CN105710380A - Aluminum-contained metal printing powder and preparation method thereof - Google Patents

Aluminum-contained metal printing powder and preparation method thereof Download PDF

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Publication number
CN105710380A
CN105710380A CN201610231510.9A CN201610231510A CN105710380A CN 105710380 A CN105710380 A CN 105710380A CN 201610231510 A CN201610231510 A CN 201610231510A CN 105710380 A CN105710380 A CN 105710380A
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powder
preparation
prints
aluminiferous metals
ball
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杨金文
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Material Technology Innovations Ltd
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Material Technology Innovations Ltd
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    • 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
    • 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
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C26/00Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • 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
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/041Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
    • 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
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C26/00Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • C22C2026/002Carbon nanotubes

Abstract

The invention discloses aluminum-contained metal printing powder and a preparation method thereof. The preparation method includes the following steps that an intermetallic compound block is prepared, specifically, aluminum powder, carbon nano tubes and a process control agent are mixed and then placed in a ball-milling blender, and the ball-milled mixture is subjected to cold-press molding to obtain the intermetallic compound block; and all raw materials and the intermetallic compound block are mixed according to the alloy raw material ratio of the aluminum-contained metal printing powder, and the mixture is smelted and atomized to obtain the aluminum-contained metal printing powder. By means of the preparation method, the problem that after the carbon nano tubes are added to the alloy materials, the alloy materials and a matrix can not get good wettability is solved; and besides, the carbon nano tubes are evenly distributed in the metal powder, so that the good abrasion resistance and long fatigue life are achieved.

Description

Aluminiferous metals prints powder and preparation method thereof
Technical field
The present invention relates to 3D printing technique field, particularly relate to a kind of aluminiferous metals and print powder and preparation method thereof.
Background technology
In recent years, 3D printing technique develops owing to can be directly produced complicated shape part rapidly, is applied in fields such as Aero-Space, hygiene medical treatment, automobile, art, buildings.3D prints and requires the features such as metal dust good sphericity, narrow particle size distribution (particle size distribution is between 15~53 μm), low, the good fluidity of oxygen content.Research emphasis present both at home and abroad is substantially on guarantee metal dust sphericity and oxygen content in power, test for the metal parts after molding is relatively fewer, generally can do Part Surface Roughness, density and stretching experiment, these performances can be met preferably after 3D prints, but when being by the testing fatigue of part, the general requirement being all extremely difficult to be correlated with, compared with forge piece, its fatigue life is all relatively poor, this is because enough internal stress can be produced in print procedure, the fatigue life of part is fatal by this.
The technology of current comparative maturity is to adopt aerosolization, plasma atomization and rotary electrode method carry out the production of spherical powder, its major product is for educating, medical treatment and space industry, part at printing shaping, under the premise that intensity and other performances reach requirement, its wear-resisting and fatigue behaviour is difficult to arrive expection requirement, compare with traditional casting and forged material, its wearability and fatigue life all differ greatly, its main cause is derived from two aspects: the first is in 3D print procedure, the rate of cooling of part is very fast, there is bigger internal stress, even if the later stage has carried out internal stress annealing, inside parts still can retain substantial amounts of internal stress, it two be the formation of hard phase second phase particles is need certain forming core and grow up the time, but in 3D print procedure, thawing and the solidification of metal all complete in very short time, and the temperature in print procedure can not be completely secured the temperature range grown up at second phase particles forming core, moreover the temperature of part can be reduced to relatively low temperature in a short period of time.
The material that current 3D prints seldom adds the trace element that wearability and fatigue behaviour is favourable, even if there is a small amount of trace element also because the internal stress of accumulation cannot be completely eliminated and make all to can not get its wearability of metal parts after 3D prints and fatigue life ensureing in 3D print procedure.
In order to generate the equally distributed Second Phase Particle of disperse in the alloy, general alloy is add C element to form the carbides such as MC, M23C6, but improves C content and cause that the fragility of material increases, be unfavorable for the combination property of material.Also have by adding CNT, but the CNT problem with the wettability between matrix material can not be solved, which results in the reduction of material function in use or disappearance.
Metal parts after 3D printing goes for good mechanical performance needs complicated postprocessing working procedures, and this adds manufacturing cost to a certain extent.
Summary of the invention
Based on this, it is an object of the invention to provide a kind of preparation method that can improve aluminiferous metals printing powder wearability and anti-fatigue performance.
Concrete technical scheme is as follows:
The preparation method that a kind of aluminiferous metals prints powder, comprises the steps:
The preparation of intermetallic compound composite block:
Being placed in ball grinding stirring machine by the mixing of aluminium powder, CNT and process control agent, the technological parameter of ball milling is: control ratio of grinding media to material is 5-25:1, and rotating speed is 700-1300r/min, and Ball-milling Time is 60-180min, and milling atmosphere is noble gas;Mixture after ball milling, through cold moudling, obtains described intermetallic compound composite block;
The addition of described CNT is the 1-20wt% of described aluminium powder consumption, and the addition of described process control agent is the 1-5wt% of described aluminium powder consumption;
The alloy raw material proportioning printing powder by described aluminiferous metals mixes each raw material and described intermetallic compound composite block, and the addition of described intermetallic compound composite block is the 1-20% that described aluminiferous metals prints powder gross mass;Then carry out melting, atomization, obtain described aluminiferous metals and print powder.
Wherein in some embodiments, described process control agent is ethanol and/or sodium stearate.
Wherein in some embodiments, described process control agent is mass ratio is ethanol and the sodium stearate of 1:1.
Wherein in some embodiments, the diameter of described CNT is 20-40nm, and length is 5-30 μm.
Wherein in some embodiments, in described aluminium powder, the weight/mass percentage composition of aluminium element is more than 99.5wt%.
Wherein in some embodiments, the technological parameter of described ball milling is: control ratio of grinding media to material is 10-20:1, and rotating speed is 900-1300r/min, and Ball-milling Time is 60-120min.
It is a further object of the present invention to provide a kind of wearability and the good aluminiferous metals of anti-fatigue performance prints powder.
Concrete technical scheme is as follows:
The aluminiferous metals that above-mentioned preparation method prepares prints powder.
Wherein in some embodiments, described aluminiferous metals prints the alloy of powder and consists of Ti6Al4V or ALSi10Mg.
Wherein in some embodiments, described aluminiferous metals prints the oxygen content of powder less than 1200ppm, and less than 53 μm powder occupation rates are 50-70wt%.
Principles of the invention and advantage are as follows:
The preparation method of the present invention overcomes in alloy material adds after CNT, it is impossible to the problem obtaining good wettability with matrix, and enables to CNT and be uniformly distributed in metal dust, and then obtains good anti-wear performance and good fatigue life.
1. the high speed ball milling of CNT and aluminium powder ensure that CNT and aluminum define intermetallic compound, and in fusion process, CNT is not exposed in hot environment, it is ensured that CNT not being melted in follow-up fusion process;
2. the preparation method of the present invention ensure that CNT will not by a large amount of scaling loss in high temperature alloy liquid, ensure that and last alloy powder can contain substantial amounts of CNT, CNT prints in powder printing becomes metallic element as the fine particle of even dispersion powder, can play reinforced metal part machinery performance and abrasion and fatigue behaviour at aluminiferous metals;
3. adopting the preparation method of the present invention to obtain aluminiferous metals powder and carry out the post processing of routine after printing, the product obtained all can obtain good anti-wear performance and good fatigue life, meets the requirement of conventional mechanical performance test.
Detailed description of the invention
By the following examples the application is further elaborated.
Embodiment 1
A kind of aluminiferous metals prints powder, and alloy consists of AlSi10Mg, and its preparation method comprises the steps:
(1) it it is 70 μm by D50, aluminum content is that the aluminium powder of 99.5wt% is as raw material, aluminium powder adds CNT, its content is the 5wt% of aluminium powder, its length is 5-15 μm, diameter is 20-25nm, batch mixing is carried out according to aforementioned proportion, adding procedure controlling agent (is specially sodium stearate), the content of process control agent is the 2% of content of aluminium powder, by aluminum powder, CNT and process control agent are mixed into raw material, weight is 2kg, above-mentioned raw material is carried out ball-milling treatment, nodularization medium is stainless steel ball, its ratio of grinding media to material is 10:1, ball-milling treatment is carried out under argon gas is protected, ball milling speed is 900r/min, Ball-milling Time is 60min, powder good for ball milling is carried out cold pressing treatment and obtains intermetallic compound composite block.
(2) according to the ratio requirement of AlSi10Mg alloy, intermetallic compound composite block obtained above is carried out proportioning with other raw materials, the ratio that wherein intermetallic compound composite block accounts in raw material is 3%, adopt heating in vacuum technology that raw material is carried out melting, aerosolization technology is adopted to be prepared, the temperature controlling gas in atomization process is 500 DEG C, atomizing pressure is 1MPa, air velocity is that the ratio 8:1 of 500m/s and gas flow and fluid flow is to control whole atomization process, the aluminiferous metals obtained is printed powder (AlSi10Mg) carry out sieving and batch mixing, test relevant parameter, the particle size distribution of such as metal dust, oxygen content in powder, and with not adding CNT and adopting the metal dust that identical device and technology obtain to carry out 3D printing, SLS technology is all adopted to print, obtain stretching standard component, carry out stretching experiment after the annealing process, test its intensity, the result obtained is as follows:
It can be seen from the above results that tensile strength and yield strength at the AlSi10Mg alloy added after CNT have lifting.
Embodiment 2:
A kind of aluminiferous metals prints powder, and alloy consists of AlSi10Mg, and its preparation method comprises the steps:
(1) it it is 100 μm by D50, aluminum content is that the aluminium powder of 99.8wt% is as raw material, aluminium powder adds CNT, its content is the 15wt% of aluminium powder, its length is 20-30 μm, diameter is 25-30nm, batch mixing is carried out according to aforementioned proportion, adding procedure controlling agent (is specially ethanol), the content of process control agent is the 5wt% of content of aluminium powder, by aluminum powder, CNT and process control agent are mixed into raw material, weight is 5kg, above-mentioned raw material is carried out ball-milling treatment, nodularization medium is stainless steel ball, its ratio of grinding media to material is 15:1, ball-milling treatment is carried out under argon gas is protected, ball milling speed is 1000r/min, Ball-milling Time is 120min, powder good for ball milling is carried out cold pressing treatment and obtains intermetallic compound composite block.
(2) according to the ratio requirement of AlSi10Mg alloy, intermetallic compound composite block obtained above is carried out proportioning with other raw materials, the ratio that wherein intermetallic compound composite block accounts in raw material is 10wt%, adopt heating in vacuum technology that raw material is carried out melting, aerosolization technology is adopted to be prepared, atomization process controls the temperature 550 DEG C of gas, atomizing pressure 1.5MPa, the ratio 10:1 of air velocity 450m/s and gas flow and fluid flow controls whole atomization process, the aluminiferous metals obtained is printed powder (AlSi10Mg) carry out sieving and batch mixing, test relevant parameter, the particle size distribution of such as metal dust, oxygen content in powder, and with not adding CNT and adopting the metal dust that identical device and technology obtain to carry out 3D printing, SLS technology is all adopted to print, obtain stretching standard component, carry out stretching experiment after the annealing process, test its intensity, the result obtained is as follows:
It can be seen from the above results that tensile strength and yield strength at the AlSi10Mg alloy added after CNT have lifting.
Embodiment 3:
A kind of aluminiferous metals prints powder, and alloy consists of AlSi10Mg, and its preparation method comprises the steps:
(1) it it is 100 μm by D50, aluminum content is that the aluminium powder of 99.8wt% is as raw material, aluminium powder adds CNT, its content is the 15wt% of aluminium powder, its length is 20-30 μm, diameter is 25-30nm, batch mixing is carried out according to aforementioned proportion, adding procedure controlling agent (is specially ethanol and sodium stearate that mass ratio is 1:1), the content of process control agent is the 5wt% of content of aluminium powder, by aluminum powder, CNT and process control agent are mixed into raw material, weight is 5kg, above-mentioned raw material is carried out ball-milling treatment, nodularization medium is stainless steel ball, its ratio of grinding media to material is 15:1, ball-milling treatment is carried out under argon gas is protected, ball milling speed is 1000r/min, Ball-milling Time is 100min, powder good for ball milling is carried out cold pressing treatment and obtains intermetallic compound composite block.
(2) according to the ratio requirement of AlSi10Mg alloy, intermetallic compound composite block obtained above is carried out proportioning with other raw materials, the ratio that wherein intermetallic compound composite block accounts in raw material is 10wt%, adopt heating in vacuum technology that raw material is carried out melting, aerosolization technology is adopted to be prepared, atomization process controls the temperature 580 DEG C of gas, atomizing pressure 2MPa, the ratio 9:1 of air velocity 480m/s and gas flow and fluid flow controls whole atomization process, the aluminiferous metals obtained is printed powder (AlSi10Mg) carry out sieving and batch mixing, test relevant parameter, the particle size distribution of such as metal dust, oxygen content in powder, and with not adding CNT and adopting the metal dust that identical device and technology obtain to carry out 3D printing, SLS technology is all adopted to print, obtain stretching standard component, carry out stretching experiment after the annealing process, test its intensity, the result obtained is as follows:
It can be seen from the above results that tensile strength and yield strength at the AlSi10Mg alloy added after CNT have lifting.
Embodiment 4:
A kind of aluminiferous metals prints powder, and alloy consists of Ti6Al4V, and its preparation method comprises the steps:
(1) it it is 130 μm by D50, aluminum content is that the aluminium powder of 99.8wt% is as raw material, aluminium powder adds CNT, its content is the 20wt% of aluminium powder, its length is 15-30 μm, diameter is 25-40nm, batch mixing is carried out according to aforementioned proportion, adding procedure controlling agent (is specially ethanol and sodium stearate that mass ratio is 1:1), the content of process control agent is the 5wt% of content of aluminium powder, by aluminum powder, CNT and process control agent are mixed into raw material, weight is 5kg, above-mentioned raw material is carried out ball-milling treatment, nodularization medium is stainless steel ball, its ratio of grinding media to material is 20:1, ball-milling treatment is carried out under argon gas is protected, ball milling speed is 1300r/min, Ball-milling Time is 120min, powder good for ball milling is carried out cold pressing treatment and obtains intermetallic compound composite block.
(2) according to the ratio requirement of Ti6Al4V alloy, intermetallic compound composite block obtained above is carried out proportioning with other raw materials, the ratio that wherein intermetallic compound composite block accounts in raw material is 20wt%, adopt heating in vacuum technology that raw material is carried out melting, aerosolization technology is adopted to be prepared, atomization process controls the temperature 700 DEG C of gas, atomizing pressure 2.1MPa, the ratio 7:1 of air velocity 480m/s and gas flow and fluid flow controls whole atomization process, the aluminiferous metals obtained is printed powder (Ti6Al4V) carry out sieving and batch mixing, test relevant parameter, the particle size distribution of such as metal dust, oxygen content in powder, and with not adding CNT and adopting the metal dust that identical device and technology obtain to carry out 3D printing, SLS technology is all adopted to print, obtain stretching standard component, carry out stretching experiment after the annealing process, test its intensity, the result obtained is as follows:
It can be seen from the above results that tensile strength and yield strength at the Ti6Al4V alloy added after CNT have lifting.
Sample after printing is carried out wear test, and experimental result is as follows:
Can be seen that its anti-wear performance is greatly improved by upper table.
Carrying out fatigue experiment with PLG-100 HF fatigue testing machine after finished product after printing is carried out grinding and polishing process, experimental result is as shown in the table:
Test result indicate that, being added to by CNT in alloy, the fatigue behaviour of alloy there has also been very big lifting.
The present invention is not limited only to single or a kind metal dust, identical method can be adopted to carry out interpolation and the powder process of CNT for the alloy containing aluminium element, for 3D metallic print aspect, can effectively carry heavy alloyed properties, be conducive to alloy application in 3D printing technique.
Each technical characteristic of embodiment described above can combine arbitrarily, for making description succinct, the all possible combination of each technical characteristic in above-described embodiment is not all described, but, as long as the combination of these technical characteristics is absent from contradiction, all it is considered to be the scope that this specification is recorded.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes comparatively concrete and detailed, but can not therefore be construed as limiting the scope of the patent.It should be pointed out that, for the person of ordinary skill of the art, without departing from the inventive concept of the premise, it is also possible to making some deformation and improvement, these broadly fall into protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.

Claims (9)

1. the preparation method that an aluminiferous metals prints powder, it is characterised in that comprise the steps:
The preparation of intermetallic compound composite block:
Being placed in ball grinding stirring machine by the mixing of aluminium powder, CNT and process control agent, the technological parameter of ball milling is: control ratio of grinding media to material is 5-25:1, and rotating speed is 700-1300r/min, and Ball-milling Time is 60-180min, and milling atmosphere is noble gas;Mixture after ball milling, through cold moudling, obtains described intermetallic compound composite block;
The addition of described CNT is the 1-20wt% of described aluminium powder consumption, and the addition of described process control agent is the 1-5wt% of described aluminium powder consumption;
The alloy raw material proportioning printing powder by described aluminiferous metals mixes each raw material and described intermetallic compound composite block, and the addition of described intermetallic compound composite block is the 1-20% that described aluminiferous metals prints powder gross mass;Then carry out melting, atomization, obtain described aluminiferous metals and print powder.
2. the preparation method that aluminiferous metals according to claim 1 prints powder, it is characterised in that described process control agent is ethanol and/or sodium stearate.
3. the preparation method that aluminiferous metals according to claim 2 prints powder, it is characterised in that described process control agent is mass ratio is ethanol and the sodium stearate of 1:1.
4. the preparation method that aluminiferous metals according to claim 1 prints powder, it is characterised in that the diameter of described CNT is 20-40nm, and length is 5-30 μm.
5. the preparation method that aluminiferous metals according to claim 1 prints powder, it is characterised in that in described aluminium powder, the weight/mass percentage composition of aluminium element is more than 99.5wt%.
6. the preparation method that the aluminiferous metals according to any one of claim 1-5 prints powder, it is characterised in that the technological parameter of described ball milling is: control ratio of grinding media to material is 10-20:1, and rotating speed is 900-1300r/min, and Ball-milling Time is 60-120min.
7. the aluminiferous metals that the preparation method described in any one of claim 1-6 prepares prints powder.
8. aluminiferous metals according to claim 7 prints powder, it is characterised in that described aluminiferous metals prints the alloy of powder and consists of Ti6Al4V or AlSi10Mg.
9. aluminiferous metals according to claim 7 prints powder, it is characterised in that described aluminiferous metals prints the oxygen content of powder less than 1200ppm, and less than 53 μm powder occupation rates are 50-70wt%.
CN201610231510.9A 2016-04-13 2016-04-13 Aluminum-contained metal printing powder and preparation method thereof Pending CN105710380A (en)

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CN106735269A (en) * 2016-12-16 2017-05-31 南通金源智能技术有限公司 The method for preparing the 3D printing Al alloy powder of excellent sintering character
CN106735268A (en) * 2016-12-16 2017-05-31 南通金源智能技术有限公司 Preparation method for reducing the 3D printing metal powder material of hollow powder
CN107695338A (en) * 2017-09-21 2018-02-16 北京宝航新材料有限公司 A kind of AlSi7Mg dusty materials and preparation method thereof and its application
CN107716918A (en) * 2017-09-21 2018-02-23 北京宝航新材料有限公司 A kind of AlSi10Mg dusty materials and preparation method thereof and its application

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CN104226980A (en) * 2014-07-29 2014-12-24 中国科学院重庆绿色智能技术研究院 Method for enhancing laser energy absorption efficiency of metal powder material
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106735269A (en) * 2016-12-16 2017-05-31 南通金源智能技术有限公司 The method for preparing the 3D printing Al alloy powder of excellent sintering character
CN106735268A (en) * 2016-12-16 2017-05-31 南通金源智能技术有限公司 Preparation method for reducing the 3D printing metal powder material of hollow powder
CN107695338A (en) * 2017-09-21 2018-02-16 北京宝航新材料有限公司 A kind of AlSi7Mg dusty materials and preparation method thereof and its application
CN107716918A (en) * 2017-09-21 2018-02-23 北京宝航新材料有限公司 A kind of AlSi10Mg dusty materials and preparation method thereof and its application

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