CN104741614B - A kind of high Zr content Ti50.5‑xNi49.5ZrxThe preparation method of manganese ternary alloy powder - Google Patents
A kind of high Zr content Ti50.5‑xNi49.5ZrxThe preparation method of manganese ternary alloy powder Download PDFInfo
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Abstract
A kind of high Zr content Ti50.5‑xNi49.5ZrxThe preparation method of manganese ternary alloy powder, the present invention relates to the preparation method of alloy powder.The invention solves the problems that prepared by existing method TiNiZr alloy efficiency is low, complex process, and the low technical problem of Zr content.Method：First, Ti powder, Ni powder and Ti are weighed10Zr90Alloyed powder；2nd, raw material is loaded in ball grinder；3rd, ball milling.The inventive method can make stable components with precise control composition, can prepare the material with special component content, especially prepare the Ti containing high Zr content50.5‑ xNi49.5ZrxManganese ternary alloy powder.The present invention is used for preparing high Zr content Ti50.5‑xNi49.5ZrxManganese ternary alloy powder.
Description
Technical field
The present invention relates to the preparation method of alloy powder.
Background technology
Ternary shape memory alloy TiNiZr has high transformation temperature, mechanical performance, corrosion resistance, wearability, high damping,
SME and super-elasticity all show excellent performance.TiNiZr alloyed powder, used as high phase transformation ternary shape of new generation
The primary raw material of shape memory alloys TiNiZr material, with stable components, purity is high, the controlled feature of crystallite dimension.
Mechanical alloying prepares the application of multicomponent alloy powder body material widely, is wherein compared with representative with ball grinding technique
Property.Ball milling causes the size of two or more metal powder granulates to there occurs change under outside energy-activation, typically
Several material powders can be caused Particle Breakage under mechanical external force effect, alloy is caused by constantly fracture seam process
The particle diameter of powder changes, the phase counterdiffusion in mechanical milling process of various atoms, mutual solid solution.But it is each in mechanical milling process
Selection such as ball mill mode, ratio of grinding media to material, ball milling speed, Ball-milling Time, process control agent and gaseous environment etc. of kind of parameter but
Alloying process will be affected, and then affects the performance of final alloy powder.
In recent years, the atom content for preparing Zr in TiNiZr alloy is at maximum up to 25% (HSIEH S F, WU S
K.Materials characterization,1998,41(4):151-162.), seldom have and prepared by mechanical alloying
The method of higher Zr content.The Ti of high Zr content50.5-xNi49.5ZrxManganese ternary alloy powder can promote the ternary shape for eventually forming
Shape memory alloys phase transition temperature is improved, and how to make suitable ball-milling technology to prepare the Ti containing high Zr content50.5- xNi49.5ZrxManganese ternary alloy powder is very necessary.
Content of the invention
The invention solves the problems that prepared by existing method TiNiZr alloy efficiency is low, complex process, and the low technology of Zr content is asked
Topic, and a kind of high Zr content Ti is provided50.5-xNi49.5ZrxThe preparation method of manganese ternary alloy powder.
A kind of high Zr content Ti50.5-xNi49.5ZrxThe preparation method of manganese ternary alloy powder, specifically enters according to following steps
Capable：
First, the atomic ratio according to Ti, Ni and Zr is (50.5-X): 49.5: X, weigh Ti powder, Ni powder and Ti10Zr90Alloy
Powder, wherein 20≤X≤35；
2nd, Ti powder, Ni powder and the Ti for step one being weighed10Zr90Alloyed powder is mixed and is put in ball grinder, is added
Stearic acid and abrading-ball, then suction filtration vacuum 3 times, are re-filled with argon gas；
3rd, the ball grinder that processes of step 2 is loaded in planetary ball mill, carries out ball milling, control per rotating 10～
30min, then 10～20min of air cooling, drum's speed of rotation are 250rpm～450rpm, and Ball-milling Time is 6～60h, are obtained a kind of high
Zr content Ti50.5-xNi49.5ZrxManganese ternary alloy powder.
The invention has the beneficial effects as follows：
(1), the inventive method low cost, efficiency high, process is simple, high with yield, and good industrialization prospect；
(2), the inventive method can prepare conventional method be difficult to the refractory metal that obtains or alloy material and those
The powder of chemical reaction can not be participated in；
(3), the inventive method can make stable components with precise control composition, can prepare with special component content
Material, especially prepares the Ti containing high Zr content50.5-xNi49.5ZrxManganese ternary alloy powder.
The present invention is used for preparing high Zr content Ti50.5-xNi49.5ZrxManganese ternary alloy powder.
Description of the drawings
Fig. 1 is Ti obtained in embodiment one30.5Ni49.5Zr20Manganese ternary alloy powder surface topography map；
Fig. 2 is Ti obtained in embodiment two20.5Ni49.5Zr30Manganese ternary alloy powder surface topography map；
Fig. 3 is Ti obtained in embodiment three15.5Ni49.5Zr35Manganese ternary alloy powder surface topography map.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, also include each specific embodiment it
Between any combination.
Specific embodiment one：A kind of high Zr content Ti of present embodiment50.5-xNi49.5ZrxThe preparation of manganese ternary alloy powder
Method, specifically follows the steps below：
First, the atomic ratio according to Ti, Ni and Zr is (50.5-X): 49.5: X, weigh Ti powder, Ni powder and Ti10Zr90Alloy
Powder, wherein 20≤X≤35；
2nd, Ti powder, Ni powder and the Ti for step one being weighed10Zr90Alloyed powder is mixed and is put in ball grinder, is added
Stearic acid and abrading-ball, then suction filtration vacuum 3 times, are re-filled with argon gas；
3rd, the ball grinder that processes of step 2 is loaded in planetary ball mill, carries out ball milling, control per rotating 10～
30min, then 10～20min of air cooling, drum's speed of rotation are 250rpm～450rpm, and Ball-milling Time is 6～60h, are obtained a kind of high
Zr content Ti50.5-xNi49.5ZrxManganese ternary alloy powder.
Specific embodiment two：Present embodiment from unlike specific embodiment one：The purity of Ti powder in step one
Purity >=99.9% of >=99.9%, Ni powder, Ti10Zr90Purity >=99.5% of alloyed powder, and Ti powder, Ni powder and Ti10Zr90Close
The granularity of bronze is 200～400 mesh.
Specific embodiment three：Present embodiment from unlike specific embodiment one：Ti powder in step 2, Ni powder and
Ti10Zr90The gross mass of alloyed powder is (100～200) with stearic mass ratio: 1.Other are identical with specific embodiment one.
Extend with Ball-milling Time, powder reunion, slimeball, wall sticking phenomenon can become apparent from.Resistance increases, and abrading-ball is held with ball milling
Device inwall also wears out and increases, and affects the composition of flour extraction and powder.Select to add stearic acid as process control agent, increase profit
Sliding effect, when stearic acid adds excessive, may produce some unnecessary side reactions.
Specific embodiment four：Present embodiment from unlike specific embodiment one：Ball in ball grinder in step 2
Material mass ratio is (8～15):1.Other are identical with specific embodiment one.
Ratio of grinding media to material has important impact to reaction rate, and it determines the amount of powder and unit interval captured during collision
The number of times of interior effective collision.
Specific embodiment five：Present embodiment from unlike specific embodiment one：In step 2, abrading-ball is stainless
Steel abrading-ball, a diameter of 10mm.Other are identical with specific embodiment one.
Specific embodiment six：Present embodiment from unlike specific embodiment one：Drum's speed of rotation in step 3
For 250rpm, Ball-milling Time is 12h.Other are identical with specific embodiment one.
Specific embodiment seven：Present embodiment from unlike specific embodiment one：Drum's speed of rotation in step 3
For 350rpm, Ball-milling Time is 24h.Other are identical with specific embodiment one.
Specific embodiment eight：Present embodiment from unlike specific embodiment one：Drum's speed of rotation in step 3
For 450rpm, Ball-milling Time is 36h.Other are identical with specific embodiment one.
Specific embodiment nine：Present embodiment from unlike specific embodiment one：Control per positive and negative in step 3
Turn 15min, then air cooling 15min.Other are identical with specific embodiment one.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：
A kind of high Zr content Ti of the present embodiment50.5-xNi49.5ZrxThe preparation method of manganese ternary alloy powder, specifically according to
Lower step is carried out：
First, according to Ti, Ni and Zr atomic ratio be 30.5: 49.5: 20, weigh 9.4g Ti powder, 23.5g Ni powder and
17.8g Ti10Zr90Alloyed powder；Purity >=99.9% of Ti powder, purity >=99.9% of Ni powder, Ti10Zr90The purity of alloyed powder
>=99.5%, and Ti powder, Ni powder and Ti10Zr90The granularity of alloyed powder is 300 mesh；
2nd, Ti powder, Ni powder and the Ti for step one being weighed10Zr90Alloyed powder is mixed and is put in ball grinder, is added
0.3g stearic acid and abrading-ball, then suction filtration vacuum 3 times, are re-filled with argon gas；Abrading-ball is stainless steel abrading-ball, a diameter of 10mm, ball milling
In tank, ball material mass ratio is 10:1；
3rd, the ball grinder for processing step 2 loads in planetary ball mill, carries out ball milling, the every rotating 15min of control,
Air cooling 15min again, drum's speed of rotation are 250rpm, and Ball-milling Time is 12h, and a kind of high Zr content Ti is obtained30.5Ni49.5Zr20Three
First alloy powder.
Ti obtained in the present embodiment30.5Ni49.5Zr20Manganese ternary alloy powder surface topography map is as shown in Figure 1, it can be seen that ball
Particle size after mill is at 1-3 μm or so；Ti30.5Ni49.5Zr20The power spectrum of manganese ternary alloy powder is as shown in table 1, as seen from table
Ti30.5Ni49.5Zr20The atomic fraction of middle Ti, Ni, Zr is respectively 30.4%, 49.5% and 20.1%, it can be seen that after ball milling
Differ very little between component content and standard design component content.
Table 1
| Element | Wt% | At% |
| ZrL | 29.61 | 20.11 |
| TiK | 23.46 | 30.36 |
| NiK | 46.93 | 49.53 |
| Matrix | Correction | ZAF |
Embodiment two：
A kind of high Zr content Ti of the present embodiment50.5-xNi49.5ZrxThe preparation method of manganese ternary alloy powder, specifically according to
Lower step is carried out：
First, according to Ti, Ni and Zr atomic ratio be 20.5: 49.5: 30, weigh 4.0g Ti powder, 22.0g Ni powder and
25.0g Ti10Zr90Alloyed powder；Purity >=99.9% of Ti powder, purity >=99.9% of Ni powder, Ti10Zr90The purity of alloyed powder
>=99.5%, and Ti powder, Ni powder and Ti10Zr90The granularity of alloyed powder is 300 mesh；
2nd, Ti powder, Ni powder and the Ti for step one being weighed10Zr90Alloyed powder is mixed and is put in ball grinder, is added
0.3g stearic acid and abrading-ball, then suction filtration vacuum 3 times, are re-filled with argon gas；Abrading-ball is stainless steel abrading-ball, a diameter of 10mm, ball milling
In tank, ball material mass ratio is 10:1；
3rd, the ball grinder for processing step 2 loads in planetary ball mill, carries out ball milling, the every rotating 15min of control,
Air cooling 15min again, drum's speed of rotation are 350rpm, and Ball-milling Time is 24h, and a kind of high Zr content Ti is obtained20.5Ni49.5Zr30Three
First alloy powder.
Ti obtained in the present embodiment20.5Ni49.5Zr30Manganese ternary alloy powder surface topography map is as shown in Figure 2, it can be seen that ball
Particle size after mill is at 1 μm or so；Ti20.5Ni49.5Zr30In energy spectrum analysis, the atomic fraction of Ti, Ni, Zr is respectively
20.6%th, 50.2% and 29.2%, it can be seen that the component content after ball milling is near the mark design component content.
Embodiment three：
A kind of high Zr content Ti of the present embodiment50.5-xNi49.5ZrxThe preparation method of manganese ternary alloy powder, specifically according to
Lower step is carried out：
First, according to Ti, Ni and Zr atomic ratio be 15.5: 49.5: 35, weigh 0.6g Ti powder, 21.3g Ni powder and
28.2g Ti10Zr90Alloyed powder；Purity >=99.9% of Ti powder, purity >=99.9% of Ni powder, Ti10Zr90The purity of alloyed powder
>=99.5%, and Ti powder, Ni powder and Ti10Zr90The granularity of alloyed powder is 300 mesh；
2nd, Ti powder, Ni powder and the Ti for step one being weighed10Zr90Alloyed powder is mixed and is put in ball grinder, is added
0.3g stearic acid and abrading-ball, then suction filtration vacuum 3 times, are re-filled with argon gas；Abrading-ball is stainless steel abrading-ball, a diameter of 10mm, ball milling
In tank, ball material mass ratio is 10:1；
3rd, the ball grinder for processing step 2 loads in planetary ball mill, carries out ball milling, the every rotating 15min of control,
Air cooling 15min again, drum's speed of rotation are 450rpm, and Ball-milling Time is 36h, and a kind of high Zr content Ti is obtained15.5Ni49.5Zr35Three
First alloy powder.
Ti obtained in the present embodiment15.5Ni49.5Zr35Manganese ternary alloy powder surface topography map is as shown in Figure 3, it can be seen that ball
Particle size after mill is at 0.5 μm or so；Ti20.5Ni49.5Zr30In energy spectrum analysis, the atomic fraction of Ti, Ni, Zr is respectively
16.2%th, 49.3% and 34.4%, it can be seen that between component content after ball milling and standard design component content, error is little.
Claims (4)
1. a kind of high Zr content Ti50.5-xNi49.5ZrxThe preparation method of manganese ternary alloy powder, it is characterised in that the method is specifically
Follow the steps below：
First, the atomic ratio according to Ti, Ni and Zr is (50.5-X): 49.5: X, weigh Ti powder, Ni powder and Ti10Zr90Alloyed powder, its
In 20≤X≤35；
2nd, Ti powder, Ni powder and the Ti for step one being weighed10Zr90Alloyed powder is mixed and is put in ball grinder, adds stearic acid
And abrading-ball, then suction filtration vacuum 3 times, are re-filled with argon gas；
3rd, the ball grinder for processing step 2 loads in planetary ball mill, carries out ball milling, and control is per rotating 15min then empty
Cold 15min, drum's speed of rotation are 250rpm～450rpm, and Ball-milling Time is 6～60h, and a kind of high Zr content Ti is obtained50.5- xNi49.5ZrxManganese ternary alloy powder；
Purity >=99.9% of Ti powder, purity >=99.9% of Ni powder, Ti wherein in step one10Zr90The purity of alloyed powder >=
99.5%, and Ti powder, Ni powder and Ti10Zr90The granularity of alloyed powder is 200～400 mesh；
Ti powder, Ni powder and Ti in step 210Zr90The gross mass of alloyed powder is (100～200) with stearic mass ratio: 1；Step
In rapid two, abrading-ball is stainless steel abrading-ball, a diameter of 10mm, and in control ball grinder, ball material mass ratio is (8～15):1.
2. a kind of high Zr content Ti according to claim 150.5-xNi49.5ZrxThe preparation method of manganese ternary alloy powder, its feature
It is in step 3 that drum's speed of rotation is 250rpm, Ball-milling Time is 12h.
3. a kind of high Zr content Ti according to claim 150.5-xNi49.5ZrxThe preparation method of manganese ternary alloy powder, its feature
It is in step 3 that drum's speed of rotation is 350rpm, Ball-milling Time is 24h.
4. a kind of high Zr content Ti according to claim 150.5-xNi49.5ZrxThe preparation method of manganese ternary alloy powder, its feature
It is in step 3 that drum's speed of rotation is 450rpm, Ball-milling Time is 36h.
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