CN111519147B - Tantalum target material with preferred orientation and preparation method thereof - Google Patents
Tantalum target material with preferred orientation and preparation method thereof Download PDFInfo
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- CN111519147B CN111519147B CN202010191434.XA CN202010191434A CN111519147B CN 111519147 B CN111519147 B CN 111519147B CN 202010191434 A CN202010191434 A CN 202010191434A CN 111519147 B CN111519147 B CN 111519147B
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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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
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Abstract
The invention relates to the technical field of target preparation, and provides a preferred orientation tantalum target and a preparation method thereof. The orientation of the internal texture of the tantalum ingot is controlled by torsional deformation, tangential deformation along the diameter direction is generated in the tantalum ingot by twisting, and the direction of the internal texture of the tantalum ingot is changed directionally, so that the aim of controlling the texture of a material is fulfilled; in addition, the preparation method provided by the invention does not need forging and rolling of the tantalum ingot, and can reduce the content of impurities mixed into the target material.
Description
Technical Field
The invention relates to the technical field of target preparation, in particular to a preferred orientation tantalum target and a preparation method thereof.
Background
Physical Vapor Deposition (PVD) is one of the key technologies for manufacturing high-end semiconductor chips, and is capable of depositing a metal or a metal compound in the form of a thin film on the surface of a silicon wafer or other substrate to manufacture the high-end semiconductor chip. The physical vapor deposition is completed by a sputtering machine, so that the sputtering target is a key consumable material for preparing high-end chips.
The preparation of most of the existing tantalum target materials is mainly realized by forging and rolling tantalum ingots, and the finished target materials are finally obtained by controlling the deformation rate, heat treatment and the like to realize grain refinement. For example, patents with publication numbers CN103572225A, CN104419901A and CN104451567A all prepare tantalum target material by forging and rolling. However, in the forging process, oxides and stains on the surface of the tantalum ingot are easily pressed into the tantalum ingot, so that the problems of uneven internal structure, high impurity content, unstable sputtering speed, target scrapping and the like of the target are caused; more importantly, the crystal grain orientation of the tantalum ingot is easy to change by forging, the preferred orientation of the internal structure of the tantalum ingot cannot be realized, and the ratio of (111) texture components to (100) texture components in the target material is low.
Disclosure of Invention
In view of the above, the present invention provides a tantalum target material with preferred orientation, a method for preparing the same, and a twisting device. The method provided by the invention can reduce the content of impurities mixed in the target material, improve the uniformity of the target material structure, reduce the grain size of the target material, and realize the preferred orientation of the internal structure of the tantalum target material, and the (111) and (100) textures in the obtained target material are superior.
In order to achieve the above object, the present invention provides the following technical solutions:
a preparation method of a preferred orientation tantalum target material comprises the following steps:
(1) carrying out acid washing, annealing heat treatment and cooling on the tantalum ingot in sequence to obtain a pretreated tantalum ingot; the tantalum ingot is a cylindrical tantalum ingot;
(2) carrying out torsional deformation on the pretreated tantalum ingot, wherein the torsional deformation angle is more than or equal to 180 degrees;
(3) sequentially carrying out annealing heat treatment and cooling on the tantalum ingot after the torsional deformation;
(4) repeating the steps (2) to (3) for 2-3 times to obtain a tantalum target blank;
(5) and cutting off two ends of the tantalum target blank, and cutting the rest part into sheets to obtain the tantalum target with preferred orientation.
Preferably, the ratio of the length to the diameter of the tantalum ingot is not less than 2; the total impurity content of the tantalum ingot is not higher than 5 wt%.
Preferably, the acid for pickling comprises one or more of hydrofluoric acid, sulfuric acid and nitric acid.
Preferably, the temperature of the annealing heat treatment in the step (1) is 800-1300 ℃, and the heat preservation time is 30-360 min; the cooling mode in the step (1) is furnace cooling.
Preferably, the torsional deformation is implemented by rotating two ends of the tantalum ingot in opposite directions or in a differential speed manner, or by fixing one end of the tantalum ingot and rotating the other end of the tantalum ingot.
Preferably, the torsional deformation is performed in a twisting device, the twisting device comprises a machine tool and a first clamping end and a second clamping end which are arranged on the machine tool, and the first clamping end and the second clamping end can fix two ends of the tantalum ingot and can rotate under the driving of the machine tool.
Preferably, the temperature of the annealing heat treatment in the step (3) is 800-1300 ℃, and the heat preservation time is 30-360 min; and (4) cooling in the step (3) in a furnace cooling mode.
The invention provides a preferred orientation tantalum target material prepared by the preparation method in the scheme, and the predominant textures in the tantalum target material are (111) and (100).
The invention also provides a twisting device which comprises a machine tool and a first clamping end and a second clamping end which are arranged on the machine tool, wherein the first clamping end and the second clamping end can fix two ends of a tantalum ingot and can rotate under the driving of the machine tool.
The invention provides a preparation method of a tantalum target material, which controls the orientation of internal texture of a tantalum ingot through torsional deformation, generates tangential deformation along the diameter direction in the tantalum ingot through torsion, and further changes the orientation of the internal texture direction of the tantalum ingot so as to achieve the aim of controlling the texture of a material; in addition, the preparation method provided by the invention does not need forging and rolling of the tantalum ingot, and can reduce the content of impurities mixed into the target material. The embodiment result shows that the tantalum target material prepared by the method has uniform internal structure, the (111) and (100) textures are superior, the crystal grains are fine, the proportion of the crystal grains with the sizes smaller than 80 mu m is more than 98%, and the purity of the obtained tantalum target material can reach 5N grade.
The invention also provides a twisting device which is simple in structure and easy to operate and can be used for twisting the high-purity tantalum ingot.
Drawings
FIG. 1 is a schematic diagram of the grain structure of an ingot of tantalum obtained by electron beam melting;
FIG. 2 is a schematic diagram of the construction of the twisting apparatus, wherein 1-the machine tool, 2-the first holding end, 3-the second holding end, 4-the tantalum ingot;
FIG. 3 is a schematic view of a tantalum ingot secured by a first and second clamping ends;
fig. 4 is a gold phase diagram of the tantalum target material prepared in example 1.
Detailed Description
The invention provides a preparation method of a preferred orientation tantalum target material, which comprises the following steps:
(1) carrying out acid washing, annealing heat treatment and cooling on the tantalum ingot in sequence to obtain a pretreated tantalum ingot; the tantalum ingot is a cylindrical tantalum ingot;
(2) carrying out torsional deformation on the pretreated tantalum ingot, wherein the torsional deformation angle is more than or equal to 180 degrees;
(3) sequentially carrying out annealing heat treatment and cooling on the tantalum ingot after the torsional deformation;
(4) repeating the steps (2) to (3) for 2-3 times to obtain a tantalum target blank;
(5) and cutting off two ends of the tantalum target blank, and cutting the rest part into sheets to obtain the tantalum target with preferred orientation.
According to the invention, the tantalum ingot is subjected to acid washing, annealing heat treatment and cooling in sequence to obtain the pretreated high-purity tantalum ingot. In the invention, the material of the tantalum ingot is preferably tantalum or tantalum alloy, the tantalum ingot is a high-purity tantalum ingot, and the total content of impurity elements in the tantalum ingot is preferably not higher than 5 wt%; the tantalum ingot is preferably obtained by electron beam melting, and crystal grains in the tantalum ingot after the electron beam melting are in a long strip shape along the axial direction, as shown in the attached drawing 1; the tantalum ingot is a cylindrical tantalum ingot, and the ratio of the length to the diameter of the cylindrical tantalum ingot is preferably not less than 2, and more preferably 2-3; according to the invention, by controlling the ratio of the length to the diameter of the tantalum ingot, the subsequent torsional deformation can be operated more easily, and the difficulty of torsional deformation is reduced.
In the invention, the acid for pickling preferably comprises one or more of hydrofluoric acid, sulfuric acid and nitric acid; the purity of the acid used for the acid washing is preferably chemical purity. The method removes oxide skins and stains on the surface of the tantalum ingot through acid washing; the invention has no special requirements on the specific conditions of the acid washing, and is suitable for full washing.
After the acid cleaning is finished, the tantalum ingot after the acid cleaning is subjected to annealing heat treatment. In the invention, the temperature of the annealing heat treatment is preferably 800-1300 ℃, more preferably 900-1200 ℃, and the heat preservation time is preferably 30-360 min, more preferably 60-300 min; the invention improves the plasticity of the tantalum ingot through annealing heat treatment, and is beneficial to subsequent torsional deformation. And after the annealing heat treatment is finished, cooling the annealed high-purity tantalum ingot to room temperature along with the furnace.
After the pretreated tantalum ingot is obtained, the pretreated tantalum is subjected to torsional deformation. In the invention, the torsion angle is more than or equal to 180 degrees, preferably 180-720 degrees, and more preferably 240-360 degrees; the torsional deformation is particularly preferably that two ends of the tantalum ingot are reversely rotated or differentially rotated, or one end of the tantalum ingot is fixed and the other end of the tantalum ingot is rotated; the torsional deformation angle is based on the angle difference of the two ends of the tantalum ingot, for example, if one end of the tantalum ingot rotates forwards by 180 degrees and the other end of the tantalum ingot rotates backwards by 180 degrees, the torsional angle is 360 degrees, if one end of the tantalum ingot rotates forwards by 360 degrees and the other end rotates forwards by 180 degrees, the torsional angle is 180 degrees, if one end of the tantalum ingot is fixed and the other end rotates forwards by 180 degrees, the torsional angle is 180 degrees.
In the present invention, the torsional deformation is preferably performed in a twisting device, the structural schematic diagram of the twisting device is shown in fig. 2, the twisting device preferably comprises a machine tool and a first clamping end and a second clamping end which are arranged on the machine tool, the first clamping end and the second clamping end can fix two ends of a tantalum ingot and can rotate under the driving of the machine tool; a groove is preferably arranged between the first clamping end and the second clamping end so as to facilitate the installation and torsion of the tantalum ingot; the specific structures of the first clamping end and the second clamping end are not required, and the tantalum ingot can be clamped and fixed by using a structure well known by the technical personnel in the field; the invention has no special requirements on the mounting mode of the first clamping end and the second clamping end on the machine tool, can firmly mount the first clamping end and the second clamping end, and can realize the rotation function; the schematic diagram after fixing the tantalum ingot by the first clamping end and the second clamping end is shown in fig. 3.
After the torsional deformation is finished, the tantalum ingot after the torsional deformation is subjected to annealing heat treatment and cooling in sequence. In the invention, the temperature of the annealing heat treatment is preferably 800-1300 ℃, more preferably 900-1200 ℃, and the heat preservation time is preferably 30-360 min, more preferably 60-300 min; according to the invention, the stress generated by torsion in the tantalum ingot is removed through annealing heat treatment, the deformation potential stored by torsional deformation is released, the crystal grains of the tantalum ingot are greatly reduced, the texture is reconstructed, the plasticity of the tantalum ingot can be improved, and the tantalum ingot can be conveniently twisted again. In the present invention, the cooling is preferably furnace-cooled to room temperature.
The steps of torsional deformation, annealing heat treatment and cooling are repeated for 2-3 times to obtain the tantalum target blank. In the present invention, in the process of repeating the twisting-annealing heat treatment-cooling, the conditions of the respective steps are preferably the same as those in the above-mentioned scheme, and will not be described herein again. The invention leads the tantalum ingot to generate tangential deformation along the diameter direction through repeated torsional deformation and annealing heat treatment, and further leads the texture direction to generate directional change, thereby achieving the purpose of controlling the texture of the material, improving the uniformity of the texture of the target material, reducing the grain size of the target material, realizing the preferred orientation of the tantalum target material and leading the texture components (111) and (100) in the target material to be superior.
After the tantalum target blank is obtained, the two ends of the tantalum target blank are cut off, and the rest part is cut into sheets to obtain the tantalum target with preferred orientation. In the invention, the cutting is specifically to cut off the clamping part in the twisting process of the tantalum ingot, and the rest middle part is the part subjected to torsional deformation treatment. The specific cutting method and the size of the sheet target obtained after cutting are not required in the invention, and the cutting method can be carried out according to a method well known by the skilled in the art.
The invention also provides a preferred orientation tantalum target material prepared by the method in the scheme, in the invention, the tantalum target material has the advantages that the predominant textures are (111) and (100), the internal structure of the tantalum target material is uniform in crystallization, the grain size is small, and the proportion of grains with the size lower than 80 mu m is more than 98%.
The invention also provides a twisting device, which comprises a machine tool and a first clamping end and a second clamping end which are arranged on the machine tool, wherein the first clamping end and the second clamping end can fix two ends of a tantalum ingot and can rotate under the driving of the machine tool; a groove is preferably arranged between the first clamping end and the second clamping end, so that the high-purity tantalum ingot can be conveniently installed and twisted. The twisting device provided by the invention can conveniently perform the twisting deformation on the tantalum ingot, so that the tantalum target material with excellent performance is prepared.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1
(1) Selecting a high-purity tantalum ingot smelted by an electron beam, wherein the total content of alloy elements and impurity elements of the tantalum ingot is not higher than 5%, the diameter of the tantalum ingot is 300mm, and the length of the tantalum ingot is 600 mm; acid cleaning is carried out on the tantalum ingot, and the acid cleaning solution is chemical pure hydrofluoric acid;
(2) carrying out annealing heat treatment on the tantalum ingot after acid washing, wherein the annealing temperature is 800 ℃, the heat preservation time is 30min, and cooling along with the furnace;
(3) clamping the tantalum ingot subjected to annealing heat treatment in a twisting device shown in fig. 2 for twisting, wherein the twisting mode is that two ends are reversely rotated, and the rotation angle is 180 degrees;
(4) carrying out annealing heat treatment on the twisted tantalum ingot, wherein the heat treatment temperature is 800 ℃, the heat preservation time is 30min, and cooling along with the furnace;
(5) repeating the steps (3) to (4) for 2 times to obtain a tantalum target blank with preferred orientation;
(6) and cutting off the clamping part of the chain segment of the tantalum target blank, and cutting the rest part into pieces to obtain the final tantalum target.
The gold phase diagram of the obtained tantalum target material is shown in FIG. 4, and it can be seen from FIG. 4 that the tantalum target material has uniform internal structure and fine grains, and the grain sizes are all about 10-30 μm; the texture of the target was detected by the EBSD (electron back scattering) method, and the obtained textures of the targets (111) and (100) were found to be superior.
The content of the internal impurities of the tantalum target material is detected according to YS/T935-containing 2013 electronic film high-purity metal sputtering target material purity grade and impurity content analysis and report standard guidelines, and the result shows that the content of the internal impurities of the target material is 1000ppm and reaches 5N grade purity.
Example 2
Otherwise, as in example 1, only the torsion angle in step (3) was changed to 360 °.
Example 3
Otherwise, as in example 1, only the torsion angle in step (3) was changed to 720 °.
Example 4
Otherwise, as in example 1, only the annealing temperature in step (2) was changed to 1200 ℃ and the holding time was changed to 120min, and the annealing temperature in step (4) was changed to 1100 ℃ and the holding time was changed to 360 min.
The tantalum target materials prepared in the embodiments 2 to 4 are tested, and the results show that the obtained target materials have uniform internal structures, fine crystal grains, the proportion of the crystal grains with the sizes smaller than 80 mu m is more than 98%, and the (111) and (100) textures are superior; the purity of the tantalum target materials prepared in the embodiments 2 to 4 is detected according to the method in the embodiment 1, and the result shows that the purity of the obtained target materials can reach 5N grade purity.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. The preparation method of the tantalum target material with preferred orientation is characterized by comprising the following steps:
(1) carrying out acid washing, annealing heat treatment and cooling on the tantalum ingot in sequence to obtain a pretreated tantalum ingot; the tantalum ingot is a cylindrical tantalum ingot;
(2) carrying out torsional deformation on the pretreated tantalum ingot, wherein the torsional deformation is to carry out reverse rotation or differential rotation on two ends of the tantalum ingot, or to fix one end of the tantalum ingot and rotate the other end of the tantalum ingot; the torsion angle of the torsion deformation is more than or equal to 180 degrees;
(3) sequentially carrying out annealing heat treatment and cooling on the tantalum ingot after the torsional deformation;
(4) repeating the steps (2) to (3) for 2-3 times to obtain a preferred orientation tantalum target blank;
(5) and cutting off two ends of the preferred orientation tantalum target blank, and cutting the rest part into sheets to obtain the preferred orientation tantalum target.
2. The method of claim 1, wherein the ratio of the length to the diameter of the tantalum ingot is not less than 2; the total impurity content of the tantalum ingot is not higher than 5 wt%.
3. The method of claim 1, wherein the acid wash comprises one or more of hydrofluoric acid, sulfuric acid, and nitric acid.
4. The preparation method according to claim 1, wherein the temperature of the annealing heat treatment in the step (1) is 800-1300 ℃, and the holding time is 30-360 min; the cooling mode in the step (1) is furnace cooling.
5. The method of claim 1, wherein the torsional deformation is performed in a twisting device comprising a machine tool and first and second holding ends mounted on the machine tool, the first and second holding ends being capable of holding both ends of the tantalum ingot and being driven by the machine tool to rotate.
6. The preparation method according to claim 1, wherein the temperature of the annealing heat treatment in the step (3) is 800 to 1300 ℃, and the holding time is 30 to 360 min; and (4) cooling in the step (3) in a furnace cooling mode.
7. The tantalum target material with preferred orientation prepared by the preparation method of any one of claims 1 to 6, wherein the predominant textures in the tantalum target material are (111) and (100).
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| CN1380437A (en) * | 2000-12-14 | 2002-11-20 | Gkss-研究中心盖斯特哈赫特有限公司 | Method for strengthening metal material tissue and metal blank |
| EP2226828A1 (en) * | 2007-12-28 | 2010-09-08 | Institute For Metals Superplasticity Problems Of The Russian Academy Of Sciences (IMSP RAS) | Cold cathode and a method for the production thereof |
| CN104498848A (en) * | 2015-01-21 | 2015-04-08 | 西南大学 | Processing method of magnesium alloy bar material |
| CN104862628A (en) * | 2015-05-27 | 2015-08-26 | 西南大学 | Method for increasing copper tensile strength |
| CN206133060U (en) * | 2016-10-14 | 2017-04-26 | 中国建筑材料科学研究总院 | Rotatory differential of optic fibre image inverter twists reverse forming device |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7699946B2 (en) * | 2005-09-07 | 2010-04-20 | Los Alamos National Security, Llc | Preparation of nanostructured materials having improved ductility |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1380437A (en) * | 2000-12-14 | 2002-11-20 | Gkss-研究中心盖斯特哈赫特有限公司 | Method for strengthening metal material tissue and metal blank |
| EP2226828A1 (en) * | 2007-12-28 | 2010-09-08 | Institute For Metals Superplasticity Problems Of The Russian Academy Of Sciences (IMSP RAS) | Cold cathode and a method for the production thereof |
| CN104498848A (en) * | 2015-01-21 | 2015-04-08 | 西南大学 | Processing method of magnesium alloy bar material |
| CN104862628A (en) * | 2015-05-27 | 2015-08-26 | 西南大学 | Method for increasing copper tensile strength |
| CN206133060U (en) * | 2016-10-14 | 2017-04-26 | 中国建筑材料科学研究总院 | Rotatory differential of optic fibre image inverter twists reverse forming device |
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