CN106825589A - A kind of mechanical alloying preparation method of niobium silica flour - Google Patents
A kind of mechanical alloying preparation method of niobium silica flour Download PDFInfo
- Publication number
- CN106825589A CN106825589A CN201611265515.XA CN201611265515A CN106825589A CN 106825589 A CN106825589 A CN 106825589A CN 201611265515 A CN201611265515 A CN 201611265515A CN 106825589 A CN106825589 A CN 106825589A
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- CN
- China
- Prior art keywords
- ball
- abrading
- element powder
- ethylene glycol
- silica flour
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/042—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Silicon Compounds (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of mechanical alloying preparation method of niobium silica flour, including selecting suitable powder, add stirring in ethylene glycol, after concentration in addition high-energy planetary ball mill machine, ball milling is carried out using different size abrading-ball, glucose carries out varied angle ball milling as antioxidant, present invention inhibits the oxidative phenomena in alloying process, the component uniformity of alloying process is improve.
Description
Technical field
The invention belongs to materials processing technology field, more particularly, to a kind of mechanical alloying preparation method of niobium silica flour.
Background technology
NbSi alloys, also known as NbSi compound based ultra-high temperature alloys, be by parent metal niobium with alloying element silicon and other
The alloy of alloying element composition, it has good Room-Temperature Fracture Toughness, elevated temperature strength, high temperature creep strength and resistance to high temperature oxidation
Ability, while having the advantages that high-melting-point and moderate density, thus is expected to turn into the superhigh temperature knot for being applied to more than 1350 DEG C
Structure material, one of good candidates structural material as fields such as contemporary aerospace industry, civilian industries, particularly exists
Blade of aviation engine field has broad application prospects.3D printing, or increasing material manufacturing is used as one kind of rising in recent years
Quick shaping process, using successively powdering, laser or electron beam melt the mode being molded, and realize being finish-machined to for precise part
Type, and the defects such as the shrinkage cavity shrinkage porosity of casting process appearance are avoided, as a kind of emerging material manufacturing process.Current 3D beats
Print powder used, main preparation methods have an atomization, involved by chemical reduction method and mechanical alloying etc., wherein atomization
Complex process, apparatus expensive, component prepared by chemical reduction method is uniform, but preparation yield is small, while chemical reagent can be produced to give up
Water, and mechanical alloying method major advantage is cheap equipment, processing method is simple, but its problem being primarily present is powder
Easily there is oxidation etc. in grain size skewness, process, limit the large-scale application of further development.
The content of the invention
In order to solve the above technical problems, the invention provides a kind of mechanical alloying preparation method of niobium silica flour.
The complete technical scheme of the present invention includes：
The mechanical alloying preparation method of niobium silica flour, comprises the following steps, the alloy compositions of selection are by atomic percent
Including Al：12-14%, Cr：1-1.6%, V：0.2-0.5%, balance of Nb,
According to the corresponding element powder of above-mentioned atomic percent selection said components, described powder particles are that 150-200 is micro-
Rice, is then added into obtaining mixture in ethylene glycol solvent, and the quality of ethylene glycol solvent is 4 times of element powder gross mass, with
After carry out ultrasonic activation stirring, heating concentration is carried out to above-mentioned solvent under conditions of continuing to stir after stirring 10min, by second
Glycol is concentrated into 0.8 times of element powder gross mass, in concentration process when quantity of solvent is reduced, it is also possible to uses rotation shaft mechanical instead and stirs
Mix.Said process is in order that all of element powder can be sufficiently mixed uniformly.
During element powder after above-mentioned concentration and ethylene glycol mixture added into high-energy planetary ball mill machine, the mill room of the ball mill
Rotatable 90 °, by ratio of grinding media to material 30:1 (mass ratio) selects ZrO2Ceramic Balls as abrading-ball, the abrading-ball include 10mm abrading-balls and
3mm abrading-balls, proportion 10mm abrading-balls：3mm abrading-ball=6.5:3.5, while adding the glucose for accounting for 0.2 times of element powder gross mass
Ball milling is carried out as antioxidant.
Then mill room is rotated by 90 °, i.e., by vertically becoming with the rotating speed ball milling 30h of 800r/min first in the mechanical milling process
It is level, then with the rotating speed ball milling 6h of 800r/min.
Gained ball milling slurry is vacuum dried, the niobium silica flour after mechanical alloying is obtained after sieving.
The present invention is relative to the advantage of prior art：
1. the problem of oxidation during mechanical alloying method is always a subject matter for restricting its application, conventional method
In the organic solvent that generally uses can only play the fierce collision of alloy in isolation itself and air contact, but high speed mechanical milling process, no
Occur that powder causes oxidation with air contact with can avoiding, and cost can then be significantly increased using inert gas purge, thus
The present invention is proposed using ethylene glycol and glucose as ball-milling additive, and in addition to completely cutting off air, above-mentioned auxiliary agent is also with micro-
Weak reproducibility, it is suppressed that the oxidative phenomena in alloying process, while be unlikely to cause powder corrosion again.
2. by the way of first stirring and concentrating again, the powder of various ingredients is sufficiently mixed, improve alloying mistake
The component uniformity of journey.
3. the stirring of varied angle, it is to avoid occur dead angle in mechanical milling process in ball grinder, powder is piled up.
4., according to multiple experiment, selection is adapted to the ball milling ginsengs such as the ratio of grinding media to material of niobium silica flour, abrading-ball composition and rotating speed, time
Number, makes the alloying effect optimized in the case of energy resource consumption as small as possible.
Specific embodiment
With reference to specific embodiment, the present invention will be further described.
The mechanical alloying preparation method of niobium silica flour, comprises the following steps, the alloy compositions of selection are by atomic percent
Including Al：12-14%, Cr：1-1.6%, V：0.2-0.5%, balance of Nb,
According to the corresponding element powder of above-mentioned atomic percent selection said components, described powder particles are that 150-200 is micro-
Rice, is then added into obtaining mixture in ethylene glycol solvent, and the quality of ethylene glycol solvent is 4 times of element powder gross mass, with
After carry out ultrasonic activation stirring, heating concentration is carried out to above-mentioned solvent under conditions of continuing to stir after stirring 10min, by second
Glycol is concentrated into 0.8 times of element powder gross mass, in concentration process when quantity of solvent is reduced, it is also possible to uses rotation shaft mechanical instead and stirs
Mix.Said process is in order that all of element powder can be sufficiently mixed uniformly.
During element powder after above-mentioned concentration and ethylene glycol mixture added into high-energy planetary ball mill machine, the mill room of the ball mill
Rotatable 90 °, by ratio of grinding media to material 30:1 (mass ratio) selects ZrO2Ceramic Balls as abrading-ball, the abrading-ball include 10mm abrading-balls and
3mm abrading-balls, proportion 10mm abrading-balls：3mm abrading-ball=6.5:3.5, while adding the glucose for accounting for 0.2 times of element powder gross mass
Ball milling is carried out as antioxidant.
Then mill room is rotated by 90 °, i.e., by vertically becoming with the rotating speed ball milling 30h of 800r/min first in the mechanical milling process
It is level, then with the rotating speed ball milling 6h of 800r/min.
Gained ball milling slurry is vacuum dried, the niobium silica flour after mechanical alloying is obtained after sieving.
The above, is only presently preferred embodiments of the present invention, and not the present invention is imposed any restrictions, every according to the present invention
Any simple modification, change and equivalent structure change that technical spirit is made to above example, still fall within skill of the present invention
In the protection domain of art scheme.
Claims (1)
1. the mechanical alloying preparation method of niobium silica flour, comprises the following steps, the alloy compositions of selection are by atomic percent bag
Include Al：12-14%, Cr：1-1.6%, V：0.2-0.5%, balance of Nb,
According to the corresponding element powder of above-mentioned atomic percent selection said components, described powder particles are 150-200 microns, with
After be added into obtaining mixture in ethylene glycol solvent, the quality of ethylene glycol solvent is 4 times of element powder gross mass, is then carried out
Ultrasonic activation is stirred, and heating concentration is carried out to above-mentioned solvent under conditions of continuing to stir after stirring 10min, and ethylene glycol is dense
0.8 times of element powder gross mass is reduced to, in concentration process when quantity of solvent is reduced, it is also possible to use rotary shaft mechanical agitation instead.On
The process of stating is in order that all of element powder can be sufficiently mixed uniformly.
By in the element powder after above-mentioned concentration and ethylene glycol mixture addition high-energy planetary ball mill machine, the mill room of the ball mill can revolve
Turn 90 °, by ratio of grinding media to material 30:1 (mass ratio) selects ZrO2Used as abrading-ball, the abrading-ball includes that 10mm abrading-balls and 3mm grind to Ceramic Balls
Ball, proportion 10mm abrading-balls：3mm abrading-ball=6.5:3.5, while adding the glucose conduct for accounting for 0.2 times of element powder gross mass
Antioxidant carries out ball milling.
Then mill room is rotated by 90 °, i.e., from being vertically changed into water with the rotating speed ball milling 30h of 800r/min first in the mechanical milling process
It is flat, then with the rotating speed ball milling 6h of 800r/min.
Gained ball milling slurry is vacuum dried, the niobium silica flour after mechanical alloying is obtained after sieving.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611265515.XA CN106825589B (en) | 2016-12-30 | 2016-12-30 | A kind of mechanical alloying preparation method of niobium metal powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611265515.XA CN106825589B (en) | 2016-12-30 | 2016-12-30 | A kind of mechanical alloying preparation method of niobium metal powder |
Publications (2)
| Publication Number | Publication Date |
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| CN106825589A true CN106825589A (en) | 2017-06-13 |
| CN106825589B CN106825589B (en) | 2018-07-17 |
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| CN201611265515.XA Expired - Fee Related CN106825589B (en) | 2016-12-30 | 2016-12-30 | A kind of mechanical alloying preparation method of niobium metal powder |
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| WO2020102200A1 (en) * | 2018-11-14 | 2020-05-22 | Sun Chemical Corporation | Metallic bismuth pigments |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1094283A (en) * | 1965-05-25 | 1967-12-06 | Ciba Ltd | Method for the manufacture of tantalum and/or niobium powder |
| JPH04350105A (en) * | 1991-05-27 | 1992-12-04 | Kawasaki Steel Corp | Production of high fusion point active metal or alloy fine powder |
| CN1328889A (en) * | 2001-06-26 | 2002-01-02 | 中国科学院长春应用化学研究所 | Tungsten aluminium carbide hard alloy nanometer powder preparation method |
| CN1498707A (en) * | 2002-11-09 | 2004-05-26 | 昆明贵金属研究所 | Micropowder method for producing copper based sheet with rare-noble metal contained |
| CN1513628A (en) * | 2003-05-21 | 2004-07-21 | 昆明理工恒达科技有限公司 | Production method of scale shpared zinc powler |
| CN104148656A (en) * | 2014-07-14 | 2014-11-19 | 中山大学 | Flake copper powder preparation method |
-
2016
- 2016-12-30 CN CN201611265515.XA patent/CN106825589B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1094283A (en) * | 1965-05-25 | 1967-12-06 | Ciba Ltd | Method for the manufacture of tantalum and/or niobium powder |
| JPH04350105A (en) * | 1991-05-27 | 1992-12-04 | Kawasaki Steel Corp | Production of high fusion point active metal or alloy fine powder |
| CN1328889A (en) * | 2001-06-26 | 2002-01-02 | 中国科学院长春应用化学研究所 | Tungsten aluminium carbide hard alloy nanometer powder preparation method |
| CN1498707A (en) * | 2002-11-09 | 2004-05-26 | 昆明贵金属研究所 | Micropowder method for producing copper based sheet with rare-noble metal contained |
| CN1513628A (en) * | 2003-05-21 | 2004-07-21 | 昆明理工恒达科技有限公司 | Production method of scale shpared zinc powler |
| CN104148656A (en) * | 2014-07-14 | 2014-11-19 | 中山大学 | Flake copper powder preparation method |
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| CN106825589B (en) | 2018-07-17 |
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Granted publication date: 20180717 Termination date: 20181230 |