CN101352759A - Method for preparing special type molybdenum powder - Google Patents

Method for preparing special type molybdenum powder Download PDF

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Publication number
CN101352759A
CN101352759A CNA2008101465316A CN200810146531A CN101352759A CN 101352759 A CN101352759 A CN 101352759A CN A2008101465316 A CNA2008101465316 A CN A2008101465316A CN 200810146531 A CN200810146531 A CN 200810146531A CN 101352759 A CN101352759 A CN 101352759A
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China
Prior art keywords
molybdenum powder
granularity
powder
preparing
special
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CNA2008101465316A
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Chinese (zh)
Inventor
陈强
张常乐
冯鹏发
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Jinduicheng Molybdenum Co Ltd
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Jinduicheng Molybdenum Co Ltd
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Priority to CNA2008101465316A priority Critical patent/CN101352759A/en
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Abstract

A method for preparing a special molybdenum powder relates to a method for preparing the molybdenum powder specially used for the industries of thermal spraying and machining as well as pressing fine apparatuses. The powder is characterized in that the preparing process includes the steps as follows: (1) sintering normal molybdenum powder for increasing the granularity; (2) grading the molybdenum powder, the granularity of which is increased; carrying out spheroidisation on the molybdenum powder with approximate granularity by a plasma device, then cooling and collecting the molybdenum powder; (3) reducing the molybdenum powder after being spheroidized, screening, grading and then obtaining the special molybdenum powder. The molybdenum powder prepared by the method of the invention has the advantages of good fluidity, simple technique, high finished product rate and relates to a technique for preparing the special molybdenum powder used in the fields of thermal spraying and pressing fine apparatuses.

Description

A kind of method of producing molybdenum powder special
Technical field
A kind of method of producing molybdenum powder special relates to a kind of method that is used to prepare thermal spraying, mechanical processing industry and accurate device compacting special molybdenum powder.
Background technology
Metal-powder is widely used in fields such as thermal spraying and welding, accurate device compactings.The granularity of powder, mobile most important for its result of use, granularity is excessive, influences coating surface quality and device pressed density; Undersized, it is not good that then spray efficiency lowly reaches the filling capacity of molybdenum powder.The flowability of molybdenum powder is very big to its spraying effect and suppression performance influence, and powder fluidity and its sphericity are closely bound up, and good sphericity is then mobile good, otherwise, mobile poor.Therefore, spraying effect that metal-powder will be obtained and good suppression performance generally need carry out subsequent treatment, improve its granularity mobile and acquisition is suitable.Low-melting-point metal is easier to improve by its granularity of Technology for Heating Processing, sphericity ratio, and refractory metal is malleable microscopic appearance not then.Metal molybdenum has higher high temperature strength, high-wearing feature, favorable conductive thermal conductivity, the lower coefficient of expansion and workability, thereby coating molybdenum powder has a wide range of applications in the parts field of thermal spray.Conventional molybdenum powder grain shape is irregular, does not have flowability, can not use as direct sprayed product, because flowability is not good, green density is lower, thereby need improve its microscopic appearance and improve performance.Technology mist projection granulating commonly used, sintering ball milling then finally makes the finished product molybdenum powder of better performances.Along with the development of technology, the more harsh requirement, particularly physical index of physical and chemical index proposition to molybdenum powder requires less than 20s/50g such as flowability, and pine also has requirement than greater than 3.5g/cm3 to granularity.And the molybdenum powder by atomizing granulating technology preparation, because the limitation of technology self, its flowability, pine all are difficult to reach requirement than, granularity.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provide a kind of and can effectively improve the molybdenum powder microscopic appearance, improve its flowability, increase its loose ratio, granularity suitably, the preparation method of the molybdenum powder special that uses in spraying and other fields of excellent performance.
The objective of the invention is to be achieved through the following technical solutions.
A kind of method of producing molybdenum powder special is characterized in that the step of its preparation process comprises:
(1) conventional molybdenum powder is carried out sintering, increase granularity;
(2) molybdenum powder that increases granularity is carried out classification, the molybdenum powder that granularity is close plasma apparatus spheroidising, cooling is collected;
(3) molybdenum powder reduces after the nodularization, obtains molybdenum powder behind the sieve classification excessively.
A kind of method for preparing molybdenum powder special of the present invention is characterized in that described conventional molybdenum powder being carried out the sintering granulation process, and sintering carries out under the hydrogen shield in Muffle furnace, and temperature is 900~1200 ℃, and the time is 3~6hr.
A kind of method for preparing molybdenum powder special of the present invention is characterized in that at first crossing sieve classification after the molybdenum powder granularity increases, and the molybdenum powder that granularity is close carries out the spheroidising of plasma high temperature, and powder feeding gas, working gas are N 2, powder feeding gas pressure 0.5-0.8MPa, air pressure 0.2-0.5MPa.
A kind of method for preparing molybdenum powder special of the present invention, the operating current that it is characterized in that the plasma spheroidization process is the 300-500 ampere, operating voltage 50-80 volt.
A kind of method for preparing molybdenum powder special of the present invention is characterized in that molybdenum powder after the nodularization reduces processing, and reduction is carried out under the hydrogen shield in Muffle furnace, and temperature is 700~950 ℃, and the time is 5~8hr.
Method production technology of the present invention is easy to control, and is easy and simple to handle, safe, reliable, is suitable for fairly large production.The molybdenum powder of the plasma spheroidization explained hereafter that it adopts is compared with common employing spray-drying, the molybdenum powder of sintered balls grinding process production, and the nodularization rate height of its product particle, apparent density are big, consistency of product, good fluidity.Gained molybdenum powder spraying surface of the work of the present invention can improve its intensity and anti-wear performance, prolongs the service life of workpiece.In addition, gained molybdenum powder particle nodularization degree height of the present invention, good fluidity can significantly improve its suppression performance, can improve green density, reduces sintering energy consumption.Molybdenum powder product good filling property can also be opened up its use at other field, for example fields such as welding, accurate device production.The present invention is intended to by loose sintering, increase conventional molybdenum powder granularity, adopt plasma technology then, the molybdenum powder that granularity is increased carries out spheroidising, improve molybdenum powder particle microscopic appearance, improve its compactness, finally prepare the molybdenum powder special that is used for fields such as thermal spraying, accurate device compacting of excellent performance.
Description of drawings
Fig. 1 produces molybdenum powder special configuration of surface figure for embodiment 1.
Fig. 2 produces molybdenum powder special configuration of surface figure for embodiment 2.
The specific embodiment
A kind of method of producing molybdenum powder special, the step of its preparation process comprises: (1) increases the molybdenum powder granularity with the granulation of conventional molybdenum powder sintering; (2) after the molybdenum powder granularity increases, cross sieve classification, carry out plasma spheroidization, improve the molybdenum powder granule-morphology; (3) cooling of the molybdenum powder of high temperature nodularization is collected, and reduces under Muffle furnace, hydrogen shield, and finished product obtains molybdenum powder special after crossing sieve classification.
Concrete operations are:
(1) with the molybdenum powder is raw material, adopts the molybdenum powder that MP-1 requires in accord with Q/JDC013-2002 standard;
(2) molybdenum powder is carried out sintering under the hydrogen shield in Muffle furnace, temperature is 900~1200 ℃, and the time is 3~6hr;
(3), carry out the spheroidising of plasma high temperature, plasma spheroidization equipment operating current 300-500 ampere, operating voltage 50-80 volt with the molybdenum powder classification of sintering granulation;
(4) the nodularization molybdenum powder is reduced under the hydrogen shield in Muffle furnace, temperature is 700~950 ℃, and the time is 5~8hr;
(5) the molybdenum powder grading system that sieves with reduction obtains molybdenum powder special of the present invention.
The average Fisher particle size of above-mentioned raw materials molybdenum powder is at 2.0~4.0 μ m, and apparent density is 1.0~1.4g/cm 3
The above-mentioned raw materials molybdenum powder carries out the sintering granulation in Muffle furnace, sintering temperature is 900~1200 ℃, and the time is 3~6hr, needs hydrogen shield.
Molybdenum powder after the above-mentioned sintering granulation is crossed sieve classification, dwindles the size distribution interval, and the molybdenum powder that granularity is close carries out the spheroidising of plasma high temperature.
Above-mentioned nodularization molybdenum powder reduces under the hydrogen shield in Muffle furnace, and temperature is 700~950 ℃, and the time is 5~8hr.
The molybdenum powder of the above-mentioned reduction grading system that sieves obtains molybdenum powder special of the present invention.
Embodiment 1
The MP-1 molybdenum powder 2kg that gets accord with Q/JDC013-2002 standard is standby, and its average Fisher particle size is 3.20 μ m, and apparent density is 1.04g/cm 3With the sintering granulation in Muffle furnace, under the hydrogen shield of the molybdenum powder that takes by weighing, sintering temperature is 980 ℃, and the time is 5hr; Molybdenum powder after the sintering granulation is crossed sieve classification, and the molybdenum powder that granularity is close carries out the high temperature spheroidising at the DH-1080 plasma apparatus, 350 amperes of plasma spheroidization equipment operating currents, 70 volts of operating voltages; The nodularization molybdenum powder reduces under the hydrogen shield in Muffle furnace, and temperature is 800 ℃, and the time is 6hr; The molybdenum powder grading system that sieves of reduction obtains molybdenum powder special of the present invention.
The detection index of molybdenum powder special is as follows:
Chemical composition Apparent density (g/cm3) Cross grit number Hall flow velocity (s/50g) Particle size range (μ m)
Mo≥99.20% 4.8 -200~+270 17.6 53~80
Embodiment 2
The MP-1 molybdenum powder 5kg that gets accord with Q/JDC013-2002 standard is standby, and its average Fisher particle size is 3.60 μ m, and apparent density is 1.10g/cm 3With the sintering granulation in Muffle furnace, under the hydrogen shield of the molybdenum powder that takes by weighing, sintering temperature is 1100 ℃, and the time is 6hr; Molybdenum powder after the sintering granulation is crossed sieve classification, and the molybdenum powder that granularity is close carries out the high temperature spheroidising at the DH-1080 plasma apparatus, 400 amperes of plasma spheroidization equipment operating currents, 80 volts of operating voltages; The nodularization molybdenum powder reduces under the hydrogen shield in Muffle furnace, and temperature is 850 ℃, and the time is 8hr; The molybdenum powder grading system that sieves of reduction obtains molybdenum powder special of the present invention.
The detection index of molybdenum powder special is as follows:
Chemical composition Apparent density (g/cm3) Cross grit number Hall flow velocity (s/50g) Particle size range (μ m)
Mo≥99.20% 4.5 -150~+240 13.5 63~100

Claims (5)

1. method of producing molybdenum powder special is characterized in that the step of its preparation process comprises:
(1) conventional molybdenum powder is carried out sintering, increase granularity;
(2) molybdenum powder that increases granularity is carried out classification, the molybdenum powder that granularity is close plasma apparatus spheroidising, cooling is collected;
(3) molybdenum powder reduces after the nodularization, obtains molybdenum powder behind the sieve classification excessively.
2. a kind of method for preparing molybdenum powder special according to claim 1 is characterized in that described conventional molybdenum powder being carried out the sintering granulation process, and sintering carries out under the hydrogen shield in Muffle furnace, and temperature is 900~1200 ℃, and the time is 3~6hr.
3. a kind of method for preparing molybdenum powder special according to claim 1 is characterized in that at first crossing sieve classification after the molybdenum powder granularity increases, and the molybdenum powder that granularity is close carries out the spheroidising of plasma high temperature, and powder feeding gas, working gas are N 2, powder feeding gas pressure 0.5-0.8MPa, air pressure 0.2-0.5MPa.
4. a kind of method for preparing molybdenum powder special according to claim 1, the operating current that it is characterized in that the plasma spheroidization process is the 300-500 ampere, operating voltage 50-80 volt.
5. a kind of method for preparing molybdenum powder special according to claim 1 is characterized in that molybdenum powder after the nodularization reduces processing, and reduction is carried out under the hydrogen shield in Muffle furnace, and temperature is 700~950 ℃, and the time is 5~8hr.
CNA2008101465316A 2008-09-02 2008-09-02 Method for preparing special type molybdenum powder Pending CN101352759A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101642811B (en) * 2009-06-29 2011-01-05 金堆城钼业股份有限公司 Preparation method of molybdenum product with heavy single weight
CN102294490A (en) * 2011-08-03 2011-12-28 成都虹波实业股份有限公司 Crude molybdenum powder preparing method
CN103157801A (en) * 2013-04-12 2013-06-19 金堆城钼业股份有限公司 Equipment of restraining spheroidized molybdenum powder of direct current plasma temperature field and method
CN103691933A (en) * 2013-12-18 2014-04-02 浙江帕特尼触头有限公司 Metal powder granulation method
CN103797153A (en) * 2011-09-13 2014-05-14 株式会社爱发科 Mo-W target and method for manufacturing same
CN104070175A (en) * 2014-06-30 2014-10-01 西安建筑科技大学 Method for producing metal molybdenum spherical fine powder or superfine powder
CN106512849A (en) * 2016-10-09 2017-03-22 四川恒创博联科技有限责任公司 Micro powder spheroidizing system
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
CN108237231A (en) * 2016-12-26 2018-07-03 龙岩紫荆创新研究院 A kind of manufacturing method of spherical shape molybdenum powder

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101642811B (en) * 2009-06-29 2011-01-05 金堆城钼业股份有限公司 Preparation method of molybdenum product with heavy single weight
CN102294490A (en) * 2011-08-03 2011-12-28 成都虹波实业股份有限公司 Crude molybdenum powder preparing method
CN102294490B (en) * 2011-08-03 2016-06-29 成都虹波实业股份有限公司 A kind of method producing thick molybdenum powder
CN103797153A (en) * 2011-09-13 2014-05-14 株式会社爱发科 Mo-W target and method for manufacturing same
CN103157801B (en) * 2013-04-12 2015-06-10 金堆城钼业股份有限公司 Equipment of restraining spheroidized molybdenum powder of direct current plasma temperature field and method
CN103157801A (en) * 2013-04-12 2013-06-19 金堆城钼业股份有限公司 Equipment of restraining spheroidized molybdenum powder of direct current plasma temperature field and method
CN103691933A (en) * 2013-12-18 2014-04-02 浙江帕特尼触头有限公司 Metal powder granulation method
CN104070175A (en) * 2014-06-30 2014-10-01 西安建筑科技大学 Method for producing metal molybdenum spherical fine powder or superfine powder
CN106512849A (en) * 2016-10-09 2017-03-22 四川恒创博联科技有限责任公司 Micro powder spheroidizing system
CN106512849B (en) * 2016-10-09 2019-06-07 四川恒创博联科技有限责任公司 A kind of system of nodularization fine powder
CN108237231A (en) * 2016-12-26 2018-07-03 龙岩紫荆创新研究院 A kind of manufacturing method of spherical shape molybdenum powder
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

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