CN103409662A - Scale-like multi-component zinc aluminum silicon alloy powder containing Ce and Nd and preparation method thereof - Google Patents
Scale-like multi-component zinc aluminum silicon alloy powder containing Ce and Nd and preparation method thereof Download PDFInfo
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- CN103409662A CN103409662A CN2013103316919A CN201310331691A CN103409662A CN 103409662 A CN103409662 A CN 103409662A CN 2013103316919 A CN2013103316919 A CN 2013103316919A CN 201310331691 A CN201310331691 A CN 201310331691A CN 103409662 A CN103409662 A CN 103409662A
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Abstract
The invention relates to scale-like multi-component zinc aluminum silicon alloy powder containing Ce and Nd and a preparation method thereof. The particle thickness of each particle of scale-like multi-component zinc aluminum silicon alloy powder is 0.1-1 micron, and the average particle diameter of the scale-like multi-component zinc aluminum silicon alloy powder is 5-35 microns. The powder comprises the following particles with different particle sizes: less than or equal to 20% of particles with the particle diameters of less than 5 microns, equal to or greater than 70% of particles with the particle diameters of 5-33 microns, and less than or equal to 10% of particles with the particle diameters of greater than 33 microns, and the radius-thickness ratio of the average particle diameter to the average particle thickness of the scale-like multi-component zinc aluminum silicon alloy powder is 35-200. The scale-like metal powder and the preparation method thereof both provided by the invention are particularly applied in the field of the production of Dacromet coating liquid, inorganic zinc rich paint, heavyduty anticorrosive coatings and the like.
Description
Technical field
The present invention relates to the polynary aluminium zinc of a kind of flakey silicon alloy powder and preparation method thereof.
Background technology
Dacromet Technology is born in later 1950s the earliest, it is a kind of metallic coating treatment technology of similar electro-galvanizing, the scientist Mai Ke Martin of the U.S. has developed take the metal zinc metal sheet and is the main high dispersive water soluble paint that adds simultaneously aluminium flake, chromic acid, deionized water to make solvent, coating sticks on metallic matrix, through the circulation of full cut-off road, apply baking, form very thin coating.Dacromet/steel is successfully resisted the erosion of chlorion, and aseptic technic has entered new step, has reformed short defect of anticorrosion life-span of traditional technology.The Dacromet/steel outward appearance is uniform silver gray, in coating, contains 80% thin zinc metal sheet and aluminium flake, and all the other are chromic salt, have good performance, as extremely strong erosion resistance etc.; Be specially adapted to the high strength stressed member, as the high strength bolt for subway engineering; High heat resistance; Heat resisting temperature can reach 300 ℃.In addition, also have the advantages such as hypertonicity, high tack, high antifriction quality, high weather resistance, high resistance to chemicals product stability and non-environmental-pollution.In the various fields such as the automobile of industrially developed country, civil construction, electric power, chemical industry, oceanographic engineering, household electrical appliance, railway, highway, bridge, tunnel, war industry, obtained applying very widely.The Dacroment masking liquid is of a great variety at present, but it is further perfect generally still to exist defect to need, and realizes dechromising and needs further to improve its performance etc. such as needs, and the performance of the flakey alloy powder of especially comparatively common employing still can't meet processing requirement fully.
In addition, the manufacture method at domestic existing scaled metal powder end mainly contains mechanical process, Physical and chemical method etc. at present.Wherein mechanical process mainly contains ball milled and ultrasonication method, and wherein ball milled comparatively generally adopts in actual production.Ball milled is divided into again dry grinding and two kinds of complete processings of wet-milling, and wherein wet milling process mainly is included in the process of metal powder grinding the operation that adds solvent wet goods medium for example to grind, then by sorting, filter drying, screening, redrying, the operations such as packing are achieved.Above-mentioned wet milling process drying process complexity, the cycle is long, and efficiency is low, the easy oxidation of metal powder, more seriously after drying metal powder can residual a part of medium, affects use range and the quality of metal powder.And dry mill process needs long dispersed with stirring, increase energy consumption, and Superfine Zn powder, the aluminium powder of dry mill process manufacture acquisition, its shape and performance all have again larger gap with the powder that Dacroment technique needs, thereby have limited the process of Non-chromium Zn-al Coating technology industrialization.
Therefore, provide a kind of improved flakey alloy powder and preparation method thereof just to become this field and be badly in need of the technical barrier solved.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of polynary Zn-Al alloy powder of high-quality flakey that can meet extraordinary coating process requirement, and provide that a kind of efficiency is high, cost is low and be applicable to the preparation method of actual production.
The polynary Zn-Al alloy powder of flakey provided by the present invention, its components based on weight percentage is: Al: 15%-69%; Si: 0.2-3%; Mg: 0.1-5%; The total amount of at least two kinds of rare earth elements: 0.02-0.9%, and wherein said at least two kinds of rare earth elements mainly comprise Ce and Nd; Total amount is no more than 1% impurity; Surplus is Zn, the sheet of the polynary Zn-Al alloy powder of wherein said flakey is thick is 0.1～1 μ m, average sheet footpath is 5～35 μ m, and specifically consisting of of granularity wherein: the sheet footpath is less than 5 μ m and accounts for≤and 20%, sheet footpath 5～33 μ m account for >=and 70%, the sheet footpath is greater than 33 μ m≤10%, and the average sheet footpath of the polynary Zn-Al alloy powder of described flakey and the thick radius-thickness ratio of sheet are 35～200.
Preferably, the radius-thickness ratio that the average sheet footpath of the polynary Zn-Al alloy powder of wherein said flakey and sheet are thick is 50～150.
Preferably, the loose density of the polynary Zn-Al alloy powder of wherein said flakey is 1.0～3.0gcm
-3.
Preferably, the lid water area of the polynary Zn-Al alloy powder of wherein said flakey is 0.4～2.0m
2G
-1.
Preferably, the content of Ce and Nd and account for the per-cent of rare earth element total amount >=85% wherein.
On the other hand, the present invention is the manufacture method of the polynary Zn-Al alloy powder of a kind of flakey that provides also, weight percent according to polynary each component of Zn-Al alloy powder of described flakey is got the raw materials ready, each component is made to aluminium zinc in smelting furnace by proportioning, by the deep-well forging type, pour into the aluminium zinc rod again, then, the aluminium zinc rod is put into to the vacuum atomizing powder manufacturing apparatus and be atomized into the spherical aluminium zinc powder of 200～500 purpose, again described spherical aluminium zinc powder is joined in ball mill, add simultaneously grinding aid and ball-milling medium to carry out ball milling, and after first vacuumizing, pass into again in rare gas element ball mill interlayer and pass into cooling liqs and take and control temperature in mechanical milling process and be 20-60 ℃, Ball-milling Time is 8～20 hours, keeping drum's speed of rotation is 30～100 rev/mins, thereby the described spherical polynary aluminium zinc sphere of powder is worn into to the sheet alloy powder, prepare the polynary Zn-Al alloy powder of described flakey.
Preferably, wherein grinding aid is one or more mixing in Zinic stearas, calcium stearate, moly-sulfide, polyvinyl alcohol, Sodium dodecylbenzene sulfonate, glyceryl alcohol.
Preferably, wherein grinding aid adds according to 1%～10% ratio of described spherical polynary zinc-aluminium powder weight.
Preferably, wherein ball-milling medium is Ceramic Balls or steel ball, and its particle diameter is the 1-15 millimeter.
Preferably, wherein ball-milling medium and described spherical polynary zinc-aluminium powder are (6～20) by weight: 1.
Average sheet footpath 5～35 μ m of the polynary Zn-Al alloy powder of flakey of the present invention, and specifically consisting of of granularity wherein: the sheet footpath is less than 5 μ m and accounts for≤20%, and sheet footpath 5～33 μ m account for >=and 70%, the sheet footpath is greater than 33 μ m≤10%.The concrete composition of this granularity of the present invention has not only guaranteed the requirement in average sheet footpath, and make the powder geometrical dimension be evenly distributed, and size-grade distribution is conducive to reduce the defects such as hole in coating uniformly, form the structure of " layer upon layer of " uniformly, thereby be conducive to suppress the infiltration of corrosive medium, thereby improve the antiseptic property of coating.
The sheet of the polynary Zn-Al alloy powder of flakey of the present invention is thick is 0.1～1 μ m, average sheet footpath is 5～35 μ m, average sheet footpath and the thick radius-thickness ratio of sheet are 35～200, have improved greatly the radius-thickness ratio of the polynary aluminium zinc powder of flakey, and this is of great immediate significance.Because the raising of radius-thickness ratio, in the time of can reducing on the one hand the coating coating, the usage quantity of per unit area aluminium zinc powder, reduce production cost greatly; On the other hand, the raising of radius-thickness ratio, the sheet aluminium zinc powder that can make to be coated in workpiece spare surface is more closely knit, reduces while applying because the sheet alloy powder is blocked up or the space caused in uneven thickness, sheet footpath, improves the antiseptic property after coating applies.Therefore, the polynary Zn-Al alloy powder of flakey of the present invention is obtained important breakthrough with respect to prior art.
Further, the loose density of the polynary Zn-Al alloy powder of flakey of the present invention is 1.0～3.0gcm
-3, this is also that the contriver has paid just finally acquisition of performing creative labour.Because it is a lot of to affect the factor of apparent density of powder, as powder particle shape, size and size-grade distribution etc.And these factors can have again significant difference because of the preparation method of powder and the difference of processing condition thereof.And the polynary Zn-Al alloy powder of flakey described in the present invention is to meet particle size less, under the higher precondition of sheet degree, by the improvement on production technique, further realized less loose density, thereby improved the dispersiveness of the polynary aluminium zinc powder of flakey in coating, also further more met the service requirements of Dyclo paint.
Further, by the improvement on production technique, to make the lid water area of the polynary Zn-Al alloy powder of described flakey be 0.4～2.0m in the present invention
2G
-1, illustrating that the polynary aluminium zinc powder of flakey of the present invention sheet degree is higher, spreadability is better, good dispersity in water.The lid water area of the polynary aluminium zinc powder of the flakey in the present invention has surpassed the lid water area of domestic simple zinc powder, even can reach the standard of external simple zinc powder product, has obtained very outstanding technique effect.
On the other hand, the preparation method of scaled metal powder provided by the present invention has compared with prior art replaced in the wet-milling by the defect of liquid as the grinding medium, by adding grinding aid and ball-milling medium to grind, metal powder after drying can residual any medium, has guaranteed use range and the quality of metal powder.
Further, the grinding aid wherein added and ball-milling medium, also guaranteed can not produce the cold welding phenomenon between metal powder.
Further, pass into rare gas element in airtight ball mill, can avoid oxygen to enter, prevent the metal powder oxidation.
Further, the temperature of controlling metal powder by the method for regulating the cooling water inflow in the ball mill interlayer in mechanical milling process is between 20～60 ℃, and the rotating speed of regulating simultaneously ball mill carries out ball milling at 30-100 rev/min, can be by spherical metal powder ball milling slabbing metal powder.
In addition, by controlling different rotational speed of ball-mill, can also improve quality and the use range of metal powder, make prepared metal powder not only can be used for Dyclo paint, also can be used for other protective systems such as zinc rich paint.
Further, in the present invention ball mill by the sandwich structure of setting up, make cooling liqs for example water be to be passed into by the ball mill interlayer, rather than directly with powder, contact.With traditional wet-milling and long dry grind process, compare, and adopt water-cool control ball milling temperature, not only still avoided the defect of wet-milling, also overcome and needed long-time dry deficiency, improved greatly production efficiency.
In addition, the polynary aluminium zinc powder of flakey provided by the present invention adopts the dry type ball milling method to obtain, the impact on follow-up coating property of the medium that while having avoided wet grinding fully, powder surface coats such as solvent oil.
Finally, aluminium zinc powder provided by the invention is due to the passivation of aluminium, greatly slowed down the wear rate of zinc, for the powder or its mixed powder of the domestic and international single zinc that there is no alloying of producing, aluminium, antiseptic property and the anticorrosion life-span of having improved greatly coating.
In sum, scaled metal powder provided by the invention end and preparation method thereof, be particularly suitable for producing the Dacroment masking liquid, inorganic zinc rich paint, the fields such as heavy duty system.Moreover, adopt the preparation method who provides of the present invention to go for equally the production of other flake metal powders, for example: aluminium powder, copper powder, cu-zn alloy powder, silver powder etc.
The accompanying drawing explanation
Fig. 1 horizontal ball mill sandwich structure figure
Embodiment
The polynary aluminium zinc of flakey of the present invention silicon alloy powder is elementary composition by A1, Si, Mg, Zn and rare earth etc., some preferred specific embodiments of each composition weight percent in the present invention in table 1, have been listed, but the content of each moiety of the present invention is not limited to concrete numerical value listed in table 1, to those skilled in the art, fully can on the basis of the listed concrete numerical value of table 1, rationally summarize and derive.
It should be noted that, the present invention is on the basis that a kind of polynary Zn-Al alloy powder of high-quality flakey that can meet extraordinary coating process requirement is provided, by the further improvement on production technique, make the performance of described flakey aluminium zinc silicon alloy powder all be more than flakey powdered alloy of the prior art far away, the interior microscopic that flakey aluminium zinc silicon alloy powder of the present invention is described is organized very large variation has also been occurred, although these micro-variations can't with the structure of flakey aluminium zinc silicon alloy powder and/or composition etc. further restriction described, but by further describing of table 1 performance parameter, those skilled in the art can clearly be known its restriction effect of playing to flakey aluminium zinc silicon alloy powder of the present invention.
But in table 1, the performance perameter such as related loose density and lid water area is not but to solve the requisite technical characterictic of the present invention, it is only the more excellent technical scheme that the present invention further obtains with respect to prior art.For the present invention, the content of core is the setting of the polynary Zn-Al alloy powder composition of flakey, especially the setting of the concrete composition of thick, the sheet footpath of sheets of powder, granularity and radius-thickness ratio and reach the goal of the invention that is suitable for producing the masking liquids such as Dacroment.And on this basis, the further improvement by production technique is all to make this technique effect more outstanding, more superior.Therefore, in following table 1 in specification sheets, put down in writing simultaneously loose density and these two performance perameters of lid water area, be also in order to introduce more in detail, easily technical scheme of the present invention, and not as the essential features that solves the technology of the present invention problem, described.
Similar therewith, table 1 further provides composition and the concrete content thereof of the concrete rare earth element adopted of the present invention and is described as preferred embodiment, those skilled in the art should determine not to be only to adopt the rare earth element and the content thereof that in table 1, provide can solve its technical problem, those skilled in the art must determine, as long as meet the total amount of rare earth element in the scope of 0.02-0.9%, in table 1, provide on the basis of two kinds of rare earth elements and content thereof, add in right amount other rare earth elements and can solve its technical problem equally.Therefore, two kinds of rare earth elements in table 1 are not described as prerequisite equally.
Each composition of table 1 (weight percent) and performance perameter thereof
Below in conjunction with accompanying drawing 1, illustrate the present invention and prepare the polynary Zn-Al alloy powder embodiment of flakey, at first, get the raw materials ready on request, and each component is made to aluminium zinc by proportioning in smelting furnace, then pour into the aluminium zinc rod by the deep-well forging type.Then, the aluminium zinc rod is put into to the vacuum atomizing powder manufacturing apparatus and be atomized into 200～500 purpose spherical powders, again spherical aluminium zinc powder is joined in ball mill, add simultaneously grinding aid, ball-milling medium carries out ball milling, after first vacuumizing, pass into again rare gas element, in ball mill interlayer 1, passing into cooling liqs take and control the ball milling temperature and be 20-60 ℃, Ball-milling Time is 8～20 hours, keeping drum's speed of rotation is 30～100 rev/mins, the spherical polynary aluminium zinc sphere of powder is worn into to the sheet alloy powder, prepare the polynary Zn-Al alloy powder of flakey.
The ball mill that the present invention adopts is to have set up a ball mill interlayer 1 on the basis of horizontal ball mill of prior art, thereby can in interlayer 1, pass into cooling liqs to control the ball milling temperature, thereby realize that cooling liqs and powder separation do not contact to overcome the goal of the invention of wet-milling defect.
Preferably, ball-milling additive comprises Zinic stearas, calcium stearate, moly-sulfide, polyvinyl alcohol, Sodium dodecylbenzene sulfonate, glyceryl alcohol etc.Stearate, moly-sulfide consumption are the 1-10% of metal-powder weight.
Preferably, adopting the ball-milling medium diameter is 1-15mm, preferably ceramic ball or steel ball etc., and the ratio of itself and raw material aluminium zinc silicon alloy powder is 6: 1 to 20: 1.
Preferably, the ball mill running speed is not less than 30r/min, and preferred range of choice is 30-100r/min.
Embodiment 1:
Get 300 order aluminium zinc silicon alloy powder raw material 10Kg, Zinic stearas 0.4Kg, steel ball 200Kg drops in ball mill, passes into nitrogen after vacuumizing, and connects water coolant, guarantees in mechanical milling process that temperature is between 30-40 ℃.With discharging after the rotating speed ball milling 10h of 50r/min, the powder after ball milling is dropped in polishing machine and carries out polishing, after the powder after polishing is classified, make flaky aluminum zinc silicon alloy powder.
Embodiment 2:
Get 200 order aluminium zinc silicon alloy powder raw material 10Kg, polyvinyl alcohol 0.1Kg, calcium stearate 0.2Kg, steel ball 120Kg drops in ball mill, passes into nitrogen after vacuumizing, and connects water coolant, guarantee in mechanical milling process that temperature is between 30-40 ℃, with the rotating speed ball milling 14h discharging of 100r/min, the powder after ball milling is dropped in polishing machine and carries out polishing, after the powder after polishing is classified, make flaky aluminum zinc silicon alloy powder.
Claims (10)
1. polynary Zn-Al alloy powder of flakey, its components based on weight percentage is: Al:15%-69%; Si:0.2-3%; Mg:0.1-5%; The total amount of at least two kinds of rare earth elements: 0.02-0.9%, and wherein said at least two kinds of rare earth elements mainly comprise Ce and Nd; Total amount is no more than 1% impurity; Surplus is Zn, the sheet of the polynary Zn-Al alloy powder of wherein said flakey is thick is 0.1～1 μ m, average sheet footpath is 5～35 μ m, and specifically consisting of of granularity wherein: the sheet footpath is less than 5 μ m and accounts for≤and 20%, sheet footpath 5～33 μ m account for >=and 70%, the sheet footpath is greater than 33 μ m≤10%, and the average sheet footpath of the polynary Zn-Al alloy powder of described flakey and the thick radius-thickness ratio of sheet are 35～200.
2. the polynary Zn-Al alloy powder of flakey as claimed in claim 1, the radius-thickness ratio that the average sheet footpath of the polynary Zn-Al alloy powder of wherein said flakey and sheet are thick is 50～150.
3. the polynary Zn-Al alloy powder of flakey as claimed in claim 1, the loose density of the polynary Zn-Al alloy powder of wherein said flakey is 1.0～3.0gcm
-3.
4. the polynary Zn-Al alloy powder of flakey as claimed in claim 1, the lid water area of the polynary Zn-Al alloy powder of wherein said flakey is 0.4～2.0m
2G
-1.
5. the polynary Zn-Al alloy powder of flakey as claimed in claim 1, the wherein content of Ce and Nd and account for the per-cent of rare earth element total amount >=85%.
6. method for preparing the polynary Zn-Al alloy powder of the described flakey of claim 1, weight percent according to polynary each component of Zn-Al alloy powder of the described flakey of claim 1 is got the raw materials ready, each component is made to aluminium zinc in smelting furnace by proportioning, by the deep-well forging type, pour into the aluminium zinc rod again, then, the aluminium zinc rod is put into to the vacuum atomizing powder manufacturing apparatus and be atomized into the spherical aluminium zinc powder of 200～500 purpose, again described spherical aluminium zinc powder is joined in ball mill, add simultaneously grinding aid and ball-milling medium to carry out ball milling, and after first vacuumizing, pass into again rare gas element, in the ball mill interlayer, passing into cooling liqs take and control temperature in mechanical milling process and be 20-60 ℃, Ball-milling Time is 8～20 hours, keeping drum's speed of rotation is 30～100 rev/mins, thereby the described spherical polynary aluminium zinc sphere of powder is worn into to the sheet alloy powder, prepare the polynary Zn-Al alloy powder of described flakey.
7. method as claimed in claim 6, wherein grinding aid is one or more mixing in Zinic stearas, calcium stearate, moly-sulfide, polyvinyl alcohol, Sodium dodecylbenzene sulfonate, glyceryl alcohol.
8. method as claimed in claim 6, wherein grinding aid adds according to 1%～10% ratio of described spherical polynary zinc-aluminium powder weight.
9. method as claimed in claim 6, wherein ball-milling medium is Ceramic Balls or steel ball, its particle diameter is the 1-15 millimeter.
10. method as claimed in claim 6, wherein ball-milling medium and described spherical polynary zinc-aluminium powder are by weight being (6～20): 1.
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| CN112517912A (en) * | 2020-11-11 | 2021-03-19 | 西安理工大学 | Surface anticorrosion treatment method for powder metallurgy iron-based part |
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