CN111057905B - Method for preparing niobium-titanium alloy through powder metallurgy - Google Patents
Method for preparing niobium-titanium alloy through powder metallurgy Download PDFInfo
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- CN111057905B CN111057905B CN202010033339.7A CN202010033339A CN111057905B CN 111057905 B CN111057905 B CN 111057905B CN 202010033339 A CN202010033339 A CN 202010033339A CN 111057905 B CN111057905 B CN 111057905B
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- C22C1/00—Making non-ferrous alloys
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Abstract
The invention discloses a method for preparing niobium-titanium alloy by powder metallurgy, which comprises the steps of uniformly mixing niobium powder and titanium powder, pressing into a green body, carrying out atmosphere protection hot-pressing sintering, and cooling along with a furnace to obtain compact niobium-titanium alloy. Compared with the traditional smelting method, the method for preparing the niobium-titanium alloy by the simple powder metallurgy method has the advantages of simple process, high efficiency and low cost. The grain size range of the alloy prepared by the method is well controlled to be 43-54, and the compactness is about 97.83%, so that a simple and efficient method is provided for the preparation of the niobium-titanium alloy.
Description
Technical Field
The invention belongs to the technical field of alloy target preparation, and particularly relates to a method for preparing niobium-titanium alloy through powder metallurgy.
Background
With the continuous improvement of the requirements on the comprehensive performance and the use environment of electronic products, higher and higher requirements are also put forward on the performance of sputtering targets. In particular, electrode and wiring materials of flat panel displays and thin film solar cells and barrier layer materials of semiconductors have strict requirements on the grain size, density and uniformity inside the target materials used by the materials. Niobium-titanium alloy, which is one of the main raw materials of the target, is more and more preferred because it can balance various properties such as high temperature resistance and corrosion resistance of the sputtered film after sputtering. These are based on the high melting point, high conductivity, good corrosion resistance and good environmental protection properties of niobium-titanium alloys.
The prior technology for preparing niobium-titanium alloy mainly comprises smelting, and the main process steps comprise material preparation, material charging, heating and melting and the like. However, in actual production, because the melting point of the niobium-titanium alloy is high, it is difficult to heat the niobium-titanium alloy to the melting point, and the production cost is increased. Therefore, the alloy target material is difficult to prepare quickly, environmentally and at low cost by adopting the traditional method.
Disclosure of Invention
The invention aims to provide a method for preparing niobium-titanium alloy by powder metallurgy, which solves the problem that the conventional niobium-titanium alloy preparation method is difficult to prepare the alloy target material quickly, environmentally and at low cost.
The technical scheme adopted by the invention is as follows: a method for preparing niobium-titanium alloy by powder metallurgy comprises the following steps:
step 1, uniformly mixing niobium powder and titanium powder to obtain mixed powder;
step 2, pressing the mixed powder obtained in the step 1 into a green body;
and 3, putting the green body pressed in the step 2 into a hot-pressing sintering furnace filled with protective gas for sintering, and cooling after sintering to obtain the niobium-titanium compact alloy.
And (2) mixing the niobium powder and the titanium powder for 4 hours in the step 1, wherein the mass of the niobium powder accounts for 45-50%, and the balance is the titanium powder.
The condition for pressing the mixed powder into a green compact in step 2 was that the pressure was 40 t.
And (3) sintering process: firstly heating to 900 ℃ and preserving heat for 30min, then heating to 1200-1300 ℃ again and starting pressurizing, and preserving heat for 2-3 h.
And 3, the protective gas is argon.
And (3) keeping the pressure at 30Mpa for 2-3 h.
The cooling mode is furnace cooling.
The beneficial effect of the invention is that,
1. the simple method for preparing the niobium-titanium alloy is based on a powder metallurgy method, adopts atmosphere protection hot-pressing sintering, can ensure that the formed alloy has high density by applying certain pressure in the sintering process, and can ensure that the finally obtained niobium-titanium alloy has fewer impurities by the protection of argon.
2. Through long-time powder mixing, titanium atoms and niobium atoms are uniformly mixed, and the two atoms are fully contacted with each other during sintering, so that uniform diffusion is ensured, and the powder is further well combined and has high density.
The process is easy to operate, the prepared niobium-titanium alloy is uniform, the purity and the relative density of the niobium-titanium alloy meet the use requirements of the coating field of high-end electronic products, the production cost is low, the product size is wide, and the industrialized mass production is facilitated. The process is suitable for industrial mass production of high-quality niobium-titanium alloy.
Drawings
FIG. 1 is a statistical distribution diagram of the particle size of the sample prepared in example 2 of the present invention.
Detailed Description
The present invention is described in detail below with reference to examples, which are provided to illustrate the technical solutions of the present invention and to provide detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following examples.
Example 1
Step 1, mixing niobium powder and titanium powder on a mixer for 4 hours, wherein the mass ratio of the niobium powder to the titanium powder is 45:55, and pressing the mixed powder into a green body at the pressure of 40 t;
and 2, putting the green body pressed in the step 1 into an atmosphere protection hot-pressing sintering furnace, heating to 900 ℃ and preserving heat for 30min, then heating to 1200 ℃ and starting pressurization, preserving heat for 3h under the pressure of 30MPa, introducing argon for protection in the whole process, and finally cooling along with the furnace to obtain the niobium-titanium alloy.
The niobium-titanium alloy obtained in example 1 was subjected to wire cutting to prepare a metallographic sample, and it was found that the grain size was 54 and the density was 99.83%.
Example 2
Step 1, mixing niobium powder and titanium powder for 4 hours, wherein the mass ratio of the mixed niobium powder to the titanium powder is 50:50, and pressing the mixed powder into a green body at the pressure of 40 t;
and 2, putting the green body pressed in the step 1 into an atmosphere protection hot-pressing sintering furnace, firstly heating to 900 ℃, preserving heat for 30min, then heating to 1250 ℃, starting pressurization, preserving heat for 2.5h at the pressure of 30MPa, and introducing argon for protection in the whole process. And finally, cooling along with the furnace to obtain the niobium-titanium alloy.
The niobium-titanium alloy obtained in example 2 was subjected to wire cutting to prepare a metallographic sample, and it was found that the grain size was 48 and the density was 99.84%.
Example 3
Step 1, mixing niobium powder and titanium powder on a mixer for 4 hours, wherein the mass ratio of the mixed niobium powder to the titanium powder is 48:52, and pressing the mixed powder into a green body at the pressure of 40 t;
and 2, putting the pressed green body into an atmosphere protection hot-pressing sintering furnace, heating to 900 ℃ and preserving heat for 30min, then heating to 1300 ℃ and starting pressurization, preserving heat for 2h under the pressure of 30MPa, and introducing argon for protection in the whole process. And finally, cooling along with the furnace to obtain the niobium-titanium alloy.
The niobium-titanium alloy obtained in example 3 was subjected to wire cutting to prepare a metallographic sample, and it was found that the grain size was 43 and the density was 99.77%.
Example 4
Step 1, mixing niobium powder and titanium powder on a mixer for 4 hours, wherein the mass ratio of the mixed niobium powder to the titanium powder is 48:52, and pressing the mixed powder into a green body at the pressure of 40 t;
and 2, putting the pressed green body into an atmosphere protection hot-pressing sintering furnace, heating to 900 ℃, preserving heat for 30min, then heating to 1300 ℃, starting pressurization, preserving heat for 2h under the pressure of 30MPa, introducing argon for protection in the whole process, and finally cooling along with the furnace to obtain the niobium-titanium alloy.
The niobium-titanium alloy obtained in example 4 was subjected to wire cutting to prepare a metallographic sample, and it was found that the grain size was 45 and the density was 99.35%.
As can be seen from figure 1, the niobium-titanium alloy prepared by the method has uniform particle size distribution and basically follows normal distribution, and completely meets the alloy preparation requirement.
The simple method for preparing the niobium-titanium alloy is based on a powder metallurgy method, adopts atmosphere protection hot-pressing sintering, can ensure that the formed alloy has high density by applying certain pressure in the sintering process, and can ensure that the finally obtained niobium-titanium alloy has fewer impurities by the protection of argon.
According to the invention, through long-time powder mixing, titanium atoms and niobium atoms are uniformly mixed, and the two atoms are fully contacted with each other during sintering, so that uniform diffusion is ensured, and the powder is better combined and has high density. The process is easy to operate, the prepared niobium-titanium alloy is uniform, the purity and the relative density of the niobium-titanium alloy meet the use requirements of the coating field of high-end electronic products, the production cost is low, the product size is wide, and the industrialized mass production is facilitated. The process is suitable for industrial mass production of high-quality niobium-titanium alloy. Meanwhile, the preparation method is simple, and other chemical reagents are not used in the preparation process, so that the green and environment-friendly requirements of modern industrial manufacturing are met.
Claims (3)
1. A method for preparing niobium-titanium alloy by powder metallurgy, which is characterized in that,
step 1, uniformly mixing niobium powder and titanium powder to obtain mixed powder;
the niobium powder and the titanium powder are mixed for 4 hours, wherein the mass of the niobium powder accounts for 45-50%, and the balance is the titanium powder;
step 2, pressing the mixed powder obtained in the step 1 into a green body;
the condition that the mixed powder was pressed into a green compact was that a pressure of 40t was used for pressing;
step 3, putting the green body pressed in the step 2 into a hot-pressing sintering furnace filled with protective gas for sintering, and cooling to obtain niobium-titanium compact alloy after sintering;
the sintering process comprises the steps of firstly heating to 900 ℃ and preserving heat for 30min, then heating to 1200-1300 ℃ again and starting pressurization, and preserving heat for 2-3 h; and (3) keeping the pressure at 30Mpa for 2-3 h.
2. The method for powder metallurgy preparation of niobium titanium alloy as claimed in claim 1, wherein the protective gas in step 3 is argon.
3. The method for powder metallurgy preparation of niobium-titanium alloy according to claim 1, wherein the cooling manner is furnace cooling.
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| CN112063867A (en) * | 2020-08-07 | 2020-12-11 | 西安理工大学 | Preparation method of gamma-phase Zn-Ni alloy |
| CN112126809A (en) * | 2020-08-24 | 2020-12-25 | 西部超导材料科技股份有限公司 | Method for preparing NbTi alloy bar by powder metallurgy method |
| CN113462917A (en) * | 2021-07-12 | 2021-10-01 | 赣州启源新材料有限公司 | Preparation method of high-temperature-resistant titanium-aluminum alloy for aircraft engine |
| CN113584366B (en) * | 2021-07-16 | 2022-07-12 | 洛阳高新四丰电子材料有限公司 | Niobium alloy sputtering target material and preparation method thereof |
| CN114507790B (en) * | 2021-12-28 | 2022-08-16 | 西安理工大学 | Preparation method of high-density zinc-nickel alloy |
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