CN109226768A - A kind of preparation method of transient metal doped antimony telluride alloy target material - Google Patents
A kind of preparation method of transient metal doped antimony telluride alloy target material Download PDFInfo
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- CN109226768A CN109226768A CN201811177004.1A CN201811177004A CN109226768A CN 109226768 A CN109226768 A CN 109226768A CN 201811177004 A CN201811177004 A CN 201811177004A CN 109226768 A CN109226768 A CN 109226768A
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- 239000000956 alloy Substances 0.000 title claims abstract 16
- 229910045601 alloy Inorganic materials 0.000 title claims abstract 16
- 239000013077 target material Substances 0.000 title claims abstract 13
- 238000002360 preparation method Methods 0.000 title claims abstract 10
- MRPWWVMHWSDJEH-UHFFFAOYSA-N antimony telluride Chemical compound [SbH3+3].[SbH3+3].[TeH2-2].[TeH2-2].[TeH2-2] MRPWWVMHWSDJEH-UHFFFAOYSA-N 0.000 title claims abstract 9
- 229910052751 metal Inorganic materials 0.000 title claims 8
- 239000002184 metal Substances 0.000 title claims 8
- 230000001052 transient effect Effects 0.000 title claims 8
- 239000000843 powder Substances 0.000 claims abstract 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract 4
- 229910002804 graphite Inorganic materials 0.000 claims abstract 4
- 239000010439 graphite Substances 0.000 claims abstract 4
- 229910052804 chromium Inorganic materials 0.000 claims abstract 2
- 238000007731 hot pressing Methods 0.000 claims abstract 2
- 229910052753 mercury Inorganic materials 0.000 claims abstract 2
- 229910052706 scandium Inorganic materials 0.000 claims abstract 2
- 229910052719 titanium Inorganic materials 0.000 claims abstract 2
- 229910052723 transition metal Inorganic materials 0.000 claims abstract 2
- 150000003624 transition metals Chemical class 0.000 claims abstract 2
- 229910052727 yttrium Inorganic materials 0.000 claims abstract 2
- 229910052725 zinc Inorganic materials 0.000 claims abstract 2
- 229910052582 BN Inorganic materials 0.000 claims 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims 1
- 238000005245 sintering Methods 0.000 claims 1
- 238000001816 cooling Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000012423 maintenance Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 abstract 1
- 230000007704 transition Effects 0.000 abstract 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Powder Metallurgy (AREA)
Abstract
本发明提供一种过渡金属掺杂的碲化锑合金靶材的制备方法,过渡金属包括Sc,Y,Ti,Cr,Hg,Zn等。本发明中合金靶材的制备方法是：1)将适量合金粉末装入石墨模具，并密封于真空热压炉当中；2)室温下施加70％的目标压强，保压约5分钟后缓慢卸压；3)调节温度至200℃后，施加目标压强，保压约5分钟后缓慢卸压；4)加热升温至目标温度后，再次施加目标压强并保压约5分钟；5)保压结束后，自然降温，且每降低20℃卸载20％目标压强，待冷却至室温即得靶材。本发明所涉及的制备方法具有成本低廉，操作简单，环境友好等特点，制备得到的靶材纯度高，致密度高且元素分布均匀。
The present invention provides a method for preparing a transition metal-doped antimony telluride alloy target material. The transition metals include Sc, Y, Ti, Cr, Hg, Zn and the like. The preparation method of the alloy target material in the present invention is as follows: 1) put an appropriate amount of alloy powder into a graphite mold, and seal it in a vacuum hot pressing furnace; 2) apply 70% of the target pressure at room temperature, and slowly unload after about 5 minutes of pressure maintenance 3) After adjusting the temperature to 200°C, apply the target pressure, and release the pressure slowly after maintaining the pressure for about 5 minutes; 4) After heating to the target temperature, apply the target pressure again and maintain the pressure for about 5 minutes; 5) The pressure maintaining is over After that, the temperature is naturally lowered, and the target pressure is unloaded by 20% every time the temperature is lowered by 20°C, and the target material is obtained after cooling to room temperature. The preparation method involved in the invention has the characteristics of low cost, simple operation, environmental friendliness and the like, and the prepared target material has high purity, high density and uniform element distribution.
Description
Technical field
The invention belongs to material processing techniques, are related to a kind of preparation side of transient metal doped antimony telluride alloy target material
Method.
Background technique
Since the 1990s, the synchronized development of sputtering target material and sputtering technology is greatly met various novel
The growth requirement of electronic component.The swift and violent growth of information data amount all proposes memory integrated technique and storage material itself
Requirements at the higher level are gone out.Currently, the thin-film material for being applied to area information storage mostly uses magnetron sputtering method to prepare, this just needs to make
The sputtering target material of standby high quality out.
Traditional preparation methods in phase change memory field, transient metal doped antimony telluride alloy target material are melting and castings
Method.Melting and casting method is mainly nonmetallic as raw material using bulk metal or bulk metal and block, by melting and castable,
Target needed for preparing.This method is at high cost, complex process, and target material composition is not easy to control, easily causes Elemental redistribution uneven
The problems such as.In addition, the target of fusion casting preparation is easily-deformable and cracks.Therefore, it is badly in need of finding a kind of novel alloy target material preparation
Technique, the technique should have low in cost, and easy to operate, environmental-friendly, density is high, the uniform equal spies of purity is high and Elemental redistribution
Point.
Summary of the invention
Environmental-friendly the object of the present invention is to provide a kind of low in cost, simple process, purity is high, consistency is high, element
The transient metal doped antimony telluride alloy target material preparation method being evenly distributed.
The preparation method of transient metal doped antimony telluride alloy target material of the invention a kind of the following steps are included:
1) appropriate alloy powder is added in the graphite jig for being coated with boron nitride；
2) mold that powder is housed in step 1) is packed into hot pressing furnace, seals furnace body, vacuumizes, keep low pressure in furnace；
3) under room temperature state, apply 70% target, pressure, complete release after pressure maintaining 5-10 minutes to mold；
4) in-furnace temperature is risen to 200 DEG C, under conditions of 200 DEG C, target, pressure and pressure maintaining 5-10 points is applied to mold
Complete release after clock；
5) in-furnace temperature is risen to by target temperature T with the speed of 10 DEG C/min1, in T1At a temperature of, target pressure is applied to mold
It is simultaneously pressure maintaining 5-10 minutes strong；
6) in step 5) after pressure maintaining period, cooled to room temperature, every 20 DEG C of 20% mesh of release in temperature-fall period
Mark pressure；
7) target prepared in step 6) is taken out to get alloy target material.
In step 1) of the present invention, the alloy powder dosage is about 54g and purity is 99% or more, and graphite jig internal diameter is
50mm；
In step 3) of the present invention, the target, pressure is that graphite jig can carry maximum pressure, about 40MPa；
In step 4) of the present invention, the dwell time is 5 minutes；
In step 5) of the present invention, the target temperature T1For 0.7Tm(TmFor alloy powder fusing point), the dwell time is 5 points
Clock；
Compared with the prior art, the invention has the following advantages that
1, the present invention directly carries out hot forming sintering using alloy powder, low in cost, easy to operate, and environment friend
It is good；
2, the target purity is high being prepared, consistency is high and Elemental redistribution is uniform；
3, temperature is low in target preparation process, and product controllability is good.
Detailed description of the invention
Fig. 1 is Sc prepared by the embodiment of the present invention 30.25Sb1.75Te3The X-ray diffractogram of target.
Fig. 2 is Sc prepared by the embodiment of the present invention 30.25Sb1.75Te3The scanning electron microscope pattern and elemental map of target
Figure.
Specific embodiment
For a better understanding of the present invention, below with reference to example the present invention is further explained content, but the contents of the present invention
It is not limited solely to following example.
Embodiment 1
Prepare Sb2Te3Target
It 1) will about 54g Sb2Te3It is in 50mm graphite jig that powder, which is added to and is coated with the internal diameter of boron nitride,；
2) by step 1) powder and mold be packed into hot pressing furnace in, closed furnace body vacuumizes, keep furnace in low pressure extremely
0.01Pa or less；
3) under room temperature state, apply the pressure of about 28MPa, pressure maintaining complete release after five minutes to mold；
4) in-furnace temperature is risen to 200 DEG C, under conditions of 200 DEG C, the pressure of 40MPa is applied to mold and pressure maintaining 5 divides
Complete release after clock；
5) in-furnace temperature is risen to 400 DEG C with the speed of 10 DEG C/min, at 400 DEG C, applies the pressure of 40MPa to mold
And pressure maintaining 5 minutes；
6) in step 5) after pressure maintaining period, cooled to room temperature discharges 8MPa's every 20 DEG C in temperature-fall period
Pressure is to complete release；
7) taking out the target prepared in step 6) to get diameter is 50mm, the Sb that thickness is about 4mm2Te3Target.
Embodiment 2
Prepare Y0.25Sb1.75Te3Target
It 1) will about 54g Y0.25Sb1.75Te3It is in 50mm graphite jig that powder, which is added to and is coated with the internal diameter of boron nitride,；
2) by step 1) powder and mold be packed into hot pressing furnace in, closed furnace body vacuumizes, keep furnace in low pressure extremely
0.01Pa or less；
3) under room temperature state, apply the pressure of about 28MPa, pressure maintaining complete release after five minutes to mold；
4) in-furnace temperature is risen to 200 DEG C, under conditions of 200 DEG C, the pressure of 40MPa is applied to mold and pressure maintaining 5 divides
Complete release after clock；
5) in-furnace temperature is risen to 400 DEG C with the speed of 10 DEG C/min, at 400 DEG C, applies the pressure of 40MPa to mold
And pressure maintaining 5 minutes；
6) in step 5) after pressure maintaining period, cooled to room temperature discharges 8MPa's every 20 DEG C in temperature-fall period
Pressure is to complete release；
7) taking out the target prepared in step 6) to get diameter is 50mm, the Y that thickness is about 4mm0.25Sb1.75Te3Target
Material.
Embodiment 3
Prepare Sc0.25Sb1.75Te3Target
It 1) will about 54g Sc0.25Sb1.75Te3It is in 50mm graphite jig that powder, which is added to and is coated with the internal diameter of boron nitride,；
2) by step 1) powder and mold be packed into hot pressing furnace in, closed furnace body vacuumizes, keep furnace in low pressure extremely
0.01Pa or less；
3) under room temperature state, apply the pressure of about 28MPa, pressure maintaining complete release after five minutes to mold；
4) in-furnace temperature is risen to 200 DEG C, under conditions of 200 DEG C, the pressure of 40MPa is applied to mold and pressure maintaining 5 divides
Complete release after clock；
5) in-furnace temperature is risen to 400 DEG C with the speed of 10 DEG C/min, at 400 DEG C, applies the pressure of 40MPa to mold
And pressure maintaining 5 minutes；
6) in step 5) after pressure maintaining period, cooled to room temperature discharges 8MPa's every 20 DEG C in temperature-fall period
Pressure is to complete release；
7) taking out the target prepared in step 6) to get diameter is 50mm, the Sc that thickness is about 4mm0.25Sb1.75Te3Target
Material.
Claims (7)
1. the present invention relates to a kind of preparation methods of transient metal doped antimony telluride alloy target material, it is characterised in that directly use
Alloy powder carries out hot forming sintering.
2. a kind of preparation method of transient metal doped antimony telluride alloy target material as described in claim 1, it is characterised in that
The transition metal includes Sc, Y, Ti, Cr, Hg, Zn etc..
3. a kind of preparation method of transient metal doped antimony telluride alloy target material as described in claim 1, it is characterised in that
The following steps are included:
1) appropriate alloy powder is added in the graphite jig for being coated with boron nitride；
2) mold that powder is housed in step 1) is packed into hot pressing furnace, seals furnace body, vacuumizes, keep low pressure in furnace；
3) under room temperature state, apply 70% target, pressure, complete release after pressure maintaining 5-10 minutes to mold；
4) in-furnace temperature is risen to 200 DEG C, under conditions of 200 DEG C, after applying target, pressure and pressure maintaining 5-10 minutes to mold
Complete release；
5) in-furnace temperature is risen to by target temperature T with the speed of 10 DEG C/min1, in T1At a temperature of, target, pressure is applied simultaneously to mold
Pressure maintaining 5-10 minutes；
6) in step 5) after pressure maintaining period, cooled to room temperature, every 20 DEG C of 20% target pressures of release in temperature-fall period
By force to complete release；
7) target prepared in step 6) is taken out to get alloy target material.
4. a kind of preparation method of transient metal doped antimony telluride alloy target material as claimed in claim 3, it is characterised in that
In step 1), the alloy powder dosage is about 54g and purity is 99% or more, and graphite jig internal diameter is 50mm.
5. a kind of preparation method of transient metal doped antimony telluride alloy target material as claimed in claim 3, it is characterised in that
In step 3), the target, pressure is that graphite jig can bear maximum pressure, about 40MPa.
6. a kind of preparation method of transient metal doped antimony telluride alloy target material as claimed in claim 3, it is characterised in that
In step 4), the dwell time is 5 minutes.
7. a kind of preparation method of transient metal doped antimony telluride alloy target material as claimed in claim 3, it is characterised in that
In step 5), the target temperature T1For 0.7Tm(TmFor alloy powder fusing point), the dwell time is 5 minutes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811177004.1A CN109226768A (en) | 2018-10-09 | 2018-10-09 | A kind of preparation method of transient metal doped antimony telluride alloy target material |
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| CN201811177004.1A CN109226768A (en) | 2018-10-09 | 2018-10-09 | A kind of preparation method of transient metal doped antimony telluride alloy target material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110635033A (en) * | 2019-10-11 | 2019-12-31 | 东华大学 | A kind of B-Sb-Te phase change material, phase change memory unit and preparation method thereof |
| CN112786781A (en) * | 2021-01-05 | 2021-05-11 | 东华大学 | Superhard Re element composite Re-Sb-Te phase change material and application thereof |
| CN116079055A (en) * | 2023-02-08 | 2023-05-09 | 苏州六九新材料科技有限公司 | CrAlFe-based alloy target and preparation method thereof |
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| CN101522940A (en) * | 2006-10-13 | 2009-09-02 | 日矿金属株式会社 | Sb-Te base alloy sinter sputtering target |
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Patent Citations (5)
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| JP2005294538A (en) * | 2004-03-31 | 2005-10-20 | Yamaha Corp | Thermoelectric element, manufacturing method thereof and thermoelectric module |
| CN101103134A (en) * | 2005-01-18 | 2008-01-09 | 日矿金属株式会社 | Sb-Te alloy powder for sintering, method for producing the same, and sintered sputtering target obtained by sintering the powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110635033A (en) * | 2019-10-11 | 2019-12-31 | 东华大学 | A kind of B-Sb-Te phase change material, phase change memory unit and preparation method thereof |
| CN112786781A (en) * | 2021-01-05 | 2021-05-11 | 东华大学 | Superhard Re element composite Re-Sb-Te phase change material and application thereof |
| CN112786781B (en) * | 2021-01-05 | 2022-09-27 | 东华大学 | Superhard Re element composite Re-Sb-Te phase change material and application thereof |
| CN116079055A (en) * | 2023-02-08 | 2023-05-09 | 苏州六九新材料科技有限公司 | CrAlFe-based alloy target and preparation method thereof |
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