CN107321994A - A kind of preparation method of supersaturated Al (Ti) metal solid solution powder - Google Patents
A kind of preparation method of supersaturated Al (Ti) metal solid solution powder Download PDFInfo
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- CN107321994A CN107321994A CN201710331038.0A CN201710331038A CN107321994A CN 107321994 A CN107321994 A CN 107321994A CN 201710331038 A CN201710331038 A CN 201710331038A CN 107321994 A CN107321994 A CN 107321994A
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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
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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
- 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
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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
- 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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- 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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/01—Reducing atmosphere
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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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/10—Inert gases
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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
- B22F2202/00—Treatment under specific physical conditions
- B22F2202/13—Use of plasma
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Abstract
The present invention provides a kind of preparation method of supersaturated Al (Ti) metal solid solution powder, alternately ground with planetary ball mill mode by using adherent ball milling method, while the plasmaassisted ball milling method for being also subject to double-dielectric barrier discharge carries out ball milling to Al powder and Ti powder and prepares supersaturation Al（Ti）Solid-solution powder.The degree of refinement and the uniformity of Al (Ti) solid-solution powder prepared using this preparation method are greatly improved, also shorten sample Ball-milling Time simultaneously, operating efficiency is improved, this method is also applied in the preparation of Al Base Metal solid-solution powders of other transition elements.
Description
Technical field
The invention belongs to solid-solution powder preparing technical field, and in particular to a kind of supersaturated Al (Ti) metal solid solution powder
The preparation method at end.
Background technology
Equilirbium solid solubilities of the Ti in Al only has 0.12% atomic ratio, to prepare the supersaturated Al that solid solubility is higher than the concentration
(Ti) solid solution must use non-equilibrium process, such as quenching method, or high energy ball mill method.Quenching method needs higher cooling speed
Rate, but quenching product is not small particle powder, and powdered supersaturated Al (Ti) solid solution can be directly made in ball-milling method.
The ball grinder and abrading-ball that current high-energy ball milling is generally used are mainly metal material, such as stainless cylinder of steel or hard are closed
Golden tank, but because Al viscosity causes during ball milling Al easily with metal tank skin and abrading-ball to stick together greatly, and Al ratio is got over
Height, adhesion degree is significantly increased.Grinding aid, such as stearic acid are usually added into, adhesion can be significantly reduced, but ball milling comes out not
It is powdery but strip.In addition ball milling product uniformity is poor, and grinding aid is difficult to complete component and has larger pollution.Even if such as
This, also is difficult to prepare supersaturated Al (Ti) solid-solution powder that solid solubility is less than 5mol% based on metal can and abrading-ball.
The content of the invention
There is provided a kind of supersaturated Al (Ti) metal solid solution for technical problem present in above-mentioned background technology by the present invention
The preparation method of powder.
A kind of preparation method of supersaturated Al (Ti) metal solid solution powder, comprises the following steps：
1）First by Al powder and Ti powder according to Al:Ti=100:X atomic ratio loads in ball grinder, and wherein X is 0.5-5, two kinds of powder
Last gross mass is 3-10g, is then charged into abrading-ball, adds 5-20ml normal heptane；
2）Electrode bar is installed on the cover plate of ball grinder, cover plate is covered, electrode bar is located in the middle of tank interior, electrode bar and ball grinder
Outer surface connects the two poles of the earth of high-voltage ac power respectively；
3）Closed ball grinder is carried out with vavuum pump to vacuumize 2min, gas medium is then charged with, 3 times are repeated, finally
Insufflation gas medium makes air pressure in ball grinder be 0.1-1atm；
4）Ball grinder is attached to the shake table of adherent ball mill device, regulation motor Starting mode, with steady-state speed carry out ball milling 1h,
Stop the 10min adherent ball milling of batch (-type), when carrying out ball milling, connect high-voltage ac power, ball grinder internal gas is occurred brightness
Light electric discharge produces plasma；
5）Ball grinder is unloaded after often carrying out adherent ball milling 5h, ball grinder, which is installed to planetary ball mill, carries out ball milling 5min, then
Step 4 is carried out again）Adherent ball milling；
6）Repeat step 4）With step 5）Sample is gathered after carrying out ball milling 30h, XRD is finally carried out and is tested with electron microscopic.
Further, step 1）The granularity of middle Al powder is less than 100 mesh, and the granularity of Ti powder is less than 100 mesh..
Further, step 1）Described in ball grinder be double-decker, its internal layer tank body uses ceramic material, such as aoxidizes
The outer layer tank body such as zirconium, silicon nitride uses metal material, such as aluminium alloy, copper, stainless steel, and the abrading-ball uses ceramic material.Ball
Grinding jar internal layer uses ceramic material with abrading-ball, can make it that Al does not stick together with ball milling top tank structure and abrading-ball during ball milling.
Further, step 1）Described in abrading-ball be divided into big abrading-ball and small abrading-ball, a diameter of 20-25mm of big abrading-ball is small
A diameter of 12-16mm of abrading-ball, wherein the quantity of big abrading-ball is 2-4, the quantity of small abrading-ball is 3-6.
Further, step 3）Described in gas medium be inert gas or reducibility gas, such as argon gas, hydrogen etc..
Further, step 4）Described in steady-state speed be 1000-1600r/min..
Further, step 4）The voltage of mesohigh AC power is 10-20kV, and frequency is 10-20kHz..
Compared with prior art, the beneficial effects of the invention are as follows：
1st, ball grinder internal layer of the invention and the ceramic material that abrading-ball is high rigidity and high abrasion so that the sample of Metal Substrate is basic
It will not be sticked together with ball grinder and abrading-ball, ball milling process will not be influenceed by any because of adhesive band；
2nd, preparation method of the invention can prepare Al (Ti) supersaturated solid solution powder that solid solubility is less than 5mol%, Gu
Solubility even can be with as little as 0.5mol%, than other method order of magnitude lower；
3rd, when the present invention uses internal layer for the ball grinder progress plasmaassisted ball milling of ceramic material, because tank body internal layer is exhausted
Edge material, it is possible to achieve double-dielectric barrier discharge, and the cold plasma of double-dielectric barrier discharge formation is all-metal than tank body
Single dielectric barrier discharge situation can be more uniform, due to all samples by plasma action intensity very close to this makes
Obtained sample distribution of particle sizes it is narrower, properties of samples also closer to；
4th, present invention employs adherent ball milling method, abrading-ball touch ball milling top tank structure and does high speed circular motion, abrading-ball not with ball milling
Top tank structure is collided, and abrading-ball is not also collided with middle electrode bar so that the service life of electrode bar is greatly improved；Secondly grind
It is also sufficiently stable that ball and sample are distributed the plasma glow formed in stabilization, tank body in ball milling；3rd, adherent ball milling method
Under, abrading-ball skid crosses powder, more has powder fining than traditional ball milling method；In addition, the mechanical energy that adherent ball milling is provided is higher,
And ballmilling energy control is more accurate；；
5th, the present invention while by planetary ball mill mode and adherent ball milling method alternately so that both obtained plasma asistance patch
The advantage of squash mill, also has the high advantage of the sample uniformity under planetary ball mill concurrently, solves adherent ball milling method because of powder and mill
The regular motion of ball makes powder spend low, lack of homogeneity shortcoming in a jumble so that the uniformity of sample is greatly improved；
6th, the present invention is using heptane as grinding aid, and with the effect for obstructing particle aggregation, heptane is volatilizable to generate heptane steam,
Plasma can be formed under dielectric impedance, and heptane is inert substance for sample, and normal heptane is easily by evaporation
Separated, pollution will not be produced to sample, while heptane can also be that powder is attached to ball milling top tank structure without kicking up so that electricity
Two electrodes of pole rod and tank body metal shell are difficult to produce short-circuit protection because kicking up conductive powder in tank；
7th, preparation method of the invention is also applied in other Al (TM) solid solution, and TM transition elements can be Zr, V, Nb
Deng being widely used.
Brief description of the drawings
Fig. 1 is the sample XRD diffracting spectrums of the embodiment of the present invention 1；
Fig. 2 is the sample Ti energy spectrum diagrams of the embodiment of the present invention 1；
Fig. 3 is that the obtained sample powder tabletting of the embodiment of the present invention 1 is carried out after the polishing of surface, and the secondary electron of burnishing surface is micro-
Figure.
Embodiment
The present invention is described below in conjunction with drawings and examples, following examples are explained with invention optimal effectiveness,
But the limitation of these embodiments and non-invention.
Embodiment 1：
A kind of preparation method of supersaturated Al (Ti) metal solid solution powder, step is as follows：
1）First by Al powder and Ti powder according to 100：2 atomic ratio loads in ball grinder, and the granularity of Al powder and Ti powder is respectively less than
100 mesh, two kinds of powder gross masses are 3g, are then charged into abrading-ball, add 12ml heptane；
2）Electrode bar is installed on the cover plate of ball grinder, cover plate is covered, electrode bar is located in the middle of tank interior, electrode bar and ball grinder
Outer surface connects the two poles of the earth of high-voltage ac power respectively；
3）Closed ball grinder is carried out with vavuum pump to vacuumize 2min, argon gas is then charged with, is repeated 3 times, by ball grinder
Internal water and oxygen content reduction, last time insufflation gas medium make air pressure in ball grinder be 0.1atm；
4）Ball grinder is attached to the shake table of adherent ball mill device, regulation motor Starting mode is entered with steady-state speed 1000r/min
Row ball milling 1h, the adherent ball milling of batch (-type) for stopping 10min, when carrying out ball milling, connect high-voltage ac power, voltage is 10kV, frequency
Rate is 10 kHz, ball grinder internal gas is occurred glow discharge and produces plasma；
5）Ball grinder is unloaded after often carrying out adherent ball milling 5h, ball grinder, which is installed to planetary ball mill, carries out ball milling 5min, then
Step 4 is carried out again）Adherent ball milling；
6）Repeat step 4）With step 5）Sample is gathered after carrying out ball milling 30h, XRD is finally carried out and is tested with electron microscopic.
In the present embodiment, ball grinder is double-decker, and its internal layer tank body uses zirconium oxide material, and outer layer tank body uses aviation
Aluminium material, the abrading-ball uses zirconium oxide material.
In the present embodiment, abrading-ball is divided into big abrading-ball and small abrading-ball, a diameter of 20mm of big abrading-ball, small abrading-ball it is a diameter of
12mm, the quantity of big abrading-ball is 4, and the quantity of small abrading-ball is 6.
Supersaturated Al (Ti) solid solution prepared by the above method, is powdered, granularity is less than 300 mesh；Such as
The XRD diffracting spectrums of sample are shown in Fig. 1, only find there is single Al (Ti) solid solution, its diffraction maximum is with respect to simple substance Al situations
Offset to high angle, do not see any phase of thing containing Ti, also can't see any impurity diffraction maximum；Such as sample Ti energy spectrum diagrams point in Fig. 2
Analysis finds distributing very evenly for Ti；As shown in figure 3, obtained sample powder tabletting is carried out after the polishing of surface, burnishing surface
Secondary electron micro image analysis show that sample basic expressions are contrast, this illustrates the composition of made solid solution
It is highly uniform.
Embodiment 2：
It is with the difference of embodiment 1, the gas medium being filled with into ball grinder is hydrogen, last time insufflation gas are situated between
Matter makes air pressure in ball grinder be 1 atm, and remaining operation principle is same as Example 1.
Embodiment 3：
It is with the difference of embodiment 1, by Al powder and Ti powder according to Al:Ti=100:0.5 atomic ratio loads ball grinder
Interior, two kinds of powder gross masses are 10g, and 20ml heptane is added into ball grinder, and remaining operation principle is same as Example 1.
Embodiment 4：
It is with the difference of embodiment 1, by Al powder and Ti powder according to Al:Ti=100:5 atomic ratio loads in ball grinder,
Two kinds of powder gross masses are 5g, and 20ml heptane is added into ball grinder, and remaining operation principle is same as Example 1.
Embodiment 5：
It is with the difference of embodiment 1, the motor steady-state speed of adherent ball mill device is 1600r/min, and remaining work is former
Reason is same as Example 1.
Embodiment 6：
It is with the difference of embodiment 1, the motor steady-state speed of adherent ball mill device is 1300r/min, and remaining work is former
Reason is same as Example 1.
Embodiment 7：
It is with the difference of embodiment 1, the voltage of high-voltage ac power is 20kV, and frequency is 20kHz, remaining operation principle
It is same as Example 1.
Embodiment 8：
It is with the difference of embodiment 1, the voltage of high-voltage ac power is 15kV, and frequency is 15kHz, remaining operation principle
It is same as Example 1.
Embodiment 9：
It is with the difference of embodiment 1, a diameter of 25mm of big abrading-ball, a diameter of 16mm of small abrading-ball, the number of big abrading-ball
Measure as 2, the quantity of small abrading-ball is 3, and remaining operation principle is same as Example 1.
Embodiment 10：
It is with the difference of embodiment 1, a diameter of 22mm of big abrading-ball, a diameter of 14mm of small abrading-ball, the number of big abrading-ball
Measure as 3, the quantity of small abrading-ball is 5, and remaining operation principle is same as Example 1.
Obviously, above-described embodiment is used for the purpose of clearly illustrating example of the present invention, and the not limit to implementation
It is fixed.For the those of ordinary skill in the field, it can also make on the basis of the above description other various forms of
Change changes.There is no need and unable to all embodiment party's formulas with exhaustion.And thus amplify out it is obvious
Among change or variation are still in protection scope of the present invention.
Claims (7)
1. a kind of preparation method of supersaturated Al (Ti) metal solid solution powder, it is characterised in that：Comprise the following steps,
1）First by Al powder and Ti powder according to Al:Ti=100:X atomic ratio loads in ball grinder, and wherein X is 0.5-5, two kinds of powder
Last gross mass is 3-10g, is then charged into abrading-ball, adds 5-20ml normal heptane；
2）Electrode bar is installed on the cover plate of ball grinder, cover plate is covered, electrode bar is located in the middle of tank interior, electrode bar and ball grinder
Outer surface connects the two poles of the earth of high-voltage ac power respectively；
3）Closed ball grinder is carried out with vavuum pump to vacuumize 2min, gas medium is then charged with, 3 times are repeated, finally
Insufflation gas medium makes air pressure in ball grinder be 0.1-1atm；
4）Ball grinder is attached to the shake table of adherent ball mill device, regulation motor Starting mode, with steady-state speed carry out ball milling 1h,
Stop the 10min adherent ball milling of batch (-type), when carrying out ball milling, connect high-voltage ac power, ball grinder internal gas is occurred brightness
Light electric discharge produces plasma；
5）Ball grinder is unloaded after often carrying out adherent ball milling 5h, ball grinder, which is installed to planetary ball mill, carries out ball milling 5min, then
Step 4 is carried out again）Adherent ball milling；
6）Repeat step 4）With step 5）Sample is gathered after carrying out ball milling 30h, XRD is finally carried out and is tested with electron microscopic.
2. a kind of preparation method of supersaturated Al (Ti) metal solid solution powder according to claim 1, it is characterised in that：
Step 1）The granularity of middle Al powder is less than 100 mesh, and the granularity of Ti powder is less than 100 mesh.
3. a kind of preparation method of supersaturated Al (Ti) metal solid solution powder according to claim 1, it is characterised in that：
Step 1）Described in ball grinder be double-decker, its internal layer tank body uses ceramic material, and outer layer tank body uses metal material, described
Abrading-ball uses ceramic material.
4. a kind of preparation method of supersaturated Al (Ti) metal solid solution powder according to claim 1, it is characterised in that：
Step 1）Described in abrading-ball be divided into big abrading-ball and small abrading-ball, a diameter of 20-25mm of big abrading-ball, a diameter of 12- of small abrading-ball
16mm, wherein the quantity of big abrading-ball is 2-4, the quantity of small abrading-ball is 3-6.
5. a kind of preparation method of supersaturated Al (Ti) metal solid solution powder according to claim 1, it is characterised in that：
Step 3）Described in gas medium be inert gas or reducibility gas.
6. a kind of preparation method of supersaturated Al (Ti) metal solid solution powder according to claim 1, it is characterised in that：
Step 4）Described in steady-state speed be 1000-1600r/min.
7. a kind of preparation method of supersaturated Al (Ti) metal solid solution powder according to claim 1, it is characterised in that：
Step 4）The voltage of mesohigh AC power is 10-20kV, and frequency is 10-20kHz.
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| CN201710331038.0A CN107321994A (en) | 2017-05-11 | 2017-05-11 | A kind of preparation method of supersaturated Al (Ti) metal solid solution powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115365501A (en) * | 2022-08-11 | 2022-11-22 | 广东工业大学 | High-entropy alloy prepared by discharge plasma assisted ball milling and application thereof in diamond tool |
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| JPH062016A (en) * | 1992-06-22 | 1994-01-11 | Suzuki Motor Corp | Al-ti intermetallic compound powder and its production |
| CN1718282A (en) * | 2005-07-29 | 2006-01-11 | 华南理工大学 | High energy ball mill method with plasma aid |
| CN101239335A (en) * | 2008-03-07 | 2008-08-13 | 华南理工大学 | Plasma auxiliary high-energy planetary ball mill device |
| CN104174856A (en) * | 2014-08-29 | 2014-12-03 | 中国科学院重庆绿色智能技术研究院 | Method for preparing TiAl-based composite powder material |
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2017
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Patent Citations (4)
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| JPH062016A (en) * | 1992-06-22 | 1994-01-11 | Suzuki Motor Corp | Al-ti intermetallic compound powder and its production |
| CN1718282A (en) * | 2005-07-29 | 2006-01-11 | 华南理工大学 | High energy ball mill method with plasma aid |
| CN101239335A (en) * | 2008-03-07 | 2008-08-13 | 华南理工大学 | Plasma auxiliary high-energy planetary ball mill device |
| CN104174856A (en) * | 2014-08-29 | 2014-12-03 | 中国科学院重庆绿色智能技术研究院 | Method for preparing TiAl-based composite powder material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115365501A (en) * | 2022-08-11 | 2022-11-22 | 广东工业大学 | High-entropy alloy prepared by discharge plasma assisted ball milling and application thereof in diamond tool |
| CN115365501B (en) * | 2022-08-11 | 2024-01-12 | 广东工业大学 | Preparation of high-entropy alloy by discharge plasma assisted ball milling and application of high-entropy alloy to diamond tool |
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