CN102615288A - Method for preparing spherical metal molybdenum particles for cold spraying - Google Patents
Method for preparing spherical metal molybdenum particles for cold spraying Download PDFInfo
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- CN102615288A CN102615288A CN201210082935XA CN201210082935A CN102615288A CN 102615288 A CN102615288 A CN 102615288A CN 201210082935X A CN201210082935X A CN 201210082935XA CN 201210082935 A CN201210082935 A CN 201210082935A CN 102615288 A CN102615288 A CN 102615288A
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Abstract
The invention relates to a method for preparing spherical metal molybdenum particles for cold spraying. The method includes the steps: mixing raw molybdenum powder with deionized water, polyethylene glycol and polyvinyl alcohol in a certain proportion; performing high-energy ball-milling mixing; performing centrifugal spray granulation; sintering dried particles at high temperature in atmosphere protection; and finally, crushing the sintered materials to obtain the spherical molybdenum powder particles in uniform particle size distribution in a classified manner. The method has the advantages that according to the performance requirements of cold spraying technology on high flowability and centralized particle size distribution of the raw powder, molybdenum powder with the small particle size is nodulized by means of combining centrifugal spraying with high-temperature sintering, flowability of the powder is improved, and particle size distribution of the nodulized particles tends to be uniform by means of secondary classification and is centralized to range from 20 micrometers to 40 micrometers applicable to the cold spraying technology.
Description
Technical field
The present invention relates to the cold spraying field, mainly is the preparation method of a kind of cold spraying with spherical metal molybdenum particle.
Background technology
Cold spraying is to use the high-speed gas nozzle that powder particle is quickened to spray to a kind of solid-state spraying coating process title of substrate, and in this technology, metal particle produces plastic deformation and under impacting, solidifies.Term " cold spraying " is meant the technology that required processing temperature is relatively low, and is general more much lower than the fusing point of sprayed on material.
Although it is early stage that the metal material cold spraying can be traced back to for 20th century to the theory on the substrate,, the applicability of this technology just displayed with application machine research institute in the Russian Academy Of Sciences theory that is positioned at Novosibirisk up to the eighties in 20th century.Because the metal dust bonding force that arrives on substrate and the deposited material makes its formation solid-state; Therefore; The characteristic of cold spraying deposition is very unique; So being highly suitable for, it precipitates tradition and advanced material widely on polytype baseplate material, particularly for the responsive non-traditional application of technological temperature.Some characteristics of cold spraying comprise that the intensive sediment oxygen content of its formation is extremely low, do not have residual-tensile stress, and particulate increases, and territory, recrystallization zone and phase change are arranged.Some materials even nano level grain refinement can occur.Owing to have these attributes, so cold spraying is particularly suitable for precipitating various senior and to temperature-sensitive material.Today, cold spraying is applied to various industrial fields more and more, comprises space flight, the energy and military industry.
Under current state; Cold spraying is applied to various industries more and more to slow down the corrosion of sensitive material, for example: WC-Co (tungsten-cobalt carbide) deposition of the bus duct manufacturing on magnadure, surface reparation, sputtering target manufacturing, the heating glass, hard chrome replacement coating, the electricity of fillet surface are led with thermal conductance coating, brazing and are connect preparation and thermal barrier and NiCrAlY adhesive coating deposition.In a lot of these types were used, it is more economical that cold spraying seems, because it can really eliminate or reduce manufacturing step.
Use for other, cold spraying only is unique feasibility solution, the particularly applied more and more in non-traditional.When environment and health and safety rules were more and more stricter, people were increasing with a kind of more green alternative of hiding the hobby of cold spraying.
Along with development of technology, estimate the cold spraying application with continuing to expand in the more non-traditional application, for example photoelectricity, wind energy, medical treatment and building field.In photovoltaic applications, cold spraying can be used for complicated conduction type solar cell manufacturing.Wind power generation can utilize cold spraying to strengthen the surface property of the element of high polymer matrix synthetic manufacturing.
At medical field, cold spraying can spray to a kind of famous biocompatible material hydroxyapatite (HAP) on a large amount of substrates effectively, but can not influence the integrality of HAP simultaneously.The architect can utilize cold spraying on any metal or ceramic substrate, to create infinite metal pattern attractive in appearance.
Because depositing temperature is low, cold spraying can be imbedded microsensor and functional coating thereof on the surface, to form intelligence structure.These structures can provide the real time information relevant with material property or environmental condition.A lot of newborn enterprises are just focusing on to bridge, electrical network, wind turbine, aircraft, automobile, steamer, pipeline and construction equipment provide induction, database and are administering and the preanalysis solution.Depend on the future of cold spraying when advanced material deposited to various substrate thermal loss and capital is near minimum.This is the following direction of this technology of definition and the foundation stone of opportunity.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned existence, and the preparation method of a kind of cold spraying with spherical metal molybdenum particle is provided.
The objective of the invention is to accomplish, comprise the steps: through following technical scheme
1), the raw material molybdenum powder is mixed with a certain proportion of deionized water, polyethylene glycol and polyvinyl alcohol, and carry out high-energy ball milling and mix;
2), the slip that obtains after the ball mill mixing is carried out centrifugal spray granulation and dry;
3), dried particle is carried out atmosphere protection and high temperature sintering;
4), the material behind the sintering is carried out fragmentation;
5), the molybdenum particle after the fragmentation is carried out the spherical molybdenum powder particle that classification can obtain even particle size distribution.
As preferably, the particle size range of described raw material molybdenum powder is 3～5 μ m.
As preferably, described proportion scale is molybdenum powder (wt%) 79.3～45.5%, deionized water content (wt%) 20～50%, polyethyleneglycol content (wt%) 0.5～3%, polyvinyl alcohol (wt%) 0.2～1.5%.
As preferably, the ratio of grinding media to material of described high-energy ball milling is 2～6: 1, and the ball milling time is 3～6 hours.
As preferably, it is N that described sintering process adopts the atmosphere of protection
2+ H
2, and volume fraction is respectively N
2Be 75%, H
2Be 25%.
As preferably, described high temperature sintering temperature is 1000～1300 ℃, and its sintering time is 1～4 hour.
As preferably, described breaking method is that the cylinder circulation is broken.
As preferably, described stage division is vibration multi-stage screening level.
Beneficial effect of the present invention is: to high fluidity, the size distribution relatively concentrated performance requirement of cold spray technique to material powder; Through using centrifugal spray to combine the method for high temperature sintering; Make the less molybdenum powder generation nodularization process of granularity; Improve the flowability of powder, the method through the secondary classification makes that the size distribution of particle is tending towards homogenising after the nodularization, concentrates between 20～40 microns that cold spray technique is suitable for.
The specific embodiment
Specify the specific embodiment of the present invention through embodiment below.
A kind of cold spraying provided by the invention is with the preparation method of spherical metal molybdenum particle; This method comprises the steps: the raw material molybdenum powder is mixed with a certain proportion of deionized water, polyethylene glycol and polyvinyl alcohol; Carrying out high-energy ball milling mixes; Carry out centrifugal spray granulation, dried particle is carried out the atmosphere protection high temperature sintering, at last the material behind the sintering is carried out the spherical molybdenum powder particle of fragmentation, classification acquisition even particle size distribution.
Preparation method according to the spherical molybdenum particle of manufacturing cold spraying provided by the invention; The effect of said a certain proportion of deionized water, polyethylene glycol and polyvinyl alcohol is in the process of atomizing granulation; For the drop that contains molybdenum powder provides necessary surface tension, make the drop nodularization in the process of drying that contains molybdenum powder.Concrete ratio is a deionized water content (wt%) 20～50%, polyethyleneglycol content (wt%) 0.5～3%, polyvinyl alcohol (wt%) 0.2～1.5%.
Method according to the spherical molybdenum particle of manufacturing cold spraying provided by the invention; Can adopt molybdenum powder well known in the art as raw material; As concrete embodiment; Said proportion scale is molybdenum powder (wt%) 79.3～45.5%, ionized water content (wt%) 20～50%, polyethyleneglycol content (wt%) 0.5～3%, polyvinyl alcohol (wt%) 0.2～1.5%.As a kind of concrete embodiment, the particle size range of said molybdenum powder is 3～5 μ m.
Said when adopting high-energy ball milling method to mix the molybdenum mixed powder, ratio of grinding media to material is 2～6: 1, and the ball milling time is 3～6 hours, and the molybdenum mixed powder is mixed, and the granularity to molybdenum powder further reduces simultaneously.
The slip that obtains behind the ball milling is carried out the centrifugal atomizing granulation, 180～350 ℃ of drying machine inlet temperatures, atomizing disk rotational frequency 150～250Hz obtains the spherical molybdenum particle of D90 size distribution at 20～50 μ m.
The purpose of said sintering process is to make the molybdenum particle of acquisition improve intensity, guarantees in the process of using, to keep its spherical pattern and have higher flowability, and it is N that sintering process adopts protective atmosphere
2+ H
2, its volume fraction is respectively N
2Be 75%, H
2Be 25%, adopt high temperature molybdenum-wound furnace to carry out sintering, sintering temperature is 1000～1300 ℃, and sintering time is 1～4 hour.
It is block that molybdenum mixed powder behind the sintering becomes, and the breaking method of employing is that the cylinder circulation is broken, and the cylinder velocity of rotation is 50～160 rev/mins.
Said stage division is vibration multi-stage screening level, and the molybdenum particle after the fragmentation is carried out multiple fractionation, and it is 250 orders, 325 orders, 400 orders, 500 orders that the order of concrete classifying screen is counted proportioning.
Embodiment 1:
The preparation slip: will contain 79.3 molybdenum powders of weight portion, 20 deionized waters of weight portion, the polyethylene glycol of 0.5 weight portion, the polyvinyl alcohol of 0.2 weight portion, 6: 1 ratios of grinding media to material were mixed 270 minutes.
Atomizing granulation parameter: 200 ℃ of baking temperatures, atomizing disk rotational frequency 150Hz.
Sintering: earlier with the powder after the granulation, in the molybdenum filament sintering furnace, carry out sintering, be incubated 240 minutes with 1000 ℃.
Broken: 50 rev/mins of drum rotation speeds.
Classification: it is 250 orders, 325 orders, 400 orders, 500 orders that the order of classifying screen is counted proportioning.
Embodiment 2:
The preparation slip: will contain 67.5 molybdenum powders of weight portion, 30 deionized waters of weight portion, the polyethylene glycol of 1.5 weight portions, the polyvinyl alcohol of 1 weight portion, 4: 1 ratios of grinding media to material were mixed 240 minutes.
Atomizing granulation parameter: 250 ℃ of baking temperatures, atomizing disk rotational frequency 200Hz.
Sintering: earlier with the powder after the granulation, in the molybdenum filament sintering furnace, carry out sintering, be incubated 180 minutes with 1150 ℃.
Broken: 80 rev/mins of drum rotation speeds.
Classification: it is 250 orders, 325 orders, 400 orders, 500 orders that the order of classifying screen is counted proportioning.
Embodiment 3:
The preparation slip: will contain 45.5 molybdenum powders of weight portion, 50 deionized waters of weight portion, the polyethylene glycol of 3 weight portions, the polyvinyl alcohol of 1.5 weight portions, 2: 1 ratios of grinding media to material were mixed 360 minutes.
Atomizing granulation parameter: 350 ℃ of baking temperatures, atomizing disk rotational frequency 250Hz.
Sintering: earlier with the powder after the granulation, in the molybdenum filament sintering furnace, carry out sintering, be incubated 90 minutes with 1300 ℃.
Broken: 120 rev/mins of drum rotation speeds.
Classification: it is 250 orders, 325 orders, 400 orders, 500 orders that the order of classifying screen is counted proportioning.
Claims (8)
1. a cold spraying is characterized in that: comprise the steps: with the preparation method of spherical metal molybdenum particle
1), the raw material molybdenum powder is mixed with a certain proportion of deionized water, polyethylene glycol and polyvinyl alcohol, and carry out high-energy ball milling and mix;
2), the slip that obtains after the ball mill mixing is carried out centrifugal spray granulation and dry;
3), dried particle is carried out atmosphere protection and high temperature sintering;
4), the material behind the sintering is carried out fragmentation;
5), the molybdenum particle after the fragmentation is carried out the spherical molybdenum powder particle that classification can obtain even particle size distribution.
2. cold spraying according to claim 1 is characterized in that with the preparation method of spherical metal molybdenum particle: the particle size range of described raw material molybdenum powder is 3～5 μ m.
3. cold spraying according to claim 1 is with the preparation method of spherical metal molybdenum particle; It is characterized in that: described proportion scale is molybdenum powder (wt%) 79.3～45.5%, deionized water content (wt%) 20～50%; Polyethyleneglycol content (wt%) 0.5～3%, polyvinyl alcohol (wt%) 0.2～1.5%.
4. cold spraying according to claim 1 is characterized in that with the preparation method of spherical metal molybdenum particle: the ratio of grinding media to material of described high-energy ball milling is 2～6: 1, and the ball milling time is 3～6 hours.
5. cold spraying according to claim 1 is characterized in that with the preparation method of spherical metal molybdenum particle: it is N that described sintering process adopts the atmosphere of protection
2+ H
2, and percent by volume is respectively N
2Be 75%, H
2Be 25%.
6. cold spraying according to claim 1 is characterized in that with the preparation method of spherical metal molybdenum particle: described high temperature sintering temperature is 1000～1300 ℃, and its sintering time is 1～4 hour.
7. cold spraying according to claim 1 is characterized in that with the preparation method of spherical metal molybdenum particle: described breaking method is that the cylinder circulation is broken.
8. cold spraying according to claim 1 is characterized in that with the preparation method of spherical metal molybdenum particle: described stage division is vibration multi-stage screening level.
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Cited By (8)
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| CN103042205A (en) * | 2012-12-18 | 2013-04-17 | 株洲弘通硬质合金有限公司 | Method for preparing hollow refractory metal and alloy spraying powder |
| CN103170635A (en) * | 2013-03-29 | 2013-06-26 | 金堆城钼业股份有限公司 | Method for preparing spherical molybdenum powder |
| WO2016000004A2 (en) | 2014-07-03 | 2016-01-07 | Plansee Se | Method for producing a layer |
| 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 |
| 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 |
| CN110607526A (en) * | 2019-09-06 | 2019-12-24 | 中国兵器科学研究院宁波分院 | Method for preparing nickel-based wide-temperature-range self-lubricating coating with nano structure by cold spraying |
| CN113617493A (en) * | 2021-06-29 | 2021-11-09 | 南京信彩科技有限公司 | Raw material grinding method for preparing color ink |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110607526B (en) * | 2019-09-06 | 2022-07-05 | 中国兵器科学研究院宁波分院 | Method for preparing nickel-based wide-temperature-range self-lubricating coating with nano structure by cold spraying |
| CN113617493A (en) * | 2021-06-29 | 2021-11-09 | 南京信彩科技有限公司 | Raw material grinding method for preparing color ink |
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Application publication date: 20120801 |