CN104785354A - Method for grading nano-sized metal powder with low-temperature high purity water as medium - Google Patents
Method for grading nano-sized metal powder with low-temperature high purity water as medium Download PDFInfo
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Abstract
The invention belongs to the technical field of nano-nickle powder grading and relates to a method for grading nano-sized metal powder with low-temperature high purity water as a medium. The method comprises the steps that the metal powder with average grain diameter less than 1500 nanometers serve as raw materials, the metal powder is added into the low-temperature high purity water and a solid-liquid system is obtained by mixing, and the solid content of the solid-liquid system is controlled to be within 20%-30%; the solid-liquid system is subjected to mechanical dispersion processing, the dispersion time is controlled to be within 10 min-30 min, and when the mechanical dispersion is conducted, the temperature of the solid-liquid system is controlled to be within 0 DEC.G to 15 DEC.G to obtain dispersed material slurry; the obtained dispersed slurry is conveyed into a cyclone through a booster pump; the time of grading of the hydraulic cyclone is controlled to be within 20 min-35 min, the material slurry overflowed at an overflow port of the cyclone is collected, the metal powder with required grain diameter distribution is obtained, and the metal powder is the nano-sized metal powder prepared through a PVD method. The method has the advantages that the production process is free of potential safety hazards, secondary pollution can not be caused to the powder, the superficial area of the powder body remains the same basically, the purity is high, the additional value is high, and the production cost is low.
Description
Technical field
The invention belongs to nano-nickel powder classification technique field, refer in particular to a kind of with low temperature high purity water for medium is to the method for nano level metal powder classification.
Background technology
CN 102327806 B discloses one " taking organic solvent as the method for media classification MLCC nano-nickel powder ", the method comprises the following steps: be 1. the metal nickel powder of below 1000nm with average grain diameter be raw material, being joined concentration is be mixed to get solid-liquid system in the organic solvent of 90 ~ 99.9%, the solid content of solid-liquid system controls 20% ~ 50%, and described organic solvent is the one of absolute ethyl alcohol, isopropyl alcohol or normal propyl alcohol; 2. carry out mechanical dispersion process to above-mentioned solid-liquid system, the temperature that jitter time controls the solid-liquid system when 10min ~ 60min, mechanical dispersion controls to obtain disperse materials slurry at 10 ~ 50 DEG C; 3. the dispersion slip of step 2. gained is sent in cyclone by booster pump, the Stress control of cyclone inlets place slip is at 0.1 ~ 2.0Mpa, the flow-control of cyclone charging aperture is at 10 ~ 200L/min, and the flow-control of cyclone underflow opening is at 2 ~ 20L/min; 4. by the time controling of hydroclone classification at 5min ~ 60min, collect the step slip that 3. cyclone overfall overflows, obtain the nickel powder of required domain size distribution, described metal nickel powder is by the standby nano-nickel powder of PVD legal system.Its weak point is: one be the method use organic solvent (as alcohol) be combustible material, misoperation hold fire hazardous; Two is that the price of organic solvent that the method uses is high, forms production cost high; Three is containing the impurity of other compositions, must can cause secondary pollution, affect the purity of product and lower its added value the metal nickel powder of classification in the organic solvent that uses of the method.
In addition, CN 102327806 B points out simultaneously: the copper nanoparticle prepared by PVD method must carry out the instructions for use that certain classification process just can reach the raw material of MLCC; Hydrocyclone is a kind of purposes wet type machinery separation classifying equipoment very widely, its operation principle relies on the centrifugal force in conical vessel to be separated from current by the particle of different-grain diameter size, with water be classification medium utilize hydroclone classification nano-nickel powder time, because nano-nickel powder particle diameter is little, specific area and surface energy large, powder surface very easily adsorbed water and with it occur chemical reaction generate new surface texture Ni-O-H, this type of mechanism will form hydrogen bond further, and cause the reunion of nickel powder, finally affect the classification efficiency of hydrocyclone.Meanwhile, the existence of Ni-O-H structure will change nickel powder surface texture form, and impelling powder surface to amass roughness increases, and the specific area showing as powder increases, and this will have a strong impact on the application of nano-nickel powder in MLCC field.
Summary of the invention
The object of this invention is to provide that a kind of production cost is low, non-secondary pollution and fire hazard, powder surface roughness are little with low temperature high purity water for medium is to the method for nano level metal powder classification.
The object of the present invention is achieved like this:
With low temperature high purity water for medium is to the method for nano level metal powder classification, comprise the steps:
(1) take average grain diameter as the metal dust of below 1500nm be raw material, joined in low temperature high purity water and be mixed to get solid-liquid system, solid content in solid-liquid system controls 20% ~ 30%, described low temperature high purity water is the high purity water of 0-15 DEG C, the high-purity resistivity of water of low temperature is 10 ~ 20 ohm meters, and described nano level metal powder is nano nickel powder or Nano Silver powder or nanometer tin powder;
(2) carry out mechanical dispersion process to above-mentioned solid-liquid system, jitter time controls when 10min ~ 30min, mechanical dispersion, and the temperature of solid-liquid system controls to obtain disperse materials slurry at 0 ~ 15 DEG C;
(3) the dispersion slip of step (2) gained is sent in cyclone by booster pump, the Stress control of cyclone inlets place slip is at 0.5 ~ 3Mpa, the flow-control of cyclone charging aperture is at 100 ~ 300L/min, and the flow-control of cyclone underflow opening is at 10 ~ 30L/min;
(4) by the time controling of hydroclone classification at 20min ~ 35min, the slip that step (3) cyclone overfall overflows is collected, obtain the metal dust of required domain size distribution, described metal dust is by the standby nano level metal powder of PVD legal system.
The average grain diameter of above-mentioned metal dust is 100nm ~ 250nm.
Solid content in above-mentioned solid-liquid system controls 20% ~ 25%.
Above-mentioned mechanical dispersion is treated to ultrasonic wave dispersion or high speed machine dispersed with stirring.
Above-mentioned slurry temperature controls at 0 ~ 5 DEG C.
Above-mentioned low temperature high purity water is the high purity water of 0 ~ 5 DEG C, and the high-purity resistivity of water of low temperature is 17 ~ 18 ohm meters.
Above-mentioned booster pump is mechanical booster pump.
The present invention gives prominence to compared to existing technology and useful technique effect is:
1. the present invention selects low temperature high purity water to be that medium carries out classification to nano level metal powder, purity due to low temperature high purity water is high and nonflammable, therefore be that medium carries out classification to nano level metal powder with low temperature high purity water, production process is without potential safety hazard, secondary pollution can not be formed, the purity of product is high, added value is high, and production cost is low.
2. the present invention selects low temperature high purity water to be that medium carries out classification to nano level metal powder, because high purity water can not produce oxidation reaction with metal dust at low temperatures, powder surface can be avoided to be subject to the erosion of classification medium, powder surface is long-pending to remain unchanged substantially, thus does not have an impact to the extensive use of metal dust.
3. the present invention selects and adopts general hydrocyclone to carry out classification to nano level metal powder, the nano level metal dust of different-grain diameter scope can be obtained, not only can carry out classification to nanoscale nickel by powder, classification can also be carried out to nanometer-level silver powder or nanoscale tin powder, the uniform particle sizes of gained powder, uniformity is good.
Detailed description of the invention
With specific embodiment, the invention will be further described below:
With low temperature high purity water for medium is to the method for nano level metal powder classification, comprise the steps:
(1) take average grain diameter as the metal dust of below 1500nm be raw material, joined in low temperature high purity water and be mixed to get solid-liquid system, solid content in solid-liquid system controls 20% ~ 30%, described low temperature high purity water is the high purity water of 0-15 DEG C, the high-purity resistivity of water of low temperature is 10 ~ 20 ohm meters, and described nano level metal powder is nano nickel powder or Nano Silver powder or nanometer tin powder;
(2) carry out mechanical dispersion process to above-mentioned solid-liquid system, jitter time controls when 10min ~ 30min, mechanical dispersion, and the temperature of solid-liquid system controls to obtain disperse materials slurry at 0 ~ 15 DEG C;
(3) the dispersion slip of step (2) gained is sent in cyclone by booster pump, the Stress control of cyclone inlets place slip is at 0.5 ~ 3Mpa, the flow-control of cyclone charging aperture is at 100 ~ 300L/min, and the flow-control of cyclone underflow opening is at 10 ~ 30L/min;
(4) by the time controling of hydroclone classification at 20min ~ 35min, the slip that step (3) cyclone overfall overflows is collected, obtain the metal dust of required domain size distribution, described metal dust is by the standby nano level metal powder of PVD legal system.
The average grain diameter of above-mentioned metal dust is 100nm ~ 250nm.
Solid content in above-mentioned solid-liquid system controls 20% ~ 25%.
Above-mentioned mechanical dispersion is treated to ultrasonic wave dispersion or high speed machine dispersed with stirring.
Above-mentioned slurry temperature controls at 0 ~ 5 DEG C.
Above-mentioned low temperature high purity water is the high purity water of 0 ~ 5 DEG C, and the high-purity resistivity of water of low temperature is 17 ~ 18 ohm meters.
Above-mentioned booster pump is mechanical booster pump.
Experimental comparison shows:
Upper table is take average grain diameter as the metallic nickel powder of below 1500nm is raw material, joined in low temperature high purity water and be mixed to get solid-liquid system, solid content in solid-liquid system controls about 20%, low temperature high purity water to be resistivity be 10 ~ 20 ohm meters, the high purity water of 0 DEG C, jitter time controls when 25min, mechanical dispersion, and the temperature of solid-liquid system controls to obtain disperse materials slurry at 1 DEG C; The Stress control of cyclone inlets place slip is at 1.5Mpa, the flow-control of cyclone charging aperture is at 200L/min, the flow-control of cyclone underflow opening is at 20L/min, the time controling of hydroclone classification is at 25min, collect the slip that cyclone overfall overflows, the average grain diameter obtaining the nickel powder of required domain size distribution is 200nm.
As seen from the above table: the present invention be with an organic solvent absolute ethyl alcohol, deionized water, low temperature high purity water is (slurry temperature only during the high-purity water as medium of low temperature is 0-5 DEG C) under the akin condition of classification condition of medium, resistivity is used to be 17 ~ 18 ohm meters, the high-purity water as medium of low temperature of zero degree, its product yield is with an organic solvent close, and its cost declines greatly, purity is made organic solvent relative to absolute ethyl alcohol and is improved 20%, the surface smoothness of nickel powder particle contrasts under 1000 power microscopes, use absolute ethyl alcohol suitable with the surface smoothness of the nickel powder particle using the high-purity water as medium of low temperature, and do not catch fire and cause the risk of fire, therefore, use the high-purity water as medium of low temperature to the classification of nano level metal powder, breach the constraint of traditional concept, overcome technology prejudice, achieve low cost, the classification of high-quality nano level metal powder, its added value of product is high.
Above-described embodiment is only preferred embodiment of the present invention, not limits the scope of the invention according to this, therefore: all equivalence changes done according to structure of the present invention, shape, principle, all should be covered by within protection scope of the present invention.
Claims (7)
1. with low temperature high purity water for medium is to the method for nano level metal powder classification, it is characterized in that: comprise the steps:
(1) take average grain diameter as the metal dust of below 1500nm be raw material, joined in low temperature high purity water and be mixed to get solid-liquid system, solid content in solid-liquid system controls 20% ~ 30%, described low temperature high purity water is the high purity water of 0-15 DEG C, the high-purity resistivity of water of low temperature is 10 ~ 20 ohm meters, and described nano level metal powder is nano nickel powder or Nano Silver powder or nanometer tin powder;
(2) carry out mechanical dispersion process to above-mentioned solid-liquid system, jitter time controls when 10min ~ 30min, mechanical dispersion, and the temperature of solid-liquid system controls to obtain disperse materials slurry at 0 ~ 15 DEG C;
(3) the dispersion slip of step (2) gained is sent in cyclone by booster pump, the Stress control of cyclone inlets place slip is at 0.5 ~ 3Mpa, the flow-control of cyclone charging aperture is at 100 ~ 300L/min, and the flow-control of cyclone underflow opening is at 10 ~ 30L/min;
(4) by the time controling of hydroclone classification at 20min ~ 35min, the slip that step (3) cyclone overfall overflows is collected, obtain the metal dust of required domain size distribution, described metal dust is by the standby nano level metal powder of PVD legal system.
2. according to claim 1 with low temperature high purity water for medium is to the method for nano level metal powder classification, it is characterized in that: the average grain diameter of described metal dust is 100nm ~ 250nm.
3. according to claim l with the method for low temperature high purity water for media classification nano level metal powder, it is characterized in that: the solid content in described solid-liquid system controls 20% ~ 25%.
4. according to claim 1 with low temperature high purity water for medium is to the method for nano level metal powder classification, it is characterized in that: described mechanical dispersion be treated to ultrasonic wave dispersion or high speed machine dispersed with stirring.
5. according to claim 1 with low temperature high purity water for medium is to the method for nano level metal powder classification, it is characterized in that: described slurry temperature controls at 0 ~ 5 DEG C.
6. according to claim 1 with low temperature high purity water for medium is to the method for nano level metal powder classification, it is characterized in that: described low temperature high purity water is the high purity water of 0 ~ 5 DEG C, and the high-purity resistivity of water of low temperature is 17 ~ 18 ohm meters.
7. according to claim 1 with low temperature high purity water for medium is to the method for nano level metal powder classification, it is characterized in that: described booster pump is mechanical booster pump.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112893830A (en) * | 2020-12-29 | 2021-06-04 | 宁波广新纳米材料有限公司 | Liquid phase grading method for magnetic metal powder |
| CN115806304A (en) * | 2021-09-13 | 2023-03-17 | 中国科学院过程工程研究所 | Method for preparing ultrafine heavy calcium carbonate by classifying marble waste residues |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112893830A (en) * | 2020-12-29 | 2021-06-04 | 宁波广新纳米材料有限公司 | Liquid phase grading method for magnetic metal powder |
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