CN104538542A - Technology for preparing multilayer film thermoelectric materials through physical vapor deposition method - Google Patents
Technology for preparing multilayer film thermoelectric materials through physical vapor deposition method Download PDFInfo
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- CN104538542A CN104538542A CN201410823870.9A CN201410823870A CN104538542A CN 104538542 A CN104538542 A CN 104538542A CN 201410823870 A CN201410823870 A CN 201410823870A CN 104538542 A CN104538542 A CN 104538542A
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Abstract
The invention discloses a technology for preparing multilayer film thermoelectric materials through a physical vapor deposition method. The technology is applied to the field of preparing of multilayer film thermoelectric materials. A proper base is selected, and the multilayer film thermoelectric materials are prepared through reactive magnetron sputtering. In the preparing process, different bases can be selected for deposition, and meanwhile material kinds, film layer thicknesses, film layer numbers and the like can be selected. Compared with other methods for preparing multilayer film thermoelectric materials, the physical vapor deposition method is obvious in layered structure, high in precision, capable of reaching the nanometer level and improving the thermoelectric performance, easy to operate, capable achieving batched production, good in controllability and capable of preparing diverse multilayer film thermoelectric materials.
Description
Technical field
The present invention relates to a kind of thermoelectric material preparation method, particularly relate to a kind of multilayer film thermoelectric material preparation technology, be applied to the preparing technical field being made into the function element such as Thermoelectric Generator and thermoelectric cooling device material.
Background technology
Thermoelectric material is a kind of a kind of material realizing heat energy and electric energy and directly change, and it may be used for thermo-electric generation and energising refrigeration.Thermoelectricity capability can characterize its performance by a dimensionless thermoelectric figure of merit ZT, and it expresses T=α ^2 σ/κ T, and wherein α is Seebeck coefficient, and σ is conductivity, and κ is thermal conductance, and T is temperature.Therefore reducing thermal conductivity is improve a more direct method of the ZT figure of merit.
Find when the size of device narrows down to micro-nano-scale after deliberation, due to quantum size effect and surface and interface effect, its many microphysical phenomena compared with Macroscopic physical phenomenon, have very large difference, and due to the microminiaturization of device dimension, make the relative importance of original various influencing factor also there occurs change, therefore dimensional effect and interfacial effect play very very important effect at microscopic fields.From heat transfer angle, the thermophysical property of material and the design of device and performance closely related, above-mentioned space microscopic heat conduction has been there is after the characteristic size microminiaturization of device, the thermophysical parameter of material is made to show obvious specificity, the thermal conductivity coefficient of such as material can reduce along with the reduction of film thickness, even can be changed into heat guard, so micro-nano-scale material and multi-layer film structure material play an important role gradually in thermoelectric material.
Current making multilayer film heat structure mainly contains Physical and the large class of chemical method two.
Chemical method mainly contains double flute method and single channel process, has following shortcoming time it prepares multilayer film: the solution of different layers easily produces cross pollution thus affects multi-layer film structure purity; In course of reaction, factors causes experimental result repeatability bad, such as ambient humidity, medicine purity and gaseous impurity etc.; The associativity of sample and substrate is bad; Sample preparation restriction is more, can only prepare metallized multilayer film, cannot prepare oxide, the compound multilayer films such as nitride.
And use physical method to solve the problem, realize the target preparing high-performance multilayer film thermoelectric material simultaneously.Physical method preparation is by the gas ion that produces under high vacuum atmosphere or molecule deposition in substrate, thus the multilayer film thermoelectric material of system.Therefore, improve the purity preparing gained film largely.Physical method comprises vacuum evaporation, molecular beam epitaxy film deposition and mechanical processing method etc.But temperature required when this method prepares multilayer film thermoelectric material is high, and film formation time is long, can not meet the development of thermoelectric material and the needs of application.
Summary of the invention
In order to solve prior art problem, the object of the invention is to the deficiency overcoming prior art existence, a kind of technique utilizing physical gas-phase deposite method to prepare multilayer film thermoelectric material is provided, can different materials be selected according to different field demand and regulate each layer thickness and the number of plies, then produce low thermal conducting material thus promote thermoelectricity capability, simple to operate, controllability is strong, reproducible and be easy to suitability for industrialized production.
Create object for reaching foregoing invention, the present invention adopts following technical proposals:
Utilize physical gas-phase deposite method to prepare a technique for multilayer film thermoelectric material, comprise the following steps:
A. the selection of substrate and process thereof: select substrate as after substrate as required, processed by the substrate of selection, processing method is hydrofluoric acid treatment, then cleans and dry for standby; Substrate preferably adopts semiconductor, sheet glass, sheet metal, polymer sheet or microdevice; When target is selected, the carrier material of selection more preferably in gold, silicon and SiGe three kinds or arbitrarily bi-materials;
B. the selection of target: select purity to be not less than the material of 99.99% as target, target at least adopts two or more different carrier materials; When target is selected, the carrier material of selection be preferably in metal, semiconductor and insulator any one or several arbitrarily;
C. in substrate, multilayer film thermoelectric material is made: adopt physical gas-phase deposite method to interlock on the substrate of stratified sedimentation after process in step a successively by the target chosen in stepb, prepare multilayer film, the multilayer film number of plies of accumulative deposition is at least greater than the species number of the target chosen in stepb, preparing in multilayer film process, the thickness of any one deck monofilm is all greater than 5nm; Physical gas-phase deposite method preferably adopts that electron beam evaporation, molecular beam epitaxy film deposit, in direct current reaction magnetron sputtering and radio frequency magnetron sputtering method any one or several arbitrarily; By preferably controlling any one or any several parameter in substrate temperature, sputtering time, reacting gas content and sputtering power, be controlled to thicknesses of layers and film formation time; When preparing multilayer film thermoelectric material, preferably each layer non-crystal thin film prepared being heat-treated and forming crystal film material layer; As one preferred technical scheme further, adopt the heat treatment mode of being annealed in the lehr by the non-crystal thin film of preparation, the hot thin-film electro material of preparation multilayer crystal; As another kind preferred technical scheme further, prepare in thermoelectric film process at sputtering sedimentation, adopt the heat treatment mode directly substrate heated, prepare the hot thin-film electro material of multilayer crystal.
The present invention compared with prior art, has following apparent outstanding substantive distinguishing features and remarkable advantage:
1. multilayer film thermoelectric material preparation method of the present invention comprises selection substrate, selects target and in substrate, make multilayer film thermoelectric material, the mode of sputtering is utilized to prepare multi-layer film structure, thermoelectricity capability and application is controlled by controlling diaphragm layer thickness and the number of plies, overcome the feature of existing thermoelectric material thermoelectricity capability difference, simple to operate, prepared focus conducting material thermoelectricity performance is good, and material tack is good and be easy to suitability for industrialized production;
2. the adhesiveness of gained film of the present invention and substrate is good, and film purity is high, and rete border is obvious, and experimental repeatability is good, and the composition of film and thickness are all controlled;
3. the present invention makes multi-layer film structure relative to additive method has speed fast, and the feature that temperature is low, purity is high, without advantages such as cross pollutions.
Accompanying drawing explanation
Fig. 1 is multilayer film thermoelectric material structure chart prepared by the embodiment of the present invention one technique.
Fig. 2 is the electron scanning micrograph of multilayer film thermoelectric material section prepared by the embodiment of the present invention one technique.
Fig. 3 is the small angle x-ray diffraction (SAXD) figure of multilayer film thermoelectric material prepared by the embodiment of the present invention one technique.
Fig. 4 is multilayer film thermoelectric material structure chart prepared by the embodiment of the present invention two technique.
Fig. 5 is multilayer film thermoelectric material structure chart prepared by the embodiment of the present invention three technique.
Embodiment
Details are as follows for the preferred embodiments of the present invention:
embodiment one:
In the present embodiment, see Fig. 1 ~ Fig. 3, a kind of technique utilizing physical gas-phase deposite method to prepare multilayer film thermoelectric material, comprises the following steps:
A. the selection of substrate and process thereof: selection type of substrate is Si<100>, and its resistivity is 1000 Ω cm.First use BOE solution (hydrogen fluoride: ammonium fluoride=1:5) to soak Si<100> substrate and carry out hydrofluoric acid treatment in 5 minutes, use acetone and ethanolic solution ultrasonic cleaning 10 minutes more respectively, then acetone is used, absolute ethyl alcohol, deionized water is cleaning silicon chip in succession, high pure nitrogen dries up again, is finally placed in drying box dry 15 min under 80 DEG C of conditions after for subsequent use;
B. the selection of target: select mass percent purity purity be 99.99% silicon and silicon germanium material as target, wherein silicon germanium material comprises the germanium of 25wt% silicon and 75wt%;
C. in substrate, multilayer film thermoelectric material is made: base vacuum is 5 × 10
-7torr, substrate does not heat, and keeps the substrate rotating speed of 20rpm in addition, uses rf-mode sputtered silicon and SiGe, both are 100 W by sputtering power, wherein the deposition rate of silicon is approximately 0.2/s, and the deposition rate of SiGe is about 0.21 s, and the thickness controlling silicon and SiGe is respectively 12 nm and 8nm, first deposited silicon layer 2, rear deposition SiGe 3 layers, and alternating deposit totally 20 layers, made multilayer film thermoelectric material structure out as shown in Figure 1.
In the present embodiment, see Fig. 1, in step c, the following order sequential deposition of PVD sample:
[SiGe (8nm)/Si (12nm)] × 10 layers, on substrate 4, deposit 20 layers of thermoelectric material layer composite membrane altogether.
In the present embodiment, Fig. 2 is its sectional drawing of scanning electronic microscope observation for silicon and germanium-silicon layer, and its stratiform is obvious as seen, and border is clearly demarcated.It is obvious that small angle x-ray diffraction (SAXD) figure in Fig. 3 also well describes its stratiform.The thermal conductivity that can obtain this sample by carrying out measurement to thermal conductivity is 1.01W/mK, much smaller than the 5W/mK of buik silicon germanium material.So the multilayer film thermoelectric material rete border adopting the present embodiment method to make is obvious, experimental repeatability is good, and the composition of film and thickness are all controlled.Making multi-layer film structure relative to additive method has speed fast, and the feature that temperature is low, purity is high, all embodies without advantages such as cross pollutions.The present embodiment selects suitable substrate, prepares multilayer film thermoelectric material by reaction magnetocontrol sputtering.In preparation process, different substrates not only can be selected to deposit, also have material category, thicknesses of layers, rete quantity etc. is selected simultaneously.The method layer structure compared with other prepare multilayer film thermoelectric material method is obvious, and precision is high, can reach Nano grade, increase on thermoelectricity capability.Simple to operate, can mass, controllability is good, can prepare rich and varied multilayer film thermoelectric material.The multilayer film thermoelectric material that the present embodiment has prepared rear formation can produce voltage under a fixed difference difference, or forms the temperature difference under certain voltage, can be applied to and be made into Thermoelectric Generator or thermoelectric cooling device.
In the present embodiment, magnetron sputtering technique is divided into again magnetically controlled DC sputtering and rf magnetron sputtering.Magnetron sputtering plating is normally with the positive ion bombardment solid target that argon gas ionization produces, and the neutral atom spilt deposits on substrate, forms rete, thus has " low temperature " and " fast " two major features.Prepare by magnetically controlled sputter method the material with special nature that additive method is not easy to acquisition, therefore applied comparatively extensive.Can be applicable to prepare electroluminescent device, extensive use in electronics and optics; The biomaterial of multilayer film modification can be prepared for bio-medical material aspect; Also can prepare ultrathin membrane system for bioreactor and biology sensor aspect etc.Reaction magnetocontrol sputtering is by introducing some reactivity gas to change or control deposition characteristics when sputter coating, thus controls the composition of film and character.By changing magnetron sputtering parameter and carry out controlling diaphragm layer thickness and rete quantity making multilayer film thermoelectric material, this method is simple, operate substrate without particular/special requirement, the adhesiveness of gained film and substrate is good, film purity is high, rete border is obvious, and experimental repeatability is good, and the composition of film and thickness are all controlled.Therefore this method being applied to the preparation of multilayer film thermoelectric material and research etc. is all play a very important role to thermoelectric material development, in addition this method prepares the shortcoming that multilayer film thermoelectric material overcomes the temperature height time length of the making multilayer film thermoelectric material of traditional a few class Physicals, thus has very large help to the development of thermoelectric material.
embodiment two:
The present embodiment is substantially identical with embodiment one, and special feature is:
In the present embodiment, see Fig. 4, a kind of technique utilizing physical gas-phase deposite method to prepare multilayer film thermoelectric material, comprises the following steps:
A. the selection of substrate and process thereof: this step is identical with embodiment one;
B. the selection of target: select mass percent purity purity be 99.99% silicon and gold as target;
C. in substrate, multilayer film thermoelectric material is made: base vacuum is 5 × 10
-7torr, substrate does not heat, and keeps the substrate rotating speed of 20rpm in addition, use rf-mode sputtered silicon, with DC mode sputtering gold, the sputtering power of silicon is 100 W, its deposition rate is approximately 0.2/s, the sputtering power of gold is 25W, and its deposition rate is about 0.6/s, and the thickness controlling silicon and gold is respectively 12 nm and 16nm, first deposition thereof 1, rear deposited silicon layer 3, alternating deposit totally 20 layers, made multilayer film thermoelectric material structure out as shown in Figure 4.
In the present embodiment, see Fig. 4, in step c, the following order sequential deposition of PVD sample:
[Au (16nm)/Si (12nm)] × 10 layers, on substrate 4, deposit 20 layers of thermoelectric material layer composite membrane altogether.
embodiment three:
The present embodiment and previous embodiment are substantially identical, and special feature is:
In the present embodiment, see Fig. 5, a kind of technique utilizing physical gas-phase deposite method to prepare multilayer film thermoelectric material, comprises the following steps:
A. the selection of substrate and process thereof: this step is identical with embodiment one;
B. the selection of target: select mass percent purity purity be 99.99% silicon, gold and silicon germanium material as target, wherein silicon germanium material comprises the germanium of 25wt% silicon and 75wt%;
C. in substrate, multilayer film thermoelectric material is made: base vacuum is 5 × 10
-7torr, substrate does not heat, and keeps the substrate rotating speed of 20rpm in addition, use rf-mode sputtered silicon and SiGe, the sputtering mode of gold is DC mode, and the sputtering power of silicon is 100 W, and its deposition rate is approximately 0.2/s, the sputtering power of SiGe is 100 W, its deposition rate is approximately 0.21/s, and the sputtering power of gold is 25W, and its deposition rate is about 0.6/s, the thickness controlling silicon, gold and SiGe is respectively 12 nm, 16nm and 8nm.First deposition thereof 1, rear deposited silicon layer 2, then silicon Germanium layer 3, last deposited silicon layer 2, so replace 5 cycle codepositions 20 layers, made multilayer film thermoelectric material structure out as shown in Figure 5.
In the present embodiment, see Fig. 5, in step c, the following order sequential deposition of PVD sample:
[Au (16nm)/Si (12nm)/SiGe (8nm)/Si (12nm)] × 5 layers, on substrate 4, deposit 20 layers of thermoelectric material layer composite membrane altogether.
By reference to the accompanying drawings the embodiment of the present invention is illustrated above; but the invention is not restricted to above-described embodiment; multiple change can also be made according to the object of innovation and creation of the present invention; change, the modification made under all Spirit Essences according to technical solution of the present invention and principle, substitute, combination, to simplify; all should be the substitute mode of equivalence; as long as goal of the invention according to the invention; only otherwise deviating from the present invention utilizes physical gas-phase deposite method to prepare know-why and the inventive concept of the technique of multilayer film thermoelectric material, all protection scope of the present invention is belonged to.
Claims (9)
1. utilize physical gas-phase deposite method to prepare a technique for multilayer film thermoelectric material, it is characterized in that, comprise the following steps:
A. the selection of substrate and process thereof: select substrate as after substrate as required, processed by the substrate of selection, processing method is hydrofluoric acid treatment, then cleans and dry for standby;
B. the selection of target: select purity to be not less than the material of 99.99% as target, described target at least adopts two or more different carrier materials;
C. in substrate, multilayer film thermoelectric material is made: adopt physical gas-phase deposite method to interlock on the substrate of stratified sedimentation after process in described step a successively by the target chosen in described step b, prepare multilayer film, the multilayer film number of plies of accumulative deposition is at least greater than the species number of the target chosen in described step b, preparing in multilayer film process, the thickness of any one deck monofilm is all greater than 5nm.
2. utilize physical gas-phase deposite method to prepare the technique of multilayer film thermoelectric material according to claim 1, it is characterized in that: in described step a, semiconductor, sheet glass, sheet metal, polymer sheet or microdevice are chosen in described substrate.
3. utilize physical gas-phase deposite method to prepare the technique of multilayer film thermoelectric material according to claim 1, it is characterized in that: in described step b, when target is selected, the carrier material of selection be in metal, semiconductor and insulator any one or several arbitrarily.
4. utilize physical gas-phase deposite method to prepare the technique of multilayer film thermoelectric material according to claim 3, it is characterized in that: in described step a, when target is selected, the carrier material of selection is three kinds or any bi-materials in gold, silicon and SiGe.
5. utilize physical gas-phase deposite method to prepare the technique of multilayer film thermoelectric material according to claim 1, it is characterized in that: in described step c, physical gas-phase deposite method adopt in electron beam evaporation, molecular beam epitaxy film deposition, direct current reaction magnetron sputtering and radio frequency magnetron sputtering method any one or several arbitrarily.
6. utilize physical gas-phase deposite method to prepare the technique of multilayer film thermoelectric material according to claim 5, it is characterized in that: in described step c, by any one in control substrate temperature, sputtering time, reacting gas content and sputtering power or any several parameter, be controlled to thicknesses of layers and film formation time.
7. according to utilizing physical gas-phase deposite method to prepare the technique of multilayer film thermoelectric material in claim 1 ~ 6 described in any one, it is characterized in that: in described step c, when preparing multilayer film thermoelectric material, each layer non-crystal thin film prepared being heat-treated and forms crystal film material layer.
8. utilize physical gas-phase deposite method to prepare the technique of multilayer film thermoelectric material according to claim 7, it is characterized in that: in described step c, adopt the heat treatment mode of being annealed in the lehr by the non-crystal thin film of preparation, the hot thin-film electro material of preparation multilayer crystal.
9. utilize physical gas-phase deposite method to prepare the technique of multilayer film thermoelectric material according to claim 7, it is characterized in that: in described step c, prepare in thermoelectric film process at sputtering sedimentation, adopt the heat treatment mode directly substrate heated, prepare the hot thin-film electro material of multilayer crystal.
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Cited By (4)
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| CN105576111A (en) * | 2016-01-26 | 2016-05-11 | 电子科技大学 | Preparation method of bismuth-layered compound superlattice |
| WO2017028467A1 (en) * | 2015-08-17 | 2017-02-23 | 宁波中车时代传感技术有限公司 | Semiconductor silicon-germanium thin film preparation method |
| CN106505046A (en) * | 2016-10-17 | 2017-03-15 | 中国石油大学(华东) | A kind of carbon aluminium carbon semiconductor film material with insulating substrate as substrate and preparation method thereof |
| WO2018084727A1 (en) | 2016-11-03 | 2018-05-11 | Aic Spółka Akcyjna | Thin thermoelectric layer |
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| CN101969095A (en) * | 2010-08-26 | 2011-02-09 | 中山大学 | Quasi one-dimensional nano structural thermoelectric material, device and preparation method thereof |
| US8841539B2 (en) * | 2012-03-25 | 2014-09-23 | Fayetteville State University | High efficiency thermoelectric device |
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| US20070235070A1 (en) * | 2006-04-10 | 2007-10-11 | Alabama A&M University Research Institute | Efficient thermoelectric device |
| US20100221861A1 (en) * | 2006-04-10 | 2010-09-02 | Alabama A&M University Research Institute | Efficient Thermoelectric Device and Associated Method |
| CN101969095A (en) * | 2010-08-26 | 2011-02-09 | 中山大学 | Quasi one-dimensional nano structural thermoelectric material, device and preparation method thereof |
| US8841539B2 (en) * | 2012-03-25 | 2014-09-23 | Fayetteville State University | High efficiency thermoelectric device |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017028467A1 (en) * | 2015-08-17 | 2017-02-23 | 宁波中车时代传感技术有限公司 | Semiconductor silicon-germanium thin film preparation method |
| US10392691B2 (en) | 2015-08-17 | 2019-08-27 | Ningbo CRRC Times Transducer Technology Co., Ltd. | Semiconductor silicon-germanium thin film preparation method |
| CN105576111A (en) * | 2016-01-26 | 2016-05-11 | 电子科技大学 | Preparation method of bismuth-layered compound superlattice |
| CN105576111B (en) * | 2016-01-26 | 2017-12-29 | 电子科技大学 | A kind of preparation method of bismuth layer-like compound superlattices |
| CN106505046A (en) * | 2016-10-17 | 2017-03-15 | 中国石油大学(华东) | A kind of carbon aluminium carbon semiconductor film material with insulating substrate as substrate and preparation method thereof |
| CN106505046B (en) * | 2016-10-17 | 2018-11-20 | 中国石油大学(华东) | It is a kind of using insulating substrate as carbon-aluminium-carbon semiconductor film material of substrate and preparation method thereof |
| WO2018084727A1 (en) | 2016-11-03 | 2018-05-11 | Aic Spółka Akcyjna | Thin thermoelectric layer |
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