CN103255385A - Design method for composite target for magnetron sputtering - Google Patents
Design method for composite target for magnetron sputtering Download PDFInfo
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- CN103255385A CN103255385A CN2013101818272A CN201310181827A CN103255385A CN 103255385 A CN103255385 A CN 103255385A CN 2013101818272 A CN2013101818272 A CN 2013101818272A CN 201310181827 A CN201310181827 A CN 201310181827A CN 103255385 A CN103255385 A CN 103255385A
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Abstract
The invention discloses a design method for a composite target for magnetron sputtering and relates to the fields of magnetron sputtering techniques and preparation techniques of functional films of inorganic compounds. The composite target is formed by uniformly and alternatively splicing simple-substance sheet targets, being divided into 5-degree, 10-degree, 30-degree and 60-degree fan-shaped sections, of each component according to certain angles, wherein the components are uniform in ingredient proportion, are stable and are easy to change; and the ingredients of the composite target can be adjusted by adjusting the angles of the fan-shaped sections of each component so as to adjust the stoichiometric ratio of a compound film, and the ingredients of the compound film obtained by utilizing sputtering are uniform. The design method is especially suitable for film preparation of Heusler compounds and half Heusler compounds which have brittleness and are difficultly prepared into the compound targets accordant with the stoichiometric ratio because the differences among the melting points of the components are relatively large or the ingredients of the partial components are easy to segregate and is a novel composite target design method for co-sputtering growing of the compound film or the composite film without utilizing a multi-target co-sputtering method.
Description
Technical field
The present invention relates to a kind of magnetron sputtering with the method for design of composite target material, belong to magnetron sputtering technique and mineral compound function film preparing technical field.
Background technology
Thomas Hessler (Heusler) and half Thomas Hessler (half Heusler) series material comprises the different compound of kind more than 1500, wherein comprise semi-conductor, topological isolator, superconductor, magneticsubstance, shape-memory material, semi-metallic etc., having wide application field, is one of lasting research focus in material field.Their general structure is respectively X
2YZ and XYZ, the performance of material is very responsive to the composition of its constituent element.General more and more deep to the research of body material in the research of these materials, and less to thin film study, particularly thermoelectric material wherein and topological isolator, the preparation research to its film lacks very much at present.Thomas Hessler and half Thomas Hessler film can be obtained by molecular beam epitaxy (MBE) and magnetron sputtering usually, but molecular beam epitaxy is restricted because of output, efficient and Composition Control problem.Sputtering method efficient when the common alloy firm of deposition is extensively approved, yet on the one hand a lot of heusler's alloys enbrittle, and are difficult to be made into large-area alloys target form; Some component fusing point of these materials has big difference on the other hand, perhaps is easy to volatilization or segregation in preparation process, thereby is difficult to form the compound target that meets stoichiometric ratio.In addition, prepare film for magnetron sputtering method, the thin film composition that sputter obtains generally is different from the composition of its used target, therefore accurately is adjusted to relatively difficulty of branch.Cosputtering is reasonable selection in these cases.
In having traditional cosputtering method of a plurality of targets, the number of required target is determined by the component number of the compound film of desire preparation, but the number of target and position thereof are just definite in device customizing, are difficult to increase and decrease and regulate.Though also can select for use the alloys target of certain two kinds of component and the simple substance target of other constituent elements to carry out cosputtering, adjusting brings difficulty but this is again to composition.In general cosputtering method, as Chinese patent application number 02128681 " with the method for cosputtering method deposition heusler's alloy film " though the composition of film can regulate by the sputter rate that changes each negative electrode target, but because its intrinsic inclination sputter arranges, even substrate can rotate in film process, the local composition of prepared film is always inhomogeneous.In order to obtain uniform film, the negative electrode target must be close to each other as far as possible, and the pitch angle must be as best one can little.This cosputtering system generally is that comparison is expensive and complicated.
Summary of the invention
Goal of the invention
In view of the above problems, the purpose of this invention is to provide a kind of magnetron sputtering method of design of composite target material, make in general non-cosputtering system, can obtain composition evenly, stoichiometric ratio is easy to regulating and controlling Thomas Hessler and half Thomas Hessler compound film, and is conducive to reduce cost.
Technical scheme
In order to address the above problem, the method for design of claim 1 record is utilized magnetron sputtering method to prepare simple substance membrane respectively and is utilized the step instrument to measure its thickness, obtains the growth parameter(s) curve of every kind of target, thereby calculates the sputter rate of each constituent element under the different capacity.Take all factors into consideration selected certain suitable sputtering power and air pressure, calculate the required area of the compound film of the certain stoichiometric ratio of preparation or the angle of fan-shaped section respectively according to the sputter rate of each element under this condition, and according to this angle the simple substance target is cut, cut into 5 of some amount respectively
o, 10
o, 30
o, 60
oFan-shaped section.According to the fan-shaped section that the required simple substance target area that calculates or angle are selected suitable quantity respectively for use, clean up the back and with conductive resin they are pasted on the scale copper with the target same size, as initial composition composition target on probation.When the splicing composition target, make the fan-shaped section of every kind of constituent element to be alternately distributed equably as far as possible.
Under suitable underlayer temperature, operating air pressure and sputtering power condition, prepare compound film with initial composition composition target on probation, carry out the elemental composition analysis.The area that readjusts each component in the composite target material according to analytical results compares or fan-shaped section angle ratio, repeats the process of above-mentioned preparation film, composition analysis result feedback, finally obtains the composite target material of required component proportions.According to repeatedly experiment repeatedly, composition analysis result for the third time very near the stoichiometric ratio of setting, can obtain satisfactory compound film.
Each constituent element fan-shaped section is replaceable adjusting in the design's method, and this change for stoichiometric ratio provides very convenient feasible approach.
The invention effect
As mentioned above, composite target material method of design of the present invention is a kind ofly not need to use many targets cosputtering method but can obtain cosputtering growth compound film or the NEW TYPE OF COMPOSITE target method of design of laminated film effect, its gained thin film composition is even, stoichiometric ratio is easy to regulating and controlling, and be conducive to reduce the film preparation cost, be specially adapted to as Thomas Hessler and half Thomas Hessler based compound, be difficult to prepare the alloy target material thin-film material.
Description of drawings
Fig. 1 is the sedimentation rate curve of Ti, Co and Sb simple substance film under the different sputtering powers under sputtering pressure 0.7 Pa.
Fig. 2 is simple substance target cutting synoptic diagram of the present invention, and the numeral among the figure is the angle of fan-shaped section.
Fig. 3 (a) is a ternary composition target structural representation, wherein three kinds of different constituent element simple substance A, B, C of distinct colors representative.Fig. 3 (b) utilizes the different angles fan-shaped section to carry out the synoptic diagram that composition is regulated.
Fig. 4 is the composite target material sputter that utilizes the present invention to design, the XRD spectrum of the half Thomas Hessler compound semiconductor for preparing at general magnetic control sputtering device: (a) under the normal temperature behind the spatter film forming 600
o5 minutes TiCoSb film of C short annealing; (b) 600
oThe YPtSb film of sputter preparation under the C underlayer temperature.
Description of reference numerals
1, the scale copper and the conductive adhesive layer that are used for support.
Embodiment
Use the method for design of composite target material according to magnetron sputtering according to the present invention, at first utilize magnetron sputtering method to prepare simple substance membrane respectively and utilize the step instrument to measure its thickness, obtain the growth parameter(s) curve of every kind of target, for example: double Thomas Hessler compound semiconductor TiCoSb, fixing other parameters such as sputtering pressure and underlayer temperature, obtain sputtering power-thickness curve, as shown in Figure 1.Calculate the sputter rate of each element under the different capacity.The sputter rate difference of three kinds of elements increases rapidly with the increase of sputtering power.Too high power is unfavorable for forming the TiCoSb film that meets stoichiometric ratio, and low excessively power deposit efficient is lower.Comprehensive the two consideration can be selected sputtering power 20 W.Calculate three kinds of element angles according to this than being Ti:Co:Sb=276 °: 57 °: 27 °, we select immediate Ti:Co:Sb=275 °: 55 °: 30 °, make initial composition composition target on probation according to this.
The simple substance target of each constituent element is cut into 5 of some amount
o, 10
o, 30
o, 60
oFan-shaped section, according to what of the required angle of simple substance target, can adjust concrete cutting angle and piece number thereof, as to Ti simple substance target, required angle is big, can cut low-angle secter pat less as shown in Figure 2.And to the Sb target, then need more Small angle piece.Formation according to top definite initial composition composition target on probation, choose the simple substance target fan-shaped section of proper angle and suitable quantity respectively, cleaning up the back is fixed to them on the scale copper with the target same size equably with conductive resin, as initial composition composition target on probation, shown in Fig. 3 (a).
Under suitable underlayer temperature, operating air pressure and sputtering power condition, prepare compound film with magnetron sputtering method, utilize X-ray diffraction to carry out material phase analysis, utilize X ray energy dispersion spectrum and X-ray fluorescence spectra to carry out the elemental composition analysis.According to initial composition analysis result, readjust area ratio or the fan-shaped section angle ratio of each component in the composite target material, repeat to make compound target on probation and composition analysis step, obtain composition composition target on probation and the result of composition analysis for the second time for the second time respectively; This result is fed back to again in the making of compound target on probation, can obtain composition composition target on probation and composition analysis result for the third time for the third time respectively.In experimentation, according to departing from of stoichiometric ratio, only need correspondingly regulate area or the fan-shaped section angle of each component of compound in composition target, can reach the purpose of regulating film chemical metering ratio, shown in Fig. 3 (b).
According to repeatedly experiment repeatedly, composition analysis result for the third time very near the stoichiometric ratio of setting, can obtain satisfactory compound film, for example, to the TiCoSb film, obtains Ti: Co: Sb=33.81: 34.29: 31.9.To the YPtSb film, regulate for the first time the result and be Y: Pt: Sb=24.68: 42.70: 32.62, regulate the result for the second time and be Y: Pt: Sb=29.72: 37.85: 32.43: regulate the result for the third time and be Y: Pt: Sb=31.99: 33.73: 34.28.
In the present invention carries out experiment that sputter prepares film, can heat to substrate or carry out the normal temperature sputter according to appointed condition.The film of normal temperature sputter need carry out anneal.The preparation of TiCoSb film and composition regulate process on the silica glass substrate as previously discussed are all in the normal temperature sputter, then at 500-800
oC carries out anneal, can obtain the TiCoSb polycrystal film.The preparation of YPtSb film and composition regulate process then all are 600 on MgO (100) substrate
oCarry out under the C underlayer temperature condition.Fig. 4 (a) and Fig. 4 (b) are respectively with the TiCoSb film of the method for the invention making and the XRD spectra of YPtSb film, and the two has all formed the polycrystalline structure film as can be seen.
Claims (8)
1. a magnetron sputtering is with the method for design of composite target material, and being does not a kind ofly need to use many targets cosputtering method but can obtain cosputtering growth compound film or the novel target method of design of laminated film effect.Some compound (as TiCoSb, YiNiBi etc.) be difficult for to utilize conventional powder metallurgic method or vacuum melting method to be prepared into can be for the ever-larger diameters compound target of magnetron sputtering use, and many targets cosputtering method equipment cost is higher; The composite target material that utilizes the design's method to make can carry out the preparation of compound film at general magnetic control sputtering device, and the stoichiometric ratio that is easy to regulate compound film.This method of design mainly may further comprise the steps: the preparation of a. simple substance target and the test of the sputter rate of simple substance membrane material; B. the calculating of each component area ratio in the composite target material; C. initial composition composite target material on probation is made in the splicing of the cutting of simple substance target and composite target material; D. utilize the composite target material sputter on probation of initial composition to prepare compound film and composition test thereof; E. form according to the element area of test result feedback regulation composition target on probation, finally obtain the composite target material that is suitable for.
2. the method for design of a magnetron sputtering usefulness composite target material also is applicable to the application of pulsed laser deposition (PLD) target.
3. a kind of magnetron sputtering according to claim 1 is with the method for design of composite target material, it is characterized in that the sputter rate test of described simple substance membrane material: at the simple substance target of target producer customization laminated film component, utilize magnetron sputtering method to prepare simple substance membrane respectively and utilize the step instrument to measure its thickness, obtain the growth parameter(s) curve of every kind of target, as: fixing other parameters such as sputtering pressure and underlayer temperature, obtain sputtering power-thickness curve, thereby calculate the sputter rate of each element under the different capacity.
4. a kind of magnetron sputtering according to claim 1 is with the method for design of composite target material, it is characterized in that the calculating of each component area ratio in the described composite target material: selected certain suitable sputtering power and air pressure calculate the required area of the compound film of the certain stoichiometric ratio of preparation or the angle of fan-shaped section respectively according to the sputter rate of each element under this condition.
5. a kind of magnetron sputtering according to claim 1 is with the method for design of composite target material, it is characterized in that the cutting of described simple substance target and the splicing of composite target material, make initial composition composite target material on probation: as required the simple substance target is cut into 5 of some amount respectively
o, 10
o, 30
o, 60
oFan-shaped section; According to the fan-shaped section that the required simple substance target area that calculates or angle are selected suitable quantity respectively for use, clean up the back and with conductive resin their alternate intervals ground is pasted on the scale copper with the target same size, try out composition target as initial composition.
6. a kind of magnetron sputtering according to claim 1 is with the method for design of composite target material, it is characterized in that the initial composition of described utilization Film by Sputtering of Composite Target on probation prepares compound film and composition test thereof, obtain initial composition analysis result: under suitable underlayer temperature, operating air pressure and sputtering power condition, prepare compound film with magnetron sputtering method, utilize X-ray diffraction (XRD) to carry out material phase analysis, utilize X ray energy dispersion spectrum (EDX) and X-ray fluorescence spectra (XRF) to carry out the elemental composition analysis.
7. a kind of magnetron sputtering according to claim 1 is with the method for design of composite target material, it is characterized in that described element area composition according to test result feedback regulation composition target on probation, finally obtain the composite target material that is suitable for: the area that readjusts each component in the composite target material according to initial composition analysis result than or fan-shaped section angle ratio, repeating step c and d obtain composition composition target on probation and the result of composition analysis for the second time for the second time respectively; This result is fed back to step c and d again, obtain composition composition target on probation and composition analysis result for the third time for the third time respectively; Composition analysis result for the third time is consistent with the stoichiometric ratio of requirement, so composition composition target on probation is required composite target material for the third time.
8. a kind of magnetron sputtering according to claim 1 is with the method for design of composite target material, it is characterized in that being easy to regulate the stoichiometric ratio of compound film: according to the change of stoichiometric ratio, only need correspondingly regulate area or the fan-shaped section angle of each component of compound in composition target.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103590013A (en) * | 2013-11-04 | 2014-02-19 | 南昌工程学院 | Method for predicting components by analytical process to prepare Fe-Ga alloy film |
| CN104846333A (en) * | 2015-04-22 | 2015-08-19 | 武汉理工大学 | Making method of component-controllable boron-carbon-nitrogen film |
| CN107299326A (en) * | 2017-08-16 | 2017-10-27 | 信利光电股份有限公司 | A kind of vacuum coating doping target and preparation method thereof and vacuum coating method |
| CN108677157A (en) * | 2018-05-31 | 2018-10-19 | 南京工程学院 | A kind of high-entropy alloy method for manufacturing thin film with high hard high resistivity characteristic |
| CN109161863A (en) * | 2018-11-16 | 2019-01-08 | 合肥鑫晟光电科技有限公司 | A kind of target, magnetic control sputtering device and sputtering method, sputtered film |
| CN109504946A (en) * | 2018-12-20 | 2019-03-22 | 兰州空间技术物理研究所 | A kind of planar rectangular magnetic control sputtering cathode adjustable angle type electromagnetic coil |
| CN109628891A (en) * | 2019-01-16 | 2019-04-16 | 兰州城市学院 | A kind of TiN/MoS2The preparation method of/Ag high temperature lubricating laminated film |
| CN109913771A (en) * | 2019-04-02 | 2019-06-21 | 中国科学院宁波材料技术与工程研究所 | A kind of VAlTiCrSi high-entropy alloy film and its application under briny environment |
| CN110306162A (en) * | 2019-07-04 | 2019-10-08 | 重庆斯太宝科技有限公司 | A kind of thermoelectric pile heat flow transducer and its manufacture craft |
| CN111020509A (en) * | 2019-12-25 | 2020-04-17 | 南京欧美达应用材料科技有限公司 | Large-area ceramic target assembly and manufacturing method thereof |
| CN111139455A (en) * | 2019-12-18 | 2020-05-12 | 复旦大学 | Preparation method of high-quality cadmium arsenide film |
| CN112962076A (en) * | 2021-02-04 | 2021-06-15 | 西南交通大学 | Preparation method of metal precursor film of second-generation high-temperature superconducting tape |
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| CN103590013B (en) * | 2013-11-04 | 2015-07-01 | 南昌工程学院 | Method for predicting components by analytical process to prepare Fe-Ga alloy film |
| CN103590013A (en) * | 2013-11-04 | 2014-02-19 | 南昌工程学院 | Method for predicting components by analytical process to prepare Fe-Ga alloy film |
| CN104846333A (en) * | 2015-04-22 | 2015-08-19 | 武汉理工大学 | Making method of component-controllable boron-carbon-nitrogen film |
| CN104846333B (en) * | 2015-04-22 | 2017-10-24 | 武汉理工大学 | A kind of preparation method of the controllable boron carbon nitrogen film of component |
| CN107299326A (en) * | 2017-08-16 | 2017-10-27 | 信利光电股份有限公司 | A kind of vacuum coating doping target and preparation method thereof and vacuum coating method |
| CN108677157A (en) * | 2018-05-31 | 2018-10-19 | 南京工程学院 | A kind of high-entropy alloy method for manufacturing thin film with high hard high resistivity characteristic |
| CN109161863A (en) * | 2018-11-16 | 2019-01-08 | 合肥鑫晟光电科技有限公司 | A kind of target, magnetic control sputtering device and sputtering method, sputtered film |
| CN109161863B (en) * | 2018-11-16 | 2023-08-22 | 合肥鑫晟光电科技有限公司 | Target material, magnetron sputtering device, sputtering method and sputtering film |
| CN109504946B (en) * | 2018-12-20 | 2020-12-01 | 兰州空间技术物理研究所 | Angle-adjustable electromagnetic coil for planar rectangular magnetron sputtering cathode |
| CN109504946A (en) * | 2018-12-20 | 2019-03-22 | 兰州空间技术物理研究所 | A kind of planar rectangular magnetic control sputtering cathode adjustable angle type electromagnetic coil |
| CN109628891A (en) * | 2019-01-16 | 2019-04-16 | 兰州城市学院 | A kind of TiN/MoS2The preparation method of/Ag high temperature lubricating laminated film |
| CN109913771A (en) * | 2019-04-02 | 2019-06-21 | 中国科学院宁波材料技术与工程研究所 | A kind of VAlTiCrSi high-entropy alloy film and its application under briny environment |
| CN110306162A (en) * | 2019-07-04 | 2019-10-08 | 重庆斯太宝科技有限公司 | A kind of thermoelectric pile heat flow transducer and its manufacture craft |
| CN111139455A (en) * | 2019-12-18 | 2020-05-12 | 复旦大学 | Preparation method of high-quality cadmium arsenide film |
| CN111139455B (en) * | 2019-12-18 | 2021-09-28 | 复旦大学 | Preparation method of high-quality cadmium arsenide film |
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| CN112962076B (en) * | 2021-02-04 | 2022-04-05 | 西南交通大学 | Preparation method of metal precursor film of second-generation high-temperature superconducting tape |
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Application publication date: 20130821 |