CN106169414A - A kind of preparation method of stress controllable type silica-base film - Google Patents
A kind of preparation method of stress controllable type silica-base film Download PDFInfo
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- CN106169414A CN106169414A CN201610712335.5A CN201610712335A CN106169414A CN 106169414 A CN106169414 A CN 106169414A CN 201610712335 A CN201610712335 A CN 201610712335A CN 106169414 A CN106169414 A CN 106169414A
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- base film
- stress
- preparation
- silica
- controllable type
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02524—Group 14 semiconducting materials
- H01L21/02532—Silicon, silicon germanium, germanium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
Abstract
The invention discloses the preparation method of a kind of stress controllable type silica-base film, including using single-frequency PECVD device to make unstrpped gas deposit on backing material by chemical vapour deposition technique, grow, obtain silica-base film, in unstrpped gas, during preparation, be passed through He and N2Process, process of the present invention is simple, and controllability is high, can prepare in the PECVD device in Single frequency RF source that can adjust on a large scale between compressive stress and tensile stress, uniformity is good, compactness is high, the silica-base film of low cost.
Description
Technical field
The present invention relates to the technical field of silica-base film.
Background technology
Along with the constantly extension of traditional optical, information optics, light and wireless telecommunications and computer technology, vacuum technique,
Developing rapidly of light and microelectric technique, thin-film optical filters and thin film electronic device have obtained increasingly extensive application, as
In the semiconductor device as the silica-base film of the materials'uses such as surface passivation, metal level spacer medium, condenser dielectric.
Different application is different to the requirement of silica-base film performance, and the particularly requirement to membrane stress is different, and thin film should
The character of power and size directly affect the performance of membrane element device, yield rate, stability and reliability.Therefore preparation meets difference and answers
The silica-base film that power requires is one of critical process for semiconductor device.
One of the most conventional and effectively regulation silica-base film stress method is to use to be configured with low-and high-frequency radio frequency simultaneously
The PECVD device in source prepares silica-base film, and the silica-base film deposited under the effect of high-frequency radio frequency source under normal circumstances presents to open answers
Power, the effect lower silica-base film deposited in low frequency radio frequency source presents compressive stress, by low-and high-frequency process alternately, the stress of thin film
The conversion being achieved between tensile stress and compressive stress.
The most conventional and effectively regulation silica-base film stress another kind of method is two kinds that selection stress characteristics is contrary
Silica-base film is combined, and such as nitridation silicon/oxidative silicon duplicature, obtains stress equilibrium, thus obtains the thin film fitted mutually with device
Material.Why use duplicature or the mode of multilayer film combination, rather than monofilm carried out thickness or Adjusting Shape, be because of with
Macro-scale material is different, and change in film thickness and the impact of Adjusting Shape counter stress size in nano-scale range have very much
Limit, it is impossible to obtain intended effect.
Summary of the invention
It is an object of the invention to provide a kind of that can prepare in the PECVD device in Single frequency RF source, monofilm i.e.
That can adjust on a large scale between compressive stress and tensile stress, uniformity is good, compactness is high, the preparation side of the silica-base film of low cost
Method.
Technical scheme is as follows:
The preparation method of a kind of stress controllable type silica-base film, it uses single-frequency PECVD device to be made by chemical vapour deposition technique
Unstrpped gas deposits on backing material, grows, and obtains silica-base film, is passed through He and N during preparation in unstrpped gas2。
In this technical scheme, He and N2Adding as regulation gas, wherein He forms He etc. in single-frequency PECVD device
Gas ions, for other conventional inertia regulation gas, it has higher thermal conductivity, improves reaction chamber diameter model
Enclose interior reactant and the uniformity of product heat distribution, N simultaneously2Addition have adjusted the N in plasma atmosphere2 +Dividing of ion
Cloth, the existence of He also further promotes N2 +Being uniformly distributed of ion, i.e. both have regulation silica-base film the most independently
, there is cooperative effect in the effect of Forming Quality, add SiN by common effect simultaneously each otherXThe combination of Si-N in thin film
Ability, improves uniformity and the compactness of thin film.
A kind of embodiment of above-mentioned preparation method is: described N2It is 0 ~ 10 with the flow-rate ratio of He, does not include endpoint value 0.
The stress requirement of this embodiment correspondence silica-base film, under this embodiment effect, the stress of silica-base film can
Tune scope is compressive stress-1500Mpa ~ tensile stress 2000Mpa, and along with the further raising of flow-rate ratio, tensile stress also can be further
Improve.
Its further embodiment is: described N2It is 0 ~ 1 with the flow-rate ratio of He, does not include endpoint value 0.
The stress requirement of this embodiment correspondence silica-base film, under this embodiment effect, the stress of silica-base film can
Tune scope is compressive stress-1500Mpa ~ tensile stress 500Mpa.
The another embodiment of the preparation method of described stress controllable type silica-base film is: described silica-base film is for being selected from
SiN thin film, SiO2One or more in thin film, SiON thin film.
Its further embodiment is: described unstrpped gas is for selected from SiH4、NH3、N2One or more in O.
It is understood that because the present invention is for the purpose of preparing silica-base film, above-mentioned raw materials gas at least should contain
SiH4。
The another embodiment of the preparation method of described stress controllable type silica-base film is: described backing material is for being selected from
In silicon, GaAs, GaN, SiC, sapphire one or more.
Technical scheme in the above-described embodiment, for different backing materials, all can get at tensile stress
And the most regulatable silica-base film between compressive stress, it not can only obtain simple stress because of the difference of backing material
The product of matter.
The another embodiment of the preparation method of described stress controllable type silica-base film is: the deposition of described silica-base film
Speed is 20 ~ 35 nm/min.
In this embodiment, time prepared by the relatively conventional method of sedimentation rate of silica-base film faster, but the finished product obtained
In sheet, uniformity and compactness all show excellence.
The another embodiment of the preparation method of described stress controllable type silica-base film is:: described single-frequency PECVD device
Inside cavity vacuum pressure is 500 ~ 3000mTorr, and in cavity, radio-frequency power is 100 ~ 500W, and cavity inner temperature is 230 ~ 350
℃。
The another embodiment of the preparation method of described stress controllable type silica-base film is: be passed through N2Flow be 0 ~
5000sccm, the flow being passed through He is 0 ~ 5000sccm.
The another embodiment of the preparation method of described stress controllable type silica-base film is: described single-frequency PECVD device
Frequency be 13.56MHz ~ 2.45GHz.
Beneficial effects of the present invention is as follows:
(1) silica-base film that stress is controlled can be prepared in the PECVD in Single frequency RF source, equipment cost is greatly reduced;
(2) gained silica-base film can realize the conversion between tensile stress and compressive stress under monolayer state, and material is greatly reduced
This, improve materials application scope, improves materials application rate, reduces preparation cost;
(3) silica-base film that uniformity is good, compactness is high can be prepared under higher sedimentation rate, decrease production week
Phase, improve production efficiency, reduce production cost;
(4) N is worked as2During with the flow-rate ratio of He in the range of 0 ~ 10, the stress adjustable extent of the silica-base film prepared is at least
For compressive stress-1500Mpa ~ tensile stress 2000Mpa;
(5) for different backing materials, the silica-base film can changed between compressive stress and tensile stress can all be prepared,
Reduce the selectivity to backing material, decrease production cost, improve production universality;
(6) silica-base film prepared relative to low-and high-frequency equipment, the silica-base film BOE rate of etch that the present invention prepares is put down
All reduce by more than 50%, illustrate that its compactness is more preferable;
(7) present invention prepares silica-base film under higher sedimentation rate, and in sheet, uniformity is within 4%, can meet high-quality
Amount, large-scale industrial production;
(8) present invention is simple to operate, controllability is high.
Accompanying drawing explanation
When Fig. 1 is for using Si to make backing material, preparation SiN thin film, N2/ He flow-rate ratio and membrane stress changing trend diagram;
When Fig. 2 is for using GaAs to make backing material, preparation SiN thin film, N2/ He flow-rate ratio and membrane stress changing trend diagram;
Fig. 3 makees backing material, preparation SiO for using Si2During thin film, N2/ He flow-rate ratio and membrane stress changing trend diagram.
Detailed description of the invention
Embodiment 1
Preparation SiN thin film on backing material Si:
The HCl deionized water solution using 10wt% puts into the single-frequency PECVD device that frequency is 13.56MHz after cleaning Si substrate
In cavity, thereafter by unstrpped gas SiH4、NH3And N2, He be uniformly passed through in cavity from cavity top spray aperture, in cavity temperature
Degree is set to 250 DEG C, and cavity internal pressure is set to 1500mTorr, and in preparation process, the power setting of radio frequency source is 150W, SiH4
Flow is 400sccm, NH3Flow is 20sccm, N2Flow be 0 ~ 5000sccm, He flow be 0 ~ 5000sccm, actual flow root
Being adjusted according to flow-rate ratio, film deposition rate is more than 20nm/min, and sedimentation time is 3min, starts to regulate N from close to 02/He
Flow-rate ratio to 1, obtain N as shown in Figure 12/ He flow-rate ratio and membrane stress changing trend diagram, the stress test of use sets
The standby measuring stress instrument for TOHO company, as accompanying drawing 1 demonstrates at N2During the change of/He flow-rate ratio, the SiN that correspondence obtains
Membrane stress changes to tensile stress 500Mpa from compressive stress-1500Mpa, i.e. can get stress controllable type silica-base film, from preparing
Stress controllable type silica-base film in randomly choose 4 batches carry out from the SiN thin film prepared by low-and high-frequency equipment 4 kinds different should
BOE etching test under the conditions of power, test result is as shown in the table:
The SiN film compactness that the visible present invention prepares is all good compared with SiN thin film prepared by low-and high-frequency equipment;Meanwhile, after tested
In gained SiN film thickness sheet, uniformity is within 4%.
Embodiment 2:
Preparation SiN thin film on backing material GaAs:
The HCl deionized water solution using 10wt% puts into, after cleaning GaAs substrate, the single-frequency PECVD device that frequency is 13.56MHz
Cavity in, thereafter by unstrpped gas SiH4、NH3And N2, He is uniformly passed through in cavity, in cavity from cavity top spray aperture
Temperature is set to 300 DEG C, and cavity internal pressure is set to 2000mTorr, and in preparation process, the power setting of radio frequency source is 180W,
SiH4Flow is 700sccm, NH3Flow is 50sccm, N2Flow be 0 ~ 5000sccm, He flow be 0 ~ 5000sccm, thin film
Sedimentation rate is more than 35nm/min, and sedimentation time is 5min, starts to regulate N from close to 02The flow-rate ratio of/He, to 1, obtains as attached
N shown in Fig. 22(wherein X-axis is N to/He flow-rate ratio with membrane stress changing trend diagram2/ He flow-rate ratio, Y-axis is stress) use
Stress test equipment is the measuring stress instrument of TOHO company, as accompanying drawing 2 demonstrates at N2During the change of/He flow-rate ratio, right
The SiN membrane stress that should obtain changes to tensile stress 200Mpa from compressive stress-800Mpa, i.e. obtains stress controllable type silica-based thin
Film;From prepared stress controllable type silica-base film, randomly choose 4 batches carry out 4 with the SiN thin film prepared by low-and high-frequency equipment
Planting the BOE etching test under different stress conditions, test result is as shown in the table:
The SiN film compactness that the visible present invention prepares is all good compared with SiN thin film prepared by low-and high-frequency equipment;Meanwhile, after tested
In gained SiN film thickness sheet, uniformity is within 4%.
Embodiment 3
Preparation SiN thin film on backing material SiC:
The HCl deionized water solution using 10wt% is put into, after cleaning SiC substrate, flat board single-frequency PECVD that frequency is 2.45GHz and is set
In standby cavity, thereafter by unstrpped gas SiH4、NH3And N2, He be uniformly passed through in cavity from cavity top spray aperture, cavity
Interior temperature is set to 350 DEG C, and cavity internal pressure is set to 3000mTorr, and in preparation process, the power setting of radio frequency source is 500W,
SiH4Flow is 700sccm, NH3Flow is 50sccm, N2Flow be 0 ~ 5000sccm, He flow be 0 ~ 5000sccm, thin film
Sedimentation rate is more than 30nm/min, and sedimentation time is 4min, starts to regulate N from close to 02The flow-rate ratio of/He, to 10, was regulating
Cheng Zhong, the stress test equipment of use is tested the different SiN membrane stresses obtained, is tested the stress test using TOHO company
Instrument, can be observed with N in test2/ He flow-rate ratio increases to 10 from 0, the stress of SiN from compressive stress-1500Mpa consecutive variations to
Tensile stress 2000Mpa, i.e. can get stress controllable type silica-base film by the present embodiment, in gained SiN film thickness sheet all
Even property is within 4%.
Embodiment 4
Backing material Si is prepared SiO2Thin film:
The HCl deionized water solution using 10wt% puts into the single-frequency PECVD device that frequency is 13.56MHz after cleaning Si substrate
In cavity, thereafter by unstrpped gas SiH4、N2O and N2, He be uniformly passed through in cavity from cavity top spray aperture, in cavity temperature
Degree is set to 300 DEG C, and cavity internal pressure is set to 1000mTorr, and in preparation process, the power setting of radio frequency source is 100W, SiH4
Flow is 1100sccm, N2O flow is 4400sccm, N2Flow be 50 ~ 100sccm, He flow be 2000 ~ 4500sccm, thin film
Sedimentation rate is more than 25nm/min, and sedimentation time is 3min, starts to regulate N from close to 02The flow-rate ratio of/He, to 2, obtains as attached
N shown in Fig. 32/ He flow-rate ratio and membrane stress changing trend diagram, the stress that stress test equipment is TOHO company of use is surveyed
Examination instrument, as accompanying drawing 3 demonstrates at N2During the change of/He flow-rate ratio, the SiO that correspondence obtains2Membrane stress from compressive stress-
350Mpa changes to tensile stress 50Mpa, i.e. can get stress controllable type silica-base film, gained SiO2Uniformity in film thickness sheet
Within 4%.
Embodiment 5
Backing material GaAs is prepared SiO2Thin film:
The HCl deionized water solution using 10wt% puts into, after cleaning GaAs substrate, the single-frequency PECVD device that frequency is 13.56MHz
Cavity in, thereafter by unstrpped gas SiH4、N2O and N2, He is uniformly passed through in cavity, in cavity from cavity top spray aperture
Temperature is set to 350 DEG C, and cavity internal pressure is set to 1000mTorr, and in preparation process, the power setting of radio frequency source is 150W,
SiH4Flow is 1200sccm, N2O flow is 4500sccm, N2Flow be 50 ~ 100sccm, He flow be 2000 ~ 4500sccm,
Film deposition rate is more than 30nm/min, and sedimentation time is 4min, starts to regulate N from close to 02The flow-rate ratio of/He, to 5, is being adjusted
The stress test equipment used during joint tests the different SiO obtained2Membrane stress, test uses the stress of TOHO company to survey
Examination instrument, can be observed with N in test2/ He flow-rate ratio increases to the corresponding SiO obtained during 5 from 02Membrane stress should from pressure
Power-450Mpa changes to tensile stress 100Mpa, i.e. can get stress controllable type silica-base film, gained SiO2In film thickness sheet all
Even property is within 4%.
Embodiment 6
Backing material sapphire is prepared SiO2Thin film:
The HCl deionized water solution using 10wt% puts into, after cleaning sapphire substrate, the flat board single-frequency that frequency is 2.45GHz
In the cavity of PECVD device, thereafter by unstrpped gas SiH4、N2O and N2, He be uniformly passed through cavity from cavity top spray aperture
In, cavity inner temperature is set to 300 DEG C, and cavity internal pressure is set to 500mTorr, the power setting of radio frequency source in preparation process
For 500W, SiH4Flow is 1200sccm, N2O flow is 4500sccm, N2Flow be 50 ~ 100sccm, He flow be 2000 ~
4500sccm, film deposition rate is more than 35nm/min, and sedimentation time is 4min, starts to regulate N from close to 02The flow-rate ratio of/He
To 10, during regulation, the stress test equipment of use tests the different SiO obtained2Membrane stress, test uses TOHO public
The measuring stress instrument of department, can be observed with N in test2/ He flow-rate ratio increases to 10, SiO from 02Stress from compressive stress-
600Mpa consecutive variations, to tensile stress 1000Mpa, i.e. can get stress controllable type silica-base film, gained by the present embodiment
SiO2In film thickness sheet, uniformity is within 4%.
Although reference be made herein to invention has been described for the explanatory embodiment of the present invention, and above-described embodiment is only this
Bright preferably embodiment, embodiments of the present invention are also not restricted to the described embodiments, it should be appreciated that people in the art
Member can be designed that a lot of other amendments and embodiment, and these amendments and embodiment will fall in principle disclosed in the present application
Within scope and spirit.
Claims (10)
1. the preparation method of a stress controllable type silica-base film, it is characterised in that: use single-frequency PECVD device by chemistry gas
Phase sedimentation makes unstrpped gas deposit on backing material, grows, and obtains silica-base film, is passed through He during preparation in unstrpped gas
And N2。
The preparation method of stress controllable type silica-base film the most according to claim 1, it is characterised in that: described N2With He's
Flow-rate ratio is 0 ~ 10, does not include endpoint value 0.
The preparation method of stress controllable type silica-base film the most according to claim 2, it is characterised in that: described N2With He's
Flow-rate ratio is 0 ~ 1, does not include endpoint value 0.
The preparation method of stress controllable type silica-base film the most according to claim 1, it is characterised in that: described silica-base film
For selected from SiN thin film, SiO2One or more in thin film, SiON thin film.
The preparation method of stress controllable type silica-base film the most according to claim 4, it is characterised in that: described unstrpped gas
For selected from SiH4、NH3、N2One or more in O.
The preparation method of stress controllable type silica-base film the most according to claim 1, it is characterised in that: described backing material
For in silicon, GaAs, GaN, SiC, sapphire one or more.
The preparation method of stress controllable type silica-base film the most according to claim 1, it is characterised in that: described silica-based thin
The sedimentation rate of film is 20 ~ 35 nm/min.
The preparation method of stress controllable type silica-base film the most according to claim 1, it is characterised in that: described single-frequency
PECVD device inside cavity vacuum pressure is 500 ~ 3000mTorr, and in cavity, radio-frequency power is 100 ~ 500W, cavity inner temperature
It it is 230 ~ 350 DEG C.
The preparation method of stress controllable type silica-base film the most according to claim 1, it is characterised in that: it is passed through N2Flow
Being 0 ~ 5000sccm, the flow being passed through He is 0 ~ 5000sccm.
The preparation method of stress controllable type silica-base film the most according to claim 1, it is characterised in that: described single-frequency
The frequency of PECVD device is 13.56MHz ~ 2.45GHz.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112233970A (en) * | 2020-12-15 | 2021-01-15 | 度亘激光技术(苏州)有限公司 | Method for manufacturing gallium arsenide-based semiconductor device |
CN112760615A (en) * | 2020-12-17 | 2021-05-07 | 武汉新芯集成电路制造有限公司 | Silicon dioxide film and low-temperature preparation method thereof |
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JP2004335980A (en) * | 2003-05-12 | 2004-11-25 | Sumitomo Electric Ind Ltd | Method for forming silicon nitride film and method for semiconductor device |
US20040262613A1 (en) * | 2003-06-30 | 2004-12-30 | Shinji Maekawa | Silicon nitride film, a semiconductor device, a display device and a method for manufacturing a silicon nitride film |
CN1837404A (en) * | 2005-03-23 | 2006-09-27 | 东京毅力科创株式会社 | Film-forming apparatus and film-forming method |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2004335980A (en) * | 2003-05-12 | 2004-11-25 | Sumitomo Electric Ind Ltd | Method for forming silicon nitride film and method for semiconductor device |
US20040262613A1 (en) * | 2003-06-30 | 2004-12-30 | Shinji Maekawa | Silicon nitride film, a semiconductor device, a display device and a method for manufacturing a silicon nitride film |
CN1837404A (en) * | 2005-03-23 | 2006-09-27 | 东京毅力科创株式会社 | Film-forming apparatus and film-forming method |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112233970A (en) * | 2020-12-15 | 2021-01-15 | 度亘激光技术(苏州)有限公司 | Method for manufacturing gallium arsenide-based semiconductor device |
CN112760615A (en) * | 2020-12-17 | 2021-05-07 | 武汉新芯集成电路制造有限公司 | Silicon dioxide film and low-temperature preparation method thereof |
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Application publication date: 20161130 |