CN103008654B - Carbon black and ceramic double-phase nanometer composite slurry for preparing metal-based micro-nano powder and preparation method thereof - Google Patents
Carbon black and ceramic double-phase nanometer composite slurry for preparing metal-based micro-nano powder and preparation method thereof Download PDFInfo
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- CN103008654B CN103008654B CN201310006029.6A CN201310006029A CN103008654B CN 103008654 B CN103008654 B CN 103008654B CN 201310006029 A CN201310006029 A CN 201310006029A CN 103008654 B CN103008654 B CN 103008654B
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Abstract
The invention discloses a carbon black and ceramic double-phase nanometer composite slurry for preparing a metal-based micro-nano powder and a preparation method thereof. The carbon black and ceramic double-phase nanometer composite slurry is characterized by comprising nanometer carbon black powder, nanometer ceramic powder and absolute ethyl alcohol, wherein the mass percentage of the nanometer carbon black powder in the slurry is 0.05-0.15 %, the mass percentage of the nanometer ceramic powder is 4-6 times larger than that of the nanometer carbon black powder; and the rest are the absolute ethyl alcohol; the total mass percentage of the components is 100 %. According to the invention, the carbon black and ceramic double-phase nanometer composite slurry with ethanol as medium is realized for the first time; meanwhile, nanometer carbon black with a wear reducing effect and nanometer ceramic with an anti-wear effect are introduced; therefore, the prepared laser wear resistant modified layer obtains very good wear resistance. Meanwhile, the carbon black and ceramic double-phase nanometer composite slurry for preparing the metal-based micro-nano powder, disclosed by the invention, has the advantages of pure components, good dispersion stability, very good use performance and very good engineering application value.
Description
Technical field
The present invention relates to a kind of nano pulp, especially a kind of biphase slurry, specifically a kind of Metal Substrate micro-nano powder for preparing carbon black and ceramic biphase composite mortar and preparation method.
Background technology
In recent years, a kind of structure is situated between and sees technology---the micro-nano granules complex technique of (micro/nano level) novel substance, has caused domestic and international experts and scholars' attention.Micro-nano granules complex technique is nano particle to be coated on to micron particles surface or to make its disperse be distributed in preparation in micron particles to have the technology that micro-nano is worked in coordination with multifunctional effect micro-nano composite granule.If the nano particle with anti-attrition, the characteristic such as wear-resisting is introduced in micron metal powder and is built micro-nano powder, will improve widely the wearability of prepared material.Can say, micro-nano granules complex technique has been opened up a new way for improving the anti-wear performance of metal material.
Carbon black powder is that a kind of average grain diameter is the black nano powder of 20nm, has good anti-attrition characteristic; Meanwhile, nano-ceramic powder, has high hardness the effective tissue of refinement material, is widely used in the wearability of improving metal material.According to the patent " a kind of mechanical preparation method of composite nanometer ceramic and micron metal powder (ZL 2007 10024996.X) " of Wang Hongyu etc., want to realize nano particle and be effectively coated on micron particles surface, need to adopt the nano pulp of stably dispersing to introduce mode as the nanometer of ball-milling medium.But, according to the knowledge of the applicant, not yet have a kind of carbon black/ceramic biphase composite mortar and preparation method thereof can be for the Metal Substrate micro-nano powder of preparing carbon black/ceramic biphase and strengthening.
Therefore, develop a kind of carbon black and ceramic biphase composite mortar, most important for the Metal Substrate micro-nano powder of preparing the carbon black/ceramic biphase enhancing with good wear-resisting modified effect.
Summary of the invention
The object of the invention is for not yet there being at present a kind of carbon black/ceramic biphase composite mortar and preparation method thereof can be for the problem of preparing the Metal Substrate micro-nano powder of carbon black/ceramic biphase enhancing, invent a kind of Metal Substrate micro-nano powder for preparing carbon black and ceramic biphase composite mortar, a kind of corresponding preparation method is provided simultaneously.
One of technical scheme of the present invention is:
Metal Substrate micro-nano powder for preparing carbon black and a ceramic biphase composite mortar, is characterized in that it is comprised of nanometer carbon black powder, nano-ceramic powder and absolute ethyl alcohol; Wherein, nanometer carbon black powder accounts for 0.05% ~ 0.15% of stock quality mark, and the mass fraction of nano-ceramic powder is 4 ~ 6 times of institute's plus nano carbon black powder mass fraction, and all the other are absolute ethyl alcohol, and each constituent mass mark summation is 100%.
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 ~ 28nm.
Described nano-ceramic powder is carborundum, tungsten carbide and aluminium oxide, and its average grain diameter is 10 ~ 50nm.
Two of technical scheme of the present invention is:
A preparation method for Metal Substrate micro-nano powder for preparing carbon black and ceramic biphase composite mortar, is characterized in that it comprises the following steps:
First, according to required mass fraction, take nanometer carbon black powder and add anhydrous ethanol preparation to become single phase nano carbon black suspension, the mass percent of controlling nanometer carbon black powder in single phase nano carbon black suspension is not more than 1%, to guarantee that nanometer carbon black powder is without precipitation;
Then, according to required mass fraction, weigh nano-ceramic powder and add in absolute ethyl alcohol, and be prepared into single phase nano ceramic suspension liquid;
Finally, Manufactured single phase nano carbon black suspension and single phase nano ceramic suspension liquid are carried out to ball milling 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 that 1 hour, ball radius are not more than 4mm, can obtain Metal Substrate micro-nano powder for preparing carbon black and ceramic biphase composite mortar.
Beneficial effect of the present invention:
(1) the present invention has realized first preparation and take carbon black and the ceramic biphase composite mortar that ethanol is medium, introduce the nanometer carbon black with anti-attrition effect and the nano ceramics with wear-resistant effect simultaneously, the wear-resisting modified layer tool of prepared laser is had good wearability, and compared with single phase nano, strengthening the wear-resisting modified layer of the prepared laser of micro-nano powder has significantly raising.
(2) in slurry of the present invention, nanometer carbon black powder and nano-ceramic powder have rational proportion relation, not only can give full play to both functional characteristics separately, and can give full play to the strong light absorptive of carbon black, the micro-nano powder prepared with this slurry has high absorptivity to laser.
(3) slurry of the present invention be take ethanol as liquid medium, does not need additionally to add any dispersant or surfactant, is guaranteeing that pulp components also has the dispersion stabilization that is not less than single phase nano slurry in pure, can stable dispersion not sedimentation above in 3 months.
(4) the present invention is by ball milling mixed method, guaranteed that nanometer carbon black powder and nano-ceramic powder are evenly distributed in slurry, have no obvious a certain single phase nano powder concentration of local phenomenon, be conducive to give full play to nanometer carbon black powder and nano ceramics functional characteristic separately, and through lot of experiments, obtained the optimised process combination that ball milling mixes.
Accompanying drawing explanation
Fig. 1 is the micro-nano powder SEM pattern that adopts biphase composite mortar of the present invention to prepare.
The specific embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is further illustrated.
Be below method of the present invention prepared take carbon black and the ceramic biphase composite mortar example that ethanol is medium, but be not limited only to these examples, as long as adopt the method for the invention, all can reach object of the present invention.
embodiment mono-.
Example material therefor: commercial common packed carbon black powder, average grain diameter 18nm, tinctorial strength is 135%, the addition of carbon black powder accounts for 0.05% of slurry gross mass; Commercial common packed
carborundumpowder, average grain diameter 30nm, is bottle green, and its addition accounts for 0.3% of slurry gross mass, and all the other are absolute ethyl alcohol.
First nanometer carbon black powder is carried out to dry ball milling pretreatment, to break wherein original macro aggregate particle, mix with absolute ethyl alcohol again and be stirred to and obtain the obviously carbon black slurry semi-finished product of solid-liquid layering of nothing, 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 ℃, jitter time is 30 ~ 60 minutes, can obtain the single phase nano carbon black suspension of stably dispersing, the addition of absolute ethyl alcohol should guarantee that the mass percent of the nanometer carbon black powder in formed single phase nano carbon black suspension is not more than 1%, then, silicon carbide powder is added in the absolute ethyl alcohol of surplus and stir and obtain single phase nano silicon carbide suspension, finally, Manufactured single phase nano carbon black suspension and single phase nano silicon carbide suspension are carried out to ball milling 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 that 1 hour, ball radius are not more than 4mm, can obtain Metal Substrate micro-nano powder for preparing carbon black and carborundum biphase composite mortar.The prepared composite mortar forming is and the similarly even black of single-phase carbon black slurry, has no the phenomenon of obvious a certain single phase nano powder concentration of local.If undesirable ultrasonic wave dispersion or other the conventional process for dispersing of also can adopting of mixing effect disperses when preparing single phase nano silicon carbide suspension, if have deposited phenomenon to occur, should suitably add silicon carbide powder and meet the demands to guarantee the content of silicon carbide powder in final slurry.
Embodiment bis-.
Example material therefor: commercial common packed carbon black powder, its average grain diameter is 28nm, and tinctorial strength is 120%, and the addition of carbon black powder accounts for 0.1% of slurry gross mass; Commercial common packed tungsten carbide powder, average grain diameter 10nm, is grey black, and its addition accounts for 0.5% of slurry gross mass, and all the other are absolute ethyl alcohol.
First nanometer carbon black powder is carried out to dry ball milling pretreatment, to break wherein original macro aggregate particle, mix with absolute ethyl alcohol again and be stirred to and obtain the obviously carbon black slurry semi-finished product of solid-liquid layering of nothing, 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 ℃, jitter time is 30 ~ 60 minutes, can obtain the single phase nano carbon black suspension of stably dispersing, the addition of absolute ethyl alcohol should guarantee that the mass percent of the nanometer carbon black powder in formed single phase nano carbon black suspension is not more than 1%, then, tungsten carbide powder is added in the absolute ethyl alcohol of surplus and stir and obtain single phase nano tungsten carbide suspension, finally, Manufactured single phase nano carbon black suspension and single phase nano tungsten carbide suspension are carried out to ball milling 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 that 1 hour, ball radius are not more than 4mm, can obtain Metal Substrate micro-nano powder for preparing carbon black and tungsten carbide biphase composite mortar.Prepared composite mortar is and the similarly even black of single-phase carbon black slurry, has no the phenomenon of obvious a certain single phase nano powder concentration of local.Adopt the Metal Substrate micro-nano powder that the prepared carbon black of this composite mortar/ceramic biphase strengthens to reach comparatively desirable quality.If the undesirable ultrasonic wave that also can adopt of mixing effect disperses or other conventional preparation method when preparing single phase nano tungsten carbide suspension.
Embodiment tri-.
Example material therefor: commercial common packed carbon black powder, average grain diameter 14nm, tinctorial strength is 140%, the addition of carbon black powder accounts for 0.15% of slurry gross mass; Commercial common bagged aluminum oxide powder, average grain diameter 50nm, is white in color, and its addition accounts for 0.6% of slurry gross mass, and all the other are absolute ethyl alcohol.
First nanometer carbon black powder is carried out to dry ball milling pretreatment, to break wherein original macro aggregate particle, mix with absolute ethyl alcohol again and be stirred to and obtain the obviously carbon black slurry semi-finished product of solid-liquid layering of nothing, 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 ℃, jitter time is 30 ~ 60 minutes, can obtain the single phase nano carbon black suspension of stably dispersing, the addition of absolute ethyl alcohol should guarantee that the mass percent of the nanometer carbon black powder in formed single phase nano carbon black suspension is not more than 1%, then, will in the alumina powder jointed absolute ethyl alcohol that adds surplus, stir and obtain single phase nano aluminum oxide suspension, finally, Manufactured single phase nano carbon black suspension and single phase nano aluminum oxide suspension are carried out to ball milling 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 that 1 hour, ball radius are not more than 4mm, can obtain Metal Substrate micro-nano powder for preparing carbon black and aluminium oxide biphase composite mortar.The prepared composite mortar forming is and the similarly even black of single-phase carbon black slurry, has no the phenomenon of obvious a certain single phase nano powder concentration of local.Adopt the Metal Substrate micro-nano powder that the prepared carbon black of this composite mortar/ceramic biphase strengthens to reach comparatively desirable quality.Equally, if undesirable ultrasonic wave dispersion or other the conventional process for dispersing of also can adopting of mixing effect disperses when preparing single phase nano aluminum oxide suspension, if have deposited phenomenon to occur, should suitably add alumina powder jointed to guarantee that content alumina powder jointed in final slurry meets the demands.
It is below contrast test method of the present invention.
One, adopt composite mortar of the present invention to prepare the micro-nano powder that biphase strengthens.
Step 1, prepares carbon black/carborundum (or other similar nano-ceramic powder) the biphase suspension mixing by method of the present invention;
Step 2, carries out spheroidization pretreatment by commercial Al-Si alloy powder and micron, obtains pretreated micron metal powder;
Step 3, by pretreated micron metal powder, carries out ball-milling after adding the carbon black/carborundum biphase suspension having mixed, and obtains carbon black/carborundum biphase and the compound micro-nano powder slurry of micron metal;
Step 4, is placed in drying box by micro-nano powder slurry dry, can obtain the collaborative Metal Substrate micro-nano powder strengthening of nanometer carbon black and nanometer silicon carbide.
The micro-nano powder that adopts the prepared carbon black of above-mentioned biphase composite mortar and carborundum biphase to strengthen, has reached comparatively desirable quality.As shown in Figure 1, in prepared micro-nano powder, nanometer carbon black and nanometer silicon carbide are polymolecularity feature and are evenly coated on micron particles surface; Meanwhile, 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 4mm/s again.
Two, preparation only contains the micro-nano powder of nanometer carbon black.
First, with reference to method of the present invention, nanometer carbon black and absolute ethyl alcohol are mixed and made into carbon black single phase nano suspension;
Secondly, commercial Al-Si alloy powder and micron is carried out to spheroidization pretreatment, obtain pretreated micron metal powder;
The 3rd, by pretreated micron metal powder, carry out ball-milling after adding carbon black single phase nano suspension, obtain carbon black single phase nano and the compound micro-nano powder slurry of micron metal;
The 4th, micro-nano powder slurry is placed in to drying box dry, can obtain the Metal Substrate micro-nano powder that carbon black single phase nano strengthens.
The Metal Substrate micro-nano powder that adopts above-mentioned prepared carbon black single phase nano to strengthen, 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 3mm/s again.
Three, preparation only contains the micro-nano powder of nanometer silicon carbide.
First, with reference to method of the present invention, nanometer silicon carbide and absolute ethyl alcohol are mixed and made into carborundum single phase nano suspension;
Secondly, commercial Al-Si alloy powder and micron is carried out to spheroidization pretreatment, obtain pretreated micron metal powder;
The 3rd, by pretreated micron metal powder, carry out ball-milling after adding carborundum single phase nano suspension, obtain carborundum single phase nano and the compound micro-nano powder slurry of micron metal;
The 4th, micro-nano powder slurry is placed in to drying box dry, can obtain the micro-nano powder that carborundum single phase nano strengthens.
The Metal Substrate micro-nano powder that adopts above-mentioned prepared carborundum single phase nano to strengthen, 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 2.5mm/s again.
The friction and wear behavior of above three kinds of wear-resisting modified layer of Metal Substrate micro-nano powder laser, as shown in table 1.Visible, adopt the prepared carbon black of composite mortar of the present invention and carborundum biphase to strengthen micro-nano powder, owing to introducing the nanometer carbon black with anti-attrition effect and the nanometer silicon carbide with wear-resistant effect simultaneously, the wear-resisting modified layer tool of prepared laser is had good wearability, and compared with single phase nano, strengthening the prepared wear-resisting modified layer of laser of micro-nano powder has significantly raising.
Table 1
| The powder adopting | Volume erosion rate | Surface microhardness | Coefficient of friction |
| With micro-nano powder of the present invention | 1.8×10 -3 cm 3/Nm | 332 HV0.1 | 0.33 |
| The micro-nano powder of preparing with the single-phase slurry of carborundum | 2.4×10 -3 cm 3/Nm | 318 HV0.1 | 0.51 |
| The micro-nano titanium valve of preparing with the single-phase slurry of carbon black | 5.3×10 -3 cm 3/Nm | 205 HV0.1 | 0.42 |
In addition, applicant has carried out identical test with titanium base, iron-based and Ni-based micron metal powder, and data and previous experiments data have good homoplasy.
Technical conceive of the present invention and feature and representative case study on implementation thereof have just been expressed in foregoing description and explanation; can not limit the scope of the invention with this; allly according to the present invention, conceive the equivalence that essence does and change or modify, all should be encompassed in protection scope of the present invention.
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 (4)
1. Metal Substrate micro-nano powder for preparing carbon black and a ceramic biphase composite mortar, is characterized in that it is comprised of nanometer carbon black powder, nano-ceramic powder and absolute ethyl alcohol; Wherein, nanometer carbon black powder accounts for 0.05% ~ 0.15% of stock quality mark, and the mass fraction of nano-ceramic powder is 4 ~ 6 times of institute's plus nano carbon black powder mass fraction, and all the other are absolute ethyl alcohol, and each constituent mass mark summation is 100%; The average grain diameter of described nano-ceramic powder is 10 ~ 50nm.
2. carbon black according to claim 1 and ceramic biphase composite mortar, is characterized in that 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 ~ 28nm.
3. carbon black according to claim 1 and ceramic biphase composite mortar, is characterized in that described nano-ceramic powder is carborundum, tungsten carbide and aluminium oxide.
4. a preparation method for carbon black and ceramic biphase composite mortar described in claim 1, is characterized in that it comprises the following steps:
First, according to required mass fraction, take nanometer carbon black powder and add anhydrous ethanol preparation to become single phase nano carbon black suspension, the mass percent of controlling nanometer carbon black powder in single phase nano carbon black suspension is not more than 1%, to guarantee that nanometer carbon black powder is without precipitation;
Then, according to required mass fraction, weigh nano-ceramic powder and add in absolute ethyl alcohol, and be prepared into single phase nano ceramic suspension liquid;
Finally, Manufactured single phase nano carbon black suspension and single phase nano ceramic suspension liquid are carried out to ball milling 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 that 1 hour, ball radius are not more than 4mm, can obtain to take carbon black and the ceramic biphase composite mortar that ethanol is medium.
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| CN101224397A (en) * | 2007-10-12 | 2008-07-23 | 南京航空航天大学 | Nanometer ceria sizing agent and preparing method thereof |
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