CN101748313A - Zinc-lithium alloy material and preparation method thereof - Google Patents
Zinc-lithium alloy material and preparation method thereof Download PDFInfo
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- CN101748313A CN101748313A CN200810239842A CN200810239842A CN101748313A CN 101748313 A CN101748313 A CN 101748313A CN 200810239842 A CN200810239842 A CN 200810239842A CN 200810239842 A CN200810239842 A CN 200810239842A CN 101748313 A CN101748313 A CN 101748313A
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Abstract
The invention discloses a zinc-lithium alloy material and a preparation method thereof. The content of lithium is 0.5-4.0% (by mass) in the zinc-lithium alloy material and the balance is Zn. The invention also discloses a technology of producing plasma sputtering target materials used in the silicon chip of an integrated circuit. The preparation method of the zinc-lithium alloy comprises the following steps: weighing high purity lithium and high purity zinc with the content of lithium 10-20% higher than the required ratio; putting the zinc into a high purity graphite crucible, putting the crucible into a vacuum furnace, wrapping the lithium with high purity zinc foil and placing the wrapped lithium into the feed hopper of the vacuum furnace; vacuum pumping; raising the temperature to 450-500 DEG C to melt the zinc; filling argon; adding the high purity lithium and refining for 10-15 minutes at the temperature of 600-650 DEG C; and casting to obtain the zinc-lithium alloy material.
Description
Technical field
The present invention relates to the metal alloy technology of preparing, relate in particular to a kind of zinc-Zinc-lithium alloy material and preparation method thereof, and the technology of using this kind alloy production target.
Background technology
The zinc alloy target is used for large-scale integrated circuit silicon chip plasma sputtering, is the critical material that highly reliable unicircuit and device are made.
The general method for preparing zinc alloy is under vacuum or antivacuum state, all alloying elements is placed on sequentially carries out alloying in the crucible.But lithium is a kind of low melting point metal, chemical property is very active, the rapid oxidation of meeting in air, can react with the crucible material that major part is used always in molten state, and in the process of melting, cause oxidation, scaling loss serious owing to lithium can absorb oxygen in the melt in a large number, have influence on it and in metal, form alloy.Adopt the conventional method for preparing alloy not only to can not get the high-content lithium alloy, and cause environmental pollution easily.Just might prepare the alloy material of high-content lithium so must adopt new technology.
Summary of the invention
An object of the present invention is to provide a kind of zinc-Zinc-lithium alloy material, wherein the shared quality of lithium is 0.5-4.0%, and this content satisfies the scope that the very high performance integrated circuit silicon chip requires of making.
Another object of the present invention provides the preparation method of above-mentioned zinc-Zinc-lithium alloy material, and it utilizes improved doping techniques, the lithium of low melting point, easily oxidation can be joined in the alloy, prepares the zinc-Zinc-lithium alloy material of higher li content.
Another purpose of the present invention provides a kind of sputtering target material that is used for the integrated circuit silicon chip plasma sputtering.
A further object of the present invention provides the above-mentioned preparation method who is used for the sputtering target material of integrated circuit silicon chip plasma sputtering.
For achieving the above object, the present invention takes following technical scheme:
A kind of zinc-lithium alloy, its composition and mass percent are Li:0.5-4.0%, Zn: surplus.
The preparation method of above-mentioned zinc-lithium alloy, it comprises the steps:
A, be 0.5-4.0% by the mass percent of Li, Zn is the proportioning of the surplus starting material of weighing, purity 〉=5N of Li wherein, and part Zn is the form of zinc paper tinsel, purity 〉=5N;
B, usefulness zinc paper tinsel parcel lithium, and put it in the loading hopper of vacuum oven; The zinc of remainder is put into the high purity graphite crucible, crucible is put into vacuum oven;
C, be evacuated to 100～200Pa;
D, be warming up to 450-500 ℃, make the zinc fusing;
E, in vacuum oven applying argon gas to the 0.8-1 normal atmosphere;
F, adding lithium;
G, control melt temperature make it not be higher than 550-700 ℃, zinc concentrate-lithium melt 10-15 minute;
H, solution watered cast from the water cooled copper mould, obtain zinc-Zinc-lithium alloy material.
A kind of zinc-lithium alloy sputtering target material, it is to be processed into above-mentioned zinc-lithium alloy.
The manufacture method of above-mentioned zinc-lithium alloy sputtering target material, it comprises the steps:
A, press working:
Use above-mentioned zinc-lithium alloy of the present invention as raw material, lithium content carries out cold pressure processing at normal temperatures at the alloy cast ingot of 0.5-1.0%, and it is extended to meeting the alloy sheets of thickness requirement; Lithium content is in the alloy cast ingot of 1.0-4.0% thermal pressure working method, and temperature is between 120 ℃-300 ℃, and this temperature increases with the raising of lithium content, and it is extended to meeting the alloy sheets of thickness requirement;
B, machining:
The alloy sheets that above-mentioned press working is crossed is carried out turnning and milling according to needed size;
C, surface treatment:
Above-mentioned mach alloy material is cleaned by immersion and/or paddling process with acidic cleaning solution, remove the pollution that causes in the course of processing, make material surface cleaning, light.
The manufacture method of above-mentioned zinc-lithium alloy sputtering target material, wherein, this acidic cleaning solution can be nitric acid, sulfuric acid or the hydrochloric acid soln of 1-2 for pH.
Beneficial effect of the present invention is, mixes technology by improvement, has solved the difficult problem of elemental lithium interpolation in the alloy, and lithium content height, even, the compact structure of composition can be used for the integrated circuit silicon chip sputtering target material in the zinc-lithium alloy of preparation.Preparation process of the present invention is environment friendly and pollution-free simultaneously.
Embodiment
Embodiment 1: the preparation lithium content is zinc-lithium alloy of 0.52%
Preparation technology is as follows:
1) by the proportioning that the mass percent of lithium is 0.6%, zinc the is surplus starting material of weighing, purity 〉=5N of Zn wherein, purity 〉=5N of Li;
2) zinc is put into the high purity graphite crucible, then crucible is put into vacuum oven; (purity 〉=5N) wrap up is put into the vacuum oven loading hopper with the high purity zinc paper tinsel with lithium;
3) be evacuated to 170Pa;
4) be warming up to 490 ℃, make the zinc fusing;
5) applying argon gas in vacuum oven, applying argon gas to 0.95 normal atmosphere;
6) add lithium;
7) control melt temperature makes it not be higher than 600 ℃ of zinc concentrates-lithium melt 10 minutes;
8) water and cast from the water cooled copper mould.
Use the icp analysis instrument to carry out composition analysis, the composition mass percent of prepared zinc-lithium alloy is a lithium 0.52%, and zinc is surplus.
Embodiment 2: preparation zinc-lithium alloy sputtering target material
Utilize embodiment 1 prepared zinc-lithium alloy to prepare sputtering target material, method is as follows:
Zinc-lithium alloy ingot casting that embodiment 1 is obtained is heated to 130 ℃ with box type heater, be incubated after 1 hour, it is about 40% that milling train is rolled the rolling amount of finish in back, with thermocompressor it flattened, it is identical with rolling temperature to flatten temperature, and it is extended to is of a size of 260mm * 240mm * 10mm.The alloy ingot blank that press working is good is carried out turnning and milling according to needed dimensional standard, forms sputtering target material;
With pH is that 1.5 hydrochloric acid solns clean by infusion method and paddling process, removes the pollution that causes in the course of processing, makes sputtering target material cleaning surfaces, light, overcomes the problem that target in use is difficult for build-up of luminance (arc).
Embodiment 3: the preparation lithium content is zinc-lithium alloy of 3.07%
Preparation technology is as follows:
1) by the proportioning that the mass percent of lithium is 3.50%, zinc the is surplus starting material of weighing, purity 〉=5N of Zn wherein, purity 〉=5N of Li;
2) zinc is put into the high purity graphite crucible, then crucible is put into vacuum oven; Lithium with high purity zinc paper tinsel parcel, is put into the vacuum oven loading hopper.
3) be evacuated to 190Pa;
4) be warming up to 480 ℃, make the zinc fusing;
5) applying argon gas in vacuum oven, applying argon gas to 0.9 normal atmosphere;
6) add lithium;
7) the control melt temperature changes, and makes it not be higher than 650 ℃ of zinc concentrates-lithium melt 10 minutes;
8) water and cast from the water cooled copper mould.
Use the icp analysis instrument to carry out composition analysis, the composition mass percent of prepared zinc-lithium alloy is a lithium 3.07%, and zinc is surplus.
Embodiment 4: preparation zinc-lithium alloy sputtering target material
Utilize embodiment 3 prepared zinc-lithium alloys to prepare sputtering target material, method is as follows:
Zinc-lithium alloy ingot casting that embodiment 3 is obtained is heated to 260 ℃ with box type heater, is incubated after 1 hour, is rolled rolling amount of finish about 30% with milling train.Then, with thermocompressor it is flattened, it is identical with rolling temperature to flatten temperature, and it is extended to is of a size of 240mm * 240mm * 8mm.The complete alloy ingot blank that press working is good is carried out turnning and milling according to needed dimensional standard, forms sputtering target material;
With pH is that 1.5 hydrochloric acid solns clean by infusion method and paddling process, removes the pollution that causes in the course of processing, makes sputtering target material cleaning surfaces, light, overcomes the problem that target in use is difficult for build-up of luminance (arc).
Claims (5)
1. a zinc-lithium alloy is characterized in that, its composition and mass percent are Li:0.5-4.0%, Zn: surplus.
2. the preparation method of the described zinc-lithium alloy of claim 1 is characterized in that, comprises the steps:
A, be 0.5-4.0% by the mass percent of Li, Zn is the proportioning of the surplus starting material of weighing, purity 〉=5N of Li wherein, and part Zn is the form of zinc paper tinsel, purity 〉=5N;
B, usefulness zinc paper tinsel parcel lithium, and put it in the loading hopper of vacuum oven; The zinc of remainder is put into the high purity graphite crucible, crucible is put into vacuum oven;
C, be evacuated to 100～200Pa;
D, be warming up to 450-500 ℃, make the zinc fusing;
E, in vacuum oven applying argon gas to the 0.8-1 normal atmosphere;
F, adding lithium;
G, control melt temperature be at 550-700 ℃, zinc concentrate-lithium melt 10-15 minute;
H, solution watered cast from the water cooled copper mould, obtain zinc-Zinc-lithium alloy material.
3. zinc-lithium alloy sputtering target material that is used for the integrated circuit silicon chip plasma sputtering, it is characterized in that: it is to be processed into the described zinc-lithium alloy of claim 1.
4. the manufacture method of the described zinc of claim 3-lithium alloy sputtering target material is characterized in that, comprises the steps:
A, press working:
Use the described zinc-lithium alloy of claim 1 as raw material, lithium content carries out cold pressure processing at normal temperatures at the alloy cast ingot of 0.5-1.0%, and it is extended to meeting the alloy sheets of thickness requirement; Lithium content is in the alloy cast ingot of 1.0-4.0% thermal pressure working method, and temperature extends it for meeting the alloy sheets of thickness requirement between 120 ℃-300 ℃;
B, machining:
The alloy sheets that above-mentioned press working is crossed is carried out turnning and milling according to needed size;
C, surface treatment:
Above-mentioned mach alloy material is cleaned by immersion and/or paddling process with acidic cleaning solution, remove the pollution that causes in the course of processing, make material surface cleaning, light.
5. according to the manufacture method of the described zinc of claim 4-lithium alloy sputtering target material, it is characterized in that described acidic cleaning solution is that pH is 1～2 nitric acid, sulfuric acid or hydrochloric acid soln.
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| CN200810239842A CN101748313A (en) | 2008-12-19 | 2008-12-19 | Zinc-lithium alloy material and preparation method thereof |
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| CN200810239842A CN101748313A (en) | 2008-12-19 | 2008-12-19 | Zinc-lithium alloy material and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104451261A (en) * | 2013-09-24 | 2015-03-25 | 兆阳真空动力股份有限公司 | Target material of anti-electromagnetic wave interference alloy film |
| CN105229179A (en) * | 2013-04-12 | 2016-01-06 | 本田技研工业株式会社 | The manufacture method of zinc alloy |
| CN105349952A (en) * | 2015-11-09 | 2016-02-24 | 基迈克材料科技（苏州）有限公司 | Manufacturing method for casting metal lithium target |
| CN106282664A (en) * | 2016-08-25 | 2017-01-04 | 上海交通大学 | Biodegradable medical zinc lithium binary alloy material and preparation method and application |
| CN107460371A (en) * | 2016-06-02 | 2017-12-12 | 北京大学 | A kind of Zn-Li systems kirsite and preparation method and application |
| CN108463897A (en) * | 2015-11-10 | 2018-08-28 | 诺瓦尔德股份有限公司 | Include the N-shaped doped semiconductor materials of two kinds of metal dopants |
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2008
- 2008-12-19 CN CN200810239842A patent/CN101748313A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105229179A (en) * | 2013-04-12 | 2016-01-06 | 本田技研工业株式会社 | The manufacture method of zinc alloy |
| CN104451261A (en) * | 2013-09-24 | 2015-03-25 | 兆阳真空动力股份有限公司 | Target material of anti-electromagnetic wave interference alloy film |
| CN105349952A (en) * | 2015-11-09 | 2016-02-24 | 基迈克材料科技（苏州）有限公司 | Manufacturing method for casting metal lithium target |
| CN108463897A (en) * | 2015-11-10 | 2018-08-28 | 诺瓦尔德股份有限公司 | Include the N-shaped doped semiconductor materials of two kinds of metal dopants |
| US10811608B2 (en) | 2015-11-10 | 2020-10-20 | Novaled Gmbh | N-doped semiconducting material comprising two metal dopants |
| CN108463897B (en) * | 2015-11-10 | 2021-01-29 | 诺瓦尔德股份有限公司 | N-type doped semiconductor material comprising two metal dopants |
| CN107460371A (en) * | 2016-06-02 | 2017-12-12 | 北京大学 | A kind of Zn-Li systems kirsite and preparation method and application |
| CN107460371B (en) * | 2016-06-02 | 2019-01-22 | 北京大学 | A kind of Zn-Li system kirsite and the preparation method and application thereof |
| CN106282664A (en) * | 2016-08-25 | 2017-01-04 | 上海交通大学 | Biodegradable medical zinc lithium binary alloy material and preparation method and application |
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Application publication date: 20100623 |