CN101469407B - Sputtering equipment with close packing tip anode - Google Patents
Sputtering equipment with close packing tip anode Download PDFInfo
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- CN101469407B CN101469407B CN2007103045555A CN200710304555A CN101469407B CN 101469407 B CN101469407 B CN 101469407B CN 2007103045555 A CN2007103045555 A CN 2007103045555A CN 200710304555 A CN200710304555 A CN 200710304555A CN 101469407 B CN101469407 B CN 101469407B
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- 238000012856 packing Methods 0.000 title claims abstract description 87
- 238000004544 sputter deposition Methods 0.000 title claims abstract description 44
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 238000005477 sputtering target Methods 0.000 claims abstract description 23
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 17
- 239000001301 oxygen Substances 0.000 claims abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000013077 target material Substances 0.000 claims description 20
- 239000011159 matrix material Substances 0.000 claims description 16
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 239000004020 conductor Substances 0.000 claims description 4
- 239000007769 metal material Substances 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 17
- 238000000034 method Methods 0.000 abstract description 14
- 229910021521 yttrium barium copper oxide Inorganic materials 0.000 abstract description 14
- 239000002184 metal Substances 0.000 abstract description 11
- 229910052751 metal Inorganic materials 0.000 abstract description 11
- 238000010849 ion bombardment Methods 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 8
- 238000010923 batch production Methods 0.000 abstract 1
- 239000010409 thin film Substances 0.000 description 11
- 239000010408 film Substances 0.000 description 9
- 239000000758 substrate Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 6
- -1 oxygen ion Chemical class 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000005555 metalworking Methods 0.000 description 2
- 239000003870 refractory metal Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 241000954177 Bangana ariza Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 208000002925 dental caries Diseases 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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Abstract
The invention provides a sputtering apparatus with a close packing tip anode. The sputtering apparatus is provided with a vacuum pipeline and an air feeding pipeline on a sputtering cavity body, and the sputtering cavity body is provided with a sputtering target and a heating body inside, wherein the close packing tip anode is arranged between the sputtering target and a sample and takes metal as a basal body, the middle part of the close packing tip anode is hollow, the edge at the inner side of the hollowed-out part is formed by arranging and connecting a plurality of tip bodies continuously, and the tip of each tip body faces the middle part of the hollowed-out part which is opposite to the sputtering target. The sputtering apparatus with the close packing tip anode can be applied to plane target sputtering to prepare an YBCO film material in batch production, greatly removes the influence of the negative oxygen ion bombardment, and meets the requirements on the speed of batch preparation and a process window.
Description
Technical field
The present invention relates to a kind of sputtering equipment, particularly the sputtering equipment of when large size plane oxidation thing target carries out film, coating preparation, using with close packing tip anode with close packing tip anode.
Background technology
Method with sputter (magnetron sputtering) prepares the complex oxide thin-film material, as RE, Ba and Cu oxide etc., is subjected to having a strong impact on of negative oxygen ion reverse sputtering (or claiming the negative oxygen ion bombardment) easily, causes the inhomogeneous of thin film composition and structure.For RE, Ba and Cu oxide ReBa
2Cu
3O
7-δ(ReBCO, as YBCO) etc. the high-temperature superconductor thin-film material, thin film composition must satisfy Re: Ba: Cu=1: 2: 3 proportionlity, could satisfy performance demands such as high transition temperature, high critical current densities, the influence of therefore removing the negative oxygen ion bombardment prepares above-mentioned film to sputtering method and is and important.When particularly adopting the planar targets sputter to prepare film, thin film composition, performance and surface topography are subjected to the influence of negative oxygen ion reverse sputtering even more serious.Technology is in the past addressing the above problem, and has adopted much and has improved one's methods.As adopt off-axis sputtering or off-axis sputtering, using planar target to prepare film; A kind of special scheme is: adopt rewinding cylinder target as sputter, in whole sputter area, be in plumbness between target and the substrate so always.In the various piece of whole circumference direction, target is in off-axis sputtering state (off-axis), so just can be reduced to gratifying degree to the effect of negative oxygen ion bombardment.
Adopt the hollow barrel-type target to carry out off-axis sputtering, though can greatly eliminate negative oxygen ion bombardment influence, but the sputtering yield of hollow barrel-type target is more much lower than planar targets, therefore can't satisfy the requirement of mass preparation, has greatly limited the cost of material preparation.If can carry out the sputter preparation by the using planar target, then want much economical, but must solve negative oxygen ion bombardment problem in mass sputter preparation.
Summary of the invention
The object of the present invention is to provide a kind of sputtering equipment with close packing tip anode, be a kind ofly can be applied to the sputtering equipment that planar target sputter mass prepares the ybco film material, by loading a kind of anode of close packing tip, greatly eliminate the influence of negative oxygen ion bombardment, satisfy the speed and the process window requirement of mass preparation.
For achieving the above object, the present invention takes following technical scheme:
A kind of sputtering equipment with close packing tip anode, this sputtering equipment is to be provided with vacuum-lines, admission passage on the sputter cavity, and in the sputter cavity, be provided with sputtering target material, heating member, between described sputtering target material and sample, be provided with close packing tip anode, this close packing tip anode is as matrix with metal, its middle part hollow out, the inside edge of openwork part is to be arranged continuously by several tip bodies to be formed by connecting, and the tip of each tip body is towards the middle part of openwork part, and its openwork part is relative with sputtering target material.
Close packing tip anode of the present invention at first will guarantee the good conductor characteristic of matrix, particularly should adapt with the processing condition of oxide compound preparation.Consider that the HTS YBCO film is preparation for a long time under 700 ℃～900 ℃ hot conditions, therefore should stand 700 ℃～900 ℃ pyritous as the metallic substance of matrix tests for a long time, guarantee not take place under the high temperature oxidation condition oxidation simultaneously, do not change metallic conductor character, under the said temperature environment, under the condition below the oxygen pressure 100Pa, significant oxidation does not take place promptly.Therefore as the matrix adopting of anode material metallic substance such as high temperature resistant stainless steel.
Why close packing tip anode of the present invention adopts cutting-edge structure, because following benefit is arranged: the negative oxygen ion that produces in the sputter procedure is mainly derived from the YBCO oxide target material.Because the existence of active metal makes target can't adopt metal alloy to carry out in the mode of reactive sputtering in the composition.Therefore, can only adopt the oxide ceramics target for preparing, has superperformance.In the process of Ar ion bombardment target, high-octane bombardment causes the O bond rupture, absorbs high-octane oxonium ion to move to the substrate direction at a high speed.Because O
2-The ionic radius is bigger, and therefore the area of bombardment influence is also bigger.Technology in the past attempts using large-area conductive anode when solving loading anodic problem.This be since large-area conductive anode because area is bigger, the probability that therefore contact with negative oxygen ion is high more, to improve the degree of negative oxygen ion bombardment just high more thereby carry out charge-exchange.But adopt this method, under the gas phase state of high temperature and disperse because sputter procedure is to carry out; The metal that sputters and O atom form one deck rete easily through sputter and high temperature for a long time on anode, and increase in time and thickness increases.Time is long more, and anode is easy more to be covered by rete, and the also very fast deterioration of conductive capability then can't reach due effect in the later stage of long-time preparation.Under the short period of time prepares situation, also to constantly change or clean, improve maintenance cost.
In the sputtering equipment with close packing tip anode of the present invention, the distance of described close packing tip anode and sputtering target material is 10-30mm.
The tip body of close packing tip anode can be following two kinds of structures: flush type triangle body or three-dimensional cone.
The tip body of described close packing tip anode is the flush type triangle body.Be to adopt metal plate to process, the thickness of the flush type triangle body that is processed into just in time is the thickness of metal plate.
The tip body of described close packing tip anode is three-dimensional cone.But three-dimensional cone is difficult with processing, and the mode that the flush type triangle body can program control cutting prepares with comparalive ease.For the function that guarantees tip body is normal, the ratio between its element length (or height) and the base should h/d should be greater than 5.
In the close packing tip, most advanced and sophisticated shape can be the flush type tip, also can adopt three-dimensional cone point, and the effect of cone point is better than flush type.But cone point is difficult with processing, and the mode that the flush type close packing tip can program control cutting prepares with comparalive ease.Normal for guaranteeing most advanced and sophisticated function, the ratio between its element length (or height) and the base should h/d should be greater than 5.
The shape of corresponding sputtering target material, the openwork part of close packing tip anode be shaped as cuboid or round.
The openwork part of described close packing tip anode is a cuboid.
Openwork part at close packing tip anode is under the situation of cuboid, and in described close packing tip anode, the tip body on four bights of orthogonal of its openwork part, the height of remaining tip body and the ratio on base are greater than 5.The matrix of described close packing tip anode is preferably tabular.
The openwork part of described close packing tip anode is a round.
Openwork part at close packing tip anode is under the situation of round, and the height of the tip body of described close packing tip anode and the ratio on base are greater than 5.The matrix of described close packing tip anode is preferably tabular.
For strengthening result of use, close packing tip anode can load positive bias in use.The existence that positively biased is had a meeting, an audience, etc. well under one's control makes the easier anode direction of negative oxygen ion move, and reduces the bombardment substrate effect.When loading positive bias, require close packing tip anode and cavity and substrate all to be in state of insulation.Described close packing tip anode is connected with D.C. regulated power supply, loads the 20-200V positive bias.
Advantage of the present invention is: the close packing tip anode that sputtering equipment of the present invention adopts, on the one hand because the existence of tip anode has improved surface-area; At tip portion,, can keep the surface fresh largely on the other hand even dispersing gas also is difficult to growth firmly under high temperature action; And then keep negative oxygen ion to eliminate effect.A contrast and experiment: not with the anode of close packing tip after preparing YBCO through 60 hours, 800 ℃ high temperature sputters, its inner rim has been high-impedance state substantially; And the employing close packing tip anode, under same state, most of tip still keeps good metal good conductor characteristic.Sputtering equipment with close packing tip anode of the present invention, be a kind ofly can be applied to the sputtering equipment that planar target sputter mass prepares the ybco film material, by loading a kind of anode of close packing tip, greatly eliminate the influence of negative oxygen ion bombardment, satisfy the speed and the process window requirement of mass preparation.
Description of drawings
Fig. 1 is a kind of close packing tip anode that is applied to the rectangle sputtering target material.
Fig. 2 is a kind of close packing tip anode that is applied to circular sputtering target material.
Fig. 3 prepares the synoptic diagram of YBCO high-temperature superconducting thin film for static sputter.
Fig. 4 is the synoptic diagram that dynamic dead axle rotates preparation YBCO high-temperature superconducting thin film.
Fig. 5 is the sputtering equipment structural representation with close packing tip anode of the present invention.
Embodiment
A kind of close packing tip anode that is applied to the rectangle sputtering target material as shown in Figure 1.Support 1 supports and the fixing rectangular metal matrix 2 of close packing tip anode, in the present embodiment, metallic matrix 2 and be used for supporting and fixed support 1 is plate refractory metal material, the middle part hollow out of metallic matrix 2, form rectangle hollow out sputter mouth, the inside edge of rectangle openwork part is to be arranged continuously by several tip bodies 3 to be formed by connecting, and the tip of each tip body 3 is towards the middle part of openwork part, close packing tip body 3 forms with metal working process, close packing tip body 3 carries out repeated arrangement in the orthogonal circumferential direction, wherein, because four bights of orthogonal are the corners in the rectangle, zone, 4 right angles in rectangle generally can not form the repeating structure of close packing tip body, therefore can form zone of transition 4, each zone of transition 4 has only a tip body, and the tip body on four bights can not be consistent with the structural requirement of tip body on four limits in the rectangle, so, the tip body on four bights of orthogonal of its openwork part, the height of remaining tip body and the ratio on base are greater than 5.
A kind of close packing tip anode that is applied to circular sputtering target material as shown in Figure 2.Wherein, support 11 supports and the fixing circular metal matrix 12 of close packing tip anode, in the present embodiment, metallic matrix 12 and be used for supporting and fixed support 11 is plate refractory metal material, the middle part hollow out of metallic matrix 12, form circular hollow out sputter mouth, the inside edge of circular openwork part is to be arranged continuously by several tip bodies 13 to be formed by connecting, and the tip of each tip body 13 is towards the middle part of openwork part, close packing tip body 13 forms with metal working process, close packing tip body 13 carries out repeated arrangement in the circumferential direction of interior circle, and the distribution that is centrosymmetric.
A kind of sputtering equipment with close packing tip anode as shown in Figure 5, this sputtering equipment is to be provided with vacuum-lines 52 on sputter cavity 51, admission passage 53, and in the sputter cavity, be provided with sputtering target material 54, heating member 55, heating member 55 is oppositely arranged with sputtering target material 54, and on heating member 55, be provided with sample 56, between described sputtering target 54 and sample 56, be provided with close packing tip anode 57, this close packing tip anode is as matrix with metal, its middle part hollow out, the inside edge of openwork part is to be arranged continuously by several tip bodies to be formed by connecting, and the tip of each tip body is towards the middle part of openwork part, and openwork part and sputtering target material 54, sample 56 is relative.
Embodiment 1
As shown in Figure 3, embodiment 1 is the synoptic diagram that static sputter prepares the YBCO high-temperature superconducting thin film.Circular YBCO planar targets 31 with φ 68mm carries out sputter, and the close packing tip anode 32 (in Fig. 3, the close packing tip body in the close packing tip anode 32 does not draw, and omits) of circular YBCO sputtering target material is placed at about 20mm place below planar targets 31.That relative with close packing tip anode 32 is φ 2 " oxide monocrystal substrate 34 and heating member 33.Generally be between heating member 33 and oxide monocrystal substrate 34, to be added with one deck soaking quartz plate (figure do not show), to play soaking, to prevent that sample is heated inequality and the effect that bursts.Apply the positive bias of 50V at the close packing tip anode end.
In implementation process, at 860 ℃ of Heating temperatures, Ar/O
2Under the mixed gas air pressure 20Pa condition,, obtain the thick YBCO high-temperature superconducting thin film of about 500nm with the sputtering current of 1.6A, through 6 hours sputter preparations.
Among the static preparation technology, add thermal recovery and carry out, the sample moving processes such as rotation that do not revolve round the sun in the mode of sample base plane heating.The inner edge of close packing tip anode 32 is generally got, sputtering target material slightly a little bit smaller size bigger slightly than sample, and the inner dimensions of close packing tip anode 32 is φ 60mm in the present embodiment 1.
Embodiment 2
Adopt dynamic dead axle to rotate preparation YBCO high-temperature superconducting thin film.Can adopt " a kind of batch preparation of double-faced high-temperature superconducting film device " by name patent No. is disclosed equipment in 200620119334.1, as shown in Figure 4, this equipment is to be provided with flush type high temperature superconducting materia target 41 in vacuum cavity 45, and the metal targets 42 that is used for the in-situ sputtering electrode; Be provided with collar plate shape heating wheelwork in the middle of in the vacuum cavity 45, this collar plate shape heating wheelwork is to be made of disk wheelwork and disk heating unit.The disk heating unit comprises upper heating disk 43 and following heating plate 47; The disk wheelwork is to be made of disk sample platform 61 and wheelwork, on disk sample platform 61, be provided with the circular port (figure does not show) that is used to place the large area superconducting film substrate evenly and at intervals, wheelwork comprises main rotary shaft 49, main rotary shaft 49 clutch disk sample table 61 drive sample table 61 and be rotated heating in heating, vacuum cavitys 45.
Present embodiment 2 is to improve on the basis of aforesaid device, is that close packing tip anode 48 is placed at about 20mm place below flush type high temperature superconducting materia target 41.Its position relation as shown in Figure 4.Present embodiment 2 is that the rectangular planes YBCO target with 152m * 76mm carries out sputter.The oxide monocrystal substrate of " oxide monocrystal substrate be placed on the circular port of sample table 61, φ 2 " with φ 2 is as LaAlO
3, MgO, CeO
2/ Al
2O
3/ CeO
2Deng.The main rotary shaft 49 of wheelwork drives sample table 61 and be rotated heating in heating, vacuum cavity 45.With 750 ℃ Heating temperatures, Ar/O
2Mixed gas air pressure 30Pa, sample with the sputtering current of 1.5A, through 60 hours sputter preparations, obtain the thick YBCO high-temperature superconducting thin film of about 300nm with under the 6rpm speed rotating conditions.
The mode that sample relies on central shaft to rotate with dead axle in the present embodiment 2 drives sample and carries out the rotation of revolution formula, and type of heating is two-sided heating simultaneously.The close packing tip anode of placing below sputtering target material, its inner rim is of a size of 140mm * 70mm.
Claims (11)
1. sputtering equipment with close packing tip anode, this sputtering equipment is to be provided with vacuum-lines and admission passage on the sputter cavity, and in the sputter cavity, be provided with sputtering target material and heating member, it is characterized in that: between described sputtering target material and sample, be provided with close packing tip anode, the matrix adopting of this close packing tip anode the high temperature resistant stainless steel metallic substance, this metallic substance can stand 700 ℃～900 ℃ pyritous to be tested for a long time, guarantee not take place under the high temperature oxidation condition oxidation simultaneously, do not change metallic conductor character, promptly under the said temperature environment, under the condition below the oxygen pressure 100Pa, significant oxidation does not take place, the middle part hollow out of this close packing tip anode, the inside edge of openwork part is to be arranged continuously by several tip bodies to be formed by connecting, and the tip of each tip body is towards the middle part of openwork part, and its openwork part is relative with sputtering target material.
2. the sputtering equipment with close packing tip anode according to claim 1 is characterized in that: the distance of described close packing tip anode and sputtering target material is 10-30mm.
3. the sputtering equipment with close packing tip anode according to claim 1 is characterized in that: the tip body of described close packing tip anode is the flush type triangle body.
4. the sputtering equipment with close packing tip anode according to claim 1 is characterized in that: the tip body of described close packing tip anode is three-dimensional cone.
5. according to claim 3 or 4 described sputtering equipments with close packing tip anode, it is characterized in that: the openwork part of described close packing tip anode is a cuboid.
6. the sputtering equipment with close packing tip anode according to claim 5 is characterized in that: in described close packing tip anode, the tip body on four bights of orthogonal of its openwork part, the height of remaining tip body and the ratio on base are greater than 5.
7. the sputtering equipment with close packing tip anode according to claim 6 is characterized in that: the matrix of described close packing tip anode is a tabular.
8. according to claim 2 or 3 described sputtering equipments with close packing tip anode, it is characterized in that: the openwork part of described close packing tip anode is a round.
9. the sputtering equipment with close packing tip anode according to claim 8 is characterized in that: the height of the tip body of described close packing tip anode and the ratio on base are greater than 5.
10. the sputtering equipment with close packing tip anode according to claim 9 is characterized in that: the matrix of described close packing tip anode is a tabular.
11. the sputtering equipment with close packing tip anode according to claim 1 and 2 is characterized in that: described close packing tip anode is connected with D.C. regulated power supply, loads the 20-200V positive bias.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007103045555A CN101469407B (en) | 2007-12-28 | 2007-12-28 | Sputtering equipment with close packing tip anode |
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|---|---|---|---|
| CN2007103045555A CN101469407B (en) | 2007-12-28 | 2007-12-28 | Sputtering equipment with close packing tip anode |
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|---|---|
| CN101469407A CN101469407A (en) | 2009-07-01 |
| CN101469407B true CN101469407B (en) | 2011-06-08 |
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| CN108220899A (en) * | 2018-01-02 | 2018-06-29 | 京东方科技集团股份有限公司 | A kind of sputtering equipment |
| CN111501010A (en) * | 2020-04-30 | 2020-08-07 | 军事科学院系统工程研究院军需工程技术研究所 | In-situ preparation method of metal fiber reinforced composite film |
| CN112663009A (en) * | 2020-12-11 | 2021-04-16 | 江苏特丽亮镀膜科技有限公司 | Magnetron sputtering coating device and working method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6171461B1 (en) * | 1996-03-07 | 2001-01-09 | Mark A. Bernick | Sputtering cathode |
| CN1316309A (en) * | 2001-03-16 | 2001-10-10 | 太原理工大学 | Process for preparing nm material by dual-glow discharge of hollow cathodes |
| CN2719866Y (en) * | 2004-08-13 | 2005-08-24 | 北京有色金属研究总院 | large-size column hollow sputtering cathode |
-
2007
- 2007-12-28 CN CN2007103045555A patent/CN101469407B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6171461B1 (en) * | 1996-03-07 | 2001-01-09 | Mark A. Bernick | Sputtering cathode |
| CN1316309A (en) * | 2001-03-16 | 2001-10-10 | 太原理工大学 | Process for preparing nm material by dual-glow discharge of hollow cathodes |
| CN2719866Y (en) * | 2004-08-13 | 2005-08-24 | 北京有色金属研究总院 | large-size column hollow sputtering cathode |
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Effective date of registration: 20190626 Address after: 101407 No. 11 Xingke East Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee after: Research Institute of engineering and Technology Co., Ltd. Address before: 100088, 2, Xinjie street, Beijing Patentee before: General Research Institute for Nonferrous Metals |
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