CN103028726A - Nano carbon black and nano rare earth synergistic-enhanced metal matrix micro-nano powder and preparation method thereof - Google Patents
Nano carbon black and nano rare earth synergistic-enhanced metal matrix micro-nano powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses nano carbon black and nano rare earth synergistic-enhanced metal matrix micro-nano powder and a preparation method thereof. The powder is characterized by comprising the following components in percentage by mass: 0.5-3% of nano carbon black powder, 2-4% of nano rare earth powder and 93-97.5% micron metal powder, wherein the percentage sum of the components is 100%; and core-shell structure micro-nano powder with the micron metal powder as core and with the nano carbon black powder and the nano rare earth powder as shell is formed. The preparation method comprises the following steps: single-phase nano carbon black suspension and single-phase nano rare earth suspension are prepared firstly, and are mixed to form double-phase nano suspension; then the double-phase nano suspension and spherically preprocessed micron metal powder are mixed, milled with balls, and are dried to prepare the metal matrix micro-nano powder. As the nano carbon black and the nano rare earth are synchronously guided in, the adding quantity of the nano carbon black can be further increased, so that better absorptivity for laser is achieved; produced thin-walled pieces have less deformation, narrow heat influence areas and good wear resistance, and can satisfy the requirements of powder conveying through the present laser forming mainstream technology, that is direct powder conveying type laser forming technology; and the powder has stronger engineering practicability and excellent application prospect.
Description
Technical field
The present invention relates to a kind of Metal Substrate micro-nano powder and preparation method thereof, especially a kind of laser is made with Metal Substrate micro-nano powder and preparation method thereof again, specifically collaborative Metal Substrate micro-nano powder that strengthens of a kind of nanometer carbon black and nano rare earth and preparation method thereof.
Background technology
On May 13rd, 2010,11 ministries and commissions such as National Development and Reform Committee, the Department of Science and Technology, Ministry of Industry and Information dispatch a joint document and dispose the development that advances remanufacturing industry, are promoted to a fundamental state policy that realizes China's strategy of sustainable development with developing manufacturing engineering again.The member of Chinese Academy of Engineering Xu Binshi professor who advocates, actively promotes again manufacturing engineering as taking the lead in China explicitly points out in its " again manufacturing engineering basis and use " book: the core of manufacturing engineering development is to make the development of key technology again again, and the center of gravity of making again key technical development then is the breakthrough of making again the theoretical and method of key technology towards high finished product added value object.As the thin-wall part of feature, a class has the again manufacturing object of high finished product added value exactly take " tight (performance is tight), smart (precision is high), thin (structure is thin) ".
For other re-manufacturing technologies, the laser re-manufacturing technology has many merits, and the interface is metallurgical binding, fine microstructures, composition is controlled, heat affecting is less etc. as making again, add Laser Processing high flexibility, high efficiency, lowly pollute and be easy to realize the light processing characteristic such as computer control, make it to become a thin-wall part that receives much concern and make again one of key technology.Yet, existing laser is made with powder again and is adopted the micron metal powder more, fuse the micron metal powder and need larger laser energy, cause matrix the heat input when manufacturing object is thin-wall part especially bigger than normal, and then cause thin-wall part distortion more greatly, again manufacturing district tissue deterioration, hydraulic performance decline etc., even lose the value of making again.As seen, improving laser and make with the absorptivity of powder to laser again, is the important channel that realization addresses the above problem.
Carbon black is generally the black nano powder about 20nm, has excellent spectral absorption performance, is widely used in coloured material, solar energy absorbing coating etc.Simultaneously, the nano rare earth powder has distinctive active rare-earth effect, is improving wetability between particle and matrix material, is purifying the aspect such as molten bath and have outstanding advantage.If nanometer carbon black powder and nano rare earth powder can be introduced structure micro-nano powder in the micron metal powder simultaneously, comprehensive two kinds of characteristics that nano powder has, with the wetability that not only can effectively improve between nanometer carbon black particle and matrix alloy, and then so that the addition of nanometer carbon black powder can further strengthen, thereby further improve powder to the absorptivity of laser; And, also be expected further to realize improving tissue and the performance of making again thin-wall part by giving full play to the active rare-earth effect.
Yet, up to the present, not yet there is collaborative Metal Substrate micro-nano powder that strengthens of a kind of nanometer carbon black and nano rare earth and preparation method thereof available, greatly limited the laser re-manufacturing technology in the application of making again aspect the high finished product added value thin-wall part.
Summary of the invention
The objective of the invention is to make again with powder not high and then cause the laser re-manufacturing technology to have again many circumscribed problems such as the heat input is bigger than normal in the manufacture process at thin-wall part to the absorptivity of laser for existing laser, invent collaborative Metal Substrate micro-nano powder that strengthens of a kind of nanometer carbon black and nano rare earth and preparation method thereof, for the extensive use of laser re-manufacturing technology in thin-wall part is made again provides material foundation.
One of technical scheme of the present invention is:
The collaborative Metal Substrate micro-nano powder that strengthens of a kind of nanometer carbon black and nano rare earth, it is characterized in that: it is that 0.5 ~ 3% nanometer carbon black powder, 2 ~ 4% nano rare earth powder and 93 ~ 97.5% micron metal powder form by mass percent, and various component sums are 100%; Nanometer carbon black powder and nano rare earth powder with inlay, in adhesion or the chemical bonds one or more are coated on micron metal powder surface, forms a kind of take the micron metal powder as examine, nanometer carbon black powder and nano rare earth powder be as the nuclear shell structure micro-nano powder of shell.
Described nanometer carbon black powder is not less than 120% according to the tinctorial strength of ASTMD-3849 or GB/T 7046-2003 standard detection, and its average grain diameter is 14 ~ 22nm.
Described nano rare earth powder is cerium oxide, lanthana or yittrium oxide, and its average grain diameter is 10 ~ 30nm.
The average grain diameter of described micron metal powder is 50 ~ 75 μ m, and the micron metal powder is that laser melts aluminium base, Ni-based, iron-based or the titanium-based metal powder that covers middle use.
Two of technical scheme of the present invention is:
The preparation method of the collaborative Metal Substrate micro-nano powder that strengthens of a kind of nanometer carbon black and nano rare earth is characterized in that it comprises the steps:
Step 1 is dispersed in commercial nanometer carbon black powder and nano rare earth powder respectively in the mixed solution of ethanol or ethanol and water, makes single phase nano carbon black suspension and the single phase nano rare earth suspension of stably dispersing;
Step 2 according to required proportioning weighing single phase nano carbon black suspension and single phase nano rare earth suspension, places same container to carry out the ball milling mixed processing both, obtains the carbon black rare earth biphase suspension that mixes;
Step 3 is carried out the spheroidization preliminary treatment with the former powder of commercial micron metal, obtains pretreated micron metal powder;
Step 4 according to the pretreated micron metal powder of required proportioning weighing, is carried out ball-milling behind the carbon black rare earth biphase suspension that has mixed in the adding step 2, obtains carbon black rare earth biphase and the compound micro-nano powder slurry of micron metal;
At last, place drying box dry in micro-nano powder slurry, can obtain the collaborative Metal Substrate micro-nano powder that strengthens of nanometer carbon black and nano rare earth.
Described single phase nano carbon black suspension and single phase nano rare earth suspension adopt identical liquid medium, and namely both are absolute ethyl alcohol or are the mixed solution of the second alcohol and water of equal volume mark.
Described ball milling mixed processing technological parameter is that rotational speed of ball-mill is that 500 rev/mins, ratio of grinding media to material 5:1, Ball-milling Time are 1 hour.
Described ball-milling parameter is that rotational speed of ball-mill is that 100-300 rev/min, ratio of grinding media to material 5:1-10:1, Ball-milling Time are 0.5-1.5 hour.
Beneficial effect of the present invention:
(1) introducing of nano rare earth powder, can effectively improve the wetability between nanometer carbon black particle and matrix alloy, so that the addition of nanometer carbon black powder can further increase, so working in coordination with the Metal Substrate micro-nano powder that strengthens, nanometer carbon black of the present invention and nano rare earth laser is had the higher absorptivity of Metal Substrate micro-nano powder of more only adding nanometer carbon black.For example, in other laser situation that Fabrication parameter is constant again, adopt micro-nano powder of the present invention to obtain best in qualityly to make the limit sweep speed that thin-wall part allows again and can improve more than 70% with the system powder and micron, the same system micro-nano powder that more only adds nanometer carbon black can improve more than 20%.
(2) that the thin-wall part that adopts the collaborative Metal Substrate micro-nano powder institute that strengthens of nanometer carbon black of the present invention and nano rare earth to make again is out of shape is little, the heat affected area is narrow, fine microstructures is fine and close, substantially do not have carbide inclusion, has than powder and micron and makes better mechanical property and anti-wear performance again.
(3) the collaborative Metal Substrate micro-nano powder that strengthens of nanometer carbon black of the present invention and nano rare earth has typical nucleocapsid structure, nanometer carbon black powder and nano rare earth powder with inlay, in adhesion or the chemical bonds one or more are coated on micron metal powder surface, there are not other fine particles in the micro-nano powder, can satisfy present laser forming mainstream technology--directly powder feeding formula laser forming technology is carried the requirement of powder, has very strong engineering practicability and good application prospect.
(4) the present invention makes thin-wall part with the absorptivity angle of powder to laser again from improving laser, realize breaking through existing laser re-manufacturing technology existing many limitation in thin-wall part is made again, help to promote to make again the development of the laser re-manufacturing technology of one of key technology, thereby for realizing that China's strategy of sustainable development provides technical support.
Description of drawings
Fig. 1 is micro-nano powder low power SEM pattern of the present invention.
Fig. 2 is micro-nano powder of the present invention surface high power SEM pattern.
The specific embodiment
The present invention is further illustrated below in conjunction with accompanying drawing and example.
As shown in Figure 1, 2.
The collaborative Metal Substrate micro-nano powder that strengthens of a kind of nanometer carbon black and nano rare earth, it is that 0.5 ~ 3% nanometer carbon black powder, 2 ~ 4% nano rare earth powder and 93 ~ 97.5% micron metal powder form by mass percent, various component sums are 100%; Nanometer carbon black powder and nano rare earth powder with inlay, in adhesion or the chemical bonds one or more are coated on micron metal powder surface, forms a kind of take the micron metal powder as examine, nanometer carbon black powder and nano rare earth powder be as the nuclear shell structure micro-nano powder of shell.It can adopt the following methods step to be prepared from:
At first, preparation single phase nano carbon black suspension, purchase first average grain diameter during preparation from market and be 14 ~ 22nm, be not less than 120% nanometer carbon black powder according to the tinctorial strength of ASTMD-3849 or GB/T 7046-2003 standard detection and carry out the dry ball milling preliminary treatment, breaking wherein original macro aggregate particle, thereby guarantee that carbon black powder has good dispersion in ethanol or pure water mixed solution; Account for 0.05% ~ 0.15% of carbon black stock quality mark according to carbon black powder and take by weighing nanometer carbon black powder and ethanol or pure water mixed solution, ethanol accounts for 30 ~ 70% of mixed liquor volume in the pure water mixed solution; Both are mixed and be stirred to and obtain without the obvious carbon black slurry semi-finished product of solid-liquid layering; Carbon black slurry semi-finished product after will stirring again place ultrasonic device to carry out the thermostatic ultrasonic dispersion, and the control thermostat temperature is 20 ± 5 ℃, and jitter time is 30 ~ 60 minutes, can obtain the single phase nano carbon black suspension of stably dispersing;
Secondly, the single phase nano rare earth suspension of preparation stably dispersing; With commercial nano rare earth powder (such as cerium oxide, lanthana or yittrium oxide, its average grain diameter is 10 ~ 30nm) to carry out mix and blend with the mixed solution of ethanol or ethanol and water, make mass percent and be the single phase nano rare earth suspension about 2-10%, it is for subsequent use to remove the precipitation part, and calculates the mass percent of the reality of nano rare earth in the actual single phase nano rare earth suspension; Also can adopt ball milling, ultrasonic dispersion etc. separately during the single phase nano rare earth suspension of preparation stably dispersing or complex method carries out, also can carry out with reference to the method for Chinese patent ZL200710133580.1;
The 3rd step, preparation biphase suspension; According to required proportioning weighing single phase nano carbon black suspension and single phase nano rare earth suspension, place same container to carry out the ball milling mixed processing both, obtain the carbon black rare earth biphase suspension that mixes; Ball milling mixed processing technological parameter is that rotational speed of ball-mill is that 500 rev/mins, ratio of grinding media to material 5:1, Ball-milling Time are 1 hour, convert according to the mass percent in the mass percent in the suspension and the micro-nano powder when weighing single phase nano carbon black suspension and single phase nano rare earth suspension, satisfy the component requirement to guarantee carbon black powder in the micro-nano powder and the mass percent content in the nano rare earth powder;
The 4th step, the former powder of commercial micron metal (can be the metal powders such as aluminium base, Ni-based, iron-based and titanium base) is carried out the spheroidization preliminary treatment, obtain pretreated micron metal powder;
The 5th step according to the pretreated micron metal powder of required proportioning weighing, added in the 3rd step and carries out ball-milling behind the carbon black rare earth biphase suspension that mixed, obtained carbon black rare earth biphase and the compound micro-nano powder slurry of micron metal; The ball-milling parameter is that rotational speed of ball-mill is that 100-300 rev/min, ratio of grinding media to material 5:1-10:1, Ball-milling Time are 0.5-1.5 hour;
At last, place drying box dry in micro-nano powder slurry, can obtain the collaborative Metal Substrate micro-nano powder that strengthens of nanometer carbon black and nano rare earth.
In addition, when specifically preparing, preparation single phase nano carbon black suspension should adopt identical liquid medium during with single phase nano rare earth suspension, and namely both are absolute ethyl alcohol or are the mixed solution of the second alcohol and water of equal volume mark; Ethanol accounts for 30 ~ 70% of mixed liquor volume in the mixed solution of second alcohol and water.
Example 1.
The present embodiment material therefor: nanometer carbon black powder average grain diameter is 18nm, and tinctorial strength is 135%, and mass fraction is 2%; The nano rare earth powder is cerium oxide, and its average grain diameter is 20nm, and mass fraction is 3%; The micron metal powder is the Al-Si alloyed powder, and average grain diameter is 50 μ m, and mass fraction is 95%; Adopt above-mentioned steps to prepare nanometer carbon black and the collaborative Metal Substrate micro-nano powder that strengthens of nano rare earth, its ball-milling parameter is that rotational speed of ball-mill is that 200 rev/mins, ratio of grinding media to material 8:1, Ball-milling Time are 1 hour.Through scanning electron microscopic observation, prepared micro-nano powder keeps the spherical feature (Fig. 1) of powder and micron, be coated with the nanometer carbon black powder and the nano rare earth powder (Fig. 2) that are in a large number the polymolecularity feature on its surface, almost completely cover the micron particles surface, form nucleocapsid structure of the present invention.
Adopt this micro-nano powder to carry out laser weld and make again the 0.6mm thick and thin wall spare that has penetrating crack, in the constant situation of other technological parameters, obtain that best in quality to make the limit sweep speed that thin-wall part allows be 3.5mm/s again, adopting then only is 2mm/s with the system powder and micron; As seen, micro-nano powder of the present invention has with the better light absorptive of system powder and micron.Adopt this micro-nano powder make again that thin-wall part distortion is very little, the heat affected area width is only for adopting with about 40% of system powder and micron.Adopting this micro-nano powder is that the AZ91D magnesium alloy substrate laser melting coating of 2mm prepares the thick wear-resisting modified layer of 0.25mm at thickness, under the identical frictional wear experiment condition, its Volume erosion rate adopts with the prepared wear-resisting modified layer of system powder and micron and has reduced by 47.2%, and coefficient of friction is reduced to 0.24 by 0.55.No matter be that laser weld is made tissue or laser fusion coating rubbing-layer tissue again, all tiny densifications, substantially do not have a carbide inclusion; Simultaneously, the thin-wall part distortion of making again little, the heat affected area is narrow, have than powder and micron and make better mechanical property again.
Example 2 ~ 8.
As shown in table 1, its ball-milling parameter is that rotational speed of ball-mill is that 200 rev/mins, ratio of grinding media to material 8:1, Ball-milling Time are 1 hour, all reaches example 1 similar effect.
Table 1 embodiment 2 ~ 8 micro-nano meal components
Above-mentioned several frequently seen nanometer carbon black and the collaborative Metal Substrate micro-nano powder that strengthens of nano rare earth only listed, those skilled in the art can be according to making the different micron metal powder of thin-wall part material selection again, according to proportioning of the present invention and preparation method, all can obtain the collaborative Metal Substrate micro-nano powder that strengthens of desirable nanometer carbon black and nano rare earth again.
The part that the present invention does not relate to all prior art that maybe can adopt same as the prior art is realized.
Claims (8)
1. the collaborative Metal Substrate micro-nano powder that strengthens of a nanometer carbon black and nano rare earth, it is characterized in that: it is that 0.5 ~ 3% nanometer carbon black powder, 2 ~ 4% nano rare earth powder and 93 ~ 97.5% micron metal powder form by mass percent, and various component sums are 100%; Nanometer carbon black powder and nano rare earth powder with inlay, in adhesion or the chemical bonds one or more are coated on micron metal powder surface, forms a kind of take the micron metal powder as examine, nanometer carbon black powder and nano rare earth powder be as the nuclear shell structure micro-nano powder of shell.
2. nanometer carbon black according to claim 1 and nano rare earth are worked in coordination with the Metal Substrate micro-nano powder that strengthens, it is characterized in that described nanometer carbon black powder is not less than 120% according to the tinctorial strength of ASTMD-3849 or GB/T7046-2003 standard detection, its average grain diameter is 14 ~ 22nm.
3. nanometer carbon black according to claim 1 and nano rare earth are worked in coordination with the Metal Substrate micro-nano powder that strengthens, and the kind that it is characterized in that described nano rare earth powder is cerium oxide, lanthana or yittrium oxide, and its average grain diameter is 10 ~ 30nm.
4. the collaborative Metal Substrate micro-nano powder that strengthens of nanometer carbon black according to claim 1 and nano rare earth, the average grain diameter that it is characterized in that described micron metal powder is 50 ~ 75 μ m, the micron metal powder is aluminium base, Ni-based, iron-based or titanium-based metal powder.
5. the preparation method of the collaborative Metal Substrate micro-nano powder that strengthens of a nanometer carbon black and nano rare earth is characterized in that it comprises the steps:
Step 1 is dispersed in commercial nanometer carbon black powder and nano rare earth powder respectively in the mixed solution of ethanol or ethanol and water, makes single phase nano carbon black suspension and the single phase nano rare earth suspension of stably dispersing;
Step 2 according to required proportioning weighing single phase nano carbon black suspension and single phase nano rare earth suspension, places same container to carry out the ball milling mixed processing both, obtains the carbon black rare earth biphase suspension that mixes;
Step 3 is carried out the spheroidization preliminary treatment with the former powder of commercial micron metal, obtains pretreated micron metal powder;
Step 4 according to the pretreated micron metal powder of required proportioning weighing, is carried out ball-milling behind the carbon black rare earth biphase suspension that has mixed in the adding step 2, obtains carbon black rare earth biphase and the compound micro-nano powder slurry of micron metal;
At last, place drying box dry in micro-nano powder slurry, can obtain the collaborative Metal Substrate micro-nano powder that strengthens of nanometer carbon black and nano rare earth.
6. preparation method according to claim 5 is characterized in that described single phase nano carbon black suspension and single phase nano rare earth suspension adopt identical liquid medium, and namely both are absolute ethyl alcohol or are the mixed solution of the second alcohol and water of equal volume mark.
7. method according to claim 5 is characterized in that described ball milling mixed processing technological parameter is that rotational speed of ball-mill is that 500 rev/mins, ratio of grinding media to material 5:1, Ball-milling Time are 1 hour.
8. method according to claim 5 is characterized in that described ball-milling parameter is that rotational speed of ball-mill is that 100-300 rev/min, ratio of grinding media to material 5:1-10:1, Ball-milling Time are 0.5-1.5 hour.
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| CN105754382A (en) * | 2016-01-29 | 2016-07-13 | 江苏大学 | High-dispersion and stable-suspension superfine yttrium oxide glue-containing sizing agent and preparation method thereof |
| CN107042369A (en) * | 2016-10-31 | 2017-08-15 | 江苏大学 | Flux-cored wire granule modified medicinal powder of fine rare earth and preparation method thereof |
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