CN108637241A - A kind of mining industry survey acquisition tool alloy powder and preparation method thereof - Google Patents

A kind of mining industry survey acquisition tool alloy powder and preparation method thereof Download PDF

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Publication number
CN108637241A
CN108637241A CN201810466199.5A CN201810466199A CN108637241A CN 108637241 A CN108637241 A CN 108637241A CN 201810466199 A CN201810466199 A CN 201810466199A CN 108637241 A CN108637241 A CN 108637241A
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China
Prior art keywords
alloy
powder
alloy powder
preparation
alloy melt
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CN201810466199.5A
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Inventor
逯峙
邱敬文
王辉
贾明灿
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Shaanxi Platinum Drilling Machinery Co., Ltd.
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Shaanxi Kaine Bao De New Material Co Ltd
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Priority to CN201810466199.5A priority Critical patent/CN108637241A/en
Publication of CN108637241A publication Critical patent/CN108637241A/en
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    • B22F1/0003
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/008Ferrous alloys, e.g. steel alloys containing tin
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/16Ferrous alloys, e.g. steel alloys containing copper
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0824Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
    • B22F2009/0828Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid with water

Abstract

A kind of mining industry survey acquisition tool alloy powder of present invention offer and preparation method thereof, according to mass percent meter, which includes following components:68~86% Fe, 13~25% Cu, 1~7% Sn, surplus be inevitable impurity;Preparation method includes:By in raw material Fe and Cu carry out melting under inert gas protection, after being heated to preset heating temperature and held for some time, the Sn added in raw material is stirred, and obtains alloy melt;Alloy melt is poured out, and is under inert gas protection smashed the alloy melt of whereabouts using high pressure water flow, atomized powder after cooling;Atomized powder is restored successively, is dried and crushing operation, alloy powder is obtained.Metallic element type contained in the alloy powder that preparation method provided by the invention is prepared is few, ratio is easy to control, and performance is stablized, and ingredient and tissue are more uniform, impurity is few, grain size is tiny, to make its material property more stablize.

Description

A kind of mining industry survey acquisition tool alloy powder and preparation method thereof
Technical field
The present invention relates to powder metallurgical technologies, and in particular to a kind of mining industry survey acquisition tool alloy powder and its Preparation method.
Background technology
The mining industry survey acquisition tool on superhard equipment for the fields such as digging up mine and exploring, be with diamond be cutting or Material is drilled, and by means of the tool with definite shape, performance and purposes made of alloy powder, the overwhelming majority is using mixing Metal powder or pre-alloyed powder are binder, are manufactured with diamond particles mixing hot pressed sintering.
Currently, the alloy powder in mining industry survey acquisition tool mostly uses greatly ultra-fine Fe-Cu alloy powders, but as master It wants the iron powder of one of raw material, quality to be difficult to control, is easy to introduce the impurity such as oxygen in preparation process, and its in preparation process Granularity is also difficult to control;And another raw material copper powder generally use electrolytic method production, usually there is uneven components, granularity are big The defects of.
Since there are drawbacks described above so that alloy powder in sintering to the wetability of superhard material such as diamond not It is enough, inlay that dynamics is small, and mechanical performance is bad, cause the cutting of tool and drilling results poor, reduce tool and equipment Efficiency and service life.Stabilization and the development in the fields such as mining and exploration when used for a long time, can be seriously being hindered, therefore urgent The proportioning and technology of preparing to changing traditional alloy powder are needed, to improve the above problem.
Invention content
A kind of mining industry survey acquisition tool alloy powder of offer of the embodiment of the present invention and preparation method thereof, it is existing to solve The defects of mining industry survey acquisition tool alloy powder existence component is uneven in technology, impurity is more, granularity is big and lead to alloy Powder is inadequate to the wetability of superhard material in sintering, inlays the problems such as dynamics is small, mechanical performance is bad.
In a first aspect, the embodiment of the present invention provides a kind of mining industry survey acquisition tool alloy powder, according to quality percentage Than meter, the alloy powder includes following components:68~86% Fe, 13~25% Cu, 1~7% Sn, surplus be can not The impurity avoided.
As the preferred embodiment of first aspect present invention, according to mass percent meter, the alloy powder includes with the following group Point:73~80% Fe, 17~22% Cu, 3~5% Sn, surplus be inevitable impurity.
Second aspect, the embodiment of the present invention provide a kind of preparation method of mining industry survey acquisition tool alloy powder, packet It includes:
By in raw material Fe and Cu carry out melting under inert gas protection, be heated to preset heating temperature and keep the temperature one After fixing time, the Sn added in raw material is stirred, and obtains alloy melt;Wherein, according to mass percent meter, the original Material include 63~86% Fe, 13~25% Cu, 1~7% Sn and inevitable impurity;
The alloy melt is poured out, and utilizes high pressure water flow by the alloy melt of whereabouts under inert gas protection It smashes, atomized powder after cooling;
The atomized powder is restored successively, is dried and crushing operation, alloy powder is obtained.
As the preferred embodiment of second aspect of the present invention, in the step of obtaining alloy melt, according to mass percent meter, The raw material include following component:73~80% Fe, 17~22% Cu, 3~5% Sn, surplus is inevitable Impurity.
As the preferred embodiment of second aspect of the present invention, in the step of obtaining alloy melt, it is according to 1000 DEG C or less 30 DEG C/min, the Fe in the heating rate heating raw materials that 1000 DEG C or more are 10 DEG C/min and Cu to 1430-1490 DEG C, heat preservation 30~after forty minutes be added raw material in Sn and be stirred.
As the preferred embodiment of second aspect of the present invention, the atomized powder the step of in, the water of the high pressure water flow Pressure is 65~125MPa;The high pressure water flow is sprayed by atomizer, wherein the convolution angle of the atomizer jet stream Ranging from 0.18~0.72rad.
As the preferred embodiment of second aspect of the present invention, the atomized powder the step of in, the stream of the high pressure water flow The fast velocity ratio with the alloy melt is 2:1~10:1;Cooling velocity after the alloy melt is crashed to pieces is 104~106K/ s。
As the preferred embodiment of second aspect of the present invention, in the step of obtaining alloy powder, the atomized powder drying The reducing gas for using hydrogen and argon gas to be mixed to form again afterwards is restored, and keeps the temperature 4~6 hours at 580~720 DEG C.
As the preferred embodiment of second aspect of the present invention, the volume ratio of hydrogen is 70~80% in the reducing gas.
As the preferred embodiment of second aspect of the present invention, the average grain diameter of the alloy powder is 2~4 μm.
Mining industry survey acquisition tool alloy powder provided in an embodiment of the present invention, by original alloy powder group subpackage On the basis of Cu and Fe, and a certain proportion of Sn is added to carry out the regulation and control of alloy compositions, performance is stablized.Meanwhile it preparing In the preparation method of the alloy powder, alloy powder is prepared using vacuum induction melting and high-pressure water atomization technology, is substantially dropped The low grain size of alloy powder, ingredient is more uniform, while so that alloy powder granularity is more concentrated, significantly reduces inside raw material The introducing of impurity also eliminates most of oxygen by the reduction process in later stage, increases substantially the sintered mechanical performance of tool, The efficiency and service life of tool and equipment are effectively increased, and reduces production cost.
Description of the drawings
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for For those of ordinary skill in the art, without creative efforts, other are can also be obtained according to these attached drawings Attached drawing.
Fig. 1 is a kind of preparation method flow of mining industry survey acquisition tool alloy powder provided in an embodiment of the present invention Figure;
Fig. 2 is that a kind of preparation method of mining industry survey acquisition tool alloy powder provided in an embodiment of the present invention is prepared Alloy powder X-ray diffractogram;
Fig. 3 is that a kind of preparation method of mining industry survey acquisition tool alloy powder provided in an embodiment of the present invention is prepared Alloy powder SEM figure;
Fig. 4 is that a kind of preparation method of mining industry survey acquisition tool alloy powder provided in an embodiment of the present invention is prepared Alloy powder energy spectrum analysis figure.
Specific implementation mode
In order to enable those skilled in the art to better understand the solution of the present invention, below in conjunction in the embodiment of the present invention Attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only The embodiment of a part of the invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill people The every other embodiment that member is obtained without making creative work should all belong to the model that the present invention protects It encloses.
The embodiment of the invention discloses a kind of mining industry survey acquisition tool alloy powders to close according to mass percent meter Bronze end includes following components:68~86% Fe, 13~25% Cu, 1~7% Sn, surplus be inevitable impurity.
Include Cu elements and Fe elements in the present embodiment, in the component, Cu therein can be used as good Heat Conduction Material, Its heat conductivility is much better than other common metals, therefore can make the mining industry survey acquisition tool finally prepared by the alloy powder With good heat dissipation performance;And Fe therein can have preferable intersolubility under certain proportioning with Cu so that alloy powder While heat conductivility is not remarkably decreased, and the high-strength characteristic of Fe is had both, production cost can also be reduced.
In addition, it is original include both metallic elements of Fe and Cu on the basis of, and add Sn elements, contained metal member Plain type is less, and content ratio is easy to control, and the addition of Sn elements can significantly improve the mechanicalness of alloy powder material Energy and wearability.
In addition, in the component, the mass percent that the mass percent of Fe is 68~86%, Cu is 13~25%, Sn's Mass percent is only 1~7%, and three kinds of elements can be made to be in each other and dissolved each other in range, ensure the performance of alloy powder material Stablize and uniform.In the present embodiment, impurity is generally the nonmetalloids such as C, P or O.
The performance of mining industry survey acquisition tool alloy powder provided in an embodiment of the present invention is stablized, and when used for a long time may be used Cutting and the drilling results for effectively improving tool, to further increase the efficiency and service life of tool and equipment.
On the basis of the above embodiments, alloy powder includes following components:73~80% Fe, 17~22% Cu, 3 ~5% Sn, surplus are inevitable impurity.
In the present embodiment, by the quality backup of Fe, Cu and Sn these three elements than be respectively set to 73~80%, 17~ 22%, 3~5% when, can further keep more good effect of dissolving each other between element contained by alloy powder, avoid ingredient as possible The uniform performance of tissue odds caused by segregation is unstable.
The embodiment of the present invention provides a kind of preparation method of mining industry survey acquisition tool alloy powder, which can To be completed using intermediate frequency furnace, intermediate frequency furnace includes mainly working chamber, spray chamber and reduction furnace.It, should shown in referring to Fig.1 Method includes the following steps:
S1, by raw material Fe and Cu carry out melting under inert gas protection, be heated to preset heating temperature and protect After a certain period of time, the Sn added in raw material is stirred temperature, obtains alloy melt.
In the present embodiment, according to mass percent meter, the raw material include 68~86% Fe, 13~25% Cu, 1~7% Sn and inevitable impurity, impurity be generally the nonmetalloids such as C, P or O.
Include Cu elements and Fe elements in the component, Cu therein can be used as good Heat Conduction Material, heat conductivility It is much better than other common metals, therefore can makes to be had by the mining industry survey acquisition tool that the alloy powder is finally prepared good Heat dissipation performance;And Fe therein can have preferable intersolubility under certain proportioning with Cu so that the heat conductivility of alloy powder does not have While being decreased significantly, and the high-strength characteristic of Fe is had both, production cost can also be reduced.
In addition, it is original include both metallic elements of Fe and Cu on the basis of, and add Sn elements, contained metal member Plain type is less, and content ratio is easy to control, and the addition of Sn elements can significantly improve the mechanicalness of alloy powder material Energy and wearability.
In addition, in the component, the mass percent that the mass percent of Fe is 68~86%, Cu is 13~25%, Sn's Mass percent is only 1~7%, and three kinds of elements can be made to be in each other and dissolved each other in range, ensure the performance of alloy powder material Stablize and uniform.
Melting is carried out by being fitted into working chamber according to the high-purity ingot iron and copper ingot of aforementioned proportion.Before melting, to reduce The oxygen content for the alloy powder finally prepared is re-filled with inert gas after first being vacuumized to working chamber and spray chamber and protects Shield.Specifically, working chamber and spray chamber are evacuated to when vacuum degree is 20Pa and are stopped, being then shut off evacuating valve, then beat Charging valve is opened, is finally filled with the high-purity argon gas that purity is 99.9% to working chamber and spray chamber so that working chamber and spray chamber Vacuum degree stop when reaching 1 atmospheric pressure.
Start intermediate frequency furnace and the high-purity ingot iron and copper ingot of addition be subjected to vacuum induction melting under inert gas protection, To above-mentioned raw material continuous heating to preset heating temperature in working chamber, make its abundant melting.After held for some time, then lead to It crosses micro- feeding device in intermediate frequency furnace and high-purity block tin is added, be then stirred using agitating device, when stirring Between generally 30 minutes, finally obtain alloy melt.In whipping process, in order to avoid impurity content is excessively high in alloy melt, Deslagging device may be used to remove one layer of melt of alloy melt outer surface.
S2, alloy melt is poured out, and is under inert gas protection smashed the alloy melt of whereabouts using high pressure water flow, Atomized powder after cooling.
In the step, by above-mentioned steps melting formed alloy melt from be first poured into working chamber atomization tundish in. There is heating device outside atomization tundish, there is catheter at bottom centre position, there is heating plug and thermocouple inside catheter, The heating device inside and outside heating to atomization tundish simultaneously outside plug and thermocouple combination is heated, to prevent mist Alloy melt is cooling in advance when change and blocks catheter, ensures being smoothed out for atomization process.Then, it is atomized adding in tundish Hot plug and thermocouple pop-up, make alloy melt be poured into spray chamber, start to be atomized.
Atomizer is equipped in spray chamber, while alloy melt falls at the top of spray chamber, in the protection of inert gas Under be atomized the high pressure water flow that nozzle ejects and smash, the alloy liquid droplet of formation disperses and is quickly cooled down to solidify out into atomized powder End eventually falls into spray chamber bottom.
In the process, the high pressure water flow of atomization is larger to the impact energy of alloy melt, is crushed to alloy melt Effect is notable so that and alloy melt can obtain larger surface energy, can make the alloy powder finally prepared very tiny in this way, And superfines proportion is very high.
In addition, due to the rapid cooling effect of high pressure water flow, the aluminium alloy that alloy melt is formed after being smashed by high pressure water flow Drop cooling velocity is ultrafast, and setting rate is much larger than the setting rate that its balance is spread, therefore crystal grain has little time according to phasor rule Rule is balanced diffusion and solidification, and just quick refrigeration solidifies so that in the alloy powder finally prepared when few equilibrium freezings Second phase and other balance phases, promote the degree of supersaturation of the alloying element in solid solution and solid solubility to greatly improve, to later stage system Standby material has great solid solution strengthening effect, contributes to the performance for being obviously improved material.
Raw material pass through being quickly cooled down in induction melting, mechanical agitation and atomization process so that alloying component is come not And there is being segregated just quick solidification, therefore microstructure segregation and component segregation are greatly reduced, help to significantly improve material composition With the uniformity of tissue, ensure the stabilization of the alloy powder material performance finally prepared.
Further, it is atomized the solidification of the alloy liquid droplet formed after the pattern of powder is smashed with alloy melt by high pressure water flow Time is related, and the setting time of alloy liquid droplet can pass through alloy melt flow velocity, the structure of atomizer, atomization hydraulic pressure, alloy Melt superheat degree etc. is because usually regulating and controlling.Wherein, alloy melt flow velocity is controlled by the diameter of catheter, and diameter is bigger, unit The flow velocity of time is bigger, and the setting time of such alloy liquid droplet is longer, and the atomized powder grain size of preparation will be larger, ball Shape degree is more preferable;Atomizer uses the close coupling circumferential weld nozzle in confined type nozzle, can not only effectively prevent alloy melt Adhesion spout also substantially increases the impact energy of atomization flow, improves nebulization efficiency, increases fine powder recovery rate, but meeting The pattern degree of irregularity of atomized powder is set to increase;The size of hydraulic pressure can be adjusted by force (forcing) pump when atomization, when improving atomization Hydraulic pressure help to improve fine powder recovery rate, but the pattern degree of irregularity of atomized powder will increase;The alloy melt degree of superheat can It combines and is controlled by adjusting heating power and the accurate thermometric of thermocouple, alloy melt can be increased by properly increasing the degree of superheat Mobility helps to obtain fine powder and spherical powder.
It is controlled or regulated by above-mentioned, it is easier to so that atomized powder is presented different patterns, such as subsphaeroidal, elliposoidal, Irregular pattern etc., to meet the requirement of different user.
S3, atomized powder is restored successively, is dried and crushing operation, obtaining alloy powder.
In the step, the atomized powder for falling into spray chamber bottom obtained in above-mentioned steps is collected, is re-fed into also Deoxidation and reduction is carried out in former stove, is then crushed after vacuum drying, you can obtains final alloy powder.By alloy powder mistake After sieving and testing and analyzing, vacuum packaging storage.
On the basis of the above embodiments, in step sl, according to mass percent meter, raw material include following component: 73~80% Fe, 17~22% Cu, 3~5% Sn, surplus be inevitable impurity.
In the present embodiment, by the quality backup of Fe, Cu and Sn these three elements than be respectively set to 73~80%, 17~ 22%, 3~5% when, can further keep more good effect of dissolving each other between element contained by alloy powder, avoid ingredient as possible The uniform performance of tissue odds caused by segregation is unstable.
On the basis of the above embodiments, in step sl, according to 1000 DEG C or less for 30 DEG C/min, 1000 DEG C or more be Fe in the heating rate heating raw materials of 10 DEG C/min and Cu to 1430-1490 DEG C, heat preservation 30~former material is added after forty minutes Sn in material is simultaneously stirred.
It,, can using the Fe and Cu in higher heating speed heating raw materials at 1000 DEG C or less in the present embodiment Smelting time is greatly shortened, production efficiency is significantly improved, reduces production cost.And temperature is when rising to 1000 DEG C or more, using compared with Low heating speed, the homogenization of the metal bath advantageously formed, melt have sufficient time convection current, to reduce ingredient Segregation, but too low heating speed can significantly reduce production efficiency again, increase production cost, therefore use 10 component segregations, Heating speed is more moderate.
Finally the Fe and Cu metal baths formed are heated in above-mentioned interval range and keep the temperature a period of time, are then added again Enter Sn, it is ensured that melt has more sufficient convection current, keeps ingredient more uniform.It should be noted that when Fe contents are relatively low, most Whole heating temperature can be lower, and soaking time can also shorten, and when Fe contents are higher, final heating temperature is then wanted High, soaking time also will be more long.Certainly, it if the quality requirements of the alloy powder to finally shaping are less high, can also drop Its low heating temperature, to reduce production cost.
On the basis of the above embodiments, in step s 2, the hydraulic pressure of high pressure water flow is 65~125MPa;High pressure water flow by Atomizer is sprayed, wherein convolution angle ranging from 0.18~0.72rad of atomizer jet stream.
In the present embodiment, due to including Fe in component so that have larger carry when the ratio of viscosities fine copper of the alloy melt of formation Height, therefore higher atomization hydraulic pressure should be used.It is more suitable using the hydraulic pressure within the scope of this, it both can guarantee the smooth of atomization process Implement, and can preferably control production cost, because production cost can be significantly improved using larger hydraulic pressure.
On the basis of the above embodiments, in step s 2, the velocity ratio of the flow velocity of high pressure water flow and alloy melt is 2:1 ~10:1;Cooling velocity after alloy melt is crashed to pieces is 104~106K/s。
In the present embodiment, due to including Fe in component so that the viscosity of the alloy melt of formation is larger, the stream of high pressure water flow When speed and the flow velocity of alloy melt use above-mentioned velocity ratio, the impact force of flow is relatively suitable, it can be ensured that atomization process It is smoothed out, can also there is preferable fine powder recovery rate so that product quality is stablized, and additional production cost will not be also increased.
Meanwhile within this range, it is ensured that the cooling velocity for the molten drop that alloy melt is formed after being crashed to pieces is 104~ 106K/s helps to ensure that atomization process is stablized and carries out.
On the basis of the above embodiments, in step s3, hydrogen and argon gas is used to mix shape again after atomized powder drying At reducing gas restored, and keep the temperature 4~6 hours at 580~720 DEG C.
In the present embodiment, due in component include Fe, and the binding ability of Fe and oxygen ratio Cu be eager to excel, it is therefore desirable to using compared with High temperature is restored.Under the reducing gas that atomized powder is mixed to form under above-mentioned temperature range by hydrogen and argon gas into Row reduction, when reduction temperature is higher, the recovery time is longer, can restore more atomized powder, and can make atomized powder quilt Fully reduction.Certainly, if the oxygen content requirement to the alloy powder finally shaped is less high, its reduction temperature can also be reduced Or shorten the recovery time, to reduce production cost.
Reducing gas is mixed to form using relatively stable argon gas and hydrogen, can be reduced when hydrogen carries out restoring operation Danger level improves processing safety.On the basis of the above embodiments, in step s3, in reducing gas hydrogen volume Ratio is 70~80%.
In the present embodiment, due to including Fe in component, and the binding ability of Fe and oxygen ratio Cu is eager to excel, therefore in reducing gas The volume ratio of hydrogen wants higher.When the volume ratio of hydrogen is aforementioned proportion range in reducing gas, it ensure that fully While restoring atomized powder, so that the dosage of hydrogen is reached minimum as possible, reduce production cost, also significantly improve safety Property.
On the basis of the above embodiments, the average grain diameter of alloy powder is 2~4 μm.
In the present embodiment, by the setting of above-mentioned atomization process and some parameters, high pressure water flow rushes alloy melt Hit that energy is larger, it is notable to the fragmentation of alloy melt so that alloy melt can obtain larger surface energy, can make in this way The alloy powder finally prepared is very tiny, and superfines proportion is very high.
In addition, due to the rapid cooling effect of high pressure water flow, the aluminium alloy that alloy melt is formed after being smashed by high pressure water flow Drop cooling velocity is ultrafast, and crystal grain, which has little time to grow up, just have been solidified, therefore can make the crystalline substance inside the alloy powder finally prepared Grain is finer, and the average grain diameter of alloy powder is 2~4 μm.Since alloy melt obtains very high degree of supercooling, greatly improve Material nucleation rate, crystal grain, which has little time to grow up, just to be solidified, therefore alloy powder granularity substantially reduces while, internal crystalline substance Grain tissue is finer, this helps to greatly promote the performance for preparing material in the later stage.
With reference to shown in Fig. 2, Fig. 2 is the preparation of the mining industry survey acquisition tool alloy powder provided based on above-described embodiment The X-ray diffractogram for the alloy powder that method is prepared, the wherein average grain diameter of the alloy powder are 3 μm.It is shown in the figure Diffraction maximum represent the alloy phase in alloy powder.It will be apparent from this figure that it is entirely ferrous alloy phase, no any impurity It mutually generates, illustrates that alloy powder degree of purity prepared by the present invention is higher, quality is preferable.In addition, peak value is higher to illustrate alloy powder Crystallization degree is higher or the number of crystals of the alloy is more.
With reference to shown in Fig. 3, Fig. 3 is the preparation of the mining industry survey acquisition tool alloy powder provided based on above-described embodiment The SEM for the alloy powder that method is prepared schemes, and wherein the average grain diameter of the alloy powder is between 2~4 μm.It can from the figure To find out, while ensure that alloy powder material quality, the grain size of alloy powder is very tiny, and average grain diameter is in 2 Between~4 μm, and particle size distribution is extremely concentrated, and is illustrated that atomization process when prepared by alloy powder is more successful, is realized The fine of powder diameter, contributes to mechanical property and wearability that later stage tools production is greatly improved.
With reference to shown in Fig. 4, Fig. 4 is the preparation of the mining industry survey acquisition tool alloy powder provided based on above-described embodiment The energy spectrum analysis figure for the alloy powder that method is prepared, the wherein average grain diameter of the alloy powder are 3 μm.In the figure, diffraction maximum Peak value where abscissa display elements type, ordinate reflects the energy spectral intensity of the element.It will be apparent from this figure that should Essential element in alloy powder is Fe, Cu and Sn, and the elements such as only minimal amount of O and P exist, and degree of purity is higher.Further In conjunction with Fig. 2 it is found that these minimal amount of impurity elements do not form compound, it is present in alloy powder in the form of solid solution Portion, thus have certain solid solution strengthening effect to powder organization.
The present invention is described in further detail with reference to specific preferred embodiment, but does not therefore limit this hair Bright protection domain.
Embodiment one
According to mass ratio meter, high-purity ingot iron of 25% high-purity copper ingot, 7% high purity metal tin and surplus is weighed, then High-purity ingot iron and high-purity copper ingot are fitted into the working chamber of intermediate frequency furnace, then working chamber and spray chamber are evacuated to vacuum degree For 20Pa, the air pressure for being filled with high-purity argon gas to working chamber and spray chamber that purity is 99.9% reaches 1 atmospheric pressure.
Start intermediate frequency furnace, working chamber is made to be warming up to 1430 DEG C, wherein 1000 DEG C or less heating rates are 30 DEG C/min, 1000 DEG C or more heating rates are 10 DEG C/min, then keep the temperature 40 minutes.Then it is added using micro- feeding device high-purity Tin slab, then alloy melt is stirred 30 minutes with agitating device.In whipping process, using deslagging device by alloy melt appearance One layer of melt in face is removed.
Alloy melt is poured into atomization tundish, the heating plug being then atomized in tundish and thermocouple pop-up make Alloy melt is poured into spray chamber, starts to be atomized.While alloy melt falls at the top of spray chamber, it is atomized what nozzle ejected High pressure water flow smashes, and the alloy liquid droplet of formation disperses and be quickly cooled down to solidify out into atomized powder, eventually falls into spray chamber bottom. Wherein, the hydraulic pressure of atomization process mesohigh flow is 110MPa, and the flow velocity of high pressure water flow and the velocity ratio of alloy melt are 5:1, Cooling velocity after alloy melt is crashed to pieces is 105~106K/s, the convolution angle ranging from 0.27 of atomizer jet stream~ 0.36rad。
Atomized powder is collected, and is sent into reduction furnace progress deoxidation and reduction processing, reducing gas be by hydrogen and The reducing gas that nitrogen is mixed to form, hydrogen volume ratio are 70%, and reduction temperature is 580 DEG C, soaking time 4 hours.
It is crushed after vacuum drying, after being sieved and testing and analyzing, vacuum packaging storage.
Embodiment two
According to mass ratio meter, high-purity ingot iron of 19% high-purity copper ingot, 4% high purity metal tin and surplus is weighed, then High-purity ingot iron and high-purity copper ingot are fitted into the working chamber of intermediate frequency furnace, then working chamber and spray chamber are evacuated to vacuum degree For 20Pa, the air pressure for being filled with high-purity argon gas to working chamber and spray chamber that purity is 99.9% reaches 1 atmospheric pressure.
Start intermediate frequency furnace, working chamber is made to be warming up to 1450 DEG C, wherein 1000 DEG C or less heating rates are 30 DEG C/min, 1000 DEG C or more heating rates are 10 DEG C/min, then keep the temperature 35 minutes.Then it is added using micro- feeding device high-purity Tin slab, then alloy melt is stirred 30 minutes with agitating device.In whipping process, using deslagging device by alloy melt appearance One layer of melt in face is removed.
Alloy melt is poured into atomization tundish, the heating plug being then atomized in tundish and thermocouple pop-up make Alloy melt is poured into spray chamber, starts to be atomized.While alloy melt falls at the top of spray chamber, it is atomized what nozzle ejected High pressure water flow smashes, and the alloy liquid droplet of formation disperses and be quickly cooled down to solidify out into atomized powder, eventually falls into spray chamber bottom. Wherein, the hydraulic pressure of atomization process mesohigh flow is 125MPa, and the flow velocity of high pressure water flow and the velocity ratio of alloy melt are 7:1, Cooling velocity after alloy melt is crashed to pieces is 106K/s, convolution angle ranging from 0.18~0.27rad of atomizer jet stream.
Atomized powder is collected, and is sent into reduction furnace progress deoxidation and reduction processing, reducing gas be by hydrogen and The reducing gas that nitrogen is mixed to form, hydrogen volume ratio are 75%, and reduction temperature is 630 DEG C, soaking time 5 hours.
It is crushed after vacuum drying, after being sieved and testing and analyzing, vacuum packaging storage.
Embodiment three
According to mass ratio meter, high-purity ingot iron of 13% high-purity copper ingot, 1% high purity metal tin and surplus is weighed, then High-purity ingot iron and high-purity copper ingot are fitted into the working chamber of intermediate frequency furnace, then working chamber and spray chamber are evacuated to vacuum degree For 20Pa, the air pressure for being filled with high-purity argon gas to working chamber and spray chamber that purity is 99.9% reaches 1 atmospheric pressure.
Start intermediate frequency furnace, working chamber is made to be warming up to 1470 DEG C, wherein 1000 DEG C or less heating rates are 30 DEG C/min, 1000 DEG C or more heating rates are 10 DEG C/min, then keep the temperature 30 minutes.Then it is added using micro- feeding device high-purity Tin slab, then alloy melt is stirred 30 minutes with agitating device.In whipping process, using deslagging device by alloy melt appearance One layer of melt in face is removed.
Alloy melt is poured into atomization tundish, the heating plug being then atomized in tundish and thermocouple pop-up make Alloy melt is poured into spray chamber, starts to be atomized.While alloy melt falls at the top of spray chamber, it is atomized what nozzle ejected High pressure water flow smashes, and the alloy liquid droplet of formation disperses and be quickly cooled down to solidify out into atomized powder, eventually falls into spray chamber bottom. Wherein, the hydraulic pressure of atomization process mesohigh flow is 90MPa, and the flow velocity of high pressure water flow and the velocity ratio of alloy melt are 4:1, it closes Cooling velocity after golden melt is crashed to pieces is 104~105K/s, the convolution angle ranging from 0.36 of atomizer jet stream~ 0.45rad。
Atomized powder is collected, and is sent into reduction furnace progress deoxidation and reduction processing, reducing gas be by hydrogen and The reducing gas that nitrogen is mixed to form, hydrogen volume ratio are 75%, and reduction temperature is 680 DEG C, soaking time 6 hours.
It is crushed after vacuum drying, after being sieved and testing and analyzing, vacuum packaging storage.
Example IV
According to mass ratio meter, high-purity ingot iron of 16% high-purity copper ingot, 2% high purity metal tin and surplus is weighed, then High-purity ingot iron and high-purity copper ingot are fitted into the working chamber of intermediate frequency furnace, then working chamber and spray chamber are evacuated to vacuum degree For 20Pa, the air pressure for being filled with high-purity argon gas to working chamber and spray chamber that purity is 99.9% reaches 1 atmospheric pressure.
Start intermediate frequency furnace, working chamber is made to be warming up to 1490 DEG C, wherein 1000 DEG C or less heating rates are 30 DEG C/min, 1000 DEG C or more heating rates are 10 DEG C/min, then keep the temperature 30 minutes.Then it is added using micro- feeding device high-purity Tin slab, then alloy melt is stirred 30 minutes with agitating device.In whipping process, using deslagging device by alloy melt appearance One layer of melt in face is removed.
Alloy melt is poured into atomization tundish, the heating plug being then atomized in tundish and thermocouple pop-up make Alloy melt is poured into spray chamber, starts to be atomized.While alloy melt falls at the top of spray chamber, it is atomized what nozzle ejected High pressure water flow smashes, and the alloy liquid droplet of formation disperses and be quickly cooled down to solidify out into atomized powder, eventually falls into spray chamber bottom. Wherein, the hydraulic pressure of atomization process mesohigh flow is 65MPa, and the flow velocity of high pressure water flow and the velocity ratio of alloy melt are 2:1, it closes Cooling velocity after golden melt is crashed to pieces is 104K/s, convolution angle ranging from 0.58~0.72rad of atomizer jet stream.
Atomized powder is collected, and is sent into reduction furnace progress deoxidation and reduction processing, reducing gas be by hydrogen and The reducing gas that nitrogen is mixed to form, hydrogen volume ratio are 75%, and reduction temperature is 720 DEG C, soaking time 4 hours.
It is crushed after vacuum drying, after being sieved and testing and analyzing, vacuum packaging storage.
Embodiment five
According to mass ratio meter, high-purity ingot iron of 22% high-purity copper ingot, 4% high purity metal tin and surplus is weighed, then High-purity ingot iron and high-purity copper ingot are fitted into the working chamber of intermediate frequency furnace, then working chamber and spray chamber are evacuated to vacuum degree For 20Pa, the air pressure for being filled with high-purity argon gas to working chamber and spray chamber that purity is 99.9% reaches 1 atmospheric pressure.
Start intermediate frequency furnace, working chamber is made to be warming up to 1450 DEG C, wherein 1000 DEG C or less heating rates are 30 DEG C/min, 1000 DEG C or more heating rates are 10 DEG C/min, then keep the temperature 35 minutes.Then it is added using micro- feeding device high-purity Tin slab, then alloy melt is stirred 30 minutes with agitating device.In whipping process, using deslagging device by alloy melt appearance One layer of melt in face is removed.
Alloy melt is poured into atomization tundish, the heating plug being then atomized in tundish and thermocouple pop-up make Alloy melt is poured into spray chamber, starts to be atomized.While alloy melt falls at the top of spray chamber, it is atomized what nozzle ejected High pressure water flow smashes, and the alloy liquid droplet of formation disperses and be quickly cooled down to solidify out into atomized powder, eventually falls into spray chamber bottom. Wherein, the hydraulic pressure of atomization process mesohigh flow is 80MPa, and the flow velocity of high pressure water flow and the velocity ratio of alloy melt are 3:1, it closes Cooling velocity after golden melt is crashed to pieces is 104~105K/s, the convolution angle ranging from 0.45 of atomizer jet stream~ 0.58rad。
Atomized powder is collected, and is sent into reduction furnace progress deoxidation and reduction processing, reducing gas be by hydrogen and The reducing gas that nitrogen is mixed to form, hydrogen volume ratio are 70%, and reduction temperature is 650 DEG C, soaking time 5 hours.
It is crushed after vacuum drying, after being sieved and testing and analyzing, vacuum packaging storage.
It should be noted that for the embodiment of the above method, for simple description, therefore it is all expressed as a series of Combination of actions, but those skilled in the art should understand that, the present invention is not limited by the described action sequence.Secondly, Those skilled in the art should also know that embodiment described in this description belongs to preferred embodiment, involved action It is not necessarily essential to the invention.
In the above embodiment of the present invention, all emphasizes particularly on different fields to the description of each embodiment, do not have in some embodiment The part of detailed description may refer to the associated description of other embodiment.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of mining industry survey acquisition tool alloy powder, which is characterized in that according to mass percent meter, the alloy powder Including following components:68~86% Fe, 13~25% Cu, 1~7% Sn, surplus be inevitable impurity.
2. mining industry survey acquisition tool alloy powder according to claim 1, which is characterized in that according to mass percent Meter, the alloy powder includes following components:73~80% Fe, 17~22% Cu, 3~5% Sn, surplus be can not keep away The impurity exempted from.
3. a kind of preparation method of mining industry survey acquisition tool alloy powder, which is characterized in that including:
By in raw material Fe and Cu carry out melting under inert gas protection, be heated to preset heating temperature and keep the temperature one timing Between after, the Sn added in raw material is stirred, and obtains alloy melt;Wherein, according to mass percent meter, the raw material Including 68~86% Fe, 13~25% Cu, 1~7% Sn and inevitable impurity;
The alloy melt is poured out, and is under inert gas protection hit the alloy melt of whereabouts using high pressure water flow It is broken, atomized powder after cooling;
The atomized powder is restored successively, is dried and crushing operation, alloy powder is obtained.
4. preparation method according to claim 3, which is characterized in that in the step of obtaining alloy melt, according to quality Percentages, the raw material include following component:73~80% Fe, 17~22% Cu, 3~5% Sn, surplus be not Evitable impurity.
5. preparation method according to claim 3, which is characterized in that in the step of obtaining alloy melt, according to 1000 DEG C or less be 30 DEG C/min, the Fe in the heating rate heating raw materials that 1000 DEG C or more are 10 DEG C/min and Cu to 1430- 1490 DEG C, heat preservation 30~after forty minutes be added raw material in Sn and be stirred.
6. preparation method according to claim 3, which is characterized in that in the atomized powder the step of, the high pressure The hydraulic pressure of flow is 65~125MPa;The high pressure water flow is sprayed by atomizer, wherein the atomizer jet stream Angle of circling round ranging from 0.18~0.72rad.
7. preparation method according to claim 3, which is characterized in that in the atomized powder the step of, the high pressure The velocity ratio of the flow velocity of flow and the alloy melt is 2:1~10:1;Cooling velocity after the alloy melt is crashed to pieces is 104~106K/s。
8. preparation method according to claim 3, which is characterized in that in the step of obtaining alloy powder, the atomization The reducing gas for using hydrogen and argon gas to be mixed to form again after powder drying is restored, and 4~6 are kept the temperature at 580~720 DEG C Hour.
9. preparation method according to claim 8, which is characterized in that the volume ratio of hydrogen is 70 in the reducing gas ~80%.
10. according to claim 3~9 any one of them preparation method, which is characterized in that the average grain diameter of the alloy powder It is 2~4 μm.
CN201810466199.5A 2018-05-15 2018-05-15 A kind of mining industry survey acquisition tool alloy powder and preparation method thereof Pending CN108637241A (en)

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