CN111118325B - Preparation method of fine-grain niobium-titanium alloy - Google Patents
Preparation method of fine-grain niobium-titanium alloy Download PDFInfo
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- CN111118325B CN111118325B CN202010033317.0A CN202010033317A CN111118325B CN 111118325 B CN111118325 B CN 111118325B CN 202010033317 A CN202010033317 A CN 202010033317A CN 111118325 B CN111118325 B CN 111118325B
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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
- C22C1/05—Mixtures of metal powder with non-metallic powder
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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
- B22F3/001—Starting from powder comprising reducible metal compounds
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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
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—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
- 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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- 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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- 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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
Abstract
The invention discloses a preparation method of a fine-grain niobium-titanium alloy, which is implemented by ball-milling Nb powder and TiH2And uniformly mixing the powder, then pressing and molding, and carrying out hot-pressing sintering under the protection of argon to obtain the Nb-Ti alloy. In the invention, after the Nb powder is subjected to high-energy ball milling, the particle size of the Nb powder can be further reduced, and internal defects and atom activity are increased, so that diffusion bonding of two atoms is promoted. While using TiH2Instead of Ti powder, H is decomposed during sintering2Can further reduce the generation of impurities in the alloy. The alloy prepared by the invention has the grain size of 16-19 mu m, more uniform structure and high density of 99.99%, and the density is further improved while the grain size is greatly reduced. Provides a new method for preparing the fine-grained Nb-Ti alloy.
Description
Technical Field
The invention belongs to the technical field of refractory alloy target preparation methods, and particularly relates to a preparation method of a fine-grain niobium-titanium alloy.
Background
In recent years, with the increasing development of sputtering targets and sputtering technology, the importance of sputtering targets is becoming more and more evident in sputtering technology, and the quality of the targets directly affects the quality of the coating film. With the development of the characteristic dimension of the metal interconnection line towards the nanometer grade direction, the width of the metal interconnection line is continuously reduced, the number of layers of the metal interconnection line is continuously increased, the traditional single metal target material process cannot meet the current requirement, and therefore the requirement for the alloy target material is increasingly greater. The Nb-Ti alloy has good physical properties such as heat conductivity, electric conductivity, high melting point, corrosion resistance and the like, and is widely applied to target material alloys. The performance of the alloy target is mainly determined by the density, grain size, microstructure and the like of the alloy. Therefore, the density and the uniformity of the components of the Nb-Ti alloy are improved, the grain size of the Nb-Ti alloy is reduced, and the quality of the plated film can be greatly improved.
Disclosure of Invention
The invention aims to provide a preparation method of a fine-grain niobium-titanium alloy, and the prepared Nb-Ti alloy has good combination, fine crystal grains, high density, uniform structure and few Ti-rich phases.
The technical scheme adopted by the invention is that the preparation method of the fine-grain niobium-titanium alloy comprises the following specific operation steps:
step 1, ball milling Nb powder;
step 2, mixing the ball-milled Nb powder with TiH2Uniformly mixing the powder to obtain mixed powder;
step 3, pressing the mixed powder obtained in the step 2 into a green body;
and 4, sintering the green compact pressed in the step 3 to obtain the compact Nb-Ti alloy.
The present invention is also characterized in that,
further, the ball milling in step 1 is specifically as follows: putting Nb powder into a ball milling tank, adding alcohol as a dispersing agent, adding stainless steel balls according to the ball-to-material ratio of 10-30: 1, vacuumizing the ball milling tank, filling argon, and putting the sealed ball milling tank into a ball mill to perform ball milling for 10-20 hours at the rotating speed of 400 r/min.
Further, step 2 is specifically as follows:
using TiH2Mixing the Nb powder and TiH2 powder subjected to ball milling in the step 1 on a V-shaped mixer for 4 hours, wherein the mass of the Nb powder accounts for 45-50%, and the balance is TiH2And (3) pulverizing.
Further, the condition for pressing the mixed powder of step 3 into a green compact is to press at a pressure of 1.5 GPa.
Further, step 4 is specifically as follows:
and (3) putting the green body pressed in the step (3) into a sintering furnace, firstly heating to 500 ℃ for heat preservation for 30min, secondly heating to 920 ℃ for heat preservation for 5min, thirdly heating to 970 ℃ for heat preservation for 30min, fourthly heating to 970 ℃ for heat preservation for 30min, finally heating to 1200-1300 ℃ for heat preservation for 2-3 h, and introducing argon for protection in the whole process.
Further, after the temperature is raised to 1200-1300 ℃ for the fifth time, argon is continuously introduced, and the pressure is maintained for 2-3 hours at the pressure of 30 MPa.
Further, the cooling mode of the step 4 is furnace cooling.
The specific process of the Nb powder high-energy ball milling is as follows: putting Nb powder into a ball milling tank, adding about 10% alcohol as a dispersing agent, adding stainless steel balls according to the ball-to-material ratio of 10-30: 1, vacuumizing the ball milling tank, then filling argon, and putting the sealed ball milling tank into a ball mill to perform ball milling for 10-20 hours at the rotating speed of 400 r/min.
The mixed powder is prepared by mixing ball-milled Nb powder and TiH2Mixing the powder for 4 hours to ensure that the powder is uniformly mixed, wherein the mass of the Nb powder accounts for 45-50%, and the balance is TiH2And (3) pulverizing.
The pressing is to mix Nb powder and TiH2The mixed powder of (2) was pressed into a green compact at a pressure of 1.5 GPa.
And sintering, namely putting the green body into an atmosphere protection hot-pressing sintering furnace, heating to 500 ℃, preserving heat for 30min, heating to 920 ℃, preserving heat for 5min, heating to 970 ℃, preserving heat for 30min, heating to 1200-1300 ℃, starting pressurizing, and preserving heat for 2-3 h at the pressure of 30 MPa. And finally, cooling along with the furnace. Obtaining the Nb-Ti alloy, and introducing argon for protection in the whole process.
The beneficial effect of the invention is that,
1. using TiH2Powder instead of Ti powder, TiH2In the course of sintering, TiH2The Nb-Ti alloy is heated to decompose and release hydrogen, so that a small amount of hydrogen exists in the blank, and the small amount of hydrogen has a reducing effect to ensure that the Nb-Ti alloy has lower oxygen content and higher purity.
2. The Nb powder is subjected to ball milling to be refined, the smaller the powder granularity is, the larger the surface area is, the more surface active atoms are, the easier the surface diffusion is, the Ti-rich phase is reduced, and the uniformity of the phase is ensured. In addition, the ball milling can also increase defects in the Nb powder, and increase diffusion channels of Ti into Nb, so that the Nb-Ti alloy obtained after sintering is more compact.
The niobium-titanium alloy obtained by the invention has fine crystal grains and high density, thereby providing guarantee for obtaining a film with excellent sputtering effect.
Drawings
FIG. 1 is an XRD phase diagram of an Nb-Ti alloy prepared in example 2 of the present invention;
FIG. 2 is a graph showing the distribution of the grain size of the Nb-Ti alloy prepared by the present invention.
Detailed Description
The following detailed description of specific embodiments of the invention:
the invention adopts the technical scheme that Nb powder is ball-milled and then mixed with TiH2And uniformly mixing the powder, pressing into a green body, and carrying out hot-pressing sintering under the atmosphere protection to obtain the Nb-Ti alloy.
The method comprises the following specific steps:
step 1: putting Nb powder into a ball milling tank, adding 10% alcohol as a dispersing agent, adding stainless steel balls according to the ball-to-material ratio of 10-30: 1, vacuumizing the ball milling tank, then filling argon, and putting the sealed ball milling tank into a ball mill to perform ball milling for 10-20 hours at the rotating speed of 400 r/min;
step 2: mixing the ball-milled Nb powder and TiH2Mixing the powder for 4 hours to ensure that the powder is uniformly mixed, wherein the mass of the Nb powder accounts for 45-50%, and the balance is TiH2Pulverizing; then pressing the mixed powder into a green body at the pressure of 1.5 GPa;
and step 3: and (3) putting the green body pressed in the step (2) into an atmosphere protection hot-pressing sintering furnace, heating to 500 ℃, preserving heat for 30min, heating to 920 ℃, preserving heat for 5min, heating to 970 ℃, preserving heat for 30min, heating to 1200-1300 ℃, starting pressurizing, preserving heat for 2-3 h under the pressure of 30MPa, and introducing argon for protection in the whole process. And finally, cooling along with the furnace to obtain the product.
Example 1
Step 1, putting Nb powder into a ball milling tank, adding 10% alcohol as a dispersing agent, adding stainless steel balls according to a ball-to-material ratio of 10:1, vacuumizing the ball milling tank, introducing argon for protection, putting the sealed ball milling tank into a ball mill, and performing ball milling for 10 hours at a rotating speed of 400r/min to obtain ball-milled Nb powder;
step 2, performing ball milling on the Nb powder and TiH obtained in the step 12Mixing the powder for 4 hours according to the mass ratio of 50:50 to ensure that the powder is uniformly mixed, and pressing the mixed powder into a green body at the pressure of 1.5 GPa;
and 3, putting the green body pressed in the step 2 into an atmosphere protection hot-pressing sintering furnace, heating to 500 ℃ at a heating rate of 20 ℃/min, preserving heat for 30min, heating to 920 ℃ and preserving heat for 5min, heating to 970 ℃ and preserving heat for 30min, heating to 1300 ℃ and starting pressurizing, preserving heat for 2h at the pressure of 30MPa, and introducing argon for protection in the whole process. And finally, cooling along with the furnace to obtain the compact Nb-Ti alloy.
The Nb-Ti alloy obtained in example 1 was wire-cut to prepare a metallographic specimen, and it was found that the grain size was 16 μm and the density was 99.97%.
Example 2
Step 1, putting Nb powder into a ball milling tank, adding 10% alcohol as a dispersing agent, adding stainless steel balls according to a ball-to-material ratio of 30:1, vacuumizing the ball milling tank, introducing argon, putting the sealed ball milling tank into a ball mill, and ball milling for 15 hours at a rotating speed of 400r/min to obtain ball-milled Nb powder;
step 2, performing ball milling on the Nb powder and TiH obtained in the step 12Mixing the powder for 4 hours according to the mass ratio of 45:55, ensuring that the powder is uniformly mixed, and pressing the mixed powder into a green body at the pressure of 1.5 GPa;
and 3, putting the green body pressed in the step 2 into an atmosphere protection hot-pressing sintering furnace, heating to 500 ℃ at a heating rate of 20 ℃/min, preserving heat for 30min, heating to 920 ℃ and preserving heat for 5min, heating to 970 ℃ and preserving heat for 30min, heating to 1250 ℃ and 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 compact Nb-Ti alloy.
The Nb-Ti alloy obtained in example 2 was wire-cut to prepare a metallographic specimen, and it was found that the grain size was 19 μm and the density was 99.99%.
Example 3
Step 1, putting Nb powder into a ball milling tank, adding 10% alcohol as a dispersing agent, adding stainless steel balls according to a ball-to-material ratio of 20:1, vacuumizing the ball milling tank, then filling argon, putting the sealed ball milling tank into a ball mill, and ball-milling for 20 hours at a rotating speed of 400r/min to obtain ball-milled Nb powder;
step 2, performing ball milling on the Nb powder and TiH obtained in the step 12Mixing the powder for 4 hours according to the mass ratio of 48:52, ensuring the uniform mixing, and pressing the mixed powder into a green body at the pressure of 1.5 GPa;
and 3, putting the green body pressed in the step 2 into an atmosphere protection hot-pressing sintering furnace, heating to 500 ℃ at a heating rate of 20 ℃/min, preserving heat for 30min, heating to 920 ℃ and preserving heat for 5min, heating to 970 ℃ and preserving heat for 30min, heating to 1200 ℃ and starting pressurizing, preserving heat for 3h at the pressure of 30MPa, and introducing argon for protection in the whole process. And finally, cooling along with the furnace to obtain the compact Nb-Ti alloy.
The Nb-Ti alloy obtained in example 3 was wire-cut to prepare a metallographic specimen, and it was found that the grain size was 17 μm and the density was 99.96%.
From the XRD phase diagram 1 of the Nb-Ti alloy prepared in example 2, it can be seen that the prepared sample is a single β (Nb, Ti) phase.
FIG. 2 is a distribution diagram of the Nb-Ti alloy grain size, which is seen to fit a normal distribution, illustrating that the grain size is uniform.
The right graph is the distribution graph of the particle size, and it can be seen from the graph that the particle size is in accordance with the normal distribution, which shows that the particle size is uniform.
The invention relates to a preparation method of microcrystalline Nb-Ti alloy, which is implemented by mixing raw material powder Nb powder and TiH2The powders are mixed uniformly. The mixed powder adopts ball-milled Nb powder, so that defects are increased, crystal grains are refined, and Ti diffusion to the interior is promoted. Compared with the direct sintering method, the method not only reduces the generation of impurities in the sintering process, but also further improves the compactness of the alloy, reduces the grain size and has more uniform structure.
Claims (3)
1. The preparation method of the fine-grain niobium-titanium alloy is characterized by comprising the following specific operation steps of:
step 1, ball milling Nb powder;
the ball milling is as follows: putting Nb powder into a ball milling tank, adding alcohol as a dispersing agent, adding stainless steel balls according to the ball-to-material ratio of 10-30: 1, vacuumizing the ball milling tank, filling argon, putting the sealed ball milling tank into a ball mill, and ball milling for 10-20 h at the rotating speed of 400r/min
Step 2, mixing the ball-milled Nb powder with TiH2Uniformly mixing the powder to obtain mixed powder;
using TiH2Mixing the Nb powder and TiH2 powder subjected to ball milling in the step 1 on a V-shaped mixer for 4 hours, wherein the mass of the Nb powder accounts for 45-50%, and the balance is TiH2Powder
Step 3, pressing the mixed powder obtained in the step 2 into a green body;
step 4, sintering the green compact pressed in the step 3 to obtain a compact Nb-Ti alloy;
putting the green body pressed in the step 3 into a sintering furnace, firstly heating to 500 ℃ for heat preservation for 30min for the first time, then heating to 920 ℃ for heat preservation for 5min for the second time, then heating to 970 ℃ for heat preservation for 30min for the third time, continuously heating to 970 ℃ for heat preservation for 30min for the fourth time, finally heating to 1200-1300 ℃ for heat preservation for 2-3 h for the fifth time, and introducing argon for protection in the whole process; and after the temperature is raised to 1200-1300 ℃ for the fifth time, continuously introducing argon, and maintaining the pressure for 2-3 hours at the pressure of 30 MPa.
2. The method of claim 1 wherein said pressing step 3 is carried out under a pressure of 1.5 GPa.
3. The method of claim 1 wherein said cooling of step 4 is furnace cooling.
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| CN112475303B (en) * | 2020-11-23 | 2022-03-08 | 江南大学 | Based on TiH2Powder metallurgy preparation method of Ti-Nb-Sn bone repair alloy |
| CN112809002B (en) * | 2020-12-29 | 2023-01-13 | 宁波江丰电子材料股份有限公司 | Preparation method of aluminum-silicon alloy target blank |
| CN112831703B (en) * | 2020-12-30 | 2022-04-29 | 南方科技大学 | Niobium-copper alloy material and preparation method thereof |
| 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 |
| CN114480900A (en) * | 2021-12-22 | 2022-05-13 | 西安理工大学 | Method for preparing near-beta type Ti-Nb alloy by powder metallurgy |
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| WO2016202892A1 (en) * | 2015-06-15 | 2016-12-22 | Katholieke Universiteit Leuven | Max phase ceramics and methods for producing the same |
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Non-Patent Citations (1)
| Title |
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| "Development of Ti–Nb and Ti–Nb–Fe beta alloys from TiH2 powders";C.Chirico et al;《POWDER METALLURGY》;20190107;第62卷;第1-10页 * |
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