CN103170635A - Method for preparing spherical molybdenum powder - Google Patents
Method for preparing spherical molybdenum powder Download PDFInfo
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- CN103170635A CN103170635A CN2013101086857A CN201310108685A CN103170635A CN 103170635 A CN103170635 A CN 103170635A CN 2013101086857 A CN2013101086857 A CN 2013101086857A CN 201310108685 A CN201310108685 A CN 201310108685A CN 103170635 A CN103170635 A CN 103170635A
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Abstract
The invention discloses a method for preparing spherical molybdenum powder. The method includes the following steps: pulverizing the molybdenum powder; preparing polyvinyl alcohol aqueous solution; adding the pulverized molybdenum powder into the polyvinyl alcohol aqueous solution, stirring the solution to be even and preparing the solution to be sizing agent; performing spray drying on the sizing agent to obtain granulation powder; and firstly performing ungrease treatment on the granulation powder, secondly performing heat treatment on the granulation powder, and eventually performing crushing and sieving to obtain the spherical molybdenum powder. The method for preparing the spherical molybdenum powder is simple in process, low in cost, high in finished product rate, and wide in application range. By adoption of the method, the microstructure of the molybdenum powder can be effectively improved, the properties including apparent density, mobility and the like of the powder can be improved, the apparent density of the prepared spherical molybdenum powder is 2.0-4.5g/cm<3>, the mobility is 15s/50g-30s/50g, the quality purity is larger than or equal to 99.95%, and the finished product rate is larger than or equal to 90%.
Description
Technical field
The invention belongs to the molybdenum powder preparing technical field, be specifically related to a kind of method for preparing spherical molybdenum powder.
Background technology
Refractory metal molybdenum is positioned at periodic table of elements VI A family, has A2 type body-centered cubic structure.Compare with other refractory metals such as Ta, Nb, Co etc., molybdenum not only has good heat conduction, conduction and decay resistance, and has low thermal coefficient of expansion, higher hardness, well elevated temperature strength.Therefore, be widely used in the high-technology fields such as electronics, Aero-Space, the energy, nuclear reactor.
In recent years, along with the particularly develop rapidly of the high-end technology such as electronic information, Aero-Space of modern science and technology, high-performance, miniature, special-shaped molybdenum based articles demand are sharply increased.For example, liquid crystal screen back light source molybdenum electrode, microwave oven magnetic molybdenum cathode assembly, space propulsion of new generation all belong to complex-shaped, difficult processing parts with molybdenum alloy nozzle and trunnion, adopt the conventional machining method to prepare above-mentioned part and have the drawbacks such as complex procedures, the process-cycle is long, yield rate is low.At present, clean near shaping of powder is a kind of new technology of the difficult processing parts of preparation, and its main processes is powder forming and sintering, and powder forming is the core in this technology.Conventional hydrogen reduction molybdenum powder apparent density is little, filling is bad, poor fluidity, can not satisfy the demand of this novel technique, prepares therefore that pattern rounding, apparent density are large, molybdenum powder good fluidity becomes at first needs the problem that solves.
At present, the method for the spherical molybdenum powder of preparation mainly contains radio frequency plasma nodularization method, sol-gel process, mist projection granulating-sintering process.Jiang Xianliang etc. adopt standby spherical molybdenum powder (the JIANG Xian-Liang of radio frequency plasma nodularization legal system, M.BOULOS.Induction plasma spheroidization of tungsten and molybdenum powders[J] .Trans Nonferrous Met Soc China, 2006,16 (1): 13-17.), the radio frequency plasma method is to utilize the high warm of plasma torch generation that powder Flashmelt in irregular shape is become drop, chilling subsequently, " freezing " globulate powder.The molybdenum powder density that adopts this method to produce is high, good sphericity, and therefore this technology is considered to obtain one of effective means of densification, regular spherical particle.Yet there are the shortcomings such as equipment cost is high, yield rate is low in this technology.The employing sol-gel processes such as Xu Zhichang prepare spherical powder (Sol-gel Wet Process For Preparing Shaped Microspheres of Spray Molybdenum Powder [J] .. China Molybdenum Industry, 2007,31 (3): 23-27.), the method complex process, production cycle are long, consider cost and environmental problem, be difficult for realizing suitability for industrialized production.Disclose a kind of method of producing coating molybdenum powder in CN1962133A, adopted mist projection granulating-sintering technology, first powder has been passed through spray-drying, obtained suitable powder through oversintering afterwards.The method has been added polyethylene glycol, polyvinyl alcohol, the many kinds of substances such as ethanol, and addition large (surpassing 10%) easily causes the molybdenum powder secondary pollution, follow-up sintering temperature high (greater than 1550 ℃), this has not only proposed high requirement to agglomerating plant, and is unfavorable for energy conservation.A kind of cold spraying preparation method of spherical metal molybdenum particle is disclosed in CN201210082935, the method has limited initial molybdenum powder raw material granularity, the additive kind is numerous and diverse simultaneously, make complex technical process, in addition, the purpose of sintering just improves granule strength in this invention, thereby adopts the molybdenum powder of the method preparation to only limit to the cold spraying field.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of technique simple, and cost is low, and yield rate is high, the method for the spherical molybdenum powder of preparation that accommodation is wide.Adopt the method can effectively improve the microscopic appearance of molybdenum powder on the basis that does not reduce molybdenum powder purity, improve the performances such as apparent density of powder, mobility.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of method for preparing spherical molybdenum powder, it is characterized in that, and the method comprises the following steps:
Step 1, molybdenum powder is ground;
Step 2, preparation polyvinyl alcohol water solution;
Step 3, the molybdenum powder after grinding in step 1 is added described in step 2 in polyvinyl alcohol water solution, stir and make slurry; In described slurry, the mass content of molybdenum powder is 60%～80%, and in described slurry, the polyvinyl alcohol quality is 1.5%～5% of molybdenum powder weight;
Step 4, slurry described in step 3 is carried out spray-drying, obtain prilling powder;
Step 5, prilling powder described in step 4 is first carried out ungrease treatment, then heat-treat, last fragmentation is sieved and is obtained spherical molybdenum powder.
A kind of above-mentioned method for preparing spherical molybdenum powder grinds described in step 1 and adopts ball-milling method or air-flow to grind method.
A kind of above-mentioned method for preparing spherical molybdenum powder, the ratio of grinding media to material of described ball-milling method is 1～4: 1, Ball-milling Time is 20min～240min; It is high energy fluid bed head-on collision airflow milling that described air-flow grinds method, and rotating speed is 8000rpm～15000rpm, and the processing time is 30min～240min.
A kind of above-mentioned method for preparing spherical molybdenum powder, spray-dired intake air temperature described in step 4 are 220 ℃～250 ℃, and the air outlet temperature is 110 ℃～150 ℃, and centrifugal atomizing dish rotating speed is 10500rpm～12500rpm.
A kind of above-mentioned method for preparing spherical molybdenum powder, the temperature of ungrease treatment described in step 5 are 700 ℃～900 ℃, and the time is 2h～8h, and the atmosphere of ungrease treatment is wet hydrogen.
A kind of above-mentioned method for preparing spherical molybdenum powder, the dew point of described wet hydrogen are 35 ℃～55 ℃.
A kind of above-mentioned method for preparing spherical molybdenum powder, heat treated temperature described in step 5 are 1200 ℃～1500 ℃, and the time is 2h～8h, and heat treated atmosphere is hydrogen.
A kind of above-mentioned method for preparing spherical molybdenum powder, the apparent density of spherical molybdenum powder described in step 5 is 2.0g/cm
3～4.5g/cm
3, mobility 15s/50g～30s/50g, quality purity 〉=99.95%, yield rate 〉=90%.
The present invention compared with prior art has the following advantages: method technique of the present invention is simple, cost is low, yield rate is high, accommodation is wide, adopt the method can effectively improve the microscopic appearance of molybdenum powder on the basis that does not reduce molybdenum powder purity, improve the performances such as apparent density of powder, mobility, the apparent density of the spherical molybdenum powder of preparation is 2.0g/cm
3～4.5g/cm
3, mobility 15s/50g～30s/50g, quality purity 〉=99.95%, yield rate 〉=90% is applicable to accurate device preparation, machining and thermal spraying.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is that conventional molybdenum powder is amplified the shape appearance figure of 2000 times.
Fig. 2 is that conventional molybdenum powder is amplified the shape appearance figure of 500 times.
Fig. 3 is that the spherical molybdenum powder of embodiment 1 preparation is amplified the shape appearance figure of 3000 times.
Fig. 4 is that the spherical molybdenum powder of embodiment 1 preparation is amplified the shape appearance figure of 1000 times.
Fig. 5 is that the spherical molybdenum powder of embodiment 2 preparations is amplified the shape appearance figure of 3000 times.
Fig. 6 is that the spherical molybdenum powder of embodiment 2 preparations is amplified the shape appearance figure of 1000 times.
Fig. 7 is that the spherical molybdenum powder of embodiment 3 preparations is amplified the shape appearance figure of 3000 times.
Fig. 8 is that the spherical molybdenum powder of embodiment 3 preparations is amplified the shape appearance figure of 1500 times.
Fig. 9 is that the spherical molybdenum powder of embodiment 4 preparations is amplified the shape appearance figure of 3000 times.
Figure 10 is that the spherical molybdenum powder of embodiment 4 preparations is amplified the shape appearance figure of 1500 times.
Figure 11 is that the spherical molybdenum powder of embodiment 5 preparations is amplified the shape appearance figure of 3000 times.
Figure 12 is that the spherical molybdenum powder of embodiment 5 preparations is amplified the shape appearance figure of 1500 times.
Figure 13 is that the spherical molybdenum powder of embodiment 6 preparations is amplified the shape appearance figure of 3000 times.
Figure 14 is that the spherical molybdenum powder of embodiment 6 preparations is amplified the shape appearance figure of 1000 times.
The specific embodiment
Embodiment 1
Step 1, adopting ball-milling method, is ball milling 240min under the condition of 1: 1 in ratio of grinding media to material with 3000g conventional reduction molybdenum powder;
Step 2, the 61.2g polyvinyl alcohol is dissolved in the 1230mL deionized water, is mixed with polyvinyl alcohol water solution;
Step 3, the molybdenum powder after grinding in step 1 is added described in step 2 in polyvinyl alcohol water solution, stir and make slurry;
Step 4, slurry described in step 3 is carried out spray-drying, obtain prilling powder; The intake air temperature of described spray-dired drying tower is 220 ℃, and the air outlet temperature is 120 ℃, and centrifugal atomizing dish rotating speed is 10500rpm;
Step 5, be 900 ℃ of ungrease treatment 2h under the wet hydrogen atmosphere of 35 ℃ at dew point to prilling powder described in step 4, then 1200 ℃ of heat treatment 8h under hydrogen atmosphere, last broken mistake-100～+ 325 eye mesh screens, obtaining granularity is 30 μ m～90 μ m, mobility is 30s/50g, and apparent density is the spherical molybdenum powder of 2.0g/cm3.
The quality purity of the spherical molybdenum powder of the present embodiment preparation is 99.95%, yield rate is 90%, and its shape appearance figure is seen Fig. 3 (* 3000) and Fig. 4 (* 1000), compares with conventional molybdenum powder (seeing Fig. 1 and Fig. 2), the molybdenum powder pattern rounding of the present embodiment preparation, microscopic appearance is good.
Embodiment 2
Step 1, employing air-flow grind method, and 3000g conventional reduction molybdenum powder is carried out high energy fluid bed head-on collision airflow milling, and rotating speed is 10000r/min, and the processing time is 80min;
Step 2, the 70g polyvinyl alcohol is dissolved in the 1400mL deionized water, is mixed with polyvinyl alcohol water solution;
Step 3, the molybdenum powder after grinding in step 1 is added described in step 2 in polyvinyl alcohol water solution, stir and make slurry;
Step 4, slurry described in step 3 is carried out spray-drying, obtain prilling powder; The intake air temperature of described spray-dired drying tower is 230 ℃, and the air outlet temperature is 150 ℃, and centrifugal atomizing dish rotating speed is 11500rpm;
Step 5, be 800 ℃ of ungrease treatment 4h under the wet hydrogen atmosphere of 40 ℃ at dew point to prilling powder described in step 4, then 1300 ℃ of heat treatment 6h under hydrogen atmosphere, last broken mistake-100～+ 325 eye mesh screens, obtaining granularity is 30 μ m～90 μ m, mobility is 25s/50g, and apparent density is 2.5g/cm
3Spherical molybdenum powder.
The quality purity of the spherical molybdenum powder of the present embodiment preparation is 99.96%, yield rate is 92%, and its shape appearance figure is seen Fig. 5 (* 3000) and Fig. 6 (* 1000), compares with conventional molybdenum powder (seeing Fig. 1 and Fig. 2), the molybdenum powder pattern rounding of the present embodiment preparation, microscopic appearance is good.
Embodiment 3
Step 1, adopting ball-milling method, is ball milling 20min under the condition of 4: 1 in ratio of grinding media to material with 3000g conventional reduction molybdenum powder;
Step 2, the 58g polyvinyl alcohol is dissolved in the 1200mL deionized water, is mixed with polyvinyl alcohol water solution;
Step 3, the molybdenum powder after grinding in step 1 is added described in step 2 in polyvinyl alcohol water solution, stir and make slurry;
Step 4, slurry described in step 3 is carried out spray-drying, obtain prilling powder; The intake air temperature of described spray-dired drying tower is 250 ℃, and the air outlet temperature is 115 ℃, and centrifugal atomizing dish rotating speed is 11000rpm;
Step 5, be 700 ℃ of ungrease treatment 8h under the wet hydrogen atmosphere of 55 ℃ at dew point to prilling powder described in step 4, then 1400 ℃ of heat treatment 4h under hydrogen atmosphere, last broken mistake-100～+ 325 eye mesh screens, obtaining granularity is 20 μ m～90 μ m, mobility is 20s/50g, and apparent density is 3.0g/cm
3Spherical molybdenum powder.
The quality purity of the spherical molybdenum powder of the present embodiment preparation is 99.98%, yield rate is 94%, and its shape appearance figure is seen Fig. 7 (* 3000) and Fig. 8 (* 1500), compares with conventional molybdenum powder (seeing Fig. 1 and Fig. 2), the molybdenum powder pattern rounding of the present embodiment preparation, microscopic appearance is good.
Embodiment 4
Step 1, adopting ball-milling method, is ball milling 100min under the condition of 2: 1 in ratio of grinding media to material with 3000g conventional reduction molybdenum powder;
Step 2, the 45g polyvinyl alcohol is dissolved in the 705mL deionized water, is mixed with polyvinyl alcohol water solution;
Step 3, the molybdenum powder after grinding in step 1 is added described in step 2 in polyvinyl alcohol water solution, stir and make slurry;
Step 4, slurry described in step 3 is carried out spray-drying, obtain prilling powder; The intake air temperature of described spray-dired drying tower is 240 ℃, and the air outlet temperature is 110 ℃, and centrifugal atomizing dish rotating speed is 11500rpm;
Step 5, be 750 ℃ of ungrease treatment 6h under the wet hydrogen atmosphere of 35 ℃ at dew point to prilling powder described in step 4, then 1500 ℃ of heat treatment 2h under hydrogen atmosphere, last broken mistake-100～+ 325 eye mesh screens, obtaining granularity is 20 μ m～90 μ m, mobility is 18s/50g, and apparent density is 3.5g/cm
3Spherical molybdenum powder.
The quality purity of the spherical molybdenum powder of the present embodiment preparation is 99.95%, yield rate is 93%, and its shape appearance figure is seen Fig. 9 (* 3000) and Figure 10 (* 1500), compares with conventional molybdenum powder (seeing Fig. 1 and Fig. 2), the molybdenum powder pattern rounding of the present embodiment preparation, microscopic appearance is good.
Embodiment 5
Step 1, employing air-flow grind method, and 3000g conventional reduction molybdenum powder is carried out high energy fluid bed head-on collision airflow milling, and rotating speed is 8000r/min, and the processing time is 240min;
Step 2, the 150g polyvinyl alcohol is dissolved in the 1850mL deionized water, is mixed with polyvinyl alcohol water solution;
Step 3, the molybdenum powder after grinding in step 1 is added described in step 2 in polyvinyl alcohol water solution, stir and make slurry;
Step 4, slurry described in step 3 is carried out spray-drying, obtain prilling powder; The intake air temperature of described spray-dired drying tower is 230 ℃, and the air outlet temperature is 130 ℃, and centrifugal atomizing dish rotating speed is 12000rpm;
Step 5, be 800 ℃ of ungrease treatment 6h under the wet hydrogen atmosphere of 45 ℃ at dew point to prilling powder described in step 4, then 1450 ℃ of heat treatment 6h under hydrogen atmosphere, last broken mistake-100～+ 325 eye mesh screens, obtaining granularity is 20 μ m～90 μ m, mobility is 16s/50g, and apparent density is 4.0g/cm
3Spherical molybdenum powder.
The quality purity of the spherical molybdenum powder of the present embodiment preparation is 99.95%, yield rate is 92%, and its shape appearance figure is seen Figure 11 (* 3000) and Figure 12 (* 1500), compares with conventional molybdenum powder (seeing Fig. 1 and Fig. 2), the molybdenum powder pattern rounding of the present embodiment preparation, microscopic appearance is good.
Embodiment 6
Step 1, employing air-flow grind method, and 3000g conventional reduction molybdenum powder is carried out high energy fluid bed head-on collision airflow milling, and rotating speed is 15000r/min, and the processing time is 30min;
Step 2, the 90g polyvinyl alcohol is dissolved in the 1000mL deionized water, is mixed with polyvinyl alcohol water solution;
Step 3, the molybdenum powder after grinding in step 1 is added described in step 2 in polyvinyl alcohol water solution, stir and make slurry;
Step 4, slurry described in step 3 is carried out spray-drying, obtain prilling powder; The intake air temperature of described spray-dired drying tower is 230 ℃, and the air outlet temperature is 125 ℃, and centrifugal atomizing dish rotating speed is 12500rpm;
Step 5, be 850 ℃ of ungrease treatment 8h under the wet hydrogen atmosphere of 50 ℃ at dew point to prilling powder described in step 4, then 1500 ℃ of heat treatment 8h under hydrogen atmosphere, last broken mistake-100～+ 325 eye mesh screens, obtaining granularity is 20 μ m～90 μ m, mobility is 15s/50g, and apparent density is 4.5g/cm
3Spherical molybdenum powder.
The quality purity of the spherical molybdenum powder of the present embodiment preparation is 99.97%, yield rate is 90%, and its shape appearance figure is seen Figure 13 (* 3000) and Figure 14 (* 1000), compares with conventional molybdenum powder (seeing Fig. 1 and Fig. 2), the molybdenum powder pattern rounding of the present embodiment preparation, microscopic appearance is good.
The above; it is only preferred embodiment of the present invention; be not that the present invention is done any restriction, every any simple modification, change and equivalent structure of above embodiment being done according to the invention technical spirit changes, and all still belongs in the protection domain of technical solution of the present invention.
Claims (8)
1. a method for preparing spherical molybdenum powder, is characterized in that, the method comprises the following steps:
Step 1, molybdenum powder is ground;
Step 2, preparation polyvinyl alcohol water solution;
Step 3, the molybdenum powder after grinding in step 1 is added described in step 2 in polyvinyl alcohol water solution, stir and make slurry; In described slurry, the mass content of molybdenum powder is 60%～80%, and in described slurry, the polyvinyl alcohol quality is 1.5%～5% of molybdenum powder weight;
Step 4, slurry described in step 3 is carried out spray-drying, obtain prilling powder;
Step 5, prilling powder described in step 4 is first carried out ungrease treatment, then heat-treat, last fragmentation is sieved and is obtained spherical molybdenum powder.
2. a kind of method that prepare spherical molybdenum powder described according to claims 1, is characterized in that, grinds described in step 1 to adopt ball-milling method or air-flow to grind method.
3. a kind of method that prepare spherical molybdenum powder described according to claims 2, is characterized in that, the ratio of grinding media to material of described ball-milling method is 1～4: 1, and Ball-milling Time is 20min～240min; It is high energy fluid bed head-on collision airflow milling that described air-flow grinds method, and rotating speed is 8000rpm～15000rpm, and the processing time is 30min～240min.
4. a kind of method that prepare spherical molybdenum powder described according to claims 1, it is characterized in that, spray-dired intake air temperature described in step 4 is 220 ℃～250 ℃, and the air outlet temperature is 110 ℃～150 ℃, and centrifugal atomizing dish rotating speed is 10500rpm～12500rpm.
5. a kind of method that prepare spherical molybdenum powder described according to claims 1, is characterized in that, the temperature of ungrease treatment described in step 5 is 700 ℃～900 ℃, and the time is 2h～8h, and the atmosphere of ungrease treatment is wet hydrogen.
6. a kind of method that prepare spherical molybdenum powder described according to claims 5, is characterized in that, the dew point of described wet hydrogen is 35 ℃～55 ℃.
7. a kind of method that prepare spherical molybdenum powder described according to claims 1, is characterized in that, heat treated temperature described in step 5 is 1200 ℃～1500 ℃, and the time is 2h～8h, and heat treated atmosphere is hydrogen.
8. a kind of method that prepare spherical molybdenum powder described according to claims 1, is characterized in that, the apparent density of spherical molybdenum powder described in step 5 is 2.0g/cm
3～4.5g/cm
3, mobility 15s/50g～30s/50g, quality purity 〉=99.95%, yield rate 〉=90%.
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| CN105397094A (en) * | 2015-12-23 | 2016-03-16 | 北京矿冶研究总院 | Preparation method of spherical spraying molybdenum powder |
| CN105583403A (en) * | 2016-01-21 | 2016-05-18 | 中核(天津)科技发展有限公司 | Pelletizing method for copper-nickel alloy powder |
| CN106216690A (en) * | 2016-08-24 | 2016-12-14 | 洛阳金鹭硬质合金工具有限公司 | A kind of preparation method of slug type thermal spraying tungsten powder of reuniting |
| CN106636827A (en) * | 2016-12-08 | 2017-05-10 | 苏州长风航空电子有限公司 | Ceramic metallization powder and manufacturing method thereof |
| CN107309434A (en) * | 2017-06-06 | 2017-11-03 | 中国航天空气动力技术研究院 | A kind of preparation method and application of the spherical molybdenum powder of high-purity compact |
| CN107522206A (en) * | 2016-06-21 | 2017-12-29 | 张家港市思杰五金工具有限公司 | The preparation method of conglobation molybdenum silicide powder |
| CN108115147A (en) * | 2017-12-04 | 2018-06-05 | 中国兵器科学研究院宁波分院 | A kind of complete closely knit, the spherical molybdenum powder of high apparent density the preparation method of cold spraying |
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| CN102626784A (en) * | 2012-05-10 | 2012-08-08 | 金堆城钼业股份有限公司 | Method for preparing molybdenum powder for preparing molybdenum end cap of magnetron |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105397094A (en) * | 2015-12-23 | 2016-03-16 | 北京矿冶研究总院 | Preparation method of spherical spraying molybdenum powder |
| CN105583403A (en) * | 2016-01-21 | 2016-05-18 | 中核(天津)科技发展有限公司 | Pelletizing method for copper-nickel alloy powder |
| CN107522206A (en) * | 2016-06-21 | 2017-12-29 | 张家港市思杰五金工具有限公司 | The preparation method of conglobation molybdenum silicide powder |
| CN106216690A (en) * | 2016-08-24 | 2016-12-14 | 洛阳金鹭硬质合金工具有限公司 | A kind of preparation method of slug type thermal spraying tungsten powder of reuniting |
| CN106636827A (en) * | 2016-12-08 | 2017-05-10 | 苏州长风航空电子有限公司 | Ceramic metallization powder and manufacturing method thereof |
| CN107309434A (en) * | 2017-06-06 | 2017-11-03 | 中国航天空气动力技术研究院 | A kind of preparation method and application of the spherical molybdenum powder of high-purity compact |
| CN107309434B (en) * | 2017-06-06 | 2020-06-09 | 中国航天空气动力技术研究院 | Preparation method and application of high-purity compact spherical molybdenum powder |
| CN108115147A (en) * | 2017-12-04 | 2018-06-05 | 中国兵器科学研究院宁波分院 | A kind of complete closely knit, the spherical molybdenum powder of high apparent density the preparation method of cold spraying |
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| CN103170635B (en) | 2015-10-21 |
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