CN104972108A - 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, specifically relate to a kind of ultra-fine Zinc alloy powder and preparation method thereof, the additive be mainly used in as coating uses.
Background technology
Zinc powder is a kind of important raw material of industry, and market demand is very large, and be widely used in the fields such as metallurgy, chemical industry, building, traffic, medicine, electronics, the production method of zinc powder has atomization and using vaporization condensation process.Producing Zinc Powders by Gas Atomization, as jet-impingement atomization, water-jet is atomized, and product recovery rate is low, and power consumption is large, also there is the problems such as particle is uneven.The method that current domestic industryization produces zinc powder is main mainly with using vaporization condensation process, using coal, coal gas or electricity as the energy, zinc ingot metal by zinc-melting furnace heat fused until evaporation produces zinc powder through condensation again.
Along with the development of science and technology, super-fine material attracts attention more and more and studies due to the combination property of its excellence, and super-fine zinc dust is exactly one of them.Super-fine zinc dust refers to the zinc powder of granularity at below 100nm, due to the physicochemical properties of its uniqueness, have broad application prospects in fields such as Chemical Manufacture, lubricating additive, coating, high performance electrode materials, super-fine zinc dust has become one of focus of countries in the world scientific worker research.The national demand of super-fine zinc dust is greater than 100,000 tons/year at present, and cumulative year after year, price is common zinc powder price 3 ~ 4 times.At present, maximum industry of super-fine zinc dust or coating and anticorrosion, can make zinc-rich paint or directly be plated on anticorrosive coat.Zinc powder particle diameter is more tiny, and surface-active is larger, is conducive to the formation of coating.
The preparation method of domestic and international zinc powder mainly contains the way of distillation, atomization, high-energy ball milling method, electrolysis and vacuum evaporation condensation method.Wherein the zinc powder particle diameter prepared of atomization is more than l0 μm, thus can not prepare super-fine zinc dust.The production efficiency of the way of distillation is high, but obtained super-fine zinc dust activity is lower.The super-fine zinc dust that high-energy ball milling method obtains is flakey, but easily pollutes.The technique proposed in Chinese patent CN1450182A and CN1482263A has promoted the large-scale production of alkaline process electrolytic zinc powder technique, but the zinc powder particle diameter that this flow process is produced is bigger than normal, and thickness is uneven, preparing super-fine zinc dust need grind with ball mill, energy consumption is high, complex process., by adding lead-containing compounds refinement preferably zinc powder, but also there is the problem of micro lead precipitation in China 201210034534.7.
But, at present pure zinc powder can not be met the demand for development of coating as the decay resistance that the technical problem that the additive of coating exists is pure zinc powder, use as corrosion resistant coating additive so people start little by little to attempt Zinc alloy powder being substituted pure zinc powder.Zinc alloy powder conventional at present can use mercury and lead to wait poisonous and harmful alloying element usually, uses the Zinc alloy powder of these elements to add in coating and can cause environmental pollution and ecological disruption, can not meet the requirement of current environmental protection.
In order to solve the problems of the technologies described above, the invention provides a kind of ultra-fine Zinc alloy powder and preparation method thereof, ultra-fine Zinc alloy powder prepared by the present invention can replace traditional pure zinc powder to use as the corrosion-resistant additive of coating, and not containing poisonous and harmful elements such as cadmium, mercury and lead in kirsite composition, environmental pollution and ecological disruption can not be caused, environmental protection.
Summary of the invention
The object of this invention is to provide a kind of ultra-fine Zinc alloy powder and preparation method thereof, traditional pure zinc powder can be substituted use as the corrosion-resistant additive of coating, and not containing poisonous and harmful elements such as cadmium, mercury and lead in kirsite composition, environmental pollution and ecological disruption can not be caused, environmental protection.The present invention is preferred by alloying component and content, alloy in the ultra-fine Zinc alloy powder prepared is grown in dendritic mode, and low-alloyed crystal boundary energy, falls in grain refinement, strengthen its alloying performance, and the corrosion-resistant of Zinc alloy powder and antioxygenic property can be improved significantly.
Technical scheme of the present invention 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; It is characterized in that, the quality of described kirsite is composed 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; Aluminium: 100 ~ 150ppm; Calcium: 100 ~ 200ppm; Surplus is zinc.
In a preferred technical scheme, the quality of described kirsite is composed as follows:
Nickel: 0.80wt%; Antimony: 0.15wt%; Cobalt: 0.05wt%; Lanthanum: 0.25wt%; Cerium: 0.25wt%; Gadolinium: 0.15wt%; Indium: 100ppm; Bismuth: 100ppm; Aluminium: 150ppm; Calcium: 200ppm; Surplus is zinc.
In a preferred technical scheme, the quality of described kirsite is composed as follows:
Nickel: 0.60wt%; Antimony: 0.10wt%; Cobalt: 0.15wt%; Lanthanum: 0.35wt%; Cerium: 0.15wt%; Gadolinium: 0.05wt%; Indium: 300ppm; Bismuth: 300ppm; Aluminium: 100ppm; Calcium: 100ppm; Surplus is zinc.
In a preferred technical scheme, the quality of described kirsite is composed as follows:
Nickel: 0.70wt%; Antimony: 0.12wt%; Cobalt: 0.10wt%; Lanthanum: 0.30wt%; Cerium: 0.20wt%; Gadolinium: 0.10wt%; Indium: 200ppm; Bismuth: 200ppm; Aluminium: 125ppm; Calcium: 150ppm; Surplus is zinc.
In a preferred technical scheme, the particle size range of described ultra-fine Zinc alloy powder is as follows: the Zinc alloy powder of 1nm < particle diameter≤20nm accounts for the 20wt% ~ 30wt% of total Zinc alloy powder, the Zinc alloy powder of 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.
The present invention provides a kind of preparation method of ultra-fine Zinc alloy powder on the other hand, and it is characterized in that, concrete steps are as follows:
Step 1, prepare nano zinc powder: first nano-zinc oxide powder is placed in reduction furnace, after sealing, passes into CO and H produced by methanol oxidation cracking with 80 ~ 100ml/min
2, be then warming up to 410 DEG C ~ 450 DEG C reaction 50 ~ 60min, after cooling, obtain high-purity nm zinc powder;
Step 2, melting: form according to the quality of described kirsite the high-purity nm zinc powder step 1 prepared and other analytically pure raw metal is placed in crucible type melting furnace, melt and remove surface oxidation slag at the temperature of 660 DEG C ~ 680 DEG C;
Step 3, distillation: the kirsite liquid of above-mentioned gained is joined in induction type electric heating crucible retort, distill at the temperature of 940 DEG C ~ 960 DEG C;
Step 4, backflow: the kirsite steam above-mentioned distillation produced imports in return duct, and reflux section temperature is 920 DEG C ~ 940 DEG C, realizes kirsite vapor portion condensing reflux decontamination, the high-boiling-point impurity in zinc fume returns with backflow zinc again and distills;
Step 5, hyperthermia and superheating: the pure kirsite steam after above-mentioned backflow enters in the superheat section of return duct, carry out hyperthermia and superheating process at the temperature of 1400 DEG C ~ 1500 DEG C;
Step 6, condensation: by the high-temperature zinc alloy steam after hyperthermia and superheating process under pure nitrogen gas atmosphere, sharply condensation at the temperature of 60 DEG C ~ 70 DEG C, obtains described ultra-fine Zinc alloy powder;
Step 7, surface treatment: the ultra-fine Zinc alloy powder obtained to step 6 carries out Dispersion on surface process, the ultra-fine Zinc alloy powder obtained is put into dispersant and carries out surface treatment, soak after 6 ~ 8 hours and take out oven dry, obtain the ultra-fine Zinc alloy powder of finished product.
In a preferred technical scheme, the particle size range of described ultra-fine Zinc alloy powder is as follows: the Zinc alloy powder of 1nm < particle diameter≤20nm accounts for the 20wt% ~ 30wt% of total Zinc alloy powder, the Zinc alloy powder of 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.
In a preferred technical scheme, described dispersant is one or its mixture of ethyl acetate, polyethylene glycol or polyvinyl alcohol.
Above-mentioned ultra-fine Zinc alloy powder is used for the additive as coating.
Technique effect of the present invention is as follows:
Containing LREE lanthanum, cerium and heavy rare earth element gadolinium in Zinc alloy powder provided by the invention.Rare-earth elements of lanthanum, cerium and gadolinium on the one hand can inhibiting grain growths, form fine grain intercrystalline strengthening mechanism, be enriched in due to Thermodynamic effect in crystal boundary, alloy grows in dendritic mode, produces more nucleus of crystal, thus makes grain refinement, the effect of degassed removal of impurities can be played on the other hand, because the gaseous impurity such as oxygen, hydrogen, sulphur in rare-earth elements of lanthanum, cerium and gadolinium cerium and alloy has stronger affinity, compound can be formed with it, thus reduce the harm of alloy; Meanwhile, the cooperation of LREE lanthanum, cerium and heavy rare earth element gadolinium adds can the crystal grain of refinement kirsite, reduces its crystal boundary energy.
With the addition of a small amount of nickel in Zinc alloy powder provided by the invention, its corrosion-resistant and antioxygenic property can be improved significantly.
With the addition of the indium of trace, bismuth, aluminium and calcium metal in Zinc alloy powder provided by the invention, strengthen its alloying performance.
Do not comprise the poisonous and harmful elements such as mercury, lead, cadmium in Zinc alloy powder provided by the invention, environmental pollution and ecological disruption can not be caused, environmental protection.
The present invention adopts methanol oxidation cracking reduction-oxidation zinc to prepare the primary raw material of high-purity nm zinc powder as preparation ultra-fine Zinc alloy powder of the present invention, the high-purity nm zinc powder adopting reduction-oxidation zinc to prepare greatly can improve the activity of raw material relative to the zinc powder of stock size as raw material, increase the apparent activation energy of raw material, be finally very advantageous in obtaining of ultra-fine Zinc alloy powder.
The primary raw material of high-purity nm zinc powder as preparation ultra-fine Zinc alloy powder of the present invention is prepared except adopting methanol oxidation cracking reduction-oxidation zinc, the present invention also adopts other metal analytically pure as raw material, by reasonably controlling to adjust the technique of melt temperature, vapo(u)rizing temperature, reflux temperature, hyperthermia and superheating temperature, quench temperature and correspondence, the preparation technology of the ultra-fine Zinc alloy powder after being finally optimized, has prepared the ultra-fine Zinc alloy powder of excellent combination property.
Detailed description of the invention
Embodiment one
A kind of ultra-fine Zinc alloy powder, the particle size range of described ultra-fine Zinc alloy powder is 1 ~ 100nm; The quality of described kirsite is composed as follows:
Nickel: 0.80wt%; Antimony: 0.15wt%; Cobalt: 0.05wt%; Lanthanum: 0.25wt%; Cerium: 0.25wt%; Gadolinium: 0.15wt%; Indium: 100ppm; Bismuth: 100ppm; Aluminium: 150ppm; Calcium: 200ppm; Surplus is zinc.
The particle size range of described ultra-fine Zinc alloy powder is as follows: the Zinc alloy powder of 1nm < particle diameter≤20nm accounts for the 20wt% ~ 30wt% of total Zinc alloy powder, the Zinc alloy powder of 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.
The concrete steps of the preparation method of above-mentioned ultra-fine Zinc alloy powder are as follows:
Step 1, prepare nano zinc powder: first nano-zinc oxide powder is placed in reduction furnace, after sealing, passes into CO and H produced by methanol oxidation cracking with 80 ~ 100ml/min
2, be then warming up to 410 DEG C ~ 450 DEG C reaction 50 ~ 60min, after cooling, obtain high-purity nm zinc powder;
Step 2, melting: form according to the quality of described kirsite the high-purity nm zinc powder step 1 prepared and other analytically pure raw metal is placed in crucible type melting furnace, melt and remove surface oxidation slag at the temperature of 660 DEG C ~ 680 DEG C;
Step 3, distillation: the kirsite liquid of above-mentioned gained is joined in induction type electric heating crucible retort, distill at the temperature of 940 DEG C ~ 960 DEG C;
Step 4, backflow: the kirsite steam above-mentioned distillation produced imports in return duct, and reflux section temperature is 920 DEG C ~ 940 DEG C, realizes kirsite vapor portion condensing reflux decontamination, the high-boiling-point impurity in zinc fume returns with backflow zinc again and distills;
Step 5, hyperthermia and superheating: the pure kirsite steam after above-mentioned backflow enters in the superheat section of return duct, carry out hyperthermia and superheating process at the temperature of 1400 DEG C ~ 1500 DEG C;
Step 6, condensation: by the high-temperature zinc alloy steam after hyperthermia and superheating process under pure nitrogen gas atmosphere, sharply condensation at the temperature of 60 DEG C ~ 70 DEG C, obtains described ultra-fine Zinc alloy powder;
Step 7, surface treatment: the ultra-fine Zinc alloy powder obtained to step 6 carries out Dispersion on surface process, the ultra-fine Zinc alloy powder obtained is put into dispersant and carries out surface treatment, soak after 6 ~ 8 hours and take out oven dry, obtain the ultra-fine Zinc alloy powder of finished product, described dispersant is one or its mixture of ethyl acetate, polyethylene glycol or polyvinyl alcohol.
The above-mentioned ultra-fine Zinc alloy powder of preparation is used for using as the additive of 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; The quality of described kirsite is composed as follows:
Nickel: 0.60wt%; Antimony: 0.10wt%; Cobalt: 0.15wt%; Lanthanum: 0.35wt%; Cerium: 0.15wt%; Gadolinium: 0.05wt%; Indium: 300ppm; Bismuth: 300ppm; Aluminium: 100ppm; Calcium: 100ppm; Surplus is zinc.
Its preparation method is identical with embodiment one.
The above-mentioned ultra-fine Zinc alloy powder of preparation is used for using as the additive of 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; The quality of described kirsite is composed as follows:
Nickel: 0.70wt%; Antimony: 0.12wt%; Cobalt: 0.10wt%; Lanthanum: 0.30wt%; Cerium: 0.20wt%; Gadolinium: 0.10wt%; Indium: 200ppm; Bismuth: 200ppm; Aluminium: 125ppm; Calcium: 150ppm; Surplus is zinc.
Its preparation method is identical with embodiment one.
The above-mentioned ultra-fine Zinc alloy powder of preparation is used for using as the additive of coating.
Claims (10)
1. a ultra-fine Zinc alloy powder, the particle size range of described ultra-fine Zinc alloy powder is 1 ~ 100nm; It is characterized in that, the quality of described kirsite is composed 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; Aluminium: 100 ~ 150ppm; Calcium: 100 ~ 200ppm; Surplus is zinc.
2. the ultra-fine Zinc alloy powder of one according to claim 1, is characterized in that, the quality of described kirsite is composed as follows:
Nickel: 0.80wt%; Antimony: 0.15wt%; Cobalt: 0.05wt%; Lanthanum: 0.25wt%; Cerium: 0.25wt%; Gadolinium: 0.15wt%; Indium: 100ppm; Bismuth: 100ppm; Aluminium: 150ppm; Calcium: 200ppm; Surplus is zinc.
3. the ultra-fine Zinc alloy powder of one according to claim 1, is characterized in that, the quality of described kirsite is composed as follows:
Nickel: 0.60wt%; Antimony: 0.10wt%; Cobalt: 0.15wt%; Lanthanum: 0.35wt%; Cerium: 0.15wt%; Gadolinium: 0.05wt%; Indium: 300ppm; Bismuth: 300ppm; Aluminium: 100ppm; Calcium: 100ppm; Surplus is zinc.
4. the ultra-fine Zinc alloy powder of one according to claim 1, is characterized in that, the quality of described kirsite is composed as follows:
Nickel: 0.70wt%; Antimony: 0.12wt%; Cobalt: 0.10wt%; Lanthanum: 0.30wt%; Cerium: 0.20wt%; Gadolinium: 0.10wt%; Indium: 200ppm; Bismuth: 200ppm; Aluminium: 125ppm; Calcium: 150ppm; Surplus is zinc.
5. the ultra-fine Zinc alloy powder of one according to any one of Claims 1 to 4 claim, it is characterized in that, the particle size range of described ultra-fine Zinc alloy powder is as follows: the Zinc alloy powder of 1nm < particle diameter≤20nm accounts for the 20wt% ~ 30wt% of total Zinc alloy powder, the Zinc alloy powder of 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.
6. the preparation method of a kind of ultra-fine Zinc alloy powder described in any one of Claims 1 to 4 claim, it is characterized in that, concrete steps are as follows:
Step 1, prepare nano zinc powder: first nano-zinc oxide powder is placed in reduction furnace, after sealing, passes into CO and H produced by methanol oxidation cracking with 80 ~ 100ml/min
2, be then warming up to 410 DEG C ~ 450 DEG C reaction 50 ~ 60min, after cooling, obtain high-purity nm zinc powder;
Step 2, melting: form according to the quality of described kirsite the high-purity nm zinc powder step 1 prepared and other analytically pure raw metal is placed in crucible type melting furnace, melt and remove surface oxidation slag at the temperature of 660 DEG C ~ 680 DEG C;
Step 3, distillation: the kirsite liquid of above-mentioned gained is joined in induction type electric heating crucible retort, distill at the temperature of 940 DEG C ~ 960 DEG C;
Step 4, backflow: the kirsite steam above-mentioned distillation produced imports in return duct, and reflux section temperature is 920 DEG C ~ 940 DEG C, realizes kirsite vapor portion condensing reflux decontamination, the high-boiling-point impurity in zinc fume returns with backflow zinc again and distills;
Step 5, hyperthermia and superheating: the pure kirsite steam after above-mentioned backflow enters in the superheat section of return duct, carry out hyperthermia and superheating process at the temperature of 1400 DEG C ~ 1500 DEG C;
Step 6, condensation: by the high-temperature zinc alloy steam after hyperthermia and superheating process under pure nitrogen gas atmosphere, sharply condensation at the temperature of 60 DEG C ~ 70 DEG C, obtains described ultra-fine Zinc alloy powder;
Step 7, surface treatment: the ultra-fine Zinc alloy powder obtained to step 6 carries out Dispersion on surface process, the ultra-fine Zinc alloy powder obtained is put into dispersant and carries out surface treatment, soak after 6 ~ 8 hours and take out oven dry, obtain the ultra-fine Zinc alloy powder of finished product.
7. the preparation method of a kind of ultra-fine Zinc alloy powder according to claim 6, it is characterized in that, the particle size range of described ultra-fine Zinc alloy powder is as follows: the Zinc alloy powder of 1nm < particle diameter≤20nm accounts for the 20wt% ~ 30wt% of total Zinc alloy powder, the Zinc alloy powder of 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.
8. the preparation method of a kind of ultra-fine Zinc alloy powder according to claim 6 or 7, is characterized in that, described dispersant is one or its mixture of ethyl acetate, polyethylene glycol or polyvinyl alcohol.
9. a kind of ultra-fine Zinc alloy powder described in any one of Claims 1 to 4 claim is used for the additive as coating.
10. a kind of ultra-fine Zinc alloy powder according to claim 5 is used for the additive as coating.
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