CN104972108B - Ultrafine zinc alloy powder and preparation method thereof - Google Patents
Ultrafine zinc alloy powder and preparation method thereof Download PDFInfo
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Abstract
The invention provides a ultrafine zinc alloy powder and a preparation method thereof, wherein the particle size range of the ultrafine zinc alloy powder is 1-100nm. The ultrafine zinc alloy powder comprises light rare earth element lanthanum, cerium and heavy rare earth element gadolinium, wherein the light rare earth element lanthanum, and the cerium and the heavy rare earth element gadolinium can restrain crystal particles to grow on one hand and form a fine crystal particle grain boundary strengthening mechanism, can play the role of degassing and removing impunities on the other hand, thereby reducing damage to alloy. Simultaneously, less nickel, cobalt and stibium are added into the ultrafine zinc alloy powder, can obviously improve anti-corrosion and oxidation resistance. Trace amount of indium, bismuth, aluminum and calcium metal are added into the ultrafine zinc alloy powder, and the alloy performance of the ultrafine zinc alloy powder is enhanced. The ultrafine zinc alloy powder does not comprise poisonous and harmful elements such as mercury, lead and cadmium, can not cause environment pollution and ecological damage, and is green and environmentally friendly.
Description
Technical field
The invention belongs to non-ferrous alloy dusty material technical field, be specifically related to a kind of ultra-fine Zinc alloy powder and
Its preparation method, is mainly used in using as the additive of coating.
Background technology
Zinc powder is a kind of important raw material of industry, and market demand is very big, is widely used in metallurgy, chemical industry, building, friendship
There are atomization and vaporization condensation process in the fields such as logical, medicine, electronics, the production method of zinc powder.Producing Zinc Powders by Gas Atomization, such as air-flow are sprayed
Atomization is penetrated, water-jet atomization, product recovery rate are low, and power consumption is big, also there is granule.Current country's work
The method that industry metaplasia produces zinc powder is more based on vaporization condensation process, and using coal, coal gas or electricity as the energy, zinc ingot metal is heated by zinc-melting furnace
Fusing produces zinc powder until evaporation is condensed again.
With the development of science and technology, super-fine material causes people's more and more due to its excellent combination property
Concern and research, super-fine zinc dust is exactly one of them.Super-fine zinc dust refers to zinc powder of the granularity in below 100nm, unique due to which
Physicochemical properties, there is wide application in fields such as Chemical Manufacture, lubricating additive, coating, high performance electrode materials
Prospect, super-fine zinc dust have become one of focus of countries in the world scientist research.The national demand mesh of super-fine zinc dust
Before be more than 100,000 tons/year, and cumulative year after year, price is 3～4 times of common zinc powder price.At present, most row of super-fine zinc dust
Industry or coating and anti-corrosion, can make zinc-rich paint or directly be plated on anticorrosive coat.Zinc powder particle diameter is more tiny, and surface activity is got over
Greatly, be conducive to the formation of coating.
The preparation method of zinc powder mainly has the way of distillation, atomization, high-energy ball milling method, electrolysis and is evaporated in vacuo cold both at home and abroad
Solidifying method.The zinc powder particle diameter that wherein prepared by atomization is more than l0 μm, thus can not prepare super-fine zinc dust.The production efficiency of the way of distillation
Height, but obtained super-fine zinc dust activity is relatively low.Super-fine zinc dust obtained in high-energy ball milling method is flakey, but is easily polluted.It is Chinese special
The technique proposed in sharp CN1450182A and CN1482263A has promoted the large-scale production of alkaline process electrolytic zinc powder technique, but this
The zinc powder particle diameter that flow process is produced is bigger than normal, and thickness is uneven, and preparing super-fine zinc dust need to be ground with ball mill, high energy consumption, technique
It is complicated.China 201210034534.7, has preferably refined zinc powder by adding lead-containing compounds, but there is also micro lead precipitation
Problem.
But, the decay resistance for being pure zinc powder by the technical problem that the additive that pure zinc powder is used as coating is present at present is
Jing can not meet the demand for development of coating, so people start little by little to attempt to substitute Zinc alloy powder pure zinc powder as corrosion-resistant
Coating additive is used.Conventional Zinc alloy powder would generally use the poisonous and harmful alloying element such as hydrargyrum and lead at present, use these
The Zinc alloy powder of element can cause environmental pollution and ecological disruption in being added to coating, it is impossible to enough meet current environmental protection
Require.
In order to solve above-mentioned technical problem, the invention provides a kind of ultra-fine Zinc alloy powder and preparation method thereof, this
The ultra-fine Zinc alloy powder of bright preparation can replace traditional pure zinc powder to use as the corrosion-resistant additive of coating, and zinc is closed
Without poisonous and harmful elements such as cadmium, hydrargyrum and lead in golden composition, environmental pollution and ecological disruption, environmental protection are not resulted in.
The content of the invention
It is an object of the invention to provide a kind of ultra-fine Zinc alloy powder and preparation method thereof, can substitute traditional pure zinc powder
End is used as the corrosion-resistant additive of coating, and without the poisonous and harmful elements such as cadmium, hydrargyrum and lead, Bu Huizao in kirsite composition
Into environmental pollution and ecological disruption, environmental protection.The present invention passes through the preferred of alloying component and content so that what is prepared is super
Alloy in thin Zinc alloy powder is grown in dendritic mode, and crystal grain refinement drops low-alloyed crystal boundary energy, strengthens its alloying
Can, and the corrosion-resistant and antioxygenic property of Zinc alloy powder can be significantly increased.
Technical scheme is as follows：
One aspect of the present invention provides a kind of ultra-fine Zinc alloy powder, and the particle size range of described ultra-fine Zinc alloy powder is
1～100nm；Characterized in that, the quality composition of described kirsite is as follows：
Nickel：0.60wt%～0.80wt%；Antimony：0.10wt%～0.15wt%；Cobalt：0.05wt%～0.15wt%；Lanthanum：
0.25wt%～0.35wt%；Cerium：0.15wt%～0.25wt%；Gadolinium：0.05wt%～0.15wt%；Indium：100～
300ppm；Bismuth：100～300ppm；Aluminum：100～150ppm；Calcium：100～200ppm；Balance of zinc.
In a preferred technical scheme, the quality composition of described kirsite is as follows：
Nickel：0.80wt%；Antimony：0.15wt%；Cobalt：0.05wt%；Lanthanum：0.25wt%；Cerium：0.25wt%；Gadolinium：
0.15wt%；Indium：100ppm；Bismuth：100ppm；Aluminum：150ppm；Calcium：200ppm；Balance of zinc.
In a preferred technical scheme, the quality composition of described kirsite is as follows：
Nickel：0.60wt%；Antimony：0.10wt%；Cobalt：0.15wt%；Lanthanum：0.35wt%；Cerium：0.15wt%；Gadolinium：
0.05wt%；Indium：300ppm；Bismuth：300ppm；Aluminum：100ppm；Calcium：100ppm；Balance of zinc.
In a preferred technical scheme, the quality composition of described kirsite is as follows：
Nickel：0.70wt%；Antimony：0.12wt%；Cobalt：0.10wt%；Lanthanum：0.30wt%；Cerium：0.20wt%；Gadolinium：
0.10wt%；Indium：200ppm；Bismuth：200ppm；Aluminum：125ppm；Calcium：150ppm；Balance of zinc.
In a preferred technical scheme, the particle size range of described ultra-fine Zinc alloy powder is as follows：1nm ＜ particle diameters≤
The Zinc alloy powder of 20nm accounts for the 20wt%～30wt% of total Zinc alloy powder, the Zinc alloy powder of 80nm >=particle diameter ＞ 20nm
Account for the 40wt%～60wt% of total Zinc alloy powder, the remaining Zinc alloy powder for 100nm >=particle diameter ＞ 80nm.
Another aspect of the present invention provides a kind of preparation method of ultra-fine Zinc alloy powder, it is characterised in that concrete steps
It is as follows：
Step 1, prepare nano zinc powder：First nano-zinc oxide powder is placed in reduction furnace, after sealing with 80～
100ml/min is passed through and the CO and H for producing is cracked by methanol oxidation2, 410 DEG C～450 DEG C 50～60min of reaction are then heated to,
High-purity nm zinc powder is obtained after cooling；
Step 2, melting：Quality according to described kirsite constitutes the high-purity nm zinc powder and its for preparing step 1
Its analytically pure raw metal is placed in crucible type melting furnace, melts and remove surface oxidation at a temperature of 660 DEG C～680 DEG C
Slag；
Step 3, distillation：The kirsite liquid of above-mentioned gained is added in vicariouss electric heating crucible retort, 940
DEG C～960 DEG C at a temperature of distilled；
Step 4, backflow：The kirsite steam that above-mentioned distillation is produced is imported in return duct, reflux section temperature is 920 DEG C
～940 DEG C, realize kirsite vapor portion condensing reflux decontamination, the high-boiling-point impurity in zinc fume with backflow zinc return again to into
Row distillation；
Step 5, hyperthermia and superheating：Pure kirsite steam Jing after above-mentioned backflow is entered in the superheat section of return duct,
Hyperthermia and superheating process is carried out at a temperature of 1400 DEG C～1500 DEG C；
Step 6, condensation：By the high-temperature zinc alloy steam after hyperthermia and superheating is processed under pure nitrogen gas atmosphere, at 60 DEG C
Drastically condense at a temperature of～70 DEG C, obtain described ultra-fine Zinc alloy powder；
Step 7, surface treatment：Dispersion on surface process is carried out to ultra-fine Zinc alloy powder obtained in step 6, it is super by what is obtained
Thin Zinc alloy powder is put in dispersant and is surface-treated, and immersion took out drying after 6～8 hours, obtains the ultra-fine zinc of finished product and closes
Bronze end.
In a preferred technical scheme, the particle size range of described ultra-fine Zinc alloy powder is as follows：1nm ＜ particle diameters≤
The Zinc alloy powder of 20nm accounts for the 20wt%～30wt% of total Zinc alloy powder, the Zinc alloy powder of 80nm >=particle diameter ＞ 20nm
Account for the 40wt%～60wt% of total Zinc alloy powder, the remaining Zinc alloy powder for 100nm >=particle diameter ＞ 80nm.
In a preferred technical scheme, described dispersant is the one of ethyl acetate, Polyethylene Glycol or polyvinyl alcohol
Plant or its mixture.
Above-mentioned ultra-fine Zinc alloy powder is for the additive as coating.
The technique effect of the present invention is as follows：
Contain LREE lanthanum, cerium and heavy rare earth element gadolinium in the Zinc alloy powder that the present invention is provided.Rare-earth elements of lanthanum, cerium
On the one hand fine grain intercrystalline strengthening mechanism can be formed, crystal boundary is enriched in due to Thermodynamic effect with inhibiting grain growth with gadolinium
In, alloy is grown in dendritic mode, produces more nucleus of crystal, so that crystal grain refinement, on the other hand can play degassing and remove
Miscellaneous effect, because rare-earth elements of lanthanum, cerium and the gaseous impurity such as gadolinium cerium and the oxygen in alloy, hydrogen, sulfur have stronger affinity, can
Compound is formed therewith, so as to reduce the harm to alloy；Meanwhile, the cooperation of LREE lanthanum, cerium and heavy rare earth element gadolinium
Addition can refine the crystal grain of kirsite, reduce its crystal boundary energy.
A small amount of nickel be with the addition of in the Zinc alloy powder that the present invention is provided, its corrosion-resistant and non-oxidizability can be significantly increased
Energy.
Micro indium, bismuth, aluminum and calcium metal be with the addition of in the Zinc alloy powder that the present invention is provided, strengthen its alloying performance.
Not comprising the poisonous and harmful element such as hydrargyrum, lead, cadmium in the Zinc alloy powder that the present invention is provided, do not result in environmental pollution and
Ecological disruption, environmental protection.
The present invention cracks reduction-oxidation zinc using methanol oxidation and prepares high-purity nm zinc powder as the preparation present invention's
The primary raw material of ultra-fine Zinc alloy powder, the high-purity nm zinc powder prepared using reduction-oxidation zinc is as raw material relative to normal
The zinc powder of scale cun can be greatly enhanced the activity of raw material, increase the apparent activation energy of raw material, be finally very advantageous in ultra-fine
Zinc alloy powder is obtained.
Except reduction-oxidation zinc being cracked using methanol oxidation prepare high-purity nm zinc powder as the super of the preparation present invention
The primary raw material of thin Zinc alloy powder, the present invention, are adjusted by reasonably control as raw material also using analytically pure other metals
Section melt temperature, vapo(u)rizing temperature, reflux temperature, hyperthermia and superheating temperature, quenching temperature and corresponding technique, finally give optimization
The preparation technology of ultra-fine Zinc alloy powder afterwards, has prepared the ultra-fine Zinc alloy powder of excellent combination property.
Specific embodiment
Embodiment one
A kind of ultra-fine Zinc alloy powder, the particle size range of described ultra-fine Zinc alloy powder is 1～100nm；Described zinc
The quality composition of alloy is as follows：
Nickel：0.80wt%；Antimony：0.15wt%；Cobalt：0.05wt%；Lanthanum：0.25wt%；Cerium：0.25wt%；Gadolinium：
0.15wt%；Indium：100ppm；Bismuth：100ppm；Aluminum：150ppm；Calcium：200ppm；Balance of zinc.
The particle size range of described ultra-fine Zinc alloy powder is as follows：The Zinc alloy powder of 1nm ＜ particle diameters≤20nm accounts for total
The Zinc alloy powder of the 20wt%～30wt% of Zinc alloy powder, 80nm >=particle diameter ＞ 20nm accounts for total Zinc alloy powder
40wt%～60wt%, the remaining Zinc alloy powder for 100nm >=particle diameter ＞ 80nm.
The preparation method of above-mentioned ultra-fine Zinc alloy powder is comprised the following steps that：
Step 1, prepare nano zinc powder：First nano-zinc oxide powder is placed in reduction furnace, after sealing with 80～
100ml/min is passed through and the CO and H for producing is cracked by methanol oxidation2, 410 DEG C～450 DEG C 50～60min of reaction are then heated to,
High-purity nm zinc powder is obtained after cooling；
Step 2, melting：Quality according to described kirsite constitutes the high-purity nm zinc powder and its for preparing step 1
Its analytically pure raw metal is placed in crucible type melting furnace, melts and remove surface oxidation at a temperature of 660 DEG C～680 DEG C
Slag；
Step 3, distillation：The kirsite liquid of above-mentioned gained is added in vicariouss electric heating crucible retort, 940
DEG C～960 DEG C at a temperature of distilled；
Step 4, backflow：The kirsite steam that above-mentioned distillation is produced is imported in return duct, reflux section temperature is 920 DEG C
～940 DEG C, realize kirsite vapor portion condensing reflux decontamination, the high-boiling-point impurity in zinc fume with backflow zinc return again to into
Row distillation；
Step 5, hyperthermia and superheating：Pure kirsite steam Jing after above-mentioned backflow is entered in the superheat section of return duct,
Hyperthermia and superheating process is carried out at a temperature of 1400 DEG C～1500 DEG C；
Step 6, condensation：By the high-temperature zinc alloy steam after hyperthermia and superheating is processed under pure nitrogen gas atmosphere, at 60 DEG C
Drastically condense at a temperature of～70 DEG C, obtain described ultra-fine Zinc alloy powder；
Step 7, surface treatment：Dispersion on surface process is carried out to ultra-fine Zinc alloy powder obtained in step 6, it is super by what is obtained
Thin Zinc alloy powder is put in dispersant and is surface-treated, and immersion took out drying after 6～8 hours, obtains the ultra-fine zinc of finished product and closes
Bronze end, described dispersant are one kind or its mixture of ethyl acetate, Polyethylene Glycol or polyvinyl alcohol.
The above-mentioned ultra-fine Zinc alloy powder for preparing is used for the additive as coating.
Embodiment two
A kind of ultra-fine Zinc alloy powder, the particle size range of described ultra-fine Zinc alloy powder is 1～100nm；Described zinc
The quality composition of alloy is as follows：
Nickel：0.60wt%；Antimony：0.10wt%；Cobalt：0.15wt%；Lanthanum：0.35wt%；Cerium：0.15wt%；Gadolinium：
0.05wt%；Indium：300ppm；Bismuth：300ppm；Aluminum：100ppm；Calcium：100ppm；Balance of zinc.
Its preparation method is identical with embodiment one.
The above-mentioned ultra-fine Zinc alloy powder for preparing is used for the additive as coating.
Embodiment three
A kind of ultra-fine Zinc alloy powder, the particle size range of described ultra-fine Zinc alloy powder is 1～100nm；Described zinc
The quality composition of alloy is as follows：
Nickel：0.70wt%；Antimony：0.12wt%；Cobalt：0.10wt%；Lanthanum：0.30wt%；Cerium：0.20wt%；Gadolinium：
0.10wt%；Indium：200ppm；Bismuth：200ppm；Aluminum：125ppm；Calcium：150ppm；Balance of zinc.
Its preparation method is identical with embodiment one.
The above-mentioned ultra-fine Zinc alloy powder for preparing is used for the additive as coating.
Claims (8)
1. a kind of ultra-fine Zinc alloy powder, the particle size range of described ultra-fine Zinc alloy powder is 1～100nm；Characterized in that,
The quality composition of described kirsite is as follows：
Nickel：0.60wt%～0.80wt%；Antimony：0.10wt%～0.15wt%；Cobalt：0.05wt%～0.15wt%；Lanthanum：
0.25wt%～0.35wt%；Cerium：0.15wt%～0.25wt%；Gadolinium：0.05wt%～0.15wt%；Indium：100～
300ppm；Bismuth：100～300ppm；Aluminum：100～150ppm；Calcium：100～200ppm；Balance of zinc；
The particle size range of described ultra-fine Zinc alloy powder is as follows：The Zinc alloy powder of 1nm ＜ particle diameters≤20nm accounts for total zinc and closes
20wt%～the 30wt% at bronze end, the Zinc alloy powder of 80nm >=particle diameter ＞ 20nm account for the 40wt% of total Zinc alloy powder～
60wt%, the remaining Zinc alloy powder for 100nm >=particle diameter ＞ 80nm.
2. a kind of ultra-fine Zinc alloy powder according to claim 1, it is characterised in that the quality composition of described kirsite
It is as follows：
Nickel：0.80wt%；Antimony：0.15wt%；Cobalt：0.05wt%；Lanthanum：0.25wt%；Cerium：0.25wt%；Gadolinium：0.15wt%；
Indium：100ppm；Bismuth：100ppm；Aluminum：150ppm；Calcium：200ppm；Balance of zinc.
3. a kind of ultra-fine Zinc alloy powder according to claim 1, it is characterised in that the quality composition of described kirsite
It is as follows：
Nickel：0.60wt%；Antimony：0.10wt%；Cobalt：0.15wt%；Lanthanum：0.35wt%；Cerium：0.15wt%；Gadolinium：0.05wt%；
Indium：300ppm；Bismuth：300ppm；Aluminum：100ppm；Calcium：100ppm；Balance of zinc.
4. a kind of ultra-fine Zinc alloy powder according to claim 1, it is characterised in that the quality composition of described kirsite
It is as follows：
Nickel：0.70wt%；Antimony：0.12wt%；Cobalt：0.10wt%；Lanthanum：0.30wt%；Cerium：0.20wt%；Gadolinium：0.10wt%；
Indium：200ppm；Bismuth：200ppm；Aluminum：125ppm；Calcium：150ppm；Balance of zinc.
5. the preparation method of a kind of ultra-fine Zinc alloy powder described in any one of Claims 1 to 4 claim, its feature exist
In comprising the following steps that：
Step 1, prepare nano zinc powder：First nano-zinc oxide powder is placed in reduction furnace, with 80～100ml/min after sealing
It is passed through and the CO and H for producing is cracked by methanol oxidation2, 410 DEG C～450 DEG C 50～60min of reaction are then heated to, are obtained after cooling
High-purity nm zinc powder；
Step 2, melting：High-purity nm zinc powder and other points that step 1 is prepared by the quality composition according to described kirsite
The pure raw metal of analysis is placed in crucible type melting furnace, melts and remove Surface Oxygen slugging at a temperature of 660 DEG C～680 DEG C；
Step 3, distillation：The kirsite liquid of above-mentioned gained is added in vicariouss electric heating crucible retort, 940 DEG C～
Distilled at a temperature of 960 DEG C；
Step 4, backflow：By above-mentioned distillation produce kirsite steam import in return duct, reflux section temperature be 920 DEG C～
940 DEG C, kirsite vapor portion condensing reflux decontamination is realized, the high-boiling-point impurity in zinc fume returns again to carry out with backflow zinc
Distillation；
Step 5, hyperthermia and superheating：Pure kirsite steam Jing after above-mentioned backflow is entered in the superheat section of return duct, at 1400 DEG C
Hyperthermia and superheating process is carried out at a temperature of～1500 DEG C；
Step 6, condensation：By the high-temperature zinc alloy steam after hyperthermia and superheating is processed under pure nitrogen gas atmosphere, 60 DEG C～70
Drastically condense at a temperature of DEG C, obtain described ultra-fine Zinc alloy powder；
Step 7, surface treatment：Dispersion on surface process is carried out to ultra-fine Zinc alloy powder obtained in step 6, by the ultra-fine zinc for obtaining
Alloy powder is put in dispersant and is surface-treated, and immersion took out drying after 6～8 hours, obtained the ultra-fine Zinc alloy powder of finished product
End.
6. a kind of preparation method of ultra-fine Zinc alloy powder according to claim 5, it is characterised in that described ultra-fine zinc
The particle size range of alloy powder is as follows：The Zinc alloy powder of 1nm ＜ particle diameters≤20nm account for the 20wt% of total Zinc alloy powder～
The Zinc alloy powder of 30wt%, 80nm >=particle diameter ＞ 20nm accounts for the 40wt%～60wt% of total Zinc alloy powder, and remainder is
The Zinc alloy powder of 100nm >=particle diameter ＞ 80nm.
7. the preparation method of a kind of ultra-fine Zinc alloy powder according to claim 5 or 6, it is characterised in that described point
Powder one kind or its mixture for ethyl acetate, Polyethylene Glycol or polyvinyl alcohol.
8. a kind of ultra-fine Zinc alloy powder described in any one of Claims 1 to 4 claim is for the additive as coating.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5425798A (en) * | 1991-05-16 | 1995-06-20 | Mitsui Mining & Smelting Co., Ltd. | Zinc alloy powder for alkaline cell and method to produce the same |
| BE1007443A3 (en) * | 1993-02-25 | 1995-07-04 | Union Miniere Sa | Zinc powder for alkaline batteries. |
| BE1008715A3 (en) * | 1994-09-05 | 1996-07-02 | Union Miniere Sa | Zinc powder for alkaline batteries. |
| CN100420527C (en) * | 2005-12-28 | 2008-09-24 | 北京北矿锌业有限责任公司 | Production equipment of high-purity superfine active zinc powder and method for preparing same |
| CN102039420A (en) * | 2010-11-02 | 2011-05-04 | 广东工业大学 | Method for preparing superfine zinc powder from hot galvanizing zinc slag wastes through vacuum evaporation and rapid condensation |
| CN202963462U (en) * | 2012-11-27 | 2013-06-05 | 天津滨海新区中冠锌品有限公司 | Condenser used for high-fineness zinc powder manufacturing |
| CN103831441A (en) * | 2012-11-27 | 2014-06-04 | 天津滨海新区中冠锌品有限公司 | Method for preparing high-fineness zinc powder |
| CN203530397U (en) * | 2013-09-24 | 2014-04-09 | 河北钢铁股份有限公司邯郸分公司 | Detachable condensing device for producing superfine zinc fume |
| CN103722175B (en) * | 2013-12-31 | 2016-02-17 | 昆明海创兴科技有限公司 | The manufacture method of superfine flaky zinc powder with high corrosion resistance |
| CN103862057B (en) * | 2014-02-27 | 2015-12-30 | 赵志强 | The way of distillation produces nanoscale high-purity zinc powder device |
| CN103938229B (en) * | 2014-04-10 | 2017-01-18 | 同济大学 | Method for preparing ultrafine flake zinc powder by adding antimony compound alkali liquor to electrolyze |
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