CN103572228A - Method for manufacturing high vapor pressure chalcogen alloy block - Google Patents
Method for manufacturing high vapor pressure chalcogen alloy block Download PDFInfo
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- CN103572228A CN103572228A CN201310302226.2A CN201310302226A CN103572228A CN 103572228 A CN103572228 A CN 103572228A CN 201310302226 A CN201310302226 A CN 201310302226A CN 103572228 A CN103572228 A CN 103572228A
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
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Images
Abstract
The invention relates to a method for manufacturing a high vapor pressure chalcogen alloy block. Preparing 0.5-30 atomic percent of chalcogen (one of gallium, indium, thallium, germanium, tin, lead, antimony, bismuth, selenium, tellurium or polonium) and the rest atomic percent of metal element raw materials in a predetermined atomic percent, placing the raw materials in a ceramic container for vacuum smelting operation, forcibly cooling the obtained alloy molten soup by gas or liquid, cooling, solidifying and molding the alloy molten soup into a casting blank, crushing the casting blank into alloy powder, sieving the alloy powder to obtain uniform alloy powder, and finally performing cold press molding and hot press sintering to obtain the block alloy; thus, an alloy block having a high purity of 99% or more, a controlled composition difference of + -1%, fine crystal grains, and a density of 90% or more is produced.
Description
Technical field
The present invention is relevant for a kind of manufacture method of high vapour pressure chalcogen alloy cube matherial, refer in particular to the manufacture method of the uppity chalcogen alloy cube matherial of a kind of composition accuracy, under vacuum state, for the alloy that includes chalcogen, carry out melting, be prepared into again Powdered and by consolidation sintering, make possess correct composition, high evenness, crystal grain are careful, the manufacture method of high purity, high-compactness bulk.
Background technology
Vacuum metal film plating (vacuum metallization, VM) refer to metal alloy bulk target under vacuum condition, use the specific means such as chemistry, physics to carry out organic conversion, make metal targets convert molecular particle to, deposit or be adsorbed on the surface of plastic cement or metallic substance, form metallic film, the plated film that namely we are commonly called as; And because alloy coating has excellent wear resistance, solidity to corrosion, thickness of coating homogeneity, compactness high, the technique that has been widely used in various electronic products, and along with electronic industry develop rapidly and the lifting of photovoltaic technique yield under, also more and more higher to the requirement of coating technique.
The sputtering method (sputtering) of take in coating technique is example, and sputtering method is one of gas phase deposition technology for thin film deposition of extensively knowing; This method is used for used in electronic industry thin film deposition; Its principle is under the environment of glow discharge, utilizes the mode of momentum transfer, is placed in the target of negative electrode with ion bombardment, and target atom is sputtered out and be deposited on substrate; Sputtered target material can be used on the wiring film of formation liquid crystal panel that TV, PC, indicating meter, other indicating meter use, organic electroluminescence panel etc., the formation of wiring film of the reflectance coating in optical recording field, recording film, semiconductor applications etc.
Generally speaking, can be used as the alloy manufacture method that target is used, its step is as follows: first, by alloying element, raw materials such as aluminium, copper, nickel, silver, titanium, magnesium, manganese, zinc, indium, tin, chromium, is complying with after demand percentage weighing, puts in smelting pot; Afterwards, in atmosphere, heating makes ingot casting fuse into uniform alloy soup completely; Then, will melt soup and pour in mold and become ingot, in cooling rear taking-up; Finally, more for example forge, heat is cold rolling, and the heat-treatment processing process such as high temperature annealing, so that alloy interior tissue homogenizes (homogenized), afterwards again with mechanical workout, makes required shape; But, when above-mentioned alloy manufacture method is implemented to use in reality, there is following disappearance: (a) melting is to carry out in atmosphere, if the fusing point of the element in alloy lower (being that 232 ℃, the fusing point of indium are 157 ℃ etc. such as: the fusing point of tin), and vapour pressure is higher, causes easily in melting technology, volatilizing, thereby the ratio of change alloy ingredient, even, with air generation oxidizing reaction, consequently cannot correctly control the aimed concn of alloy, cause the change of alloy material characteristic; (b) often there is composition skewness in melting casting process, causes the problem of segregation (segregation) to occur, and the high temperature properties of alloy has serious impact, and then reduce the reliability of alloy under hot environment; And (c) oxidation activity of some elements (such as chromium, titanium, silicon etc.) when high temperature is very big, make in melting in air process, very easily with take the crucible that magnesium oxide, aluminum oxide etc. are main material and produce chemical reaction, not only corrode the material of crucible, even and then affect purity and the quality of made alloy; In addition, above-mentioned alloy manufacture method is mainly the technique developing for transition metal.
And in the periodic table of elements, at the right-hand element between transition metal and elemental gas of periodictable, its character between metal and nonmetal between, these elements are referred to as chalcogen, comprising: gallium (Ga, 30 ℃ of fusing points), indium (In, 115 ℃ of fusing points), thallium (Tl, 303 ℃ of fusing points), germanium (Ge, 937 ℃ of fusing points), tin (Sn, 232 ℃ of fusing points), plumbous (Pb, 328 ℃ of fusing points), antimony (Sb, 631 ℃ of fusing points), bismuth (Bi, 271 ℃ of fusing points), selenium (Se, 217 ℃ of fusing points), the element such as tellurium (Te, 450 ℃ of fusing points), polonium (Po, 254 ℃ of fusing points); The feature of these elements is that fusing point is low above, therefore often there is special phase transformation step response, use in fields such as recording medium, mutually abnormal memory body, solar electrical energy generations in a large number, but also because its alloy configuration composition must be controlled precisely, and these because of metal vapour pressures are high simultaneously, therefore be very easy to scatter and disappear in a large number in fusion process, cause concentration and target component to produce the significantly problem of difference.
Summary of the invention
For solving the problems of the technologies described above, main purpose of the present invention is to provide the manufacture method of the uppity chalcogen alloy cube matherial of a kind of composition accuracy, under vacuum state, for the alloy that includes chalcogen, carry out melting, then be prepared into Powdered and by consolidation sintering to make, possess correct composition, high evenness, crystal grain are careful, the manufacture method of high purity, high-compactness bulk.
In order to reach above-mentioned enforcement object, the present invention proposes a kind of manufacture method of high vapour pressure chalcogen alloy cube matherial, at least comprise the following steps: first, preparation includes the chalcogen of 0.5-30 atomic percent, chalcogen is a kind of in gallium, indium, thallium, germanium, tin, lead, antimony, bismuth selenium tellurium or polonium element, and the metallic element raw material of residue atomic percent; Continue, above-mentioned all raw materials are all seated in and in earthenware porcelain receptacle, carry out vacuum melting operation; Then, the molten soup of the alloy of vacuum melting operation gained is cooling with gas or liquid pressure, make the molten soup cooled and solidified of alloy be shaped to casting embryo; Afterwards, with shredding unit, will cast embryo pulverizes or with powder spraying apparatus, makes powdered alloy; Then, powdered alloy is sieved with screen cloth, obtain the uniform uniform alloy powder of powder diameter; Finally, uniform alloy powder, sequentially through coldmoulding and hot pressing or hot pressing processing of all pressing sintering, is made to high vapour pressure chalcogen alloy cube matherial; Afterwards, block alloy cube matherial can be done secondary mechanical processing treatment according to actual need to further inserting in facility of using, to meet the demands such as required plated film target shape, size.
In addition, when preparing raw material, comprise cleaning, namely by oxide compound and the oil removal on prepared chalcogen and raw metal surface, and the raw material through this cleaning is prepared according to predetermined atomic percent, make the alloy ingredient making meet predetermined atomic percent.
The manufacture method of high vapour pressure chalcogen alloy cube matherial as above, preferred, the purity of the chalcogen raw material of preparing is more than 99.9%.
The manufacture method of high vapour pressure chalcogen alloy cube matherial as above, preferably, in earthenware porcelain receptacle, carrying out vacuum melting operation by vacuum unit (for example: the vacuum induction furnace of prior art) earthenware porcelain receptacle is pumped into the vacuum state below 0.1torr, is then passed into argon gas and make the vacuum pressure of earthenware porcelain receptacle maintain 200-600torr is; Afterwards, earthenware porcelain receptacle is inserted in well heater, temperature is heated to 800 ℃-1100 ℃, and earthenware porcelain receptacle is placed in it and continued 1～5 minute.
The manufacture method of high vapour pressure chalcogen alloy cube matherial as above, preferred, shredding unit is jaw crusher, by jaw crusher, will cast the broken granulation of embryo.
The manufacture method of high vapour pressure chalcogen alloy cube matherial as above, preferred, screen cloth is selected from 100 above meshes (mesh), makes the powder diameter of the uniform alloy powder after filtering be not more than 150 μ m.
The manufacture method of high vapour pressure chalcogen alloy cube matherial as above, preferably, the pressing processing operation of uniform alloy powder is, in vacuum oven, uniform alloy powder filling is carried out to pressing processing at graphite jig, and graphite jig both sides are provided with provides the heat pipe of thermal source row, press binding device is the uniform alloy powder in graphite jig with the pressure pressing of 50-100MPa, now, heat pipe row is heated to 300 ℃-700 ℃ by graphite jig, press binding device continued to exert pressure after 1～3 hour, can make a high purity, high vapour pressure alloy cube matherial.
Therefore, the present invention and prior art are in comparison, the manufacture method of high vapour pressure chalcogen alloy cube matherial provided by the invention is in the earthenware porcelain receptacle under vacuum state, to carry out melting operation, not only can effectively prevent raw material wherein in high melt process with air generation oxidizing reaction, except increasing technology stability, also can improve the problem of low melting point metal volatilization dissipation, make alloy ingredient can be controlled in ± 1% between; In addition by the casting embryo of vacuum melting operation gained, be to be broken into powdered alloy with jaw crusher,, through screen cloth, sieve so that powder diameter is even again, and become alloy cube matherial with hot pressed sintering, and make its composition uniformity high, can avoid single composition segregation problem being produced with melting casting in traditional technology.
And, by earthenware porcelain receptacle, under vacuum state, carry out the melting operation of alloy, in comparison, can avoid in fusion process with the technology by crucible for smelting in traditional technology, alloy ingredient and crucible produce chemical reaction, make the present invention can make the alloy cube matherial of higher degree.
The manufacture method of high vapour pressure chalcogen alloy cube matherial provided by the invention, by existing vacuum induction furnace, can in earthenware porcelain receptacle, carry out extracting vacuum and melting operation, need not design new process unit or buy more high production unit, can significantly reduce manufacturing cost.
Accompanying drawing explanation
Fig. 1 is the manufacture method flow chart of steps of the high vapour pressure chalcogen alloy cube matherial of preferred embodiment of the present invention;
Fig. 2 is that the view of vacuum melting is carried out in preferred embodiment of the present invention in earthenware porcelain receptacle;
Fig. 3 is that preferred embodiment of the present invention is ground into casting embryo with shredding unit the view of powdered alloy;
Fig. 4 is that preferred embodiment of the present invention is made into the pressing of uniform alloy powder the view of alloy cube matherial under vacuum oven.
Main element nomenclature:
1 earthenware porcelain receptacle 2 well heaters
3 shredding unit 4 press binding devices
5 graphite jig 51 heat pipe rows
6 vacuum oven S1 step 1
S2 step 2 S3 step 3
Embodiment
Advantage in object of the present invention and structure function thereof, will, according to structure shown in the drawings, coordinate specific embodiment to be explained, for making people have more deep and concrete understanding to the present invention.
First, please refer to shown in Fig. 1, the flow chart of steps for the preferred embodiment of the manufacture method of high vapour pressure chalcogen alloy cube matherial of the present invention, mainly includes following steps:
Step 1 S1: the total raw material composition atomic percent with 100% calculates, preparation includes the chalcogen of 0.5-30 atomic percent, chalcogen is a kind of in gallium, indium, thallium, germanium, tin, lead, antimony, bismuth selenium tellurium or polonium element, and the metallic element raw material of residue atomic percent; The purity of the chalcogen raw material of wherein, preparing is more than 99.9%; In addition, when step 1 S1 prepares raw material, comprise cleaning, namely by oxide compound and the oil removal on prepared chalcogen and raw metal surface, and the raw material through this cleaning is prepared according to predetermined atomic percent, make the alloy ingredient making meet predetermined atomic percent;
Step 2 S2: above-mentioned all raw materials are all seated in and carry out vacuum melting operation in earthenware porcelain receptacle 1; In the present embodiment, earthenware porcelain receptacle 1 is vitrified pipe, and by vacuum unit (for example: the vacuum induction furnace of prior art) earthenware porcelain receptacle 1 is pumped into the vacuum state below 0.1torr, then passes into argon gas and make the vacuum pressure of earthenware porcelain receptacle 1 maintain 200-600torr; Afterwards, earthenware porcelain receptacle 1 is inserted in well heater 2, refer to shown in Fig. 2, that the present embodiment carries out the view of vacuum melting in earthenware porcelain receptacle 1, well heater 2 is to utilize load coil at short notice temperature to be risen to 800 ℃-1100 ℃, and utilize inducedmagnetic field that the molten metal of melting is mixed completely, and by the accommodating 1-5 minute that continues in it of earthenware porcelain receptacle 1; Accordingly, not only can effectively prevent raw material wherein in high melt process with air generation oxidizing reaction, except increasing technology stability, also can improve the problem of low melting point metal volatilization dissipation, make alloy ingredient can be controlled in ± 1% between;
Noticeable, should be appreciated that the manufacture method of the high vapour pressure chalcogen of the present invention alloy cube matherial and not only in the alloy product of making for plated film target, apply, in other purposes are also encompassed in; Principle of the present invention is to be used in to make all kinds of containing in chalcogen alloy product, therefore, does not limit the purposes of the obtained alloy cube matherial of above-described embodiment.
Claims (10)
1. a manufacture method for high vapour pressure chalcogen alloy cube matherial, it comprises the following steps:
Step 1: the total raw material composition atomic percent with 100% calculates, preparation includes the chalcogen of 0.5-30 atomic percent, this chalcogen is a kind of in gallium, indium, thallium, germanium, tin, lead, antimony, bismuth selenium tellurium or polonium element, and the metallic element raw material of residue atomic percent;
Step 2: described total raw material is all seated in and carries out vacuum melting operation in earthenware porcelain receptacle;
Step 3: the molten soup of the alloy of vacuum melting operation gained is cooling with gas or liquid pressure, make the molten soup cooled and solidified of described alloy be shaped to casting embryo;
Step 4: with shredding unit, described casting embryo is pulverized, made powdered alloy;
Step 5: described powdered alloy is sieved with screen cloth, obtain the consistent uniform alloy powder of powder diameter; And
Step 6: described uniform alloy powder, sequentially through the pressing processing of coldmoulding and hot pressed sintering, is made to high vapour pressure chalcogen alloy cube matherial.
2. the manufacture method of high vapour pressure chalcogen alloy cube matherial as claimed in claim 1, wherein, the purity of described chalcogen raw material is more than 99.9%.
3. the manufacture method of high vapour pressure chalcogen alloy cube matherial as claimed in claim 1, wherein, described step 2 is, by vacuum unit, earthenware porcelain receptacle is pumped into the vacuum state below 0.1torr, then passes into argon gas and makes the vacuum pressure of earthenware porcelain receptacle maintain 200-600torr.
4. the manufacture method of high vapour pressure chalcogen alloy cube matherial as claimed in claim 3, wherein, described vacuum unit is vacuum induction furnace.
5. the manufacture method of high vapour pressure chalcogen alloy cube matherial as claimed in claim 1, wherein, the melting technology of described step 2 is at the temperature of 800 ℃-1100 ℃, to continue 1-5 minute.
6. the manufacture method of high vapour pressure chalcogen alloy cube matherial as claimed in claim 1, wherein, the shredding unit of described step 4 is jaw crusher, by jaw crusher, granulates described casting embryo is broken.
7. the manufacture method of high vapour pressure chalcogen alloy cube matherial as claimed in claim 1, wherein, described step 5 is the screen filtration powdered alloy by 100 above meshes, makes the powder diameter of the uniform alloy powder after filtering be not more than 150 μ m.
8. the manufacture method of high vapour pressure chalcogen alloy cube matherial as claimed in claim 1, wherein, described step 6 is that uniform alloy powder filling is carried out to pressing processing at graphite jig, and the temperature of hot pressed sintering is that 300 ℃-700 ℃, pressure are 50-100MPa, and lasting 1-3 hour.
9. the manufacture method of high vapour pressure chalcogen alloy cube matherial as claimed in claim 1, wherein, when described step 1 is prepared raw material, comprise cleaning, this cleaning is by oxide compound and the oil removal on prepared chalcogen and raw metal surface, and the raw material through this cleaning is prepared according to predetermined atomic percent.
10. the manufacture method of high vapour pressure chalcogen alloy cube matherial as claimed in claim 1, wherein, after described step 6 completes, further inserts bulk alloy in facility and does secondary mechanical processing treatment, with the needs of realistic use.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TW101127653A TWI493047B (en) | 2012-07-31 | 2012-07-31 | Method for manufacturing alloy bulk material of sulfur-free chalcogenide elements with high vapor pressure |
| TW101127653 | 2012-07-31 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103572228A true CN103572228A (en) | 2014-02-12 |
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Citations (6)
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|---|---|---|---|---|
| WO2000031316A1 (en) * | 1998-11-20 | 2000-06-02 | Japan Energy Corporation | Co-Ti ALLOY SPUTTERING TARGET AND MANUFACTURING METHOD THEREOF |
| JP2003277923A (en) * | 2002-03-27 | 2003-10-02 | Sumitomo Metal Mining Co Ltd | Ge-Bi ALLOY TARGET FOR SPUTTERING AND PRODUCTION METHOD THEREOF |
| CN1978099A (en) * | 2005-12-07 | 2007-06-13 | 中国电子科技集团公司第十八研究所 | PbTe powde material formation preparing method |
| CN101042903A (en) * | 2002-02-25 | 2007-09-26 | 日矿金属株式会社 | Method for producing sputtering target for phase-change memory |
| JP2012072467A (en) * | 2010-09-29 | 2012-04-12 | Sumitomo Metal Mining Co Ltd | Cu-Ga ALLOY SPUTTERING TARGET AND METHOD FOR MANUFACTURING Cu-Ga ALLOY SPUTTERING TARGET |
| CN102534278A (en) * | 2010-12-28 | 2012-07-04 | 北京有色金属研究总院 | Sleeve forging and pressing preparation method of bismuth-telluride-base thermoelectric material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100108503A1 (en) * | 2008-10-31 | 2010-05-06 | Applied Quantum Technology, Llc | Chalcogenide alloy sputter targets for photovoltaic applications and methods of manufacturing the same |
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- 2013-07-18 CN CN201310302226.2A patent/CN103572228A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000031316A1 (en) * | 1998-11-20 | 2000-06-02 | Japan Energy Corporation | Co-Ti ALLOY SPUTTERING TARGET AND MANUFACTURING METHOD THEREOF |
| CN101042903A (en) * | 2002-02-25 | 2007-09-26 | 日矿金属株式会社 | Method for producing sputtering target for phase-change memory |
| JP2003277923A (en) * | 2002-03-27 | 2003-10-02 | Sumitomo Metal Mining Co Ltd | Ge-Bi ALLOY TARGET FOR SPUTTERING AND PRODUCTION METHOD THEREOF |
| CN1978099A (en) * | 2005-12-07 | 2007-06-13 | 中国电子科技集团公司第十八研究所 | PbTe powde material formation preparing method |
| JP2012072467A (en) * | 2010-09-29 | 2012-04-12 | Sumitomo Metal Mining Co Ltd | Cu-Ga ALLOY SPUTTERING TARGET AND METHOD FOR MANUFACTURING Cu-Ga ALLOY SPUTTERING TARGET |
| CN102534278A (en) * | 2010-12-28 | 2012-07-04 | 北京有色金属研究总院 | Sleeve forging and pressing preparation method of bismuth-telluride-base thermoelectric material |
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| Publication number | Publication date |
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| TW201404892A (en) | 2014-02-01 |
| TWI493047B (en) | 2015-07-21 |
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