CN115925416A - Preparation method of tantalum oxide target material - Google Patents
Preparation method of tantalum oxide target material Download PDFInfo
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- CN115925416A CN115925416A CN202310056113.2A CN202310056113A CN115925416A CN 115925416 A CN115925416 A CN 115925416A CN 202310056113 A CN202310056113 A CN 202310056113A CN 115925416 A CN115925416 A CN 115925416A
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Abstract
The invention belongs to the technical field of sputtering targets, and particularly relates to a tantalum oxide target and a preparation method thereof. The preparation process of the method comprises the steps of S1, providing tantalum oxide powder; s2, pressing and molding the tantalum oxide powder by adopting a cold isostatic pressing method; s3, performing two-step sintering molding on the pressed blank in an oxygen atmosphere; s4, machining after sintering the target; the tantalum oxide sputtering target with high density and uniform grain size is obtained by the method, and meanwhile, the method is easier to prepare the large-size sputtering target, completely overcomes the limitation of hot pressing or hot isostatic pressing equipment on the size of the sputtering target, and is more favorable for meeting the practical application of preparing the tantalum oxide film layer by magnetron sputtering.
Description
Technical Field
The invention belongs to the technical field of preparation of sputtering targets, and particularly relates to a preparation method of a tantalum oxide target.
Background
At present, a conventional memory represented by a flash memory faces physical limits, and a Resistive Random Access Memory (RRAM) is a key direction of a next-generation nonvolatile memory due to characteristics of simple structure, easy integration, high erasing speed, and the like. A simple RRAM device is formed by sandwiching a Resistance Switching Layer (Resistance Switching Layer) between two Metal electrodes, namely a Top Electrode (Top Electrode) and a Bottom Electrode (Bottom Electrode), so as to generate Resistance transition, and is called a Metal-Insulator-Metal (MIM) structure. The tantalum oxide has good resistance switching characteristics and good compatibility with a CMOS (complementary metal oxide semiconductor) process, is suitable for preparing a resistance layer film layer of a resistance random access memory, and has a wide application prospect.
Magnetron sputtering is one of the main techniques for preparing thin film materials, ions generated by an ion source are accelerated and gathered in vacuum to form ion beam flow with high speed energy, the ion beam flow bombards the surface of a solid, kinetic energy exchange is carried out between the ions and atoms on the surface of the solid, the atoms on the surface of the solid leave the solid and are deposited on the surface of a substrate, and a thin film with the thickness of nanometer or micrometer level is formed. The bombarded solid is a raw material for preparing a magnetron sputtering deposition film, is generally called a sputtering target, and is often applied to industries of information storage, integrated circuits, displays and the like.
The preparation method of the tantalum oxide film layer mainly comprises the following steps: sputtering, vacuum evaporation, chemical vapor deposition, and the like. The tantalum oxide film layer prepared by the vacuum evaporation method mainly adopts powder as an evaporation raw material, the prepared film layer is seriously influenced by the granularity, the appearance, the bulk ratio and the like of the powder, the adhesion force, the uniformity and the like of the prepared film layer are poor, and the performance of the film layer cannot be ensured. The magnetron sputtering mostly adopts reactive magnetron sputtering to prepare the tantalum oxide film layer, namely, a high-purity molybdenum target material is used as a sputtering source electrode, the sputtering film layer is adjusted by controlling process parameters such as vacuum degree, oxygen flow and the like, the control difficulty of the whole process is high, and adverse phenomena such as abnormal discharge, target poisoning and the like are easy to occur. If the high-purity high-density tantalum oxide target material is adopted to prepare the film layer by magnetron sputtering, the problems can be effectively solved, and therefore, the preparation of the high-purity high-density tantalum oxide target material is the key for preparing the high-performance resistance change layer film layer. In the prior art, the research on preparing the high-purity and high-density tantalum oxide target material is few, or the performance indexes of the prepared target material can not reach the standard for sputtering target materials, such as low density, high impurity content, uneven grain size and components and the like. Therefore, the development and preparation of the tantalum oxide target material applicable to the resistive random access memory industry becomes an important problem to be solved urgently at present, and has far-reaching significance.
The Chinese invention patent CN 106958008A discloses a method for preparing a tantalum oxide film by a direct current magnetron sputtering method, which comprises the following steps: placing the pretreated substrate into a reaction chamber of a magnetron sputtering instrument, vacuumizing the reaction chamber, and filling Ar with the purity of 99.95 percent as working gas and O with the purity of 99.95 percent 2 And (3) as a reaction gas, regulating the sputtering working pressure, setting the sputtering power, sputtering a Ta target and obtaining the tantalum oxide film on the substrate. The preparation method takes metal tantalum as a sputtering target material, a tantalum oxide film layer is obtained by adjusting parameters such as equipment air pressure, sputtering power and the like, and the uniformity control difficulty of reaction gas O2 in a cavity is high, so that the film layer is uneven in composition and performance; in addition, reactive sputtering is adopted, the coating speed is low, target surface poisoning is caused due to a large amount of oxygen, abnormal electric arc and dust fall are generated, and the film quality and the device qualification rate are seriously influenced. The ceramic target material using the metal oxide only needs to be introduced with a small amount of oxygen, dust falling is not easy to cause, and the sputtering rate is greatly improved compared with that of the metal target reactive sputtering.
Chinese patent CN 112751005A discloses a preparation method of a tantalum oxide/tantalum carbide composite material, and a product and application thereof. The method comprises the steps of uniformly mixing acetylacetone, an organic solvent, a tantalum source and phenolic resin, and carrying out heat preservation and reflux to obtain a complex; carrying out solvothermal reaction on the complex to obtain precursor powder containing a tantalum source and a carbon source; and fully grinding the precursor powder, and then carrying out heat treatment under the protection of inert gas to obtain the tantalum oxide/tantalum carbide composite material. The method has the advantages of complex process, difficult control of the reaction process, adoption of a large amount of chemical reagents, no environmental pollution and no industrial production, and the prepared tantalum oxide/tantalum carbide composite material has low purity.
Disclosure of Invention
In order to overcome the technical problems disclosed above, the invention provides a preparation method of a tantalum oxide target material, which aims to obtain a tantalum oxide sputtering target material with high density and uniform grain size.
In order to achieve the purpose, the invention provides a preparation method of a tantalum oxide target material, which comprises the following steps:
(1) Providing tantalum oxide powder;
(2) Pressing and molding the tantalum oxide powder by adopting a cold isostatic pressing method;
(3) Carrying out two-step sintering molding on the pressed blank in an oxygen atmosphere;
(4) And machining the target after sintering.
Further, in the step (1), the granularity of the tantalum oxide powder is 1-5 μm, and the purity is more than or equal to 99.9%.
Further, in the step (2), the cold isostatic pressing is to put the tantalum oxide powder into a rubber mold, encapsulate and fix the tantalum oxide powder by a steel fixture, and put the tantalum oxide powder into a cold isostatic press for press forming.
Further, the cold isostatic pressing process comprises the following steps: increasing the pressure to 80-120Mpa at a rate of 3-6Mpa/min, maintaining the pressure for 2-5min, and increasing the pressure to 200-250Mpa at a rate of 8-12Mpa/min for 10-20min.
Further, in the step (3), the two-step sintering process in the oxygen atmosphere comprises: the first step is heating to 800-950 ℃ at the heating rate of 0.5-1 ℃/min, preserving the heat for 4-6h, and controlling the oxygen flow to be 30-60L/min; and the second step is to heat to 1350-1450 deg.c at the temperature raising rate of 0.8-1.2 deg.c/min, to heat to 1500-1550 deg.c at the temperature raising rate of 3-6 deg.c/min, to maintain for 5-15min, to cool to 1350-1450 deg.c at the temperature lowering rate of 1-3 deg.c/min, to maintain for 6-10 hr with oxygen flow rate of 50-80L/min.
Further, in the step (4), the machining process includes cutting, and the cutting is performed by using a diamond wire cutting device.
Further, the machining treatment also comprises surface grinding and polishing treatment after cutting.
Further, the tantalum oxide target material is obtained by the preparation method of the tantalum oxide target material.
The invention has the following positive beneficial effects:
1. in the preparation process, oxygen atmosphere sintering is adopted, so that decomposition, crystal form transformation and the like of tantalum oxide at high temperature can be avoided under the environment of positive oxygen pressure, and the target with stable chemical components can be obtained;
2. according to the invention, an oxygen atmosphere two-step sintering method is adopted for sintering, the heating rate and the oxygen flow are adjusted according to different sintering stages, the lower heating rate of the medium-low temperature can ensure the elimination of harmful impurities such as water vapor and the like in the pressed blank, and meanwhile, the shrinkage consistency of different positions of the blank can be ensured, the deformation and cracking risks can be reduced, the surface of the prepared target has no cracks, and the yield is high;
3. according to the invention, the target material is prepared by adopting an oxygen atmosphere two-step sintering method, the sintering temperature is increased to 50-200 ℃ above the highest heat preservation temperature, and the sintering temperature is reduced to the sintering temperature for heat preservation after short heat preservation, so that the method can excite the sintering activation energy in the blank, promote the sintering process to improve the density, simultaneously prevent the abnormal growth of target material grains, and obtain the target material grains with uniform and consistent sizes;
4. the tantalum oxide target material finally prepared by the method has uniform tissue and consistent chemical composition, the average grain size is less than 10 mu m, and the density is more than or equal to 8.0g/cm 3 And all performance indexes meet the technical standard of high-quality target materials, and the method can be widely applied.
5. According to the invention, the tantalum oxide target material is prepared by sintering in the cold isostatic pressing-oxygen atmosphere, compared with an HP method and an HIP method, the preparation of the target material with large size can be realized, and meanwhile, the preparation process is simple and the industrial production is easy.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings.
FIG. 1 is a flow chart of a method for preparing a tantalum oxide target according to the present invention.
Description of the preferred embodiment
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to fig. 1 of the embodiments of the present invention. It should be apparent that the described embodiments are only some of the embodiments of the present invention, and not all of them. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention, are within the scope of the invention.
To facilitate understanding of the invention, the following examples are set forth:
example 1
The embodiment provides a preparation method of a tantalum oxide target material, which comprises the following steps:
preparing tantalum oxide powder with the purity of 99.95% and the particle size of 1 mu m;
(2) Carrying out cold isostatic pressing on the tantalum oxide powder prepared in the step (1): firstly, tantalum oxide powder is filled into a rubber mold with a certain shape, then the rubber mold is sealed and fixed by a steel fixture, and finally the sealed and fixed mold is placed into a cold isostatic pressing device for compression molding; the cold isostatic pressing process comprises the following steps: increasing the pressure to 80MPa at a pressure increasing rate of 3MPa/min, maintaining the pressure for 5min, and then pressing at a maximum pressure of 12MPa/min of 200MPa for 20min;
(3) And (3) performing two-step sintering molding on the pressed blank prepared in the step (2), wherein the sintering process comprises the following steps: the first step is heating to 800 ℃ at the heating rate of 0.5 ℃/min, and keeping the temperature for 6h, wherein the oxygen flow is 30L/min; secondly, heating to 1350 ℃ at the heating rate of 0.8 ℃/min, heating to 1500 ℃ at the heating rate of 3 ℃/min, preserving heat for 15min, reducing to 1350 ℃ at the cooling rate of 1 ℃/min, preserving heat for 10h, and controlling the oxygen flow to be 50L/min; finally sintering to prepare a tantalum oxide target blank;
(4) And (4) cutting the tantalum oxide blank prepared in the step (3), wherein the cutting equipment is a diamond wire cutting machine, and then grinding and polishing the surface of the cut blank to obtain the finished tantalum oxide target.
Example 2
The embodiment provides a preparation method of a tantalum oxide target material, which comprises the following steps:
(1) Preparing tantalum oxide powder with the purity of 99.92% and the particle size of 5 mu m;
(2) Carrying out cold isostatic pressing on the tantalum oxide powder prepared in the step (1): firstly, tantalum oxide powder is filled into a rubber mould with a certain shape, then the rubber mould is sealed and fixed by a steel fixture, and finally the sealed and fixed mould is placed into cold isostatic pressing equipment for compression molding; the cold isostatic pressing process comprises the following steps: increasing the pressure to 120Mpa at a pressure increasing rate of 6Mpa/min, maintaining the pressure for 2min, and then maintaining the maximum pressure of 250Mpa at 8Mpa/min for 10min;
(3) And (3) performing two-step sintering molding on the pressed blank prepared in the step (2), wherein the sintering process comprises the following steps: the first step is heating to 950 ℃ at the heating rate of 1 ℃/min, preserving the heat for 4h, and the oxygen flow is 60L/min; secondly, heating to 1450 ℃ at a heating rate of 1.2 ℃/min, heating to 1550 ℃ at a heating rate of 6 ℃/min, preserving heat for 5min, reducing to 1450 ℃ at a cooling rate of 3 ℃/min, preserving heat for 6h, and controlling the oxygen flow to 80L/min; finally sintering to prepare a tantalum oxide target blank;
(4) And (4) cutting the tantalum oxide blank prepared in the step (3), wherein the cutting equipment is a diamond wire cutting machine, and then grinding and polishing the surface of the cut blank to obtain the finished tantalum oxide target.
Example 3
The embodiment provides a preparation method of a tantalum oxide target material, which comprises the following steps:
(1) Preparing tantalum oxide powder with the purity of 99.95% and the particle size of 2 mu m;
(2) Carrying out cold isostatic pressing on the tantalum oxide powder prepared in the step (1): firstly, tantalum oxide powder is filled into a rubber mold with a certain shape, then the rubber mold is sealed and fixed by a steel fixture, and finally the sealed and fixed mold is placed into a cold isostatic pressing device for compression molding; the cold isostatic pressing process comprises the following steps: increasing the pressure to 100Mpa at a pressure increasing rate of 5Mpa/min, maintaining the pressure for 4min, and then performing maximum pressing at a pressure of 8Mpa/min of 230Mpa for 12min;
(3) And (3) performing two-step sintering molding on the pressed blank prepared in the step (2), wherein the sintering process comprises the following steps: the first step is heating to 800 ℃ at the heating rate of 0.7 ℃/min, and keeping the temperature for 4h, wherein the oxygen flow is 45L/min; secondly, heating to 1400 ℃ at a heating rate of 1 ℃/min, heating to 1500 ℃ at a heating rate of 4 ℃/min, preserving heat for 8min, then reducing to 1400 ℃ at a cooling rate of 2 ℃/min, preserving heat for 7h, and ensuring the oxygen flow to be 60L/min; finally sintering to prepare a tantalum oxide target blank;
(4) And (4) cutting the tantalum oxide blank prepared in the step (3), wherein the cutting equipment is a diamond wire cutting machine, and then grinding and polishing the surface of the cut blank to obtain the finished tantalum oxide target.
Example 4
The embodiment provides a preparation method of a tantalum oxide target material, which comprises the following steps:
(1) Preparing tantalum oxide powder with the purity of 99.92% and the particle size of 4 mu m;
(2) Carrying out cold isostatic pressing on the tantalum oxide powder prepared in the step (1): firstly, tantalum oxide powder is filled into a rubber mould with a certain shape, then the rubber mould is sealed and fixed by a steel fixture, and finally the sealed and fixed mould is placed into cold isostatic pressing equipment for compression molding; the cold isostatic pressing process comprises the following steps: increasing the pressure to 120Mpa at a pressure increasing rate of 4Mpa/min, maintaining the pressure for 6min, and then performing maximum pressing at a pressure of 10Mpa/min of 220Mpa for 12min;
(3) And (3) performing two-step sintering molding on the pressed blank prepared in the step (2), wherein the sintering process comprises the following steps: the first step is heating to 850 ℃ at the heating rate of 0.6 ℃/min, and keeping the temperature for 5 hours, wherein the oxygen flow is 50L/min; secondly, heating to 1450 ℃ at the heating rate of 1.1 ℃/min, heating to 1550 ℃ at the heating rate of 5 ℃/min, preserving heat for 8min, reducing to 1450 ℃ at the cooling rate of 1.5 ℃/min, preserving heat for 8h, and controlling the oxygen flow to 70L/min; finally sintering to prepare a tantalum oxide target blank;
(4) And (4) cutting the tantalum oxide blank prepared in the step (3), wherein the cutting equipment is a diamond wire cutting machine, and then grinding and polishing the surface of the cut blank to obtain the finished tantalum oxide target.
The performance test of the tantalum oxide target material prepared by the invention is shown in the following table 1.
TABLE 1 Performance index of target materials prepared in each example
| Density of | Grain size | Phase of matter | |
| Example 1 | 7.94 | 6μm | Ta 2 O 5 |
| Example 2 | 7.88 | 7.5μm | Ta 2 O 5 |
| Example 3 | 8.02 | 4μm | Ta 2 O 5 |
| Example 4 | 8.1 | 5μm | Ta 2 O 5 |
The tantalum oxide target material prepared by the method has uniform and consistent grain size and chemical composition, the average grain size is less than 10 mu m, and the density is more than or equal to 8.0g/cm 3 And each performance index meets the technical standard of a high-quality target material.
Although specific embodiments of the invention have been described above, it will be understood by those skilled in the art that the specific embodiments described are illustrative only and are not limiting upon the scope of the invention, and that equivalent modifications and variations can be made by those skilled in the art without departing from the spirit of the invention, which is to be limited only by the appended claims.
Claims (8)
1. The preparation method of the tantalum oxide target is characterized by comprising the following steps:
(1) Providing tantalum oxide powder;
(2) Pressing and molding the tantalum oxide powder by adopting a cold isostatic pressing method;
(3) Carrying out two-step sintering molding on the pressed blank in an oxygen atmosphere;
(4) And machining the sintered target.
2. The method for preparing tantalum oxide target material according to claim 1, wherein in step (1), the tantalum oxide powder has a particle size of 1-5 μm and a purity of not less than 99.9%.
3. The method for preparing the tantalum oxide target material according to claim 1, wherein in the step (2), the cold isostatic pressing is performed by filling tantalum oxide powder into a rubber mold, packaging and fixing the tantalum oxide powder by using a steel fixture, and putting the tantalum oxide powder into a cold isostatic press for compression molding.
4. The method for preparing the tantalum oxide target material according to claim 3, wherein the cold isostatic pressing process comprises the following steps: increasing the pressure to 80-120Mpa at a rate of 3-6Mpa/min, maintaining the pressure for 2-5min, and increasing the pressure to 200-250Mpa at a rate of 8-12Mpa/min for 10-20min.
5. The method for preparing tantalum oxide target material according to claim 1, wherein in the step (3), the two-step sintering process in oxygen atmosphere comprises: the first step is heating to 800-950 ℃ at the heating rate of 0.5-1 ℃/min, preserving the heat for 4-6h, and controlling the oxygen flow to be 30-60L/min; the second step is to heat to 1350-1450 deg.c at the temperature raising rate of 0.8-1.2 deg.c/min, to heat to 1500-1550 deg.c at the temperature raising rate of 3-6 deg.c/min, to maintain the temperature for 5-15min, to cool to 1350-1450 deg.c at the temperature lowering rate of 1-3 deg.c/min, to maintain the temperature for 6-10 hr with oxygen flow rate of 50-80L/min.
6. The method for preparing a tantalum oxide target material according to claim 1, wherein in the step (4), the machining treatment comprises cutting, and the cutting is performed by using a diamond wire cutting device.
7. The method for preparing a tantalum oxide target according to claim 6, wherein the machining process further comprises surface grinding and polishing after cutting.
8. The tantalum oxide target material obtained by the method according to any one of claims 1 to 7.
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2023
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