentation calcining reduction, and hydrogen flowing quantity is 0.5m
3/ h, first section temperature is 750 ℃, is incubated 240 minutes, ammonium metatungstate becomes tungsten through thermal decomposition, hydrogen reduction; Second section temperature is 1000 ℃, is incubated 240 minutes, and aluminum sulfate becomes aluminium oxide through thermal decomposition, is coated on tungsten powder surface, obtains the composite granule of nano aluminum oxide coated tungsten powder, and aluminum oxide grain size is 25nm, and tungsten powder particle-size is 0.95 μ m.
Embodiment 8:
(1) mol ratio by final aluminium oxide and tungsten powder is 3: 7, and weighing 7.492 gram ammonium metatungstate white crystalline powder and 7.996 gram aluminum sulfate white crystalline powder are dissolved in 500 ml distilled waters altogether with the two respectively, wait to clarify;
(2) use the nitrogen spray gun to press, the mixed solution of clarifying is dispersed in obtains scars in the liquid nitrogen, spray gun pressure is 3.2 atmosphere:
(3) scars are placed freeze dryer to carry out vacuum drying, the performing a programme of freeze dryer is again: the operating pressure in 0～2400 minute is that 300 millitorrs, temperature are-30 ℃; Operating pressure in 2400～3800 minutes is that 120 millitorrs, temperature are-15 ℃; Operating pressure in 3800～4600 minutes is that 80 millitorrs, temperature are 0 ℃; Operating pressure in 4600～4800 minutes is that 0 millitorr, temperature are 15 ℃;
(4) mixed-powder after the freeze drying is packed into porcelain boat pushes porcelain boat in the tube furnace, and logical hydrogen carries out the segmentation calcining reduction, and hydrogen flowing quantity is 0.3m
3/ h, first section temperature is 650 ℃, is incubated 240 minutes, ammonium metatungstate becomes tungsten through thermal decomposition, hydrogen reduction; Second section temperature is 1100 ℃, is incubated 240 minutes, and aluminum sulfate becomes aluminium oxide through thermal decomposition, is coated on tungsten powder surface, obtains the composite granule of nano aluminum oxide coated tungsten powder, and aluminum oxide grain size is 31nm, and tungsten powder particle-size is 1.08 μ m.
Claims (1)
1, a kind of preparation method of nano aluminum oxide coated tungsten powder is characterized in that, it may further comprise the steps:
(1) respectively according to target in the composite granule mol ratio of aluminium oxide and tungsten be aluminium oxide: tungsten=1: 9～3: 7, weighing ammonium metatungstate [(NH
4)
6H
2W
12O
4014H
2O] white crystalline powder and aluminum sulfate [Al
2(SO
4)
318H
2O] crystal powder, and the two is dissolved in the distilled water altogether, wait to clarify;
(2) use general nitrogen spray gun, the mixed solution of clarifying is dispersed in pre-freeze in the general liquid nitrogen, obtain scars, spray gun pressure is 1.5～3.5 atmospheric pressure;
(3) will use the scars of liquid nitrogen pre-freeze to place freeze dryer to carry out vacuum drying, obtain the mixed-powder of freeze-drying; The performing a programme of freeze dryer is: the operating pressure in 0～2400 minute is that 250～350 millitorrs, temperature are-28～-24 ℃; Operating pressure in 2400～3800 minutes is that 120～180 millitorrs, temperature are-15～-12 ℃; Operating pressure in 3800～4600 minutes is that 50～100 millitorrs, temperature are-3～2 ℃; Operating pressure in 4600～4800 minutes is that 0～20 millitorr, temperature are 15～25 ℃;
(4) mixed-powder of the freeze-drying that step (3) is obtained is carried out the segmentation calcining reduction, and atmosphere is hydrogen atmosphere, and flow is 0.1～0.5m
3/ h obtains the composite granule of nano aluminum oxide coated tungsten powder; The segmentation calcining reduction comprises two sections processes: first section is reduction process, and reduction temperature is 650～850 ℃, is incubated 120～240 minutes; Second section is the calcining and decomposing process, and decomposition temperature is 900～1100 ℃, is incubated 120～360 minutes.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI416056B (en) * | 2012-12-14 | 2013-11-21 | ||
| CN105397102A (en) * | 2015-12-30 | 2016-03-16 | 河南科技大学 | Preparation method aluminum oxide coating tungsten powder |
| CN107008917A (en) * | 2017-04-17 | 2017-08-04 | 河南科技大学 | A kind of nanometer Al2O3/WO3Composite granule and preparation method thereof, Al2O3/ W alloy powder |
| CN108723382A (en) * | 2018-06-25 | 2018-11-02 | 天津大学 | A kind of freeze drying process of preparing same of ultrafine yttria doping tungsten composite powder |
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| JP3977226B2 (en) * | 2002-10-25 | 2007-09-19 | 大日本インキ化学工業株式会社 | Method of surface treatment of metal powder for forming sintered body and metal powder for forming sintered body |
| CN1182932C (en) * | 2003-04-09 | 2005-01-05 | 北京工业大学 | Nano-rare earth tungsten powder and its preparation method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI416056B (en) * | 2012-12-14 | 2013-11-21 | ||
| CN105397102A (en) * | 2015-12-30 | 2016-03-16 | 河南科技大学 | Preparation method aluminum oxide coating tungsten powder |
| CN107008917A (en) * | 2017-04-17 | 2017-08-04 | 河南科技大学 | A kind of nanometer Al2O3/WO3Composite granule and preparation method thereof, Al2O3/ W alloy powder |
| CN108723382A (en) * | 2018-06-25 | 2018-11-02 | 天津大学 | A kind of freeze drying process of preparing same of ultrafine yttria doping tungsten composite powder |
| CN116021020A (en) * | 2022-12-16 | 2023-04-28 | 辽宁省轻工科学研究院有限公司 | Thermal spraying sealing powder and preparation method thereof |
| CN116021020B (en) * | 2022-12-16 | 2024-09-06 | 辽宁省轻工科学研究院有限公司 | Thermal spraying sealing powder and preparation method thereof |
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