CN103674790A - Method for testing particle size distribution of superfine nickel powder - Google Patents
Method for testing particle size distribution of superfine nickel powder Download PDFInfo
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- CN103674790A CN103674790A CN201310694492.4A CN201310694492A CN103674790A CN 103674790 A CN103674790 A CN 103674790A CN 201310694492 A CN201310694492 A CN 201310694492A CN 103674790 A CN103674790 A CN 103674790A
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Abstract
The invention provides a method for testing particle size distribution of superfine nickel powder. The method comprises the operation steps as follows: preparing a polyamidoamine solution with the mass-to-volume percent of 0.5-20% with reverse osmosis water; enabling a laser particle size distribution detector to be located in a stable detection state; preparing a superfine nickel powder solution with the mass-to-volume percent of 0.01-1% with the reverse osmosis water, adding the polyamidoamine solution, wherein the adding amount of the polyamidoamine solution to the amount of reverse osmosis water in the superfine nickel power solution is (0.5-2 ml):150 ml; then dispersing the mixture with an ultrasonic stirrer for 15-20 min; detecting the liquid obtained in the last step by the laser particle size distribution detector to obtain the particle size distribution condition of the superfine nickel power. According to the method, the polyamidoamine is selected as a surfactant, so that the superfine nickel powder is good in hydrophilic property, and the actual particle size distribution condition of the superfine nickel power can be reflected more truly.
Description
Technical field
The present invention relates to ultra-fine powder technology field, be specifically related to a kind of for testing the method for extra-fine nickel powder size-grade distribution.
Background technology
Diameter of particle size is the fundamental property of powder, and especially for nano metal powder, particle size directly affects the character such as the temperature of fusion, oxidizing temperature, mobility of powder, further can affect production practical application.Use PVD legal system to belong to extra-fine nickel powder for the nickel powder of gained, extra-fine nickel powder is because particle diameter is little, and surface area ratio is large, is magnetic material, easily occurs agglomeration.This problem also perplexs many manufacturers and powder supplier, and therefore the correct size-grade distribution that effectively detects rapidly powder, could not affect the production of next procedure.
When metal-powder detects size-grade distribution, conventional medium is alcohol and water.But with alcohol, do medium, the one, cost is large, two meeting environmental pollutions, three because alcohol belongs to flammable and explosive substance, exists certain danger.And while selecting to do medium with pure water, between pure water and nickel powder, exist the not good problem of water wettability, and particularly powder diameter is less, and its water wettability is poorer.
Therefore, we are when detection small particle diameter nickel powder is as extra-fine nickel powder size-grade distribution, preferably select a kind of surfactant, affine for nickel powder and water two-phase respectively by different piece in molecule, make two-phase all the other side be regarded as to the composition of this phase, surfactant molecule is arranged between two-phase, make the surface of two-phase be equivalent to proceed to intramolecule, thereby reduction surface tension, increase the water wettability of nickel powder, nickel powder can fully be scatter, thereby can reflect more realistically powder actual grain size distribution situation.
Summary of the invention
Technical matters to be solved by this invention is for above the deficiencies in the prior art, provide a kind of for testing the method for extra-fine nickel powder size-grade distribution, it is surfactant that the method is selected daiamid, make extra-fine nickel powder good hydrophilic property, thereby can reflect more realistically extra-fine nickel powder actual grain size distribution situation.
The technical solution adopted in the present invention is:
For testing a method for extra-fine nickel powder size-grade distribution, the method comprises following operation steps:
(1) utilize reverse osmotic pressure device Pure-water Making, obtain pH and be 7 ± 0.2, conductivity is the reverse osmosis water of 3-4 μ s/m;
(2) adopt the reverse osmosis water that step (1) makes to prepare the daiamid solution that quality percent by volume is 0.5-20%;
(3) standard model carrying with Laser particle-size distribution detector carries out instrument self checking, makes Laser particle-size distribution detector in detecting steady state (SS);
(4) adopt the reverse osmosis water that step (1) makes to prepare the extra-fine nickel powder solution that quality percent by volume is 0.01-1%, wherein extra-fine nickel powder adopts physical vaporous deposition to make, the daiamid solution that adds step (2) to make toward extra-fine nickel powder solution again, the ︰ 150ml of the amount of reverse osmosis water in the Liang of the adding ︰ extra-fine nickel powder solution of daiamid solution=(0.5-2ml), then adds stirrer with ultrasound wave and disperses 15-20min;
(5) step (4) gained liquid is detected under Laser particle-size distribution detector, obtain the size-grade distribution situation of extra-fine nickel powder.
As preferably, in described step (2), the concentration of daiamid solution is 2-8%.
As preferably, in described step (4), the mean grain size of extra-fine nickel powder is 200 ± 20nm, is shaped as spherical.
Compared with prior art, the present invention has following remarkable advantage and beneficial effect:
Laser particle-size distribution detector can make laser produce this physical phenomenon test size-grade distribution of scattering according to particle, so use this equipment to carry out when powder granularity distributes detection making powder fully spread out, not reunite extremely important.The present invention is through large quantity research and test, final definite using daiamid as surfactant, increase the water wettability of the extra-fine nickel powder that PVD method makes, extra-fine nickel powder can fully be scatter in water, thereby the actual grain size distribution situation that reflects more realistically extra-fine nickel powder, effectively guarantees the accuracy that size-grade distribution detects.And daiamid is easily bought, cheap, be applicable to operating for actual production.
Embodiment
Below in conjunction with embodiment, the present invention is further described in detail, but is not limited to this.
Embodiment:
A kind of extra-fine nickel powder being made by PVD method, it is 3.38 ㎡/g that this nickel powder detects specific surface area by specific surface area measuring instrument, by theory, calculating mean grain size is 200nm, and sample presentation to authoritative testing agency-University Of Ningbo carries out size-grade distribution detection, obtains its real size-grade distribution situation and is:
D10：0.125-0.145um，D50：0.250-0.280um，
D90：0.450-0.600um，D99.9：1.400-1.700um。
Adopt the inventive method to carry out particle size distribution test to this extra-fine nickel powder, operation steps is as follows:
(1) open LA-950V2 Laser particle-size distribution detector, and stablize 2 hours;
(2) utilize reverse osmotic pressure device Pure-water Making, obtain pH and be 7 ± 0.2, conductivity is the reverse osmosis water of 3-4 μ S/m;
(3) get 1 500 ml beaker, add 100 milliliters of reverse osmosis waters, then add 5 grams of daiamids, be mixed with homogeneous solution;
(4) standard model carrying with Laser particle-size distribution detector (meso-position radius D50 is 1.022 ± 0.02um) carries out instrument self checking, and the D50 test value of standard specimen is 1.023um, illustrates that instrument is in steady state (SS);
(5) get 1 500 ml beaker, add 150 milliliters of reverse osmosis waters, add 0.05 gram of extra-fine nickel powder, then add 0.5 milliliter of the daiamid solution that step (3) prepares, the ultrasound wave of putting into 200W power carries out ultrasonic dispersion and adds simultaneously and stir 20min;
(6) the scattered sample of step (4) is put into scattered sample in the sample cell of LA-950V2 laser fineness gage, in opening ultrasonic (machine carries), recorded result after within 2 minutes, completing test sample, test minutes two groups is carried out, and the results are shown in Table 1.
Comparative example 1:
The extra-fine nickel powder of indication in embodiment is carried out to particle size distribution test, and the same embodiment of operation steps, is not just used surfactant daiamid (place of using daiamid in embodiment is changed into and uses reverse osmosis water), and testing result is shown in Table 1.
Comparative example 2:
The extra-fine nickel powder of indication in embodiment is carried out to particle size distribution test, and the same embodiment of operation steps, just changes use therein surfactant daiamid into use neopelex, and testing result is shown in Table 1.
Comparative example 3:
The extra-fine nickel powder of indication in embodiment is carried out to particle size distribution test, and the same embodiment of operation steps, just changes use therein surfactant daiamid to use triethanolamine soap into, and testing result is shown in Table 1.
Comparative example 4:
The extra-fine nickel powder of indication in embodiment is carried out to particle size distribution test, and the same embodiment of operation steps, just changes use therein surfactant daiamid into use benzalkonium bromide, and testing result is shown in Table 1.
Comparative example 5:
The extra-fine nickel powder of indication in embodiment is carried out to particle size distribution test, and the same embodiment of operation steps, just changes use therein surfactant daiamid into use lecithin, and testing result is shown in Table 1.
Comparative example 6:
The extra-fine nickel powder of indication in embodiment is carried out to particle size distribution test, and the same embodiment of operation steps, just changes use therein surfactant daiamid into use stearic acid, and testing result is shown in Table 1.
Comparative example 7:
The extra-fine nickel powder of indication in embodiment is carried out to particle size distribution test, and the same embodiment of operation steps, just changes use therein surfactant daiamid into use polysorbate, and testing result is shown in Table 1.
Comparative example 8:
The extra-fine nickel powder of indication in embodiment is carried out to particle size distribution test, and the same embodiment of operation steps, just changes use therein surfactant daiamid into use sucrose ester, and testing result is shown in Table 1.
Table 1:
As can be seen from Table 1, the extra-fine nickel powder of selecting daiamid of the present invention as surface dispersant, PVD method to be produced carries out particle size distribution test, the true size-grade distribution that can reflect accurately, truly extra-fine nickel powder powder, and as surface dispersant, extra-fine nickel powder is carried out to particle size distribution test with other surfactant, the result drawing all has different gaps from its real size-grade distribution.
The above embodiment of the present invention is to explanation of the present invention and can not be for limiting the present invention, and the implication suitable with claims of the present invention and any change in scope, all should think to be included in the scope of claims.
Claims (3)
1. for testing a method for extra-fine nickel powder size-grade distribution, it is characterized in that comprising following operation steps:
(1) utilize reverse osmotic pressure device Pure-water Making, obtain pH and be 7 ± 0.2, conductivity is the reverse osmosis water of 3-4 μ s/m;
(2) adopt the reverse osmosis water that step (1) makes to prepare the daiamid solution that quality percent by volume is 0.5-20%;
(3) standard model carrying with Laser particle-size distribution detector carries out instrument self checking, makes Laser particle-size distribution detector in detecting steady state (SS);
(4) adopt the reverse osmosis water that step (1) makes to prepare the extra-fine nickel powder solution that quality percent by volume is 0.01-1%, wherein extra-fine nickel powder adopts physical vaporous deposition to make, the daiamid solution that adds step (2) to make toward extra-fine nickel powder solution again, the ︰ 150ml of the amount of reverse osmosis water in the Liang of the adding ︰ extra-fine nickel powder solution of daiamid solution=(0.5-2ml), then adds stirrer with ultrasound wave and disperses 15-20min;
(5) step (4) gained liquid is detected under Laser particle-size distribution detector, obtain the size-grade distribution situation of extra-fine nickel powder.
2. according to claim 1 a kind of for testing the method for extra-fine nickel powder size-grade distribution, it is characterized in that: in described step (2), the concentration of daiamid solution is 2-8%.
3. according to claim 1 a kind of for testing the method for extra-fine nickel powder size-grade distribution, it is characterized in that: in described step (4), the mean grain size of extra-fine nickel powder is 200 ± 20nm, is shaped as spherical.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106053196A (en) * | 2016-05-23 | 2016-10-26 | 无锡帝科电子材料科技有限公司 | Dispersing method of grain size test of silver powder for photovoltaic positive silver slurry |
| CN106940284A (en) * | 2017-05-24 | 2017-07-11 | 张建平 | A kind of dispersability of titanium dioxide detection method |
| CN106970008A (en) * | 2017-04-13 | 2017-07-21 | 广州市药品检验所 | The method for determining ibuprofen pharmaceutical particle size and its distribution in ibuprofen suspension |
| CN111982763A (en) * | 2020-08-17 | 2020-11-24 | 上海普康药业有限公司 | Method for determining particle size and particle size distribution of coenzyme Q10 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106053196A (en) * | 2016-05-23 | 2016-10-26 | 无锡帝科电子材料科技有限公司 | Dispersing method of grain size test of silver powder for photovoltaic positive silver slurry |
| CN106970008A (en) * | 2017-04-13 | 2017-07-21 | 广州市药品检验所 | The method for determining ibuprofen pharmaceutical particle size and its distribution in ibuprofen suspension |
| CN106970008B (en) * | 2017-04-13 | 2019-06-18 | 广州市药品检验所 | The method for measuring ibuprofen pharmaceutical particle size and its distribution in ibuprofen suspension |
| CN106940284A (en) * | 2017-05-24 | 2017-07-11 | 张建平 | A kind of dispersability of titanium dioxide detection method |
| CN111982763A (en) * | 2020-08-17 | 2020-11-24 | 上海普康药业有限公司 | Method for determining particle size and particle size distribution of coenzyme Q10 |
| CN111982763B (en) * | 2020-08-17 | 2021-05-14 | 上海普康药业有限公司 | Method for determining particle size and particle size distribution of coenzyme Q10 |
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Effective date of registration: 20161221 Address after: 223801 Suqian province high tech Development Zone, Jiangshan Road, No. 23, No. Patentee after: Jiangsu Bo move new materials Limited by Share Ltd Address before: Yinzhou District Zhejiang city in Ningbo province where 315153 broad industrial park spring news site Patentee before: Ningbo Guangbo New Nanomaterials Stock Co.,Ltd. |
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