CN103028726B - 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 manufactured with Metal Substrate micro-nano powder and preparation method thereof again, specifically collaborative Metal Substrate micro-nano powder strengthening 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 by developing manufacturing engineering a fundamental state policy that realizes China's strategy of sustainable development again.The member of Chinese Academy of Engineering Xu Binshi professor who advocates, actively promotes manufacturing engineering as taking the lead in China explicitly points out in its " manufacturing engineering basis and application thereof again " book: the core of manufacturing engineering development is to manufacture the development of key technology again again, then the center of gravity of manufacturing key technical development is the breakthrough of manufacturing again the theoretical and method of key technology towards high finished product added value object.Taking " tight (performance is tight), essence (precision is high), thin (structure is thin) ", as the thin-wall part of feature, a class has the manufacturing object again of high finished product added value exactly.
For other re-manufacturing technologies, laser re-manufacturing technology has many merits, and as manufactured, interface is metallurgical binding, fine microstructures, composition is controlled, heat affecting is less again etc., add high flexibility, high efficiency, the low pollution of Laser Processing and be easy to realize the light processing characteristics such as computer control, making it to become a thin-wall part receiving much concern and manufacture again one of key technology.But, existing laser is manufactured and is adopted micron metal powder with powder more, fuse micron metal powder and need larger laser energy, cause heat input when manufacturing object is thin-wall part especially again to matrix bigger than normal, and then cause thin-wall part distortion more greatly, manufacturing district tissue deterioration, hydraulic performance decline etc. again, even lose the value of manufacturing again.Visible, improve laser and manufacture again the absorptivity to laser with powder, be to realize the important channel addressing 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.Meanwhile, nano rare earth powder has distinctive active rare-earth effect, has outstanding advantage at the aspect such as wetability, purification molten bath of improving between particle and matrix material.In micron metal powder, build micro-nano powder if nanometer carbon black powder and nano rare earth powder can be introduced simultaneously, comprehensive two kinds of characteristics that nano powder has, wetability between nanometer carbon black particle and matrix alloy will not only can effectively be improved, and then the addition of nanometer carbon black powder can further be strengthened, thereby further improve the absorptivity of powder to laser; And, be also expected further to improve by giving full play to the realization of active rare-earth effect tissue and the performance of manufacturing again thin-wall part.
But, up to the present, not yet there is collaborative Metal Substrate micro-nano powder strengthening of a kind of nanometer carbon black and nano rare earth and preparation method thereof available, greatly limit laser re-manufacturing technology in the application of manufacturing again aspect high finished product added value thin-wall part.
Summary of the invention
The object of the invention is to manufacture again with powder not high and then cause laser re-manufacturing technology to have again many circumscribed problems such as heat input is bigger than normal in manufacture process at thin-wall part to the absorptivity of laser for existing laser, invent collaborative Metal Substrate micro-nano powder strengthening 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 manufactured again provides material foundation.
One of technical scheme of the present invention is:
The collaborative Metal Substrate micro-nano powder strengthening of nanometer carbon black and nano rare earth, 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%; One or more inlaying, in adhesion or chemical bonds of nanometer carbon black powder and nano rare earth powder are coated on micron metal powder surface, form a kind of taking micron metal powder as core, nanometer carbon black powder and nano rare earth powder be 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 micron metal powder is that laser melts aluminium base, Ni-based, the iron-based or the titanium-based metal powder that cover middle use.
Two of technical scheme of the present invention is:
A preparation method for the collaborative Metal Substrate micro-nano powder strengthening 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, weighs single phase nano carbon black suspension and single phase nano rare earth suspension according to required proportioning, both is placed in to same container and carries out ball milling mixed processing, obtains the carbon black rare earth biphase suspension mixing;
Step 3, carries out spheroidization pretreatment by former commercial micron metal powder, obtains pretreated micron metal powder;
Step 4, weighs pretreated micron metal powder according to required proportioning, carries out ball-milling after adding the carbon black rare earth biphase suspension having mixed in step 2, obtains carbon black rare earth biphase and the compound micro-nano powder slurry of micron metal;
Finally, micro-nano powder slurry is placed in to drying box dry, can obtains the collaborative Metal Substrate micro-nano powder strengthening 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 both are absolute ethyl alcohol or are the mixed solution of the second alcohol and water of same volume mark.
Described ball milling mixed processing technological parameter is that rotational speed of ball-mill is that 500 revs/min, 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, the addition of nanometer carbon black powder can further be increased, therefore the collaborative Metal Substrate micro-nano powder strengthening of nanometer carbon black of the present invention and nano rare earth has the higher absorptivity of Metal Substrate micro-nano powder of more only adding nanometer carbon black to laser.For example, at other laser Fabrication parameter is constant again in the situation that, adopt micro-nano powder of the present invention to obtain and best in qualityly manufacture the limit sweep speed that thin-wall part allows again and can improve more than 70% with 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 strengthening of nanometer carbon black of the present invention and nano rare earth to manufacture is again out of shape is little, heat affected area is narrow, fine microstructures is fine and close, substantially there is no carbide inclusion, has compared with powder and micron and manufactures better mechanical property and anti-wear performance again.
(3) the collaborative Metal Substrate micro-nano powder strengthening of nanometer carbon black of the present invention and nano rare earth has typical nucleocapsid structure, one or more inlaying, in adhesion or chemical bonds of nanometer carbon black powder and nano rare earth powder are coated on micron metal powder surface, in micro-nano powder, there are not other fine particles, can meet current 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 manufactures the absorptivity angle of thin-wall part powder to laser again from improving laser, realize and break through existing laser re-manufacturing technology existing many limitation in thin-wall part is manufactured again, contribute to promote the development of the laser re-manufacturing technology of manufacturing again one of key technology, thereby provide technical support for realizing China's strategy of sustainable development.
Brief description of the 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.
Detailed description of the invention
Below in conjunction with accompanying drawing and example, the present invention is further illustrated.
As shown in Figure 1, 2.
The collaborative Metal Substrate micro-nano powder strengthening 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%; One or more inlaying, in adhesion or chemical bonds of nanometer carbon black powder and nano rare earth powder are coated on micron metal powder surface, form a kind of taking micron metal powder as core, nanometer carbon black powder and nano rare earth powder be the nuclear shell structure micro-nano powder of shell.It can adopt following methods step to be prepared from:
First, prepare single phase nano carbon black suspension, when preparation, first purchase average grain diameter 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 dry ball milling pretreatment, to break wherein original macro aggregate particle, thereby ensure that carbon black powder has good dispersion in ethanol or alcohol water mixed solution; Account for 0.05% ~ 0.15% of carbon black stock quality mark according to carbon black powder and take nanometer carbon black powder and ethanol or alcohol water mixed solution, in alcohol water mixed solution, ethanol accounts for 30 ~ 70% of mixed liquor volume; Both are mixed and be stirred to and obtain the obviously carbon black slurry semi-finished product of solid-liquid layering of nothing; Again the carbon black slurry semi-finished product after stirring are placed in to ultrasonic device and carry out thermostatic ultrasonic dispersion, controlling thermostat temperature is 20 ± 5 DEG C, and jitter time is 30 ~ 60 minutes, can obtain the single phase nano carbon black suspension of stably dispersing;
Secondly, prepare the single phase nano rare earth suspension of stably dispersing; By commercial nano rare earth powder (as cerium oxide, lanthana or yittrium oxide, its average grain diameter is 10 ~ 30nm) carry out mix and blend with the mixed solution of ethanol or ethanol and water, making mass percent is the single phase nano rare earth suspension of 2-10% left and right, remove precipitation part for subsequent use, and calculate the actual mass percent of nano rare earth in actual single phase nano rare earth suspension; While preparing the single phase nano rare earth suspension of stably dispersing, also can adopt ball milling, ultrasonic dispersion etc. separately or complex method carry out, also can carry out with reference to the method for Chinese patent ZL200710133580.1;
The 3rd step, prepares biphase suspension; Weigh single phase nano carbon black suspension and single phase nano rare earth suspension according to required proportioning, both are placed in to same container and carry out ball milling mixed processing, obtain the carbon black rare earth biphase suspension mixing; Ball milling mixed processing technological parameter is that rotational speed of ball-mill is that 500 revs/min, ratio of grinding media to material 5:1, Ball-milling Time are 1 hour, while weighing single phase nano carbon black suspension and single phase nano rare earth suspension, convert according to the mass percent in the mass percent in suspension and micro-nano powder, to guarantee that the mass percent content in carbon black powder and the nano rare earth powder in micro-nano powder meets component requirement;
The 4th step, carries out spheroidization pretreatment by former commercial micron metal powder (can be the metal powders such as aluminium base, Ni-based, iron-based and titanium base), obtains pretreated micron metal powder;
The 5th step, weighs pretreated micron metal powder according to required proportioning, carries out ball-milling after adding the carbon black rare earth biphase suspension having mixed in the 3rd step, obtains carbon black rare earth biphase and the compound micro-nano powder slurry of micron metal; 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;
Finally, micro-nano powder slurry is placed in to drying box dry, can obtains the collaborative Metal Substrate micro-nano powder strengthening of nanometer carbon black and nano rare earth.
In addition, while specifically preparation, while preparing single phase nano carbon black suspension and single phase nano rare earth suspension, should adopt identical liquid medium, both are absolute ethyl alcohol or are the mixed solution of the second alcohol and water of same volume mark; In the mixed solution of second alcohol and water, ethanol accounts for 30 ~ 70% of mixed liquor volume.
Example 1.
The present embodiment material therefor: nanometer carbon black powder average grain diameter is 18nm, tinctorial strength is 135%, mass fraction is 2%; Nano rare earth powder is cerium oxide, and its average grain diameter is 20nm, and mass fraction is 3%; Micron metal powder is Al-Si alloyed powder, and average grain diameter is 50 μ m, and mass fraction is 95%; Adopt above-mentioned steps to prepare the collaborative Metal Substrate micro-nano powder strengthening of nanometer carbon black and nano rare earth, its ball-milling parameter is that rotational speed of ball-mill is that 200 revs/min, 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, on its surface, be coated with the nanometer carbon black powder and the nano rare earth powder (Fig. 2) that are in a large number polymolecularity feature, almost cover micron particles surface completely, form nucleocapsid structure of the present invention.
Adopt this micro-nano powder to carry out laser weld and manufacture again the 0.6mm thick and thin wall part that has penetrating crack, in the constant situation of other technological parameters, obtain that best in quality to manufacture the limit sweep speed that thin-wall part allows be 3.5mm/s again, adopting is only 2mm/s with system powder and micron; Visible, micro-nano powder of the present invention has with the better light absorptive of system powder and micron.Adopt that this micro-nano powder manufactures that thin-wall part distortion is very little again, heat affected area width is only for adopting 40% left and right with system powder and micron.Adopt the AZ91D magnesium alloy substrate laser melting coating that this micro-nano powder is 2mm at thickness to prepare the wear-resisting modified layer that 0.25mm is thick, under identical frictional wear experiment condition, its Volume erosion rate adopts the prepared wear-resisting modified layer of same system powder and micron to reduce by 47.2%, and coefficient of friction is reduced to 0.24 by 0.55.No matter be that laser weld is manufactured tissue or laser fusion coating rubbing-layer tissue again, all tiny densifications, substantially there is no a carbide inclusion; Meanwhile, then the thin-wall part of manufacturing distortion is little, heat affected area is narrow, have compared with powder and micron and manufacture 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 revs/min, ratio of grinding media to material 8:1, Ball-milling Time are 1 hour, all reaches the similar effect of example 1.
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 strengthening of nano rare earth only listed, those skilled in the art can be according to manufacturing 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 strengthening 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 (5)
1. the collaborative Metal Substrate micro-nano powder strengthening of nanometer carbon black and nano rare earth, 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%; One or more inlaying, in adhesion or chemical bonds of nanometer carbon black powder and nano rare earth powder are coated on micron metal powder surface, form a kind of taking micron metal powder as core, nanometer carbon black powder and nano rare earth powder be 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/T7046-2003 standard detection, and its average grain diameter is 14 ~ 22nm; The kind of 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 micron metal powder is aluminium base, Ni-based, iron-based or titanium-based metal powder.
2. a preparation method for the collaborative Metal Substrate micro-nano powder strengthening of the nanometer carbon black described in claims 1 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, weighs single phase nano carbon black suspension and single phase nano rare earth suspension according to required proportioning, both is placed in to same container and carries out ball milling mixed processing, obtains the carbon black rare earth biphase suspension mixing;
Step 3, carries out spheroidization pretreatment by former commercial micron metal powder, obtains pretreated micron metal powder;
Step 4, weighs pretreated micron metal powder according to required proportioning, carries out ball-milling after adding the carbon black rare earth biphase suspension having mixed in step 2, obtains carbon black rare earth biphase and the compound micro-nano powder slurry of micron metal;
Finally, micro-nano powder slurry is placed in to drying box dry, can obtains the collaborative Metal Substrate micro-nano powder strengthening of nanometer carbon black and nano rare earth.
3. preparation method according to claim 2, is characterized in that described single phase nano carbon black suspension and single phase nano rare earth suspension adopt identical liquid medium, and both are absolute ethyl alcohol or are the mixed solution of the second alcohol and water of same volume mark.
4. method according to claim 2, is characterized in that described ball milling mixed processing technological parameter is that rotational speed of ball-mill is that 500 revs/min, ratio of grinding media to material 5:1, Ball-milling Time are 1 hour.
5. method according to claim 2, 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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| CN105754382B (en) * | 2016-01-29 | 2018-08-14 | 江苏大学 | Fine yttrium oxide material containing rubber cement of high dispersive stable suspersion and preparation method thereof |
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