CN106222611A - A kind of MF reactive magnetron sputtering preparation method of AlN piezoelectric membrane - Google Patents

A kind of MF reactive magnetron sputtering preparation method of AlN piezoelectric membrane Download PDF

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Publication number
CN106222611A
CN106222611A CN201610841057.3A CN201610841057A CN106222611A CN 106222611 A CN106222611 A CN 106222611A CN 201610841057 A CN201610841057 A CN 201610841057A CN 106222611 A CN106222611 A CN 106222611A
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sputtering
piezoelectric membrane
aln
magnetron sputtering
reactive magnetron
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王文庆
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Dongguan Lianzhou Intellectual Property Operation and Management Co Ltd
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Dongguan Lianzhou Intellectual Property Operation and Management Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0617—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
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  • Mechanical Engineering (AREA)
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  • Organic Chemistry (AREA)
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Abstract

The present invention relates to the preparation field of wide bandgap semiconductor, particularly to the MF reactive magnetron sputtering preparation method of a kind of AlN piezoelectric membrane, comprise the following steps: (1) substrate pre-treatment；(2) target pretreatment；(3) it is passed through N2, Ar mixed gas sputtering sedimentation bottom AlN thin film；(4) it is passed through N2, Ar mixed gas sputtering sedimentation AlN thin film, N2Content constant, increase gas atmosphere in cavity.The AlN thin film that the inventive method is prepared has the preferred orientation growth of (002) face, and surface grain size is uniform, the advantage that surface roughness is little, is the high-quality AlN piezoelectric membrane being suitable for making SAW device.

Description

A kind of MF reactive magnetron sputtering preparation method of AlN piezoelectric membrane
Technical field
The present invention relates to the preparation field of wide bandgap semiconductor, the intermediate frequency particularly to a kind of AlN piezoelectric membrane reacts magnetic Control sputtering preparation method.
Background technology
III-V compounds of group aluminium nitride (AlN) is a kind of semiconductor material with wide forbidden band with hexagonal Pb-Zn deposits structure, tool There are physics and the chemical characteristic of a series of excellence.In bulk acoustic wave device field, FBAR filter has body Long-pending little, be lost low, can the advantage such as integrated, high workload frequency and high power ability to bear, before being currently the only radio frequency that can be integrated End filter, it needs to have good chemical stability, high heat conductance, big disruptive field intensity, the high velocity of sound, high electromechanical coupling Number and piezoelectric compatible with semiconductor technology, aluminium nitride (AlN) thin film can meet these requirements well, become Developing the first-selected piezoelectric of bulk acoustic wave device, aluminium nitride (AlN) thin film of (002) face preferred orientation more can meet surface acoustic wave The requirement of device.
At present, there is multiple method can prepare the aluminium nitride film of (002) face preferential growth, but the most optimal Method is intermediate frequency (40KHz) reactive magnetron sputtering method.MF reactive magnetron sputtering, compared to metal-organic chemical vapor deposition equipment (MOCVD), the method for manufacturing thin film such as pulsed laser deposition (PLD), molecular beam epitaxy (MBE) there is low growth temperature, Seedling height Speed, low cost, large area film deposition can be realized, and meet the advantage such as requirement of large-scale industrial production.
But in medium frequency reactive sputtering technology, there is the phenomenon of film surface abnormal grain growth, film surface will The aluminium nitride bulky grain of some micrometer-submicrometer levels there is, the uneven piezoelectric property that can affect aluminium nitride film of crystallite dimension Harmony propagation velocity, and the bulky grain of the micrometer-submicrometer level on surface can be to the manufacture of ensuing SAW device The consequence of bringing on a disaster property, makes the interdigital electrode (IDT) of SAW device that fracture or short circuit to occur, thus causes device Can lose efficacy.
Summary of the invention
It is an object of the invention to provide the MF reactive magnetron sputtering preparation method of a kind of AlN piezoelectric membrane, the party's legal system Standby AlN piezoelectric membrane grain surface size uniform, and grow in (002) face preferred orientation.
For achieving the above object, the present invention is by the following technical solutions:
The MF reactive magnetron sputtering preparation method of a kind of AlN piezoelectric membrane, comprises the following steps:
(1) substrate pre-treatment；
(2) target pretreatment；
(3) it is passed through N2, Ar mixed gas sputtering sedimentation bottom AlN thin film, sputtering sedimentation time 20min～90min, wherein N2Content account for 20%～30%；
(4) it is passed through N2, Ar mixed gas sputtering sedimentation AlN thin film, N2Content constant, increase gas atmosphere in cavity, spatter Penetrate sedimentation time 5min～15min.
Preferably, substrate pre-treatment includes cleaning substrate and substrate being carried out reverse sputtering.
More selection of land, carries out reverse sputtering at N to substrate2, carry out under Ar mixed-gas atmosphere.
Preferably, target pretreatment includes vacuum pre-treatment, logical Ar target pre-sputtering and logical N2Target pre-sputtering.
Preferably, vacuum pre-treatment is evacuated to 1 × 10-5Below Pa.
Preferably, gas atmosphere 0.2Pa～0.5Pa in step (3) cavity.
Preferably, in step (4) cavity, gas atmosphere increases to 0.7Pa～1Pa.
Preferably, in regulation sputtering chamber body during gas atmosphere, slowly regulating gas atmosphere, regulations speed is maintained at 1sccm/ Between min～4sccm/min.
Preferably, step (3), (4) are circulated repeatedly.
Preferably, step (3), (4) circulation repeat 2～5 times.
Preferably, sputtering power 2000W～2300W.
Compared with prior art, the invention have the advantages that
(1) low N is started2Content 20%～30% is conducive to (002) face preferential growth, if to substrate at N2, Ar mixed gas Carrying out reverse sputtering under atmosphere, the substrate surface that nitrogen terminates is more conducive to (002) face preferential growth；
(2) relatively low gas atmosphere is conducive to (002) face preferential growth, and of a relatively high gas atmosphere can make film surface Crystallite dimension is the most tiny, and surface roughness is less, and low gas atmosphere and high gas atmosphere interval growth can make thin film At (002) face preferential growth, crystallite dimension and roughness can be reduced, it is thus achieved that smooth surface simultaneously.
Therefore, the AlN thin film that the inventive method is prepared has the preferred orientation growth of (002) face, and surface grain size is equal Even, that surface roughness is little advantage, is the high-quality AlN piezoelectric membrane being suitable for making SAW device.
Detailed description of the invention
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving Release the present invention, the present invention will not be constituted any restriction.
Gases used purity Ar of the embodiment of the present invention (99.999%), N2And H (99.999%)2(99.999%), target Purity Al (99.999%), target-substrate distance 80mm, sputtering power 2100W, sputter under the non-heating state of underlayer temperature room temperature.
In order to prove that AlN thin film prepared by the present invention is the high-quality having significant application value in SAW device Film, uses D/MAX-2200 type X-ray diffractometer (XRD) of science to characterize the structure of AlN thin film, with chemistry institute of Chinese Academy of Sciences basis Nanometer instrument company produce CSPM-3100 type atomic force microscope (AFM) come the pattern on viewing film surface, granular size and Surface roughness.
Embodiment 1
The MF reactive magnetron sputtering preparation method of a kind of AlN piezoelectric membrane, comprises the following steps:
(1) substrate pre-treatment；
Substrate pre-treatment includes cleaning substrate and substrate being carried out reverse sputtering.
Substrate selects the Al atom N row of the Si (111) of finishing polish, the arrangement of Si (111) surface atom and wurtzite structure Arrange similar, it is thus possible to obtain high-quality Al N thin film；
Clean substrate: the Si (111) of polishing is immersed in acetone soln and carries out ultrasonic Treatment 15 minutes, then mixed by essence Close in liquid 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l) and boil 5 minutes, then with mixed liquor 2 (deionized water: peroxidating Hydrogen: hydrochloric acid=7:2:1) boil 5 minutes, carry out ultrasonic Treatment the most in deionized water 20 minutes, to remove silicon chip surface Organic substance that may be present, puts into after taking-up and is filled with pure N2Drying baker in be heated to 100 DEG C dry 1 hour.
Substrate is carried out reverse sputtering: cleaned Si (111) substrate is positioned over the sample of medium frequency magnetron reaction sputtering system In sample platform, close cavity；Normally start magnetron sputtering apparatus, cavity is evacuated to 0.8 × 10-5Pa；Then pass to Ar gas, To Si (111) substrate reverse sputtering 15 minutes, remove silicon chip surface oxide layer that may be present, to obtain pure growing surface.
(2) target pretreatment；
Al target is arranged on main sputtering chamber, finally with sample guide rod, the main sputtering chamber that silicon chip feeding has been pumped through vacuum is prepared Deposition, closes cavity, normally starts magnetron sputtering apparatus, cavity is evacuated to 0.8 × 10-5Pa, first keeps off baffle plate before deposition On, it is filled with Ar gas, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer, turns off Ar gas, is passed through N2Gas, spatters in advance Penetrate 10min.
(3) in vacuum cavity, it is passed through N simultaneously2, Ar mixed gas, and make wherein N2Content account for 23%, gas atmosphere 0.27Pa, opens baffle plate after aura is stable, starts sputtering sedimentation bottom AlN thin film, sputtering sedimentation 60min；
(4) baffle plate is blocked, continue to be passed through N2, Ar, N2Content constant, gas atmosphere increases to 0.72Pa, treats that aura is stable After open baffle plate, start sputtering sedimentation middle level AlN thin film, sputtering sedimentation 13min；
XRD result shows, the present embodiment AlN thin film only goes out AlN (002) crystallographic plane diffraction peak near 36 °, illustrates that thin film exists (002) face preferential growth；AFM plane attempts result and shows, the intercrystalline of AlN thin film is fine and close and uniform, grain size distribution 50nm～70nm, AFM 3-D view display film surface is smooth, uniformity, and its r.m.s. roughness (RMS) is 4.7nm。
Embodiment 2
The MF reactive magnetron sputtering preparation method of a kind of AlN piezoelectric membrane, comprises the following steps:
(1) substrate pre-treatment；
Substrate pre-treatment includes cleaning substrate and substrate being carried out reverse sputtering.
Substrate selects the Si (111) of finishing polish；
Clean substrate: the Si (111) of polishing is immersed in acetone soln and carries out ultrasonic Treatment 15 minutes, then mixed by essence Close in liquid 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l) and boil 5 minutes, then with mixed liquor 2 (deionized water: peroxidating Hydrogen: hydrochloric acid=7:2:1) boil 5 minutes, carry out ultrasonic Treatment the most in deionized water 20 minutes, to remove silicon chip surface Organic substance that may be present, puts into after taking-up and is filled with pure N2Drying baker in be heated to 100 DEG C dry 1 hour.
Substrate is carried out reverse sputtering: cleaned Si (111) substrate is positioned over the sample of medium frequency magnetron reaction sputtering system In sample platform, close cavity；Normally start magnetron sputtering apparatus, cavity is evacuated to 0.8 × 10-5Pa；Then pass to N2, Ar mix Close gas, to Si (111) substrate reverse sputtering 15 minutes, remove silicon chip surface oxide layer that may be present, to obtain pure life Long surface, is passed through N2A large amount of nitrogen particles arrive surface of silicon, are formed the surface of silicon that nitrogen terminates, prevent silicon further Sheet surface oxidation, more effectively removes the impurity such as deoxygenation, advantageously reduces the defect of deposition thin film, makes thin film crystallization better quality, with Time nitrogen terminate surface of silicon be more conducive to thin film at (002) face preferential growth.
(2) target pretreatment；
Al target is arranged on main sputtering chamber, finally with sample guide rod, the main sputtering chamber that silicon chip feeding has been pumped through vacuum is prepared Deposition, closes cavity, normally starts magnetron sputtering apparatus, cavity is evacuated to 0.9 × 10-5Pa, first keeps off baffle plate before deposition On, it is filled with Ar gas, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer, turns off Ar gas, is passed through N2Gas, spatters in advance Penetrate 10min.
(3) in vacuum cavity, it is passed through N simultaneously2, Ar mixed gas, and make wherein N2Content account for 23%, gas atmosphere 0.41Pa, opens baffle plate after aura is stable, starts sputtering sedimentation bottom AlN thin film, sputtering sedimentation 60min；
(4) baffle plate is blocked, continue to be passed through N2, Ar, N2Content constant, gas atmosphere increases to 0.72Pa, treats that aura is stable After open baffle plate, start sputtering sedimentation middle level AlN thin film, sputtering sedimentation 10min；
In the present embodiment regulation sputtering chamber body during gas atmosphere, gas regulation speed is maintained at 1sccm/min～4sccm/ Between min.
XRD result shows, the present embodiment AlN thin film only goes out AlN (002) crystallographic plane diffraction peak near 36 °, illustrates that thin film exists (002) face preferential growth；AFM plane attempts result and shows, the intercrystalline of AlN thin film is fine and close and uniform, grain size distribution 50nm～65nm, AFM 3-D view display film surface is smooth, uniformity, and its r.m.s. roughness (RMS) is 4.3nm。
Embodiment 3
The MF reactive magnetron sputtering preparation method of a kind of AlN piezoelectric membrane, comprises the following steps:
(1) substrate pre-treatment；
Substrate pre-treatment includes cleaning substrate and substrate being carried out reverse sputtering.
Substrate selects the Si (111) of finishing polish；
Clean substrate: the Si (111) of polishing is immersed in acetone soln and carries out ultrasonic Treatment 15 minutes, then mixed by essence Close in liquid 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l) and boil 5 minutes, then with mixed liquor 2 (deionized water: peroxidating Hydrogen: hydrochloric acid=7:2:1) boil 5 minutes, carry out ultrasonic Treatment the most in deionized water 20 minutes, to remove silicon chip surface Organic substance that may be present, puts into after taking-up and is filled with pure N2Drying baker in be heated to 100 DEG C dry 1 hour.
Substrate is carried out reverse sputtering: cleaned Si (111) substrate is positioned over the sample of medium frequency magnetron reaction sputtering system In sample platform, close cavity；Normally start magnetron sputtering apparatus, cavity is evacuated to 0.9 × 10-5Pa；Then pass to N2, Ar mix Close gas, to Si (111) substrate reverse sputtering 15 minutes, remove silicon chip surface oxide layer that may be present, to obtain pure life Long surface, is passed through N2A large amount of nitrogen particles arrive surface of silicon, are formed the surface of silicon that nitrogen terminates, prevent silicon further Sheet surface oxidation, more effectively removes the impurity such as deoxygenation, advantageously reduces the defect of deposition thin film, makes thin film crystallization better quality.
(2) target pretreatment；
Al target is arranged on main sputtering chamber, finally with sample guide rod, the main sputtering chamber that silicon chip feeding has been pumped through vacuum is prepared Deposition, closes cavity, normally starts magnetron sputtering apparatus, cavity is evacuated to 0.7 × 10-5Pa, first keeps off baffle plate before deposition On, it is filled with Ar gas, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer, turns off Ar gas, is passed through N2Gas, spatters in advance Penetrate 10min.
(3) in vacuum cavity, it is passed through N simultaneously2, Ar mixed gas, and make wherein N2Content account for 27%, gas atmosphere 0.32Pa, opens baffle plate after aura is stable, starts sputtering sedimentation bottom AlN thin film, sputtering sedimentation 70min；
(4) baffle plate is blocked, continue to be passed through N2, Ar, N2Content constant, gas atmosphere increases to 0.87Pa, treats that aura is stable After open baffle plate, start sputtering sedimentation middle level AlN thin film, sputtering sedimentation 15min；
In the present embodiment regulation sputtering chamber body during gas atmosphere, gas regulation speed is maintained at 1sccm/min～4sccm/ Between min.
XRD result shows, the present embodiment AlN thin film only goes out AlN (002) crystallographic plane diffraction peak near 36 °, illustrates that thin film exists (002) face preferential growth；AFM plane attempts result and shows, the intercrystalline of AlN thin film is fine and close and uniform, grain size distribution 45nm～55nm, AFM 3-D view display film surface is smooth, uniformity, and its r.m.s. roughness (RMS) is 4.1nm。
Embodiment 4
The MF reactive magnetron sputtering preparation method of a kind of AlN piezoelectric membrane, comprises the following steps:
(1) substrate pre-treatment；
Substrate pre-treatment includes cleaning substrate and substrate being carried out reverse sputtering.
Substrate selects the Si (111) of finishing polish；
Clean substrate: the Si (111) of polishing is immersed in acetone soln and carries out ultrasonic Treatment 15 minutes, then mixed by essence Close in liquid 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l) and boil 5 minutes, then with mixed liquor 2 (deionized water: peroxidating Hydrogen: hydrochloric acid=7:2:1) boil 5 minutes, carry out ultrasonic Treatment the most in deionized water 20 minutes, to remove silicon chip surface Organic substance that may be present, puts into after taking-up and is filled with pure N2Drying baker in be heated to 100 DEG C dry 1 hour.
Substrate is carried out reverse sputtering: cleaned Si (111) substrate is positioned over the sample of medium frequency magnetron reaction sputtering system In sample platform, close cavity；Normally start magnetron sputtering apparatus, cavity is evacuated to 0.8 × 10-5Pa；Then pass to N2, Ar mix Close gas, to Si (111) substrate reverse sputtering 15 minutes, remove silicon chip surface oxide layer that may be present, to obtain pure life Long surface, is passed through N2A large amount of nitrogen particles arrive surface of silicon, are formed the surface of silicon that nitrogen terminates, prevent silicon further Sheet surface oxidation, more effectively removes the impurity such as deoxygenation, advantageously reduces the defect of deposition thin film, makes thin film crystallization better quality.
(2) target pretreatment；
Al target is arranged on main sputtering chamber, finally with sample guide rod, the main sputtering chamber that silicon chip feeding has been pumped through vacuum is prepared Deposition, closes cavity, normally starts magnetron sputtering apparatus, cavity is evacuated to 0.7 × 10-5Pa, first keeps off baffle plate before deposition On, it is filled with Ar gas, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer, turns off Ar gas, is passed through N2Gas, spatters in advance Penetrate 10min.
(3) in vacuum cavity, it is passed through N simultaneously2, Ar mixed gas, and make wherein N2Content account for 25%, gas atmosphere 0.35Pa, opens baffle plate after aura is stable, starts sputtering sedimentation bottom AlN thin film, sputtering sedimentation 30min；
(4) baffle plate is blocked, continue to be passed through N2, Ar, N2Content constant, gas atmosphere increases to 0.80Pa, treats that aura is stable After open baffle plate, start sputtering sedimentation middle level AlN thin film, sputtering sedimentation 10min；
Next step (3), (4) circulation are repeated 2 times.
In the present embodiment regulation sputtering chamber body during gas atmosphere, gas regulation speed is maintained at 1sccm/min～4sccm/ Between min.
XRD result shows, the present embodiment AlN thin film only goes out AlN (002) crystallographic plane diffraction peak near 36 °, illustrates that thin film exists (002) face preferential growth；AFM plane attempts result and shows, the intercrystalline of AlN thin film is fine and close and uniform, grain size distribution 48nm～55nm, AFM 3-D view display film surface is smooth, uniformity, and its r.m.s. roughness (RMS) is 3.5nm。
Embodiment 5
The MF reactive magnetron sputtering preparation method of a kind of AlN piezoelectric membrane, comprises the following steps:
(1) substrate pre-treatment；
Substrate pre-treatment includes cleaning substrate and substrate being carried out reverse sputtering.
Substrate selects the Si (111) of finishing polish；
Clean substrate: the Si (111) of polishing is immersed in acetone soln and carries out ultrasonic Treatment 15 minutes, then mixed by essence Close in liquid 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l) and boil 5 minutes, then with mixed liquor 2 (deionized water: peroxidating Hydrogen: hydrochloric acid=7:2:1) boil 5 minutes, carry out ultrasonic Treatment the most in deionized water 20 minutes, to remove silicon chip surface Organic substance that may be present, puts into after taking-up and is filled with pure N2Drying baker in be heated to 100 DEG C dry 1 hour.
Substrate is carried out reverse sputtering: cleaned Si (111) substrate is positioned over the sample of medium frequency magnetron reaction sputtering system In sample platform, close cavity；Normally start magnetron sputtering apparatus, cavity is evacuated to 0.6 × 10-5Pa；Then pass to N2, Ar mix Close gas, to Si (111) substrate reverse sputtering 15 minutes, remove silicon chip surface oxide layer that may be present, to obtain pure life Long surface, is passed through N2A large amount of nitrogen particles arrive surface of silicon, are formed the surface of silicon that nitrogen terminates, prevent silicon further Sheet surface oxidation, more effectively removes the impurity such as deoxygenation, advantageously reduces the defect of deposition thin film, makes thin film crystallization better quality.
(2) target pretreatment；
Al target is arranged on main sputtering chamber, finally with sample guide rod, the main sputtering chamber that silicon chip feeding has been pumped through vacuum is prepared Deposition, closes cavity, normally starts magnetron sputtering apparatus, cavity is evacuated to 0.9 × 10-5Pa, first keeps off baffle plate before deposition On, it is filled with Ar gas, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer, turns off Ar gas, is passed through N2Gas, spatters in advance Penetrate 10min.
(3) in vacuum cavity, it is passed through N simultaneously2, Ar mixed gas, and make wherein N2Content account for 20%, gas atmosphere 0.47Pa, opens baffle plate after aura is stable, starts sputtering sedimentation bottom AlN thin film, sputtering sedimentation 20min；
(4) baffle plate is blocked, continue to be passed through N2, Ar, N2Content constant, gas atmosphere increases to 0.80Pa, treats that aura is stable After open baffle plate, start sputtering sedimentation middle level AlN thin film, sputtering sedimentation 8min；
Next step (3), (4) circulation are repeated 3 times.
In the present embodiment regulation sputtering chamber body during gas atmosphere, gas regulation speed is maintained at 1sccm/min～4sccm/ Between min.
XRD result shows, the present embodiment AlN thin film only goes out AlN (002) crystallographic plane diffraction peak near 36 °, illustrates that thin film exists (002) face preferential growth；AFM plane attempts result and shows, the intercrystalline of AlN thin film is fine and close and uniform, grain size distribution 40nm～50nm, AFM 3-D view display film surface is smooth, uniformity, and its r.m.s. roughness (RMS) is 2.9nm。
Embodiment 6
The MF reactive magnetron sputtering preparation method of a kind of AlN piezoelectric membrane, comprises the following steps:
(1) substrate pre-treatment；
Substrate pre-treatment includes cleaning substrate and substrate being carried out reverse sputtering.
Substrate selects the Si (111) of finishing polish；
Clean substrate: the Si (111) of polishing is immersed in acetone soln and carries out ultrasonic Treatment 15 minutes, then mixed by essence Close in liquid 1 (deionized water: hydrogen peroxide: fluorine water=5:2:l) and boil 5 minutes, then with mixed liquor 2 (deionized water: peroxidating Hydrogen: hydrochloric acid=7:2:1) boil 5 minutes, carry out ultrasonic Treatment the most in deionized water 20 minutes, to remove silicon chip surface Organic substance that may be present, puts into after taking-up and is filled with pure N2Drying baker in be heated to 100 DEG C dry 1 hour.
Substrate is carried out reverse sputtering: cleaned Si (111) substrate is positioned over the sample of medium frequency magnetron reaction sputtering system In sample platform, close cavity；Normally start magnetron sputtering apparatus, cavity is evacuated to 0.8 × 10-5Pa；Then pass to N2, Ar mix Close gas, to Si (111) substrate reverse sputtering 15 minutes, remove silicon chip surface oxide layer that may be present, to obtain pure life Long surface, is passed through N2A large amount of nitrogen particles arrive surface of silicon, are formed the surface of silicon that nitrogen terminates, prevent silicon further Sheet surface oxidation, more effectively removes the impurity such as deoxygenation, advantageously reduces the defect of deposition thin film, makes thin film crystallization better quality.
(2) target pretreatment；
Al target is arranged on main sputtering chamber, finally with sample guide rod, the main sputtering chamber that silicon chip feeding has been pumped through vacuum is prepared Deposition, closes cavity, normally starts magnetron sputtering apparatus, cavity is evacuated to 0.8 × 10-5Pa, first keeps off baffle plate before deposition On, it is filled with Ar gas, by Al target elder generation pre-sputtering 15min, to remove the Al of target surface2O3Layer, turns off Ar gas, is passed through N2Gas, spatters in advance Penetrate 10min.
(3) in vacuum cavity, it is passed through N simultaneously2, Ar mixed gas, and make wherein N2Content account for 20%, gas atmosphere 0.39Pa, opens baffle plate after aura is stable, starts sputtering sedimentation bottom AlN thin film, sputtering sedimentation 20min；
(4) baffle plate is blocked, continue to be passed through N2, Ar, N2Content constant, gas atmosphere increases to 0.92Pa, treats that aura is stable After open baffle plate, start sputtering sedimentation middle level AlN thin film, sputtering sedimentation 7min；
Next step (3), (4) circulation are repeated 4 times.
In the present embodiment regulation sputtering chamber body during gas atmosphere, gas regulation speed is maintained at 1sccm/min～4sccm/ Between min.
XRD result shows, the present embodiment AlN thin film only goes out AlN (002) crystallographic plane diffraction peak near 36 °, illustrates that thin film exists (002) face preferential growth；AFM plane attempts result and shows, the intercrystalline of AlN thin film is fine and close and uniform, grain size distribution 45nm～55nm, AFM 3-D view display film surface is smooth, uniformity, and its r.m.s. roughness (RMS) is 2.7nm。

Claims (10)

1. the MF reactive magnetron sputtering preparation method of an AlN piezoelectric membrane, it is characterised in that comprise the following steps:
(1) substrate pre-treatment；
(2) target pretreatment；
(3) it is passed through N2, Ar mixed gas sputtering sedimentation bottom AlN thin film, sputtering sedimentation time 20min～90min, wherein N2's Content accounts for 20%～30%；
(4) it is passed through N2, Ar mixed gas sputtering sedimentation AlN thin film, N2Content constant, increase gas atmosphere in cavity, sputtering is heavy Long-pending time 5min～15min.
The MF reactive magnetron sputtering preparation method of AlN piezoelectric membrane the most according to claim 1, it is characterised in that: lining End pretreatment includes cleaning substrate and substrate being carried out reverse sputtering.
The MF reactive magnetron sputtering preparation method of AlN piezoelectric membrane the most according to claim 2, it is characterised in that: right Substrate carries out reverse sputtering at N2, carry out under Ar mixed-gas atmosphere.
The MF reactive magnetron sputtering preparation method of AlN piezoelectric membrane the most according to claim 1, it is characterised in that: target Material pretreatment includes vacuum pre-treatment, logical Ar target pre-sputtering and logical N2Target pre-sputtering.
The MF reactive magnetron sputtering preparation method of AlN piezoelectric membrane the most according to claim 4, it is characterised in that: true Empty pretreatment is evacuated to 1 × 10-5Below Pa.
The MF reactive magnetron sputtering preparation method of AlN piezoelectric membrane the most according to claim 1, it is characterised in that: step Suddenly gas atmosphere 0.2Pa～0.5Pa in (3) cavity.
The MF reactive magnetron sputtering preparation method of AlN piezoelectric membrane the most according to claim 1, it is characterised in that: step Suddenly in (4) cavity, gas atmosphere increases to 0.7Pa～1Pa.
The MF reactive magnetron sputtering preparation method of AlN piezoelectric membrane the most according to claim 1, it is characterised in that: adjust Joint sputtering chamber body in gas atmosphere time, slowly regulate gas atmosphere, regulations speed be maintained at 1sccm/min～4sccm/min it Between.
The MF reactive magnetron sputtering preparation method of AlN piezoelectric membrane the most according to claim 1, it is characterised in that: step Suddenly (3), (4) are circulated repeatedly.
The MF reactive magnetron sputtering preparation method of AlN piezoelectric membrane the most according to claim 1, it is characterised in that: step Suddenly (3), (4) circulation repeat 2～5 times.
CN201610841057.3A 2016-09-22 2016-09-22 A kind of MF reactive magnetron sputtering preparation method of AlN piezoelectric membrane Pending CN106222611A (en)

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CN109962129A (en) * 2019-01-28 2019-07-02 华灿光电（浙江）有限公司 The preparation method of AlN template and gallium nitride based LED epitaxial slice
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