CN101758226B

CN101758226B - Preparation method of special iron powder for metal object surface spraying and embedding technology

Info

Publication number: CN101758226B
Application number: CN2009101797015A
Authority: CN
Inventors: 王惠民
Original assignee: Individual
Current assignee: Individual
Priority date: 2008-09-30
Filing date: 2009-09-28
Publication date: 2012-05-30
Anticipated expiration: 2029-09-28
Also published as: CN101758226A

Abstract

The invention relates to a preparation method of metal nano powder, in particular to a preparation method of special iron powder for metal object surface spraying and embedding technology; the preparation method solves the problem that the form of iron powder particles used for spraying and embedding on the metal surface is not ideal in the prior art; the method comprises the following steps: under the condition that the high-frequency cutting times are set as 6000-6500 times per minute, the raw material is processed into nano iron powder with spherical particles at -5-5 DEG C, and then the powder material with particle distribution that D3=21nm, D25-32.5nm, D50=50nm, D75=63.2nm and D97=77.3nm is respectively sorted out, and a DQ cladding method is used to carry out anti-oxidation cladding of the iron powder particle with 2nm-3nm of thickness, and then the surface of the cladded powder particle is ground. The performance of iron powder prepared by the method is good, and the effect is good.

Description

The preparation method of iron powder special for metalized product surface spray-embedding technique

Technical field

The present invention relates to a kind of preparation method of metal nano powder, be specially a kind of preparation method of iron powder special for metalized product surface spray-embedding technique.

Background technology

The metal nano powder material sprays embedding in the metal surface be present a kind of ten minutes frontier science and technology technology in the world.The advantage of spray-embedding technique is, the monomer particle of metal nano powder material can be effectively and firm the combining of metallics, forms unique metal surface protection layer.Compare with technologies such as other spraying, injections, have precision height, even tissue, excellent performance, low, the metal powder material saving 81.31% of cost.

Its product is widely used in industrial circles such as Aero-Space, national defense industry, Electronics and Information Engineering, biologic medical apparatus, automobile, machinery, five metals, sports apparatus, timepiece industry, weapon industry.Therefore, the development that generally believes this technology in the world will cause the industrialization overlay coating, be coated with combine together the new shape technology of development of course industrialization.

The subject matter of the world and domestic spray-embedding technique existence at present is: not having perfect metal nano powder material spray-embedding technique, its reason in the world basically at present mainly is that the shape problem of metal nano powder material granule solves bad always.Because what at present spray-embedding technique used in the world almost all is inequilateral sheet, dendroid, metal nano powder material such as fibrous, the requirement that does not almost reach spray-embedding technique in actual use.U.S. B-2A stealth bomber for example, when just equipping our troops, the maintenance task all is that the technical staff by each major company accomplishes basically, 1 hour maintenance time of every flight is 132 hours.After each aerial mission was accomplished, high velocity air all can cause wearing and tearing to the body top layer.The unlikely decline of stealthy performance in order to ensure aircraft; After each flight; The technical staff will rebuild the radar absorbing on B-2A top layer with the method for spray-embedding technique; And newly spray the absorbing material of embedding because grain shape undesirable causes the overlapping wave-sucking performance that weakens aircraft of finite sum spray embedding in service life.Owing to lack desirable metal nano powder sphere material, so B-2A base deployment in overseas always, this is for the septic yanks that fight with global deployment, and this is an intolerable shortcoming.Since although B-2A equips our troops, U.S. army once repeatedly made by force in overseas, and B-2A never appears at the battlefield.U.S. latest model stealth fighter F-22A exists the problem of B-2A equally at present.

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 of producing 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.

Summary of the invention

The preparation method that the present invention provides a kind of iron powder special for metalized product surface spray-embedding technique in order to solve the metal surface that exists in the prior art and to spray the dissatisfactory problem of ferrous powder granules shape that embedding uses.

The present invention is realized by following technical scheme; A kind of preparation method of iron powder special for metalized product surface spray-embedding technique; May further comprise the steps: at-5 ℃---under 5 ℃ the condition; High frequency cutting number of times is set in per minute 6000 times---and under 6500 times the situation raw material is processed into the nanometer iron powder that powder granule is shaped as spheroid, sub-elects the powder body material of the distribution of particles of D3=21nm D25=32.5nm D50=50nm D75=63.2nm D97=77.3nm more respectively, then; Using " DQ coats method " that ferrous powder granules is continued thickness again is the anti-oxidation coating of 2nm-3nm, and the powder granule surface grinding after coating is handled.

Technical advantage of the present invention

1, technical advantage one of the present invention is; Shortcomings such as the life-span of spray-embedding technique is short in the world at present, cost is high, the spray embedding is overlapping, wave-absorbing effect difference have thoroughly been changed.

2, technical advantage two of the present invention is; Thoroughly changed the melting property of parent of spraying embedding nano-powder material and metal surface at present in the world; Formed metal nano powder material granule 2/3 embedding metal surface; Formed effectively the parent and melted integraty, solved metal object in high-speed cruising with permanent friction in and coming off and etching problem in the adverse circumstances corrosion.

3, technical advantage three of the present invention is; The metal nano powder material uses few, and cost is low.Data shows that the B-2A stealth bomber surface area of the U.S. is that 300 square metres, F-22A stealth fighter surface area are 35 square metres, and using the consumption of the every square meter metal nano powder of spray-embedding technique material is 97g.If use the spray embedding use amount of every square metre of the present invention's technology to have only 2g, be the U.S. spray the embedding use amount at present 1/49.

4, technical advantage four of the present invention is; Durability is in the world particularly 37 of the U.S. times at present.The particle that the metal nano powder material of embedding use is sprayed at present in the U.S. is dendroid basically; Spray is embedded in the degree of depth of aircraft metal surface and has only about 1/10 of powder granule relative diameter; At 2 Mach; Spray embedding powder granule expulsion rate under the 1h current intelligence is 42%, and technology of the present invention is at 2 Mach, and the spray embedding powder granule expulsion rate under 1h (wind-tunnel) current intelligence is 1.13%.

5, technical advantage five of the present invention is; With the suction ripple rate of amount under the unit are be at present in the world particularly the U.S. can't compare.For example, the spray-embedding technique of the U.S. on state-of-the art in the world stealth fighter F-22A at present, according to 35 square metres of amount unit ares, spray engaged column nano-powder material particle.

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 preparation method of iron powder special for metalized product surface spray-embedding technique; May further comprise the steps: (concrete processing method referenced patent application number is the cutting production technology of metal nanometer powder zero boundry particle of 2006100481685 records;) under-5 ℃ condition; High frequency cutting number of times is set under the situation of per minute 6500 times and produces, processing powder grain shape is the nanometer iron powder of the special-purpose spray-embedding technique of spheroid; Sub-elect the powder body material of the distribution of particles of (50nm is an example) D3=21nm D25=32.5nm D50=50nm D75=63.2nm D97=77.3nm more respectively; Then, using " DQ coats method " that ferrous powder granules is continued thickness again is the anti-oxidation coating of 2nm-3nm, and its anti-oxidization time was reached more than 90 hours; Powder body material after coating is input to the surface grinding of carrying out powder granule in the high-speed grinder handles, make it reach that the powder granule material surface is smooth, spheroid is perfectly round.

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 13% when producing, processing under the environment of protective gas (N)---the purity oxygen of 18% (volume ratio); Forming thickness on the metal powder particles surface is 2nm---the oxide layer of 3nm, 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 interval (100 μ m---the metal particle product of 10nm) concentrating relatively of various distribution of particles 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; Certainly also tentatively sorting earlier constantly in the practical operation; Instrument detecting product specification 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.

Embodiment 2: a kind of preparation method of iron powder special for metalized product surface spray-embedding technique; May further comprise the steps: under 5 ℃ condition; High frequency cutting number of times is set under the situation of per minute 6000 times and produces, processing powder grain shape is the nanometer iron powder of the special-purpose spray-embedding technique of spheroid; Sub-elect the powder body material of the distribution of particles of (50nm is an example) D3=21nm D25=32.5nm D50=50nm D75=63.2nm D97=77.3nm more respectively; Then; Using " DQ coats method " that ferrous powder granules is continued thickness again is the anti-oxidation coating of 2nm-3nm, and its anti-oxidization time was reached more than 90 hours, the powder body material after coating is input to the surface grinding of carrying out powder granule in the high-speed grinder handles.

Embodiment 3: a kind of preparation method of iron powder special for metalized product surface spray-embedding technique; May further comprise the steps: under 0 ℃ condition; High frequency cutting number of times is set under the situation of per minute 6250 times and produces, processing powder grain shape is the nanometer iron powder of the special-purpose spray-embedding technique of spheroid; Sub-elect the powder body material of the distribution of particles of (50nm is an example) D3=21nm D25=32.5nm D50=50nm D75=63.2nm D97=77.3nm more respectively; Then; Using " DQ coats method " that ferrous powder granules is continued thickness again is the anti-oxidation coating of 2nm-3nm, and its anti-oxidization time was reached more than 90 hours, the powder body material after coating is input to the surface grinding of carrying out powder granule in the high-speed grinder handles.

Claims

1. the preparation method of an iron powder special for metalized product surface spray-embedding technique; It is characterized in that: may further comprise the steps: at-5 ℃---under 5 ℃ the condition; High frequency cutting number of times is set in per minute 6000 times---under 6500 times the situation raw material is processed into the nanometer iron powder that powder granule is shaped as globoid; Sub-elect the powder body material of the distribution of particles of D3=21nm D25=32.5nm D50=50nm D75=63.2nm D97=77.3nm more respectively; Then using " DQ coats method " that ferrous powder granules is continued thickness again is the anti-oxidation coating of 2nm-3nm, and the powder granule surface grinding after coating is handled; The step of described " DQ coats method " is: ferrous powder granules is 50 ℃-510 ℃ and protective gas N is arranged in temperature ₂Environment under to add the purity oxygen of 3%-20% when carrying out production and processing; Forming thickness on the ferrous powder granules surface is the oxide layer of 2nm-3nm, in the high temp tunnel stove, temperature is adjusted between 350 ℃-510 ℃; Ferrous powder granules is under this temperature conditions; The surface oxide layer structure begins to soften, under the situation of sealing, in inert gas N and the He of 4: 6 ratio injection dew point≤6-10; Injection length was controlled at 30 minutes-45 minutes, let inert gas fully be penetrated in the oxide layer on ferrous powder granules surface.

2. the preparation method of iron powder special for metalized product surface spray-embedding technique according to claim 1; It is characterized in that: may further comprise the steps: under 0 ℃ condition; High frequency cutting number of times is set under the situation of per minute 6250 times raw material is processed into the nanometer iron powder that powder granule is shaped as globoid; Sub-elect the powder body material of the distribution of particles of D3=21nm D25=32.5nm D50=50nm D75=63.2nm D97=77.3nm more respectively; Then using " DQ coats method " that ferrous powder granules is continued thickness again is the anti-oxidation coating of 2nm-3nm; Its anti-oxidization time was reached more than 90 hours, the powder body material after coating is input to the surface grinding of carrying out powder granule in the high-speed grinder handles.

3. the cutting machine of processing such as claim 1,2 said iron powder special for metalized product surface spray-embedding technique; It is characterized in that: structure comprises the body (4) that has cooling system; Body (4) is provided with charging aperture (2), inert gas entrance (1); In body (4), be provided with some cutter groups; Each cutter group comprises two cutters (5,14) that working face is relative, and the working face of cutter (5,14) is zigzag or file shape, and two cutters (5,14) are exported the rotating part combination through separately connecting rod (6,13) and frequency modulation vibrating motor (9) respectively.