CN101758223B - Metal nano powder surface tension and particle agglomeration processing technology - Google Patents
Metal nano powder surface tension and particle agglomeration processing technology Download PDFInfo
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- CN101758223B CN101758223B CN2009101790976A CN200910179097A CN101758223B CN 101758223 B CN101758223 B CN 101758223B CN 2009101790976 A CN2009101790976 A CN 2009101790976A CN 200910179097 A CN200910179097 A CN 200910179097A CN 101758223 B CN101758223 B CN 101758223B
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Abstract
The invention relates to the metal nano particle surface processing technology, in particular to a metal nano powder surface tension and particle agglomeration processing technology; the technology solves the problem of particle agglomeration caused by nano powder surface tension in the prior art; the method comprises the following steps: under the condition that the cutting frequency is set as 5500-6000 times per minute, the nano iron powder or non-ferrous metal nano powder particle material is produced at -5 DEG C - 0 DEG C, and then the powder material with particle distribution that D3=31nm, D25=61.1nm, D50=80nm, D75=86.13nm and D97=100.6nm is respectively sorted out, and then anti-oxidation cladding of the iron powder particle with 2nm-3nm of thickness is carried out, and then the iron powder particle is ground by rotation at from 6000r per minute to 8000r per minute at -5-0 DEG C, the grinding time is controlled from 5 to 8 minutes, the surface tension of the powder particle material is almost zero, so as to achieve the purpose of zero agglomeration of the powder particle material.
Description
Technical field
The present invention relates to a kind of process for treating surface of metal nanoparticle, be specially a kind of metal nano powder surface tension and particle agglomeration processing technology.
Background technology
At present countries in the world when using metal nano powder material and nonmetal nano powder granular material all in various degree exist the problem that powder granule is reunited, so just caused very big difficulty in use.Like novel process such as spraying, spray embedding, injections is exactly because the reunion of nano metal powder particle causes difficult forming or can't carry out technology basically and cause the technology apparatus badly damaged or greatly reduce service life of apparatus.
The subject matter of the world and domestic metal powder material operation technique existence at present does; Majority state all uses chemical method to make metal nano powder granular material in the world at present; Chemical method is made and has been solved agglomeration traits on the make; But after metal becomes nano powder granular material, do not eliminate the tension force of surface of metal particles,, carry out the decomposition of agglomerated particle and could normally use thereby cause in use adding the chemical breakdown agent so cause the metal powder particles material in use owing to the particle agglomeration that forms due to the surface of metal particles tension force; But will bring increase and the chemical contamination of using difficulty like this, reduce service efficiency simultaneously.
In addition chemical method also exist can't industrial-scale production, energy consumption is high, pollute big and machine-shaping secondary pollution problems.
Number of patent application is 2006100481685 to have put down in writing a kind of cutting production technology of metal nanometer powder zero boundry particle, and a kind of brand-new zero boundry particle cutting metal nano-powder material technology has been put down in writing in this patent application, is example with the iron powder; Step comprises; Iron powder is placed under-10 ℃～+ 15 ℃ the processing temperature state, then ferrous powder granules is carried out high-speed cutting, per minute is controlled at 5000～6000 times; Then the ferrous powder granules after the cutting 6000 rev/mins high frequency is ground; Carry out the physics reduction again, the surface coats handles, and last classification and sorting can obtain product.This technology can process the iron powder of different Nano grades; The iron powder that utilizes this method to produce the particular particles diameter has the technological in the past excellent specific property that can't produce; And discovering through the inventor; Raising or reduction processing " cutting " frequency are also correspondingly adjusted nanometer iron powder or other metal powder of each different stage that also can produce after " processing temperature " in this technology; And characteristic has tangible difference, through being widely used in different industries or field after classification and sorting and the proportioning.The technical scheme that this patent application is put down in writing is the applicant has proposed " cutting " this processing first in nano metal powder materials processing technology field a notion; Utilize the relative high speed reciprocating collision between the abrasive media can the feed metal powder be machined to Nano grade with friction; And the reciprocating number of times of the high speed of this abrasive media in the unit interval can be called " frequency ", and its crushing process to raw material can be described as " cutting "; And proposed concrete machined parameters, and just can process this technical scheme of high-quality nanometer iron powder with the corresponding processing temperature of control through having facts have proved through setting corresponding " cutting " frequency.
Number of patent application is 2006101620469 to disclose little, the nano particle cladding process of a kind of metal; The technical scheme of this application can form the high-quality protection against oxidation layer that a layer thickness is 1nm-3nm on the surface of metal powder material, below is called " DQ coats method ".Think the cladding process of more traditional nano metal powder, this technical scheme clad ratio is higher, and anti oxidation time is longer.
Go out more effective anti-agglomeration technology in conjunction with above technological development and just become the current technical problem that needs to be resolved hurrily.
Summary of the invention
The present invention is in order to solve due to the nano powder surface tension that exists in the prior art and the problem of the particle agglomeration that forms and a kind of metal nano powder surface tension and particle agglomeration processing technology are provided.
The present invention is realized by following technical scheme; A kind of metal nano powder surface tension and particle agglomeration processing technology; Method is at-5 ℃---under 0 ℃ the situation; Cutting frequency is set in per minute 5500 times---and producing under 6000 times the situation, processing the powder grain shape is the nanometer iron powder or the non-ferrous metal nano powder granular material of spheroid; Sub-elect the concentrated powder body material of distribution of particles of (80nm is an example) D3=31nm D25=61.1nmD50=80nm D75=86.13nm D97=100.6nm more respectively, then to metal nanoparticle continuation thickness be again: the anti-oxidation coating of 2nm-3nm reaches more than 90 hours its anti-oxidization time; With the metal nano powder granular material after coating; 8000 rev/mins run up, grind---to carry out 6000 rev/mins of per minutes under 0 ℃ of situation--at-5 ℃, and the powder granule material is progressively eliminated the surface tension of itself in running up, grinding, and requires milling time to be controlled at 5 minutes--between-8 minutes; The surface tension of powder granule material at this moment is almost nil, thereby has reached the purpose that powder granule material zero is reunited.When reaching powder granule material zero reunion purpose, can also grind modification to the surface of powder granule material, make its powder granule smooth surface, be beneficial to following moulding process.
Technical advantage of the present invention
1, technical advantage one of the present invention is: fundamentally solved the agglomeration traits of powder granule material in depositing and using.
2, technical advantage two of the present invention is: solved novel process in using metal nano powder granular material, a difficult problem that causes because reunite.
3, technical advantage three of the present invention is: greatly reduce powder granule material cost in use, the use cost of present technique has only 1/5 of U.S.'s powder granule material use cost.
4, technical advantage four of the present invention is: increased substantially the use value of metal nano powder granular material in novel process.
5, technical advantage five of the present invention is: reduced the probability that apparatus damages in the novel forming technology, be reduced to 1.31% of present technique from original 21%.
6, technical advantage six of the present invention is: solved that density differs in the moulding, intensity is different, a rough difficult problem.
Description of drawings
Fig. 1 is the structural representation of cutting machine
Fig. 2 is the grinding machine structure sketch map
Fig. 3,4,5 is for processing the electromicroscopic photograph of the metallic particles that obtains
1-inert gas entrance among the figure; The 2-charging aperture; The 3-cooling water inlet; The 4-body; The 5-cutter; The 6-connecting rod; The 7-support; The 8-discharging opening; 9-frequency modulation vibrating motor; The 10-foundation of incision machine; 11-vibrates air bag; The 12-cooling water inlet; The 13-connecting rod; The 14-cutter; The 15-vibrating spring; 16-vulcanie pad; The 17-discharging opening; The 18-hollow rotating shaft; 19-grinds body; 20-is by abrasive grains; 21 charging gas ports; The 22-variable-frequency motor; The 23-support; The 24-frame; 25-spherical grinding body
The specific embodiment
Embodiment 1; A kind of metal nano powder surface tension and particle agglomeration processing technology; Method is under-5 ℃ situation; Cutting frequency is set under the situation of per minute 6000 times and produces, processing powder grain shape is the nanometer iron powder or the non-ferrous metal nano powder granular material of spheroid; Sub-elect the concentrated powder body material of distribution of particles of (80nm is an example) D3=31nm D25=61.1nm D50=80nm D75=86.13nm D97=100.6nm more respectively, then to metal nanoparticle continuation thickness be again: the anti-oxidation coating of 2nm-3nm reaches more than 90 hours its anti-oxidization time; With the metal nano powder granular material after coating; Under-5 ℃ of situations, carry out per minute and run up, grind for 8000 rev/mins, the powder granule material is progressively eliminated the surface tension of itself in running up, grinding, and requires milling time to be controlled at 5 minutes--between-8 minutes.
Used cutting machine meaning as shown in Figure 1; Cutting machine structure comprises the body that has cooling system; Body is provided with charging aperture 2, inert gas entrance 1, is provided with some cutter groups in the lower end of charging aperture 2, and each cutter group comprises two cutters 5,14 that working face is relative; The working face of cutter 5,14 is zigzag or file shape, and two cutters 5,14 are exported the rotating parts combination through separately connecting rod 6,13 and frequency modulation vibrating motor 9 respectively.Cutting machine is designed to the dual-vibration system, and outer VIBRATION DESIGN is the gasbag-type vibrating device, and the internal vibration system is designed to the spring vibration device.The frequency modulation vibrating motor; Adopt the mode of frequency modulation to carry out the control of vibration frequency; Pass through adjusting rotating speed of motor 1500/minute---6000 biographies/minute, vibration frequency is controlled at 1500 times/minute---6000 times/minute, reaching the unlimited cutting of designing requirement---" zero boundry particle patterning method ".Cutting machine is when work, and indoor design adds inert gas and keeps the constant of processing temperature, in interlayer, adds the temperature processing that cooling water is set simultaneously.Its operation principle is to do relative motion through two cutters that frequency modulation motor drives each cutter group; Make the working face relative motion of two cutters; Move each other in its surperficial zigzag or file shape protruding part then; Major diameter feed metal particle about 80 orders-100 order of charging aperture adding is constantly rubbed, collides, pushes, and the effect that reaches at last is to make oarse-grained metallic particles be divided into the small diameter particles object.The surface of cutter is just as the structure on file surface, and its gap is adjustable, so that adapt to the size of raw material particle.After cutting machine work begins; Metallic particles powder irregular particle has been carried out in the motion process cutting for N time between two cutters from top to bottom; Certainly the frequency modulation motor rotating speed is high more; The probability that metallic particles is cut in unit interval is also big more, and the distribution probability of the metallic particles of the small diameter particles that it processes is also big more, and sorting is got up also easier.Generally to just can reach the nano metal powder particle more than 80% through six circulation cuttings.
Anti-oxidation coating process; Metal powder material is in temperature (100 ℃-310 ℃) and have and will add 10% when producing, processing under the environment of protective gas (N)---the purity oxygen of 15% (volume ratio); Forming thickness on the metal powder particles surface is 1nm---the oxide layer of 2nm, in the high temp tunnel stove, temperature is adjusted between 350 ℃-510 ℃ then; The metal powder particles material is under this temperature conditions; The surface oxide layer structure begins to soften, under the situation of sealing, in the inert gas N and the He of 4: 6 ratio injection dew point≤6; Injection length was controlled at 30 minutes---and 45 minutes, let inert gas fully be penetrated in the oxide layer on metal powder material surface.
The grinder of meaning as shown in Figure 2 comprises frame 24, and variable-frequency motor 22 is provided with hollow grinding body 19 through hollow rotating shaft 18 on the frame 24, and grinding body 19 is provided with charging and advances inertia gas port 21, and discharging opening 17 grinds in the body 19 and is provided with some mill balls 25.Operation principle like octahedral grinder among the figure is; Utilize adjustable frequency motor to control the rotating speed of grinder (1000 rev/mins---6000 rev/mins); Utilize the angle of anistree body; Reach 270 of metal species spherical particles and spend the counter-rotating that does not stop, thereby reach through the powder granule smooth surface spherical particles after grinding.Because from the metallic particles that cutting machine processes, generally be irregular globoid, through the grinding of the inner spherical grinding body of anistree grinder, irregular globoid will become ganoid spherical particles.Metal particle and inert gas with well cutting in the time of work add in the grinding body; Start driven by motor then and grind the body upset; Mutual collision between the mill ball can grind to form spheroidal particle with metal particle, the lengthening that its surface configuration can be in time and become gradually smooth.Grinder designs the input inert gas in charging, keep the temperature stabilization in the process.
Show that the diameter range of metallic particles nanometer from tens of to hundreds of does not wait in the photo of being illustrated like Fig. 3,4,5, this just needs to adopt the pneumatic separation technical point select the product that distribution of particles is concentrated relatively.The stressed surface area and the metal particle that utilize metal particle are in the parabolic curve and deadweight falling speed, the time of ferrous powder granules in container that receive under the slinging force situation.Utilize artificial wind-force in closed container, the different ferrous powder granules of diameter to be carried out effective classification with speed.Concrete sorting process is: at first start vacuum motor and in the container of classifying equipoment, form negative pressure state, then open the clasfficiator motor respectively and in closed container, form the axial flow whirlwind.Negative pressure will need the iron powder of classification to limit the quantity of to suck first closed container; In the axial flow whirlwind, sub-elect the maximum metallic particles of particle diameter; The residual metallic particle gets into second closed container; Classification goes out required ferrous powder granules in greater than the first axial flow whirlwind, and order two, three, level Four are carried out classification step by step, can obtain distribution of particles interval (100 μ m---the metal particle product of 10nm) concentrating relatively so simultaneously.In conjunction with technical scheme of the present invention; Quantity through adjusting distinguished and admirable size and fractionated container just can obtain corresponding product, and also tentatively sorting earlier constantly in the practical operation certainly detects then; The feedback adjustment mechanical parameter makes processing equipment can stably sub-elect product then.One of purpose of sorting is come out satisfactory product selecting exactly; Little can directly get into next program than requiring; Cut again than requiring big product will return one procedure; It two is products of selecting requirement, and the product that does not reach requirement will turn back to a last operation through screening installation, once more cutting.
Claims (1)
1. metal nano powder surface tension and particle agglomeration processing method; It is characterized in that at-5 ℃---under 0 ℃ the situation; Cutting frequency is set in per minute 5500 times---and producing under 6000 times the situation, processing the powder grain shape is the nanometer iron powder or the non-ferrous metal nano powder granular material of spheroid; Sub-elect the concentrated powder body material of distribution of particles of D3=31nm D25=61.1nm D50=80nm D75=86.13nm D97=100.6nm more respectively; Then again metal nanoparticle being continued thickness is: the anti-oxidation coating of 2nm-3nm; Its anti-oxidization time was reached more than 90 hours, and with the metal nano powder granular material after coating, 8000 rev/mins run up, grind---to carry out 6000 rev/mins of per minutes under 0 ℃ of situation--at-5 ℃; The powder granule material is progressively eliminated the surface tension of itself in running up, grinding, and requires milling time to be controlled at 5 minutes--between-8 minutes;
Anti-oxidation coating process: metal powder material is 100 ℃-310 ℃ of temperature and protective gas N is arranged
2Environment under produce, will add volume ratio 10% when processing---15% purity oxygen; Forming thickness on the metal powder particles surface is 1nm---the oxide layer of 2nm, in the high temp tunnel stove, temperature is adjusted between 350 ℃-510 ℃ then; The metal powder particles material is under this temperature conditions; The surface oxide layer structure begins to soften, under the situation of sealing, in the inert gas N of 4: 6 ratio injection dew point≤6
2And He, injection length was controlled at 30 minutes---and 45 minutes, let inert gas fully be penetrated in the oxide layer on metal powder material surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101790976A CN101758223B (en) | 2008-12-15 | 2009-09-28 | Metal nano powder surface tension and particle agglomeration processing technology |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810080193.0 | 2008-12-15 | ||
| CNA2008100801930A CN101433960A (en) | 2008-12-15 | 2008-12-15 | Technique for processing surface tension and particle agglomeration of metal nano powder |
| CN2009101790976A CN101758223B (en) | 2008-12-15 | 2009-09-28 | Metal nano powder surface tension and particle agglomeration processing technology |
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| CN101758223A CN101758223A (en) | 2010-06-30 |
| CN101758223B true CN101758223B (en) | 2012-05-23 |
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| CN106622571A (en) * | 2017-02-22 | 2017-05-10 | 江苏巨鑫磁业有限公司 | High-frequency diamond vibration ultrafine grinding device of soft magnetic powder |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1911567A (en) * | 2006-08-17 | 2007-02-14 | 王惠民 | Cutting production technology of metal nanometer powder zero boundry particle |
| CN1970200A (en) * | 2006-12-11 | 2007-05-30 | 王惠民 | Metal micron nano particle cladding process |
| CN101157128A (en) * | 2007-10-29 | 2008-04-09 | 王惠民 | Medicine special-purpose powdered iron |
| CN101157137A (en) * | 2007-10-29 | 2008-04-09 | 王惠民 | Electromagnetic energy transformation special-purpose powdered iron |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1911567A (en) * | 2006-08-17 | 2007-02-14 | 王惠民 | Cutting production technology of metal nanometer powder zero boundry particle |
| CN1970200A (en) * | 2006-12-11 | 2007-05-30 | 王惠民 | Metal micron nano particle cladding process |
| CN101157128A (en) * | 2007-10-29 | 2008-04-09 | 王惠民 | Medicine special-purpose powdered iron |
| CN101157137A (en) * | 2007-10-29 | 2008-04-09 | 王惠民 | Electromagnetic energy transformation special-purpose powdered iron |
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| CN101758223A (en) | 2010-06-30 |
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