CN112760511B - Preparation method of titanium-nickel-palladium alloy - Google Patents
Preparation method of titanium-nickel-palladium alloy Download PDFInfo
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- CN112760511B CN112760511B CN202011574318.2A CN202011574318A CN112760511B CN 112760511 B CN112760511 B CN 112760511B CN 202011574318 A CN202011574318 A CN 202011574318A CN 112760511 B CN112760511 B CN 112760511B
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- nickel
- titanium
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- palladium alloy
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
Abstract
The invention provides a preparation method of a titanium-nickel-palladium alloy, which comprises the following steps: mixing titanium powder, nickel powder and palladium powder uniformly and then carrying out hot pressing; the hot pressing comprises the following conditions that the vacuum degree of the hot pressing is-0.1-1 Pa, the pressure of the hot pressing is 30-50 Mpa, and the temperature of the hot pressing is 700-950 ℃; the particle size of the titanium powder is 40-150 mu m, the particle size of the nickel powder is 40-150 mu m, and the particle size of the palladium powder is as follows: 40-150 μm. According to the preparation method of the titanium-nickel-palladium alloy, the titanium powder, the nickel powder and the palladium powder are uniformly mixed and then are subjected to hot pressing, so that the problems of high internal defect and low yield of the titanium-nickel-palladium alloy prepared from the titanium-nickel-palladium alloy ingot are solved, the internal defect of the titanium-nickel-palladium alloy is remarkably reduced, and the yield is improved.
Description
Technical Field
The invention relates to the field of sputtering targets, in particular to a preparation method of a titanium-nickel-palladium alloy.
Background
The titanium nickel palladium alloy is shape memory, attracts people's attention due to the shape memory characteristic, and is rapidly applied to the aspects of spaceflight, mechanical engineering, bioengineering, photographic equipment, medical health and the like. In the prior art, the titanium-nickel-palladium alloy cast ingot is prepared by a vacuum melting method, so that a large amount of internal defects are easily generated, and the yield is low.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a titanium-nickel-palladium alloy.
In order to realize the purpose, the invention adopts the technical scheme that: a method of making a titanium-nickel-palladium alloy, the method comprising the steps of:
mixing titanium powder, nickel powder and palladium powder uniformly and then carrying out hot pressing;
the hot pressing comprises the following conditions that the vacuum degree of the hot pressing is-0.1-1 Pa, the pressure of the hot pressing is 30-50 Mpa, and the temperature of the hot pressing is 700-950 ℃;
the particle size of the titanium powder is 40-150 mu m, the particle size of the nickel powder is 40-150 mu m, and the particle size of the palladium powder is 40-150 mu m.
The preparation method of the titanium-nickel-palladium alloy adopts a method of uniformly mixing titanium powder, nickel powder and palladium powder and then carrying out hot pressing, and the particle sizes of the titanium powder, the nickel powder and the palladium powder before hot pressing are controlled to be 40-150 mu m, so that the problems of high internal defects and low yield of the titanium-nickel-palladium alloy prepared by titanium-nickel-palladium alloy ingot casting are solved, but the inventor finds that the problems of high internal defects and low yield of the titanium-nickel-palladium alloy are not completely solved only by uniformly mixing the titanium powder, the nickel powder and the palladium powder and then carrying out hot pressing, and further researches by the inventor find that the internal defects of the titanium-nickel-palladium alloy are remarkably reduced and the yield is improved when the pressure of the hot pressing is 30-50 MPa and the temperature of the hot pressing is 700-950 ℃.
Preferably, the heat preservation time of the hot pressing is 90-120 minutes.
Preferably, in the titanium-nickel-palladium alloy, the nickel content is 20 wt% to 40 wt% and the palladium content is 20 wt% to 40 wt%.
Preferably, the temperature of the hot pressing is 750-900 ℃.
The inventor finds that the internal defects of the titanium-nickel-palladium alloy can be better reduced when the hot pressing temperature is 750-900 ℃.
Preferably, the temperature of the hot pressing is 800-850 ℃.
Preferably, the pressure of the hot pressing is 35-45 MPa.
The inventor finds that the internal defects of the titanium-nickel-palladium alloy can be better reduced when the hot pressing pressure is 35-45 Mpa.
Preferably, the pressure of the hot pressing is 40 Mpa.
Preferably, the titanium, the nickel and the palladium are ball-milled in a ball mill until the particle size is 40-150 μm and are mixed uniformly.
Preferably, the hot pressing is processed in a vacuum autoclave.
The invention has the beneficial effects that: the invention provides a preparation method of a titanium-nickel-palladium alloy, which adopts a method of uniformly mixing titanium powder, nickel powder and palladium powder and then carrying out hot pressing, overcomes the problems of high internal defect and low yield of the titanium-nickel-palladium alloy prepared by titanium-nickel-palladium alloy ingot casting, remarkably reduces the internal defect of the titanium-nickel-palladium alloy and improves the yield.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
The preparation method of the titanium-nickel-palladium alloy provided by the embodiment of the invention comprises the following steps:
uniformly mixing titanium powder, nickel powder and palladium powder in a ball mill according to a weight ratio to obtain mixed powder, wherein the titanium content is 54.8 wt%, the nickel content is 25.2 wt% and the palladium content is 20 wt%;
putting the uniformly mixed powder into a 300 x 300mm square graphite die, and carrying out hot pressing in a hot pressing furnace; preparing a titanium-nickel-palladium alloy with the thickness of 300mm by 10 mm;
the hot pressing comprises the following conditions that the vacuum degree of the hot pressing is-0.1-1 Pa, the pressure of the hot pressing is 40Mpa, the temperature of the hot pressing is 700 ℃, and the time of the hot pressing and the heat preservation is 100 min;
carrying out ball milling on titanium powder, nickel powder and palladium powder in a weight ratio on a ball mill at a rotating speed of 70r/min for 6 hours, taking the mixed powder after ball milling, and detecting the particle size distribution, wherein the particle size of the titanium powder is 40-150 mu m, the particle size of the nickel powder is 40-150 mu m, and the particle size of the palladium powder is 40-150 mu m.
And (3) preparing the titanium-nickel-palladium alloy target, taking a quantitative sample, dissolving the quantitative sample by nitric acid microwave, and carrying out ICP detection, wherein the titanium-nickel-palladium alloy target comprises the following elements: 54.78 wt%, Ni 24.93 wt%, Pd 20.02 wt%.
Comparative example 1
The only difference between the preparation method of the titanium-nickel-palladium alloy as a comparative example of the invention and the embodiment 1 is as follows: the temperature of hot pressing was 1000 c, and the mixed powder for hot pressing was prepared in the same batch as in example 1.
Comparative example 2
The only difference between the preparation method of the titanium-nickel-palladium alloy as a comparative example of the invention and the embodiment 1 is as follows: the temperature of hot pressing was 650 ℃, and the mixed powder for hot pressing was prepared in the same batch as in example 1.
Comparative example 3
The only difference between the preparation method of the titanium-nickel-palladium alloy as a comparative example of the invention and the embodiment 1 is as follows: the pressure of hot pressing was 55Mpa, and the mixed powder for hot pressing was prepared in the same batch as in example 1.
Comparative example 4
The only difference between the preparation method of the titanium-nickel-palladium alloy as a comparative example of the invention and the embodiment 1 is as follows: the pressure of hot pressing was 25Mpa, and the mixed powder for hot pressing was prepared in the same batch as in example 1.
Comparative example 5
The preparation method of the titanium-nickel-palladium alloy used as the comparative example of the invention uses a vacuum melting preparation method to prepare a TiNiPd alloy ingot, and the mass ratio of Ti: 54.8 wt%, Ni: 25.2 wt%, Pd: preparing raw materials according to the proportion of 20 wt%, wherein the raw materials comprise an electrolytic nickel block with the purity of 99.8%, a titanium block with the purity of 99.98% and palladium powder with the purity of 99.99%, pumping the vacuum degree of a vacuum smelting furnace to 0.26Pa, then filling argon to 0.08MPa, raising the temperature to 1350 ℃, melting, and casting into a TiNiPd alloy cast ingot.
Effect example 1
The titanium nickel palladium alloys of example 1 and comparative examples 1-5 were tested.
The titanium powder, the nickel powder and the palladium powder of example 1, comparative example 1 and comparative example 4 are powder prepared by the same batch of ball milling.
And testing the internal defects of the titanium-nickel-palladium alloy by using a C-scan flaw detection method. The specifications of the test samples were: 300mm 10mm, detect defects on a 100 x 100mm face 2mm from the surface, test defects on a 2mm face of a cuboid 6 faces of each sample, average, and round the average. The results of the experiment are shown in table 1.
TABLE 1 titanium Nickel Palladium alloy internal Defect Performance
As can be seen from table 1, the preparation method of the titanium-nickel-palladium alloy according to the embodiment significantly reduces the internal defects of the titanium-nickel-palladium alloy, and improves the yield.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (5)
1. A preparation method of a titanium-nickel-palladium alloy is characterized by comprising the following steps:
ball-milling titanium, nickel and palladium in a ball mill until the particle size is 40-150 mu m, uniformly mixing and then carrying out hot pressing;
the hot pressing comprises the following conditions that the vacuum degree of the hot pressing is-0.1-1 Pa, the pressure of the hot pressing is 30-50 MPa, the temperature of the hot pressing is 700-950 ℃, and the heat preservation time of the hot pressing is 90-120 minutes;
in the titanium-nickel-palladium alloy, the nickel content is 20 wt% -40 wt% and the palladium content is 20 wt% -40 wt%.
2. The method for preparing the titanium-nickel-palladium alloy as claimed in claim 1, wherein the hot pressing temperature is 750 ℃ to 900 ℃.
3. The method for preparing the titanium-nickel-palladium alloy as claimed in claim 1, wherein the pressure of the hot pressing is 35 to 45 MPa.
4. The method for preparing the titanium-nickel-palladium alloy as claimed in claim 3, wherein the pressure of the hot pressing is 40 MPa.
5. The method of claim 1, wherein the hot pressing is performed in a vacuum autoclave.
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| CN202011574318.2A CN112760511B (en) | 2020-12-24 | 2020-12-24 | Preparation method of titanium-nickel-palladium alloy |
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| CN112760511B true CN112760511B (en) | 2022-07-12 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63121629A (en) * | 1986-11-10 | 1988-05-25 | Daido Steel Co Ltd | Manufacture of shape memory alloy |
| JPS63307229A (en) * | 1987-06-05 | 1988-12-14 | Natl Res Inst For Metals | Manufacture of shape memory alloy |
| CN102925780A (en) * | 2012-11-21 | 2013-02-13 | 常熟市良益金属材料有限公司 | Titanium-nickel-aluminum alloy material and preparation technique thereof |
| CN103906850A (en) * | 2011-10-21 | 2014-07-02 | 利默里克大学 | Method of forming a sintered nickel-titanium-rare earth (ni-ti-re) alloy |
| CN109822095A (en) * | 2019-04-04 | 2019-05-31 | 哈尔滨工程大学 | Shape memory alloy particles enhance Cu-base composites and preparation method |
| CN111893348A (en) * | 2020-07-03 | 2020-11-06 | 广东省材料与加工研究所 | Preparation method of nickel-titanium alloy material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9212409B2 (en) * | 2012-01-18 | 2015-12-15 | Cook Medical Technologies Llc | Mixture of powders for preparing a sintered nickel-titanium-rare earth metal (Ni-Ti-RE) alloy |
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- 2020-12-24 CN CN202011574318.2A patent/CN112760511B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63121629A (en) * | 1986-11-10 | 1988-05-25 | Daido Steel Co Ltd | Manufacture of shape memory alloy |
| JPS63307229A (en) * | 1987-06-05 | 1988-12-14 | Natl Res Inst For Metals | Manufacture of shape memory alloy |
| CN103906850A (en) * | 2011-10-21 | 2014-07-02 | 利默里克大学 | Method of forming a sintered nickel-titanium-rare earth (ni-ti-re) alloy |
| CN102925780A (en) * | 2012-11-21 | 2013-02-13 | 常熟市良益金属材料有限公司 | Titanium-nickel-aluminum alloy material and preparation technique thereof |
| CN109822095A (en) * | 2019-04-04 | 2019-05-31 | 哈尔滨工程大学 | Shape memory alloy particles enhance Cu-base composites and preparation method |
| CN111893348A (en) * | 2020-07-03 | 2020-11-06 | 广东省材料与加工研究所 | Preparation method of nickel-titanium alloy material |
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