CN114892133A - Ru-Sb-Te alloy sputtering target material used as long-storage phase change storage medium and preparation method thereof - Google Patents
Ru-Sb-Te alloy sputtering target material used as long-storage phase change storage medium and preparation method thereof Download PDFInfo
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- 239000013077 target material Substances 0.000 title claims abstract description 93
- 229910001215 Te alloy Inorganic materials 0.000 title claims abstract description 37
- 238000003860 storage Methods 0.000 title claims abstract description 37
- 230000008859 change Effects 0.000 title claims abstract description 35
- 238000005477 sputtering target Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 60
- 239000002994 raw material Substances 0.000 claims abstract description 53
- 238000005245 sintering Methods 0.000 claims abstract description 53
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 39
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 38
- 239000000956 alloy Substances 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 36
- 239000000126 substance Substances 0.000 claims abstract description 28
- 229910052707 ruthenium Inorganic materials 0.000 claims abstract description 21
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000012545 processing Methods 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 11
- 238000005266 casting Methods 0.000 claims abstract description 10
- 230000004927 fusion Effects 0.000 claims abstract description 8
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 7
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 7
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- 239000002184 metal Substances 0.000 claims abstract description 6
- 150000002739 metals Chemical class 0.000 claims abstract description 4
- 238000000498 ball milling Methods 0.000 claims description 40
- 238000000227 grinding Methods 0.000 claims description 35
- 239000000463 material Substances 0.000 claims description 32
- 230000015654 memory Effects 0.000 claims description 15
- 238000007731 hot pressing Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- 238000012216 screening Methods 0.000 claims description 13
- 238000001513 hot isostatic pressing Methods 0.000 claims description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- 239000010431 corundum Substances 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 7
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- 238000009792 diffusion process Methods 0.000 claims description 3
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- 229910002804 graphite Inorganic materials 0.000 description 11
- 239000010439 graphite Substances 0.000 description 11
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- 238000007873 sieving Methods 0.000 description 10
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- 239000010949 copper Substances 0.000 description 8
- 238000004806 packaging method and process Methods 0.000 description 8
- 239000010453 quartz Substances 0.000 description 8
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- 238000004544 sputter deposition Methods 0.000 description 8
- 239000004615 ingredient Substances 0.000 description 7
- DDJAGKOCVFYQOV-UHFFFAOYSA-N tellanylideneantimony Chemical compound [Te]=[Sb] DDJAGKOCVFYQOV-UHFFFAOYSA-N 0.000 description 6
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- -1 Ru + Sb 2 Te Inorganic materials 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
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- 229910000618 GeSbTe Inorganic materials 0.000 description 2
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- AXJJGGUECHRLTA-UHFFFAOYSA-N [Ru].[Sb] Chemical compound [Ru].[Sb] AXJJGGUECHRLTA-UHFFFAOYSA-N 0.000 description 2
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- 229910001245 Sb alloy Inorganic materials 0.000 description 1
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- 239000004480 active ingredient Substances 0.000 description 1
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- 125000003118 aryl group Chemical group 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
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- 229910052732 germanium Inorganic materials 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
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- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
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- 239000012782 phase change material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
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- 239000010409 thin film Substances 0.000 description 1
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Classifications
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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
-
- 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
-
- 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
- B22F3/15—Hot isostatic pressing
-
- 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
- B22F3/24—After-treatment of workpieces or articles
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/04—Alloys based on a platinum group metal
-
- 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
- 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
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/247—Removing material: carving, cleaning, grinding, hobbing, honing, lapping, polishing, milling, shaving, skiving, turning the surface
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/14—Thermal energy storage
Abstract
The invention discloses a high-performance Ru-Sb-Te alloy sputtering target material used as a phase change storage medium. The Ru-Sb-Te alloy sputtering target material is an alloy target material which is composed of raw materials of Ru, Sb and Te and has a chemical formula of Rux (Sb2Te)100-x, wherein x is the atomic percent of Ru element, and x is more than or equal to 1 and less than or equal to 10; in particular x is 3 or 5; the raw materials are three elementary metals of Ru, Sb and Te or compounds of any two elements. The preparation method takes ruthenium, antimony, tellurium or compounds of any two elements as raw materials, and prepares Ru-Sb-Te alloy powder by a fusion casting method; the target blank is obtained by mechanical crushing and pressure sintering, and finally the target is obtained by processing and forming. The defects of low phase transition temperature, poor thermal stability and the like of the Sb2Te compound are overcome by adding ruthenium; through powder preparation and pressure sintering after smelting, a sputtering target with better uniformity and high density is obtained, and the defects of more smelting defects, large grains, poor processability and the like of the target prepared by direct fusion casting are avoided; the high requirement of the phase change storage field on the RST target is fully met.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy, further belongs to the technical field of alloy sputtering target materials, further belongs to the technical field of phase change storage, and particularly relates to a Ru-Sb-Te alloy sputtering target material used as a long-storage phase change storage medium and a preparation method thereof.
Background
The phase-change memory material is a novel nonvolatile random memory mode based on chalcogenide and has the advantages of nonvolatility, high reading speed, good thermal stability and the like. The mechanism is that the information is read and stored by the resistance difference between the amorphous state and the crystal through the temperature difference of the phase-change material. In the prior art, the phase change storage film is mainly prepared by a magnetron sputtering method, and has the characteristics of stable performance and strong operability.
The phase change memory material prepared by the antimony tellurium compound film has the characteristic of high phase transition speed, is a representative phase change memory material researched at present, and has the defects of poor thermal stability, low crystallization temperature and the like. Germanium antimony tellurium (Ge-Sb-Te, GST) is the most mature researchOne of the phase change memory material systems of (1), mainly comprising Ge 2 Sb 2 Te 5 、Ge 1 Sb 4 Te 7 、Ge 1 Sb 2 Te 4 And so on. However, although phase change memories based on these phase change memory materials have good performance in many aspects, there is still much room for improvement in material stability, resistivity, crystallization speed, crystallization temperature, power consumption, service life, and the like.
Different application fields have different requirements on phase change memory materials. For example, 10-year data retention temperature and threshold transition speed are indexes respectively representing system stability and data reading speed, and are higher than 85 ℃ for embedded memory application and higher than 120 ℃ for the system in the field of automotive electronics application, while Ge is currently used 2 Sb 2 Te 5 The 10-year data retention temperature of the system is only 80 ℃, the threshold transition speed is only tens of nanoseconds, and the requirements in the fields of automobile electronics and the like cannot be met completely. Therefore, it is an urgent need to develop a phase change memory system with excellent overall performance, such as good data stability, fast reading speed, low power consumption, etc., so that it is very desirable to develop a sputtering target with high density and uniformity, and capable of satisfying the requirement of long-term phase change memory.
Disclosure of Invention
The first purpose of the invention is to provide a high-performance Ru-Sb-Te alloy sputtering target material (called RST sputtering target material for short) used as a long-storage phase-change storage medium; the invention also aims to provide a preparation method of the high-performance Ru-Sb-Te alloy sputtering target material used as the long-storage phase change storage medium; a further object is the use of the Ru-Sb-Te alloy sputtering target.
The first purpose of the invention is realized by that the high-performance Ru-Sb-Te alloy sputtering target material (RST target material for short) used as the phase change storage medium with long storage time is composed of Ru, Sb and Te elements according to the chemical formula x (Sb 2 Te 3 ) 100-x The formed alloy target material, wherein x is the atomic percentage of the alloy element Ru, and x is more than or equal to 1 and less than or equal to 10; in particular, x is 5 or 8. The raw materials are three elementary metals of Ru, Sb and Te or NingMeaning a compound of two elements.
The other purpose of the invention is realized by the following steps of raw material preparation, powder preparation, pressure sintering and machine-shaping, wherein the preparation method of the high-performance Ru-Sb-Te alloy sputtering target material used as the long-storage phase change storage medium comprises the following steps:
(1) preparing raw materials: preparing ruthenium, antimony and tellurium or compounds of any two elements of ruthenium, antimony and tellurium as raw materials according to a ratio, and preparing a Ru-Sb-Te alloy by a fusion casting method, wherein Ru is added according to a stoichiometric ratio, Sb is excessive by 2-8 wt%, Te is excessive by 6-16 wt% during proportioning, and the smelting vacuum degree is 1 x 10 -2 Pa~1×10 -4 Pa, the smelting temperature is 600-1100 ℃;
(2) powder preparation: Ru-Sb-Te alloy powder is obtained by mechanical crushing and screening, and the mechanical crushing can be mechanical grinding, ball milling and the like. When planetary ball milling is adopted, zirconia grinding balls are preferably selected, the material ratio of the grinding balls is 4:1-1:1, the rotating speed is 100-300 r/min, and the time is 1-5 h;
(3) and (3) pressure sintering: obtaining a Ru-Sb-Te target material billet through pressure sintering, wherein the pressure sintering can be hot isostatic pressing or vacuum hot pressing, and when the hot isostatic pressing sintering is adopted, the sintering temperature is 450-600 ℃, the time is 1-4 h, and the pressure is 20-100 MPa; when vacuum hot pressing is adopted, the sintering temperature is 500-650 ℃, the time is 1-4 h, and the pressure is 20-60 MPa;
(4) and (3) processing and forming: the Ru-Sb-Te target material is obtained by mechanical processing, and the selected mechanical processing is preferably grinding because the target material is fragile during processing, and a grinding wheel made of silicon carbide or corundum is adopted during grinding.
The invention utilizes the excellent performance of the ruthenium-doped antimony-tellurium alloy sputtering as a film material, and the Ru-Sb-Te alloy is further optimized and modified to be used as an RST sputtering target material for preparing a phase change storage medium. The invention overcomes the technical defect that the film or device processing in the prior art usually adopts a co-sputtering mode to realize, namely, the method for preparing the Ru-Te-Sb alloy sputtering target material is specially developed according to the physicochemical characteristics of each element in the co-sputtering process of three metal target materials of Ru + Sb + Te alloy or the co-sputtering process of Ru metal + SbTe compound target material. Is not limited toThe operation is simple and convenient, and the alloy composition of the required film or device can be accurately controlled. On the one hand, Sb is improved by adding ruthenium 2 Te 3 The phase transition temperature of the compound is low, the thermal stability is poor and the like; on the other hand, through the preparation of powder after smelting and pressure sintering, the sputtering target material with better uniformity and density can be obtained, and the defects of more smelting defects, coarse grains, poor machinability and the like of the target material prepared by direct casting in the prior art are avoided; fully meets the requirements of the phase change storage field on the ruthenium antimony tellurium sputtering target material.
Drawings
FIG. 1 is an XRD spectrum of the Ru-Sb-Te alloy powder and the mixed powder prepared by the method of example 1;
FIG. 2 is a diagram of the gold phase of the Ru-Sb-Te target material prepared by the method of the embodiment 1 of the invention;
FIG. 3 is an XRD spectrum of the Ru + Sb + Te raw material system alloy target material prepared by the method of comparative example 2.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to be limiting in any way, and any modifications or alterations based on the teachings of the present invention are intended to fall within the scope of the present invention.
The invention discloses a high-performance Ru-Sb-Te alloy sputtering target material used as a phase change storage medium, which is prepared by performing chemical formula Ru on Ru, Sb and Te elements x (Sb 2 Te 3 ) 100-x The formed alloy target material, wherein x is the atomic percentage of the alloy element Ru, and x is more than or equal to 1 and less than or equal to 10; in particular x is 3 or 5.
The raw material is a compound of any two elements of three elementary metals of Ru, Sb and Te, such as Ru + Sb 2 Te、Ru+Sb 2 Te 3 And the like.
The invention relates to a preparation method of a high-performance Ru-Sb-Te alloy sputtering target material used as a phase change storage medium, which comprises the following steps:
ruthenium, antimony, tellurium or compounds of any two elements of ruthenium, antimony and tellurium are taken as raw materials, the materials are prepared according to a mixture ratio, wherein Ru is added according to a stoichiometric ratio, Sb is excessive by 2-8 wt%, and Te is excessive during the material preparationFeeding 6-16 wt.% of materials, and preparing a Ru-Sb-Te alloy by a fusion casting method; the fusion casting method is realized by vacuum melting with the vacuum degree of 1 × 10 -2 Pa~1×10 -4 Pa, and the temperature is 600-1100 ℃.
Ru-Sb-Te alloy powder is obtained by mechanical crushing and screening, and the mechanical crushing can be mechanical grinding, ball milling and the like. When planetary ball milling is adopted, zirconia grinding balls are preferably selected, the material ratio of the grinding balls is 4:1-1:1, the rotating speed is 100-300 r/min, and the time is 1-5 h;
obtaining a Ru-Sb-Te target material billet through pressure sintering; the pressure sintering is hot isostatic pressing sintering, the sintering temperature is 450-600 ℃, the time is 1-4 h, and the pressure is 20-100 MPa. The pressure sintering is vacuum hot pressing, the sintering temperature is 500-650 ℃, the time is 1-4 h, and the pressure is 20-60 MPa.
The Ru-Sb-Te target material is obtained by mechanical processing, preferably by grinding, and a grinding wheel made of silicon carbide or corundum is adopted during grinding.
The prepared Ru-Sb-Te target material is bound with the back plate by a tin soldering or diffusion welding method.
The Ru-Sb-Te alloy sputtering target material is used for preparing a phase change storage medium capable of storing data for a long time.
The RST sputtering target material of the invention takes ruthenium Ru as a doping element and takes chalcogenide compound consisting of Sb and Te as a matrix material. The antimony-tellurium compound is Sb 2 Te 3 . With Sb 2 Te 3 The phase change memory material prepared by the compound film has the characteristic of high phase transition speed, is one of representative phase change memory materials researched at present, and has the defects of poor thermal stability, low crystallization temperature and the like. It is often desirable to ameliorate these disadvantages by doping or the like. Germanium antimony tellurium (Ge-Sb-Te, GST) is one of the most mature phase change storage material systems, and researchers also research scandium (Sc) -doped (Sc-Sb-Te) alloys, but the crystallization temperature and the thermal stability of the storage materials still have a large promotion space. The inventor finds that the crystallization temperature of the target can be effectively increased and the thermal stability of the film can be improved by adding the ruthenium Ru element. Ruthenium is a noble metal elementThe element has high melting point and stable chemical property, and the content of the ruthenium element has great influence on the alloy performance and needs to be strictly controlled. The content of the active ingredients is less, and no positive effect can be produced; and a larger amount thereof reduces the overall effect by reducing the crystallization speed of the chalcogenide compound.
In order to fully exert the advantages of the single-target sputtering method in the aspect of component control, it is a necessary prerequisite to obtain raw material powder and a target material with accurate components. The elements are generally thoroughly mixed by fusion casting. Sb (425K, 1.33X 10) at the same saturation vapor pressure for the Ru-Sb-Te system -2 Pa）、Te（280K，1.33×10 -2 Pa) is far less than that of Ru (2703K, 1.33 multiplied by 10 -2 Pa), generally the lower the temperature at which the vapour pressure reaches saturation, the greater the ability of the material to volatilize, so that Te volatilizes most easily during synthesis, Sb secondly, Ru hardly volatilizes, and the different volatilization rates of the elements make precise control of the composition difficult. For example, by taking Ru, Sb and Te as raw materials, and carrying out series experiments on different feeding ratios of the Ru, the Sb and the Te at the earlier stage of the experiment, the RST alloy with accurate components can be obtained when the Ru is added according to the stoichiometric ratio, the Sb is excessive by 2-8 wt.%, and the Te is excessive by 6-16 wt.%. Meanwhile, in order to control the oxygen content of the alloy, the vacuum degree of smelting needs to be strictly controlled, and experiments show that the vacuum degree is 1 multiplied by 10 - 2 Pa~1×10 -4 Pa is suitable.
In the aspect of smelting temperature, because the melting point of ruthenium is higher, the ruthenium can be fully melted at the temperature of 600-1100 ℃; the optimized temperature condition is 600-699 ℃; 701-899 ℃; 901 to 1099 ℃.
Obtaining Ru-Sb-Te alloy powder by mechanical crushing and screening. As the antimony tellurium alloy is brittle, the alloy powder can be obtained by adding a small amount of Ru-Sb-Te alloy cast ingot, mechanically crushing and screening. Mechanical crushing may be mechanical milling, ball milling, or the like. When planetary ball milling is adopted, zirconia grinding balls are preferably selected, the material ratio of the grinding balls is 4:1-1:1, the rotating speed is 100-300 r/min, and the time is 1-5 hours.
Obtaining a Ru-Sb-Te target material billet through pressure sintering; the target blank with high density and low density can be obtained by pressure sintering. The pressure sintering can be hot isostatic pressing, and the preferred sintering temperature is 450-600 ℃ and is optimized to be 450-499 ℃ due to the lower melting points of Sb and Te; 501-549 ℃; 551-599 ℃; the time is 1-4 h, and the optimized time is 2h or 3 h; the pressure is 20-100 MPa, and the optimized pressure is 21-39 MPa; 41-59 MPa; 61-79 MPa; 81-99 MPa; the pressure sintering can also be vacuum hot pressing, the sintering temperature is 500-650 ℃, and the optimized sintering temperature is 501-549 ℃; 551-599 ℃; the temperature is 601-649 ℃, the time is 1-4 h, the optimized time is 2h, 3h or 3.5h, the pressure is 20-60 MPa, and the optimized time is 21-29 MPa; 31 to 39 MPa; 41-49 MPa; 51-59 MPa; 61-69 MP.
Example 1
Taking three elementary substance powders of 4N (with the purity of 99.99 percent) Ru, Sb and Te as raw materials, sieving the raw materials by a standard sieve of 200 meshes, and then screening the raw materials according to a chemical formula of Ru 5 (Sb 2 Te 3 ) 95 Ingredients, wherein: ru was added stoichiometrically, Sb was in excess of 4 wt.%, Te was in excess of 14 wt.% fed. The mixed powder is treated by adopting planetary ball milling, and the ball milling process comprises the following steps: the ball-material ratio is 2:1, the rotating speed is 150r/min, and the time is 3 h. Ball milling and mixing, putting the mixed powder into a quartz tube, vacuumizing and packaging, wherein the vacuum degree is 1 multiplied by 10 -4 Pa, placing the mixture in a resistance furnace, and sintering the mixture for 3 hours at 650 ℃ to obtain RST alloy powder raw materials; and (3) putting the alloy powder into a graphite die with the diameter of 50mm, and carrying out vacuum hot pressing, wherein the sintering temperature is 550 ℃, the pressure is 40MPa, and the time is 3 h. Then grinding by a silicon carbide grinding wheel to obtain Ru with the diameter of 50 multiplied by 5mm 5 (Sb 2 Te 3 ) 95 A ternary alloy target material. The processed target material and the copper back plate are bonded by tin soldering by taking indium as a solder to obtain the final target material.
Example 2
Taking three elementary substance powders of 4N (with the purity of 99.99 percent) Ru, Sb and Te as raw materials, sieving the raw materials by a standard sieve of 200 meshes, and then screening the raw materials according to a chemical formula of Ru 1 (Sb 2 Te 3 ) 99 Ingredients, wherein: ru was added stoichiometrically, Sb was in excess of 2 wt.%, Te was in excess of 6wt.% fed. The mixed powder is treated by adopting planetary ball milling, and the ball milling process comprises the following steps: the ball-material ratio is 1:1, the rotating speed is 100r/min, and the time is 1 h. Ball milling and mixing, loading the mixed powder into quartz tube, vacuumizing and packaging at vacuum degree of 1 × 10 -4 Pa, placing in a resistance furnace, and sintering at 600 ℃ for 1h to obtain RST alloyA powder raw material; and putting the alloy powder into a graphite die with the diameter of 50mm, and carrying out hot isostatic pressing, wherein the sintering temperature is 450 ℃, the pressure is 100MPa, and the time is 3 h. Then grinding by a corundum grinding wheel to obtain Ru with the diameter of 50 multiplied by 5mm 1 (Sb 2 Te 3 ) 99 A ternary alloy target material. And binding the processed target material and the copper back plate through diffusion welding to obtain the final target material.
Example 3
Taking three elementary substance powders of 4N (with the purity of 99.99 percent) Ru, Sb and Te as raw materials, sieving the raw materials by a standard sieve of 200 meshes, and then screening the raw materials according to a chemical formula of Ru 3 (Sb 2 Te 3 ) 97 Ingredients, wherein: ru is added in stoichiometric proportion, Sb is in excess of 4 wt.%, and Te is in excess of 8 wt.%. The mixed powder is treated by adopting planetary ball milling, and the ball milling process comprises the following steps: the ball-material ratio is 2:1, the rotating speed is 150r/min, and the time is 3 h. Ball milling and mixing, putting the mixed powder into a quartz tube, vacuumizing and packaging, wherein the vacuum degree is 1 multiplied by 10 -4 Pa, placing the powder in a resistance furnace, and sintering the powder for 2 hours at 700 ℃ to obtain RST alloy powder raw materials; and (3) putting the alloy powder into a graphite die with the diameter of 50mm, and carrying out vacuum hot pressing, wherein the sintering temperature is 500 ℃, the pressure is 50MPa, and the time is 2 h. Then grinding by using a silicon carbide grinding wheel to obtain Ru with the phi of 50 multiplied by 5mm 5 (Sb 2 Te 3 ) 95 A ternary alloy target material. And binding the processed target material with a copper back plate to obtain the final target material.
Example 4
4N (with the purity of 99.99%) Ru elemental powder and Sb 2 Te 3 Three are used as raw materials, and after passing through a standard sieve of 200 meshes, the raw materials are screened according to a chemical formula Ru 5 (Sb 2 Te 3 ) 95 Ingredients, wherein: ru is added according to the stoichiometric ratio, Sb is excessive by 5wt.%, and Te is excessive by 10 wt.%. The mixed powder is treated by adopting a planetary ball milling process, and the ball milling process comprises the following steps: the ball-material ratio is 3:1, the rotating speed is 250r/min, and the time is 2 h. Ball milling and mixing, putting the mixed powder into a quartz tube, vacuumizing and packaging, wherein the vacuum degree is 1 multiplied by 10 -4 Pa, placing the mixture in a resistance furnace, and sintering the mixture for 3 hours at 650 ℃ to obtain RST alloy powder raw materials; and putting the alloy powder into a graphite die with the diameter of 50mm, and carrying out hot isostatic pressing, wherein the sintering temperature is 550 ℃, the pressure is 80MPa, and the time is 2 h. Followed byGrinding corundum grinding wheel to obtain Ru with phi 50 multiplied by 5mm 5 (Sb 2 Te 3 ) 95 A ternary alloy target material. And binding the processed target material with a copper back plate to obtain the final target material.
Example 5
Taking three elementary substance powders of 4N (with the purity of 99.99 percent) Ru, Sb and Te as raw materials, sieving the raw materials by a standard sieve of 200 meshes, and then screening the raw materials according to a chemical formula of Ru 6 (Sb 2 Te 3 ) 94 Ingredients, wherein: ru is added according to the stoichiometric ratio, Sb is excessive by 5wt.%, and Te is excessive by 15 wt.%. The mixed powder is treated by adopting planetary ball milling, and the ball milling process comprises the following steps: the ball material ratio is 3:1, the rotating speed is 250r/min, and the time is 2 h. Ball milling and mixing, putting the mixed powder into a quartz tube, vacuumizing and packaging, wherein the vacuum degree is 1 multiplied by 10 -2 Pa, placing the powder in a resistance furnace, and sintering the powder for 3 hours at 750 ℃ to obtain RST alloy powder raw materials; and (3) putting the alloy powder into a graphite die with the diameter of 50mm, and carrying out vacuum hot pressing, wherein the sintering temperature is 650 ℃, the pressure is 20MPa, and the time is 1 h. Then grinding by a silicon carbide grinding wheel to obtain Ru with the diameter of 50 multiplied by 5mm 5 (Sb 2 Te 3 ) 95 A ternary alloy target material. And binding the processed target material with a copper back plate to obtain the final target material.
Example 6
Taking three elementary substance powders of Ru, Sb and Te with 4N (the purity is 99.99%) as raw materials, sieving the raw materials by a standard sieve with 200 meshes, and then screening the raw materials by a chemical formula Ru 8 (Sb 2 Te 3 ) 92 Ingredients, wherein: ru was added stoichiometrically, Sb was 6wt.% in excess, Te was 16wt.% in excess. The mixed powder is treated by adopting planetary ball milling, and the ball milling process comprises the following steps: the ball-material ratio is 3:1, the rotating speed is 200r/min, and the time is 4 h. Ball milling and mixing, putting the mixed powder into a quartz tube, vacuumizing and packaging, wherein the vacuum degree is 1 multiplied by 10 -3 Pa, placing the powder in a resistance furnace, and sintering the powder for 4 hours at 800 ℃ to obtain RST alloy powder raw material; and putting the alloy powder into a graphite die with the diameter of 50mm, and carrying out hot isostatic pressing, wherein the sintering temperature is 600 ℃, the pressure is 60MPa, and the time is 4 h. Then grinding by a corundum grinding wheel to obtain Ru with the diameter of 50 multiplied by 5mm 8 (Sb 2 Te 3 ) 92 A ternary alloy target material. And binding the processed target material with a copper back plate to obtain the final target material.
Example 7
Taking three elementary substance powders of Ru, Sb and Te with 4N (the purity is 99.99%) as raw materials, sieving the raw materials by a standard sieve with 200 meshes, and then screening the raw materials by a chemical formula Ru 10 (Sb 2 Te 3 ) 90 And (4) batching. The mixed powder is treated by adopting planetary ball milling, and the ball milling process comprises the following steps: the ball-material ratio is 4:1, the rotating speed is 300r/min, and the time is 5 h. Ball milling and mixing, putting the mixed powder into a quartz tube, vacuumizing and packaging, wherein the vacuum degree is 1 multiplied by 10 -4 Pa, placing the powder in a resistance furnace, and sintering the powder for 1 hour at 1100 ℃ to obtain RST alloy powder raw material; and (3) putting the alloy powder into a graphite die with the diameter of 50mm, and carrying out vacuum hot pressing, wherein the sintering temperature is 600 ℃, the pressure is 60MPa, and the time is 4 h. Then grinding by using a silicon carbide grinding wheel to obtain Ru with the phi of 50 multiplied by 5mm 10 (Sb 2 Te 3 ) 90 A ternary alloy target material. And binding the processed target material with a copper back plate to obtain the final target material.
Example 8
Taking three elementary substance powders of 4N (with the purity of 99.99 percent) Ru, Sb and Te as raw materials, sieving the raw materials by a standard sieve of 200 meshes, and then screening the raw materials according to a chemical formula of Ru 5 (Sb 2 Te 3 ) 95 Ingredients, wherein: ru was added stoichiometrically, Sb was in excess of 4 wt.%, Te was in excess of 16wt.% fed. The mixed powder is treated by adopting planetary ball milling, and the ball milling process comprises the following steps: the ball-material ratio is 2:1, the rotating speed is 150r/min, and the time is 3 h. Ball milling and mixing, putting the mixed powder into a quartz tube, vacuumizing and packaging, wherein the vacuum degree is 1 multiplied by 10 -4 Pa, placing the mixture in a resistance furnace, and sintering the mixture for 2 hours at 650 ℃ to obtain RST alloy powder raw materials; and putting the alloy powder into a graphite die with the diameter of 50mm, and carrying out hot isostatic pressing, wherein the sintering temperature is 500 ℃, the pressure is 40MPa, and the time is 1 h. Then grinding by a corundum grinding wheel to obtain Ru with the diameter of 50 multiplied by 5mm 5 (Sb 2 Te 3 ) 95 A ternary alloy target material. And binding the processed target material with a copper back plate to obtain the final target material.
Comparative example 1
Sb of 4N (purity 99.99 percent) 2 Te 3 Alloy powder is used as raw material, and after the alloy powder is sieved by a standard sieve with 200 meshes, the alloy powder is sieved according to a chemical formula Sb 2 Te 3 And (4) batching. The mixed powder is treated by adopting planetary ball millingFinally, the ball milling process comprises the following steps: the ball-material ratio is 2:1, the rotating speed is 150r/min, and the time is 3 h. After ball milling and mixing, the alloy powder is directly put into a graphite die with the diameter of 50mm for vacuum hot pressing, the sintering temperature is 450 ℃, the pressure is 40MPa, and the time is 3 h. Then adopting mechanical processing to obtain Sb with phi of 50 multiplied by 5mm 2 Te 3 An alloy target material. The relative density of the obtained target material was 99.70%. The target density and properties of the prepared film are shown in Table 1 by the same target analysis method as in example 1.
Comparative example 2
Taking 4N (with purity of 99.99%) elementary substance powder of Ru, Sb and Te as raw materials, sieving the raw materials by a standard sieve of 200 meshes, and then screening the raw materials according to a chemical formula of Ru 5 (Sb 2 Te 3 ) 95 And (4) batching. The mixed powder is treated by adopting planetary ball milling, and the ball milling process comprises the following steps: the ball-material ratio is 2:1, the rotating speed is 150r/min, and the time is 3 h. After ball milling and mixing, the alloy powder is directly put into a graphite die with the diameter of 50mm for vacuum hot pressing without a vacuum smelting process, the sintering temperature is 540 ℃, the pressure is 40MPa, and the time is 3 h. Then obtaining Ru with phi 50 multiplied by 5mm by adopting mechanical processing 5 (Sb 2 Te 3 ) 95 A ternary alloy target material.
Comparative example 3
4N (with the purity of 99.99%) Ru elemental powder and Sb 2 Te 3 Sieving with 200 mesh standard sieve, and sieving with Ru as chemical formula 5 (Sb 2 Te 3 ) 95 And (4) batching. The mixed powder is treated by adopting planetary ball milling, and the ball milling process comprises the following steps: the ball-material ratio is 2:1, the rotating speed is 150r/min, and the time is 3 h. After ball milling and mixing, the alloy powder is directly filled into a graphite die with the diameter of 50mm for vacuum hot pressing without vacuum melting, the sintering temperature is 540 ℃, the pressure is 40MPa, and the time is 3 h. Then obtaining Ru with phi 50 multiplied by 5mm by adopting mechanical processing 5 (Sb 2 Te 3 ) 95 A ternary alloy target material.
Chemical titration was used to analyze the chemical composition of the powder and target. And testing the phases of the alloy powder and the target material by adopting an X-ray diffractometer. FIG. 1 is the XRD spectrum of the mixed powder of the elementary powders Ru, Sb and Te in example 1 and the mixed and smelted powder. By using an aryl radicalAnd measuring the actual density of the sample blank by a Mide drainage method, and according to a formula: relative density = ρ actual/ρ theoretical × 100%, the relative density was calculated. The relative density of the target prepared by the method is 99.83 percent. To the prepared Ru 5 (Sb 2 Te 3 ) 95 The ternary alloy target material is used for sputtering a Ru-Sb-Te film on a Si substrate, measuring a resistance-temperature (R-T) curve of the Ru-Sb-Te film to obtain the crystallization temperature of the Ru-Sb-Te film, and obtaining ten-year data retention of the Ru-Sb-Te film by using an Arrhenius equation. As can be seen from the R-T curve, the crystallization temperature of the film is 280 ℃ and the ten-year data retention is 170 ℃.
Similarly, the relative densities of the targets prepared in examples 2 to 8 were measured. The prepared target material is used as a sputtering source, a Ru-Sb-Te film is sputtered on a Si substrate, the resistance-temperature (R-T) curve of the Ru-Sb-Te film is measured so as to obtain the crystallization temperature of the Ru-Sb-Te film, and the ten-year data retention of the Ru-Sb-Te film is obtained by using an Arrhenius equation. The corresponding density and film properties are shown in table 1.
Different alloy components and preparation conditions are respectively selected in comparative examples 1 to 3. Specifically, the comparative example 1 is a ruthenium-undoped antimony tellurium alloy target, the comparative example 2 is a ruthenium-antimony-tellurium target directly prepared without vacuum melting of several kinds of raw material powder, and the comparative example 3 is a ruthenium-antimony-tellurium target prepared by directly hot-pressing and sintering elemental ruthenium-antimony-tellurium alloy powder without vacuum melting. Similarly, the density of the prepared target material in the comparative example was measured, and the prepared target material was sputtered on a silicon substrate by the sputtering process as in example 1, and the R-T curve and ten-year data retention of the film were measured. Fig. 3 is an XRD spectrum of the target material prepared in comparative example 2. The relative density of the target material prepared in the comparative example and the properties of the film prepared in the comparative example are shown in Table 1.
TABLE 1 relative densities and film Properties of targets of various examples and comparative examples
As can be seen from FIG. 1, the Ru-Sb-Te alloy target material prepared in example 1 is made of RuTe 2 And Sb 2 Te 3 Composition ofAs can be seen from fig. 2, the target material prepared in example 1 has a uniform microstructure; as can be seen from FIG. 3, in comparative example 2, the Ru-Sb-Te target material is prepared from Ru and Sb 2 Te 3 Composition, Ru is not alloyed with Sb and Te. As can be seen from Table 1, the crystallization temperature and ten-year data retention temperature of the thin film of the target materials prepared in examples 1-8 are greatly increased compared with those of the target material prepared in comparative example 1, which indicates that the doping of ruthenium can effectively increase Sb 2 Te 3 Thermal stability of the system and data retention temperature. Meanwhile, the relative density of the target prepared by the method provided by the invention is generally higher and reaches more than 99.6% of the theoretical density, and the alloying reaction of ruthenium and antimony tellurium can be effectively realized (as shown in fig. 1), while the relative density of the target prepared in the comparative example 2 and the comparative example 3 is only about 96% of the theoretical density, and the film prepared by the target prepared in the comparative example 2 and the comparative example 3 has a great improvement on the proportion 1 due to the doping of ruthenium, but has a great difference compared with the example 1, the example 4 and the example 8.
In summary, in embodiments 1 to 8, by using the method provided by the present invention, the ruthenium antimony tellurium target material can be prepared by controlling parameters in the casting process, such as the material proportioning ratio, the vacuum degree, and the temperature, and combining with the pressure sintering, and the prepared target material has characteristics of high density, good stability, and simple process. Meanwhile, the film prepared by the target material in the embodiment 1-8 has higher crystallization stability and ten-year data retention temperature, so that the film has better thermal stability and is expected to be suitable for preparing the phase change storage material film.
Claims (9)
1. A high-performance Ru-Sb-Te alloy sputtering target material used as a phase change storage medium for long time storage is characterized in that the Ru-Sb-Te alloy sputtering target material is prepared from raw materials of Ru, Sb and Te according to the chemical formula Ru x (Sb 2 Te 3 ) 100-x The formed alloy target material, wherein x is the atomic percentage of Ru element, and x is more than or equal to 1 and less than or equal to 10; the raw materials are three elementary metals of Ru, Sb and Te or compounds consisting of any two elements.
2. Use according to claim 1 as a storage-durable phase change memory mediumThe high-performance Ru-Sb-Te alloy sputtering target material is characterized in that the chemical formula Ru x (Sb 2 Te 3 ) 100-x And (3), x = 3.
3. The high performance Ru-Sb-Te alloy sputtering target material used as long-storage phase change storage medium according to claim 1, wherein the chemical formula Ru x (Sb 2 Te 3 ) 100-x And (5), x = 5.
4. A preparation method of the high-performance Ru-Sb-Te alloy sputtering target material used as the long-storage phase-change storage medium according to any one of claims 1 to 3, which is characterized by comprising the following steps of raw material preparation, powder preparation, pressure sintering and machine shaping, and specifically comprises the following steps:
(1) preparing raw materials: preparing materials according to a mixture ratio by taking compounds of ruthenium, antimony and tellurium or any two elements of ruthenium, antimony and tellurium as raw materials, wherein during the material preparation, Ru is added according to a stoichiometric ratio, Sb is excessive by 2-8 wt%, Te is excessive by 6-16 wt%, and Ru-Sb-Te alloy is prepared by a fusion casting method;
(2) powder preparation: obtaining Ru-Sb-Te alloy powder through mechanical crushing and screening, wherein the mechanical crushing is mechanical grinding or ball milling; when planetary ball milling is adopted, zirconia grinding balls are preferably selected, the grinding ball material ratio is 4:1-1:1, the rotating speed is 100-300 r/min, and the time is 1-5 h;
(3) and (3) pressure sintering: obtaining a Ru-Sb-Te target material billet through pressure sintering;
(4) processing and forming: the Ru-Sb-Te target material is obtained by mechanical processing, the selected mechanical processing preferably adopts grinding, and a grinding wheel made of silicon carbide or corundum is adopted during grinding.
5. The method for preparing Ru-Sb-Te sputtering target material with high performance for long-term storage phase change storage medium according to claim 4, wherein the step (1) of fusion casting is realized by vacuum melting with the vacuum degree of 1 x 10 -2 Pa~1×10 -4 Pa, and the temperature is 600-1100 ℃.
6. The method for preparing the Ru-Sb-Te sputtering target material used as the long-storage phase change storage medium according to claim 4, wherein the step (3) of pressure sintering is hot isostatic pressing sintering, the sintering temperature is 450-600 ℃, the sintering time is 1-4 h, and the pressure is 20-100 MPa.
7. The method for preparing the Ru-Sb-Te sputtering target material used as the phase change storage medium with long storage life according to claim 4, wherein the step (3) of pressure sintering is vacuum hot pressing, the sintering temperature is 500-650 ℃, the time is 1-4 h, and the pressure is 20-60 MPa.
8. The method for preparing the Ru-Sb-Te sputtering target material used as the phase change storage medium with long storage life as claimed in claim 4, wherein the prepared Ru-Sb-Te alloy sputtering target material is bound with a back plate by soldering or diffusion welding.
9. The Ru-Sb-Te alloy sputtering target material according to any one of claims 1 to 3 and 5 to 8 for preparing a phase change memory medium capable of storing data for a long time.
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