CN108493760A - A kind of Si3N4/ SiON composite membranes, chip of laser and preparation method - Google Patents

A kind of Si3N4/ SiON composite membranes, chip of laser and preparation method Download PDF

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Publication number
CN108493760A
CN108493760A CN201810317772.6A CN201810317772A CN108493760A CN 108493760 A CN108493760 A CN 108493760A CN 201810317772 A CN201810317772 A CN 201810317772A CN 108493760 A CN108493760 A CN 108493760A
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sion
pecvd
composite membranes
film
sih
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逯心红
王忠政
洪志苍
方瑞禹
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Hisense Broadband Multimedia Technology Co Ltd
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Hisense Broadband Multimedia Technology Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S5/00—Semiconductor lasers
    • H01S5/02—Structural details or components not essential to laser action
    • H01S5/028—Coatings ; Treatment of the laser facets, e.g. etching, passivation layers or reflecting layers
    • H01S5/0282—Passivation layers or treatments

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  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Optics & Photonics (AREA)
  • Chemical Vapour Deposition (AREA)
  • Formation Of Insulating Films (AREA)

Abstract

The present invention provides a kind of Si3N4/ SiON composite membranes, chip of laser and preparation method.Si prepared by PECVD methods3N4The stress in thin film of film layer is negative stress, and the stress in thin film of SiON film layers prepared by PECVD methods is direct stress.The present invention will be by that will have the Si of negative stress3N4Film layer and SiON film layers with direct stress carry out compound, form the Si compared with low stress3N4/ SiON composite membranes, to reduce the Stress superposition effect in chip fabrication process.In addition, Si3N4Film layer and SiON film layers all have preferable water vapor performance, thus the Si prepared3N4/ SiON composite membranes can be provided simultaneously with water vapor performance and low stress in thin film performance, meet the performance requirement of high-speed laser chip.

Description

A kind of Si3N4/ SiON composite membranes, chip of laser and preparation method
Technical field
The present invention relates to technical field of optical fiber communication more particularly to a kind of Si3N4/ SiON composite membranes, chip of laser and system Preparation Method.
Background technology
Semiconductor laser has the characteristics that small, light-weight and photoelectric conversion efficiency is high, thus material process, It is used widely in the fields such as medical and beauty treatment, military project and communication.Semiconductor laser forms laser after assembling and encapsulation Chip, to form different integrated circuits.
Currently, it includes mainly air-tight packaging and non-airtight that semiconductor laser, which encapsulates the method to form chip of laser, Encapsulation.Relative to air-tight packaging, non-airtight encapsulation has lower manufacturing cost.To reduce being produced into for chip of laser This, non-airtight, which encapsulates, to be rapidly developed.It is to form passivation film that non-airtight, which encapsulates more common mode, i.e., is partly leading The surface of body laser deposits the preferable passivation film of water-resistance.Currently, most common passivation film deposition method is PECVD (Plasma Enhanced Chemical Vapor Deposition, plasma activated chemical vapour deposition).
PECVD has many advantages, such as that substrate temperature is low, quality of forming film is good and pin hole is less, and the passivation film thickness formed Thicker, water vapor performance is better.But the passivation film that PECVD is formed has certain stress in thin film, and the thickness of passivation film Bigger, stress in thin film is bigger.When the thickness of passivation film is thicker, passivation film is easy cracking, falls off, and leads to passivation film The performance requirement of chip of laser is cannot be satisfied, and then chip of laser is caused to fail.It can be seen that the water vapor of passivation film Performance and stress in thin film performance are related with the thickness of passivation film, and the thickness of passivation film is bigger, and water vapor performance is better, Stress in thin film is bigger.For high-speed laser chip, non-airtight encapsulation require simultaneously have preferable water vapor performance with Lower stress in thin film, but due to stress in thin film existing for passivation film itself, lead to passivation film used at present and difference When have both two performance requirements of preferable water vapor performance and low stress in thin film, i.e., passivation film used at present cannot meet height The performance requirement of fast chip of laser.
Invention content
The present invention provides a kind of Si3N4/ SiON composite membranes, chip of laser and preparation method are used at present blunt to solve Change the problem of film layer cannot meet high-speed laser chip performance requirement.
In a first aspect, the present invention provides a kind of Si3N4/ SiON composite membranes, including deposition reaction formed SiON film layers and The Si being deposited in the SiON film layers3N4Film layer.
Second aspect, the present invention provide a kind of Si3N4The preparation method of/SiON composite membranes, including：
PECVD chambers are vacuumized, and set temperature is 280 DEG C；
After the PECVD chamber temps reach set temperature, Ar, N are passed through into the PECVD chambers2, He and N2O, with The PECVD cavity indoor pressures are made to reach default operating pressure；
After the PECVD cavity indoor pressures are stablized, SiH is passed through into the PECVD chambers4And NH3；
Under conditions of radio-frequency power supply power is 50W, reaction generates SiON film layers；
Stopping is passed through N2O、SiH4And NH3, keep Ar, N2It is constant with the volume flow of He；
Under the radio-frequency power supply effect that power is 80W, it is passed through SiH again into the PECVD chambers4And NH3, reaction life At Si3N4Film layer obtains Si3N4/ SiON composite membranes.
The third aspect, a kind of chip of laser of present invention offer, including wafer and the Si being deposited on the wafer3N4/ SiON composite membranes, the Si3N4/ SiON composite membranes are the composite membrane of first aspect or the Si3N4/ SiON composite membranes are according to The method of two aspects is prepared.
Fourth aspect, the present invention provide the preparation method of chip of laser, including：
Wafer sulfuric acid cleaned, drying are placed in PECVD chambers；
PECVD chambers are vacuumized, and set temperature is 280 DEG C；
After the PECVD chamber temps reach set temperature, Ar, N are passed through into the PECVD chambers2, He and N2O, with The PECVD cavity indoor pressures are made to reach default operating pressure；
After the PECVD cavity indoor pressures are stablized, power is used to remove the oxygen of the crystal column surface for the radio-frequency power supply of 50W Change layer；
It is passed through SiH into the PECVD chambers4And NH3, deposited in the crystal column surface and generate SiON film layers；
Stopping is passed through N2O、SiH4And NH3, keep Ar, N2It is constant with the volume flow of He；
Under the radio-frequency power supply effect that power is 80W, it is passed through SiH again into the PECVD chambers4And NH3, described SiON film surfaces deposition generates Si3N4Film layer obtains Si3N4The chip of laser of/SiON composite membranes encapsulation.
The technical solution that the embodiment of the present invention provides can include the following benefits：
The present invention provides a kind of Si3N4/ SiON composite membranes, chip of laser and preparation method.Prepared by PECVD methods Si3N4There is film layer compression, i.e. negative stress, SiON film layers prepared by PECVD methods to have tensile stress, i.e. direct stress.The present invention By the Si with negative stress3N4Film layer and SiON film layers with direct stress carry out compound, pass through and control Si3N4Film layer and SiON The thickness of film layer forms the Si compared with low stress3N4/ SiON composite membranes, to reduce the effect of the Stress superposition in chip fabrication process It answers.In addition, Si3N4Film layer and SiON film layers all have preferable water vapor performance, thus the Si prepared3N4/ SiON composite membrane energy It is enough provided simultaneously with water vapor performance and low stress in thin film performance, meets the performance requirement of high-speed laser chip.
It should be understood that above general description and following detailed description is only exemplary and explanatory, not It can the limitation present invention.
Description of the drawings
In order to illustrate more clearly of the technical solution of the application, letter will be made to attached drawing needed in the embodiment below Singly introduce, it should be apparent that, for those of ordinary skills, without having to pay creative labor, Other drawings may also be obtained based on these drawings.
Fig. 1 is Si provided in an embodiment of the present invention3N4The flow diagram of the preparation method of/SiON composite membranes；
Fig. 2 is the preparation method flow diagram of chip of laser provided in an embodiment of the present invention；
Fig. 3 is SEM provided in an embodiment of the present invention (scanning electron microscope, scanning electron microscopy Mirror) detection figure；
Fig. 4 is SiO under different soaking times provided in an embodiment of the present invention2Film layer aquation back reflection rate variation diagram；
Fig. 5 is the partial enlarged view at a in Fig. 4 provided in an embodiment of the present invention；
Fig. 6 is SiON film layer aquation back reflection rate variation diagrams under different soaking times provided in an embodiment of the present invention；
Fig. 7 is the partial enlarged view at b in Fig. 6 provided in an embodiment of the present invention；
Fig. 8 is Si under different soaking times provided in an embodiment of the present invention3N4/ SiON composite membrane aquation back reflection rates change Figure；
Fig. 9 is the partial enlarged view at c in Fig. 8 provided in an embodiment of the present invention；
Figure 10 is SiON film layers provided in an embodiment of the present invention and Si3N4Thickness proportion-the Si of film layer3N4/ SiON composite membranes Stress in thin film relational graph.
Specific implementation mode
Although PECVD has many advantages, such as that substrate temperature is low, quality of forming film is good and pin hole is less, PECVD is formed blunt Changing film layer has certain stress in thin film, and the thickness of passivation film is bigger, and stress in thin film is bigger.When the thickness of passivation film When thicker, passivation film is easy cracking, falls off, and causes passivation film to cannot be satisfied the performance requirement of chip of laser, and then lead Cause chip of laser failure.But if the passivation film that PECVD is formed is thinner, and water vapor performance is poorer, leads to chip of laser Inside is easy to immerse moisture, and then leads to its failure.It can be seen that the water vapor performance and stress in thin film performance of passivation film are equal It is related with the thickness of passivation film, and the thickness of passivation film is bigger, water vapor performance is better, and stress in thin film is bigger.For height Fast chip of laser, non-airtight, which encapsulates, requires while having preferable water vapor performance and lower stress in thin film, but by The stress in thin film existing for passivation film itself, causes passivation film used at present not while having both preferable water vapor Energy and two performance requirements of low stress in thin film, i.e., the performance that passivation film used at present cannot meet high-speed laser chip are wanted It asks.
In view of the above-mentioned problems, the application proposes a kind of Si3N4/ SiON composite membranes, to meet preferable water vapor performance simultaneously And the requirement of low stress in thin film performance.Si provided by the present application3N4The core concept of/SiON composite membranes is：Two kinds are chosen simultaneously to have The monofilm for having preferable water vapor performance, such as SiON film layers and Si3N4Film layer.The two kinds of monofilms chosen must also have opposite Stress in thin film, as SiON film layers have tensile stress, i.e. direct stress；Si3N4Film layer has compression, i.e. negative stress.By by two Monofilm progress of the kind with different stress in thin film directions is compound, and the stress in thin film after superposition can be made to substantially reduce, thus made Standby Si3N4/ SiON composite membranes have lower stress in thin film.Due to SiON film layers and Si3N4Film layer all has preferable water vapor Performance, therefore, the Si being prepared3N4/ SiON composite membranes can have preferable water vapor performance and lower film layer to answer simultaneously Power.
Specifically, there are commonly SiO for the film layer that PECVD is formed2、Si3N4, tri- kinds of SiON, wherein SiON film layers are current Main application material.Under normal circumstances, the SiO that prepared by PECVD methods2Film layer and Si3N4The film stress of film layer is that pressure is answered The film stress of power, i.e. negative stress, SiON film layers prepared by PECVD methods is tensile stress, i.e. direct stress.To prepare stress in thin film Lower composite membrane, the application preferentially select the SiON with negative stress as one of composite membrane.Due to Si3N4Water vapor It can be between SiO2Between SiON, therefore, to make the composite membrane of preparation that there is preferable water vapor performance, the application selection to have Direct stress, water vapor Si of good performance3N4As one of composite membrane.
Based on selected single layer passivation film, the application deposits to form Si by PECVD methods3N4/ SiON composite membranes.I.e. Si provided by the present application3N4/ SiON composite membranes include the SiON film layers and be deposited in SiON film layers that deposition reaction is formed Si3N4The Si that film layer or deposition reaction are formed3N4Film layer and it is deposited on Si3N4SiON film layers in film layer.Wherein, SiON films Layer is by N2O、SiH4And NH3Deposition reaction generates, Si3N4Film layer is by SiH4And NH3Deposition reaction generates.
Since the stability of Si-O keys is better than the stability of Si-N keys, to improve Si3N4The stabilization of/SiON composite membranes Property, preferential deposition forms the SiON film layers having good stability, and then deposits to form Si on the surface of SiON film layers3N4Film layer.Separately Outside, the stress in thin film of SiON film layers is direct stress, Si3N4The stress in thin film of film layer is negative stress, therefore, Si3N4Film deposition exists After SiON film layers, the stress in thin film of composite membrane is enabled to substantially reduce under negative stress and the superposition of direct stress.As a result, Si provided by the present application3N4/ SiON composite membranes are preferably the SiON film layers and be deposited in SiON film layers that deposition reaction is formed Si3N4Film layer.
Attached drawing 1 is please referred to, attached drawing 1 shows a kind of Si provided by the present application3N4The stream of the preparation method of/SiON composite membranes Journey schematic diagram.It can be prepared by attached preparation method shown in FIG. 1 and deposit Si after first depositing SiON film layers3N4Film layer and formed Si3N4/ SiON composite membranes.
Specifically, by attached drawing 1 it is found that Si provided by the present application3N4The preparation method of/SiON composite membranes specifically includes：
S01：PECVD chambers are vacuumized, and set temperature is 280 DEG C.
PECVD is plasma activated reactive gas, promote to be chemically reacted in matrix surface or near surface space and The method for generating solid film.Based on this, to prevent plasma from other reaction gas, PECVD chambers being activated to need to be evacuated to vacuum State, to remove in PECVD chambers and the air of matrix surface.Under normal conditions, PECVD chambers are evacuated to vacuum degree and are 0.7mTorr。
Due between monofilm film quality, film layer transitionality and film layer and film layer between thickness matching be influence Therefore main three factor of composite film comprehensive performance is the excellent Si of processability3N4/ SiON composite membranes, it has to be noted that Transition between monofilm film quality, film layer and film layer and thicknesses of layers.And it deposits to form single layer passivation in PECVD methods During film layer, the principal element that influences stress in thin film includes that depositing temperature, deposition rate, operating air pressure, power source are gentle Body is passed through ratio etc..Therefore, the SiON film layers to be formed to make PECVD methods deposit have uniform stress in thin film, PECVD chambers Inside need the temperature of setting deposition reaction.
Under lower temperature conditions, CH4 +、C、CH4And SiH2Isoreactivity group is relatively low in the activity of matrix surface, is formed SiON film layers compactness it is poor, lead to that stress in thin film is uneven, water vapor performance is bad.Under higher temperature conditions, CH4 +、 C、CH4And SiH2Isoreactivity group is improved in the activity of matrix surface, and the compactness of the SiON film layers of formation improves.But When PECVD chamber indoor temperatures are higher, then to the more demanding of consersion unit, lead to Si3N4The manufacturing cost of/SiON composite membranes It is higher.For this purpose, by test of many times, it is 280 DEG C to select the indoor temperature of PECVD chambers, and the depositing temperature of film layer is formed with control. At this point, PECVD methods, which deposit the SiON film layers to be formed, has preferable compactness.To make the indoor temperature of PECVD chambers stablize, when After PECVD chamber indoor temperatures reach 280 DEG C, gas is passed through after keeping temperature 3min.
S02：After PECVD chamber temps reach set temperature, Ar, N are passed through into PECVD chambers2, He and N2O, so that PECVD cavity indoor pressures reach default operating pressure.
After PECVD chamber temps reach set temperature, Ar, N are passed through into PECVD chambers2, He and N2O, so that PECVD Cavity indoor pressure reaches default operating pressure, so that PECVD chambers are in stable air pressure, plasma gas is in steady Determine state.Under 280 DEG C of depositing temperature, to form the preferable SiON film layers of compactness, default operating pressure is 1300mTorr。
In Ar, the N being passed through2, He and N2In O, Ar easily ionizables are build-up of luminance gas；N2It is diluent gas, N with He2O is reaction One of gas.To make the indoor pressure stability of PECVD chambers, and reach pressure needed for reaction, is passed through PECVD chambers indoor Ar, N2、 He and N2The volume flow ratio of O is 1:15:1:4, e.g., the volume flow of Ar is 150sccm；N2Volume flow be 3000sccm； The volume flow of He is 100sccm；N2The volume flow of O is 800sccm.To make PECVD cavity indoor pressures stablize, work as PECVD After cavity indoor pressure reaches default operating pressure, it is passed through other gases again after keeping operating pressure 3min.
S03：After PECVD cavity indoor pressures are stablized, SiH is passed through into PECVD chambers4And NH3。
After PECVD cavity indoor pressures are stablized, SiH is passed through into PECVD chambers4And NH3, wherein SiH4And NH3It is Reaction gas.Film forming of the making a living lower SiON film layers of ply stress, N2O、SiH4And NH3Volume flow ratio be 40:1:2, such as N2O Volume flow be 800sccm, SiH4Volume flow be 20sccm, NH3Volume flow be 40sccm.
S04：Under conditions of radio-frequency power supply power is 50W, reaction generates SiON film layers.
Open radio-frequency power supply, wherein the power of radio-frequency power supply is 50W.It is deposited according to deposition thickness and deposition rate setting Time, so that N2O、SiH4And NH3In Ar, N2Certain thickness SiON film layers are generated with deposition reaction under He atmosphere.N2O、SiH4 And NH3Reaction generate SiON film layers reaction equation be：2N2O+2SiH4+2NH3=2SiON+2N2+7H2。
S05：Stopping is passed through N2O、SiH4And NH3, keep Ar, N2It is constant with the volume flow of He.
After reaching setting time between when deposited, stopping is passed through N2O、SiH4And NH3, and keep Ar, N2With the volume flow of He Measure it is constant so that remaining N in PECVD chambers2O、SiH4And NH3Reaction completely, and then deposit Si in SiON film surfaces3N4Film When layer, two deposition reactions will not be existed simultaneously.Since two deposition reactions, thus SiON film layers and Si will not be existed simultaneously3N4 Have distinct interface, and then SiON film layers and Si between film layer3N4Film layer can determine that film layer is answered according to its respective thickness Power, and then determine SiON film layers and Si3N4The Si formed after film layer is compound3N4The stress in thin film of/SiON composite membranes.
S06：Under the radio-frequency power supply effect that power is 80W, it is passed through SiH again into PECVD chambers4And NH3, reaction life At Si3N4Film layer obtains Si3N4/ SiON composite membranes.
The power of radio-frequency power supply is improved to 80W, so that build-up of luminance gas Ar ion bombardments deposit the SiON film layers to be formed, to reach To the purpose of cleaning SiON film layers.Meanwhile build-up of luminance gas Ar ion bombardment SiON film layers can also make the H of SiON film surfaces Hydrogenolysis absorption occurs, so that Si3N4Film deposition is in SiON film surfaces, SiON film layers and Si3N4Have between film layer good Associativity.
In Ar, N2With the volume flow of He it is constant under conditions of, be passed through SiH again into PECVD chambers4And NH3.Wherein, SiH4And NH3Volume flow ratio be 1:2, such as SiH4Volume flow be 20sccm, NH3Volume flow be 40sccm.According to Deposition thickness sets sedimentation time, SiH with deposition rate4And NH3In Ar, N2Si is generated with deposition reaction under He atmosphere3N4Film layer. SiH4And NH3Reaction generates Si3N4The reaction equation of film layer is 3SiH4+4NH3=Si3N4+12H2。
Further, Si provided by the present application3N4The preparation method of/SiON composite membranes further includes：
S07：Stopping is passed through SiH4And NH3, keep Ar, N2It is constant with the volume flow of He；
After reaching setting time between when deposited, stopping is passed through SiH4And NH3, and keep Ar, N2Not with the volume flow of He Become, so that remaining SiH in PECVD chambers4And NH3Reaction completely.
S08：Stopping is passed through N2And He, keep the volume flow of Ar constant；Finally stop being passed through Ar.
SiH4And NH3After stopping is passed through 3min, stopping is passed through N2And He, and keep the volume flow of Ar constant, so that remaining The reaction was continued under Ar ion bombardments for residual gas, until the reaction is complete.Finally stop being passed through Ar, vacuum breaker taking-up prepares sample Product.
First deposition forms Si3N4Deposition forms the preparation method of SiON film layers substantially with above-mentioned Si after film layer3N4/ SiON is multiple The specific preparation flow for closing film, is only N2O、SiH4And NH3Be passed through sequence and SiH4And NH3Be passed through exchange, remaining deposition temperature The setting that degree, deposition rate, operating air pressure, power source and gas are passed through ratio etc. is constant.Herein shape is not deposited first in elaboration At Si3N4Deposition forms the specific preparation flow of SiON film layers after film layer.
Based on Si provided by the present application3N4/ SiON composite membranes and Si3N4The preparation method of/SiON composite membranes, the application A kind of chip of laser is also provided.Chip of laser provided by the present application includes wafer and the Si that is deposited on wafer3N4/ SiON composite membranes, wherein Si3N4/ SiON composite membranes use the above-mentioned Si referred to3N4/ SiON composite membranes, or use above-mentioned Si3N4/ Si prepared by the preparation method of SiON composite membranes3N4/ SiON composite membranes.
Based on chip of laser provided by the present application, present invention also provides the preparation methods of chip of laser, specifically ask Refer to the attached drawing 2.By attached drawing 2 it is found that the preparation method of chip of laser provided by the present application specifically includes：
S11：Wafer sulfuric acid cleaned, drying are placed in PECVD chambers.
The wafer for preparing chip of laser is cleaned with sulfuric acid, with particle and the organic matter etc. for removing crystal column surface, And then ensure crystal column surface cleaning, enhance the adhesiveness between wafer and film layer.Since hydrochloric acid can be with the InP of crystal column surface (Indium Phosphide, indium phosphide) reacts, and nitric acid has oxidisability, therefore, using sulfuric acid to crystalline substance in the application Circle carries out surface clean.Specifically, wafer is impregnated into 3min in concentrated sulfuric acid, is then rinsed with water 10min.
Wafer after cleaning carries out spin-drying, to ensure that crystal column surface is dried.Wafer after drying is put into PECVD chambers In, in order to deposit Si in crystal column surface by PECVD methods3N4/ SiON composite membranes.
S12：PECVD chambers are vacuumized, and set temperature is 280 DEG C.
It is vacuumized in PECVD chambers, and after reaching 280 DEG C, keeps the temperature 3min, so that crystal column surface is heated evenly, and then promoted Make Si3N4The filmogen of/SiON composite membranes has good diffusivity in crystal column surface, and chemical reaction is more abundant, formation The compactness of SiON composite membranes is more preferable.
S13：After PECVD chamber temps reach set temperature, Ar, N are passed through into PECVD chambers2, He and N2O, so that PECVD cavity indoor pressures reach default operating pressure.
S14：After PECVD cavity indoor pressures are stablized, power is used to remove the oxidation of crystal column surface for the radio-frequency power supply of 50W Layer.
After PECVD cavity indoor pressures are stablized, power is used to remove the oxide layer of crystal column surface for the radio-frequency power supply of 50W.It penetrates Frequency power will produce plasma after opening, and plasma that crystal column surface is bombarded, to remove crystal column surface Oxide layer.The wafer oxidation layer fallen is bombarded with Ar, N2, the flowing of gases such as He and take PECVD chambers out of, and then prevent wafer Oxide layer participates in Si3N4In the film formation reaction of/SiON composite membranes.Since the oxide layer of crystal column surface has removed, thus PECVD The indoor crystal column surface of chamber has very strong activity, and then can preferably be combined with the film forming atom of SiON film layers, improves Adhesiveness between SiON film layers and wafer.
S15：It is passed through SiH into PECVD chambers4And NH3, deposited in crystal column surface and generate SiON film layers.
S16：Stopping is passed through N2O、SiH4And NH3, keep Ar, N2It is constant with the volume flow of He.
S17：Under the radio-frequency power supply effect that power is 80W, it is passed through SiH again into PECVD chambers4And NH3, in SiON Film surface deposition generates Si3N4Film layer obtains Si3N4The chip of laser of/SiON composite membranes encapsulation.
There is good water vapor performance and lower stress in thin film, this Shen to verify chip of laser provided by the present application Please to prepared Si3N4/ SiON composite membranes carry out Shape measure, water vapor performance detection and stress in thin film detection.
1, using SEM to the Si that is deposited on the chip of ridge-structure3N4/ SiON composite membranes are detected, and testing result is for example attached Shown in Fig. 3.By attached drawing 3 as it can be seen that Si3N4The film layer interfaces transition of/SiON composite membranes is good, without apparent lamination, and film layer Compactness is good.
2, the Si provided for embodiment application3N4The water vapor performance of/SiON composite membranes is better than single layer SiON film layers and single layer SiO2Film layer, using SiON film layers and SiO2Film layer carries out water vapor performance detection as a comparison case.Specifically, by SiON film layers, SiO2Film layer and Si3N4/ SiON composite membranes are immersed in 95 DEG C of boiling water simultaneously, detect SiON film layers, SiO respectively2Film layer and Si3N4Reflectivity of/SiON the composite membranes after impregnating 0h, 1h, 2h, 5h and 10h, testing result please refer to attached drawing 4-9.Wherein, attached Fig. 5 is the partial enlarged view that a locates in attached drawing 4, and attached drawing 7 is the partial enlarged view at b in attached drawing 6, attached drawing 9 for c in attached drawing 8 at Partial enlarged view.
By attached drawing 4-9 as it can be seen that SiO2There is forward migration 2.2% in reflectivity after film layer boiling water impregnates, i.e., after aquation, SiO2Water suction phenomenon, water vapor poor performance occurs.SiON film layers and Si3N4Reflectivity after the immersion of/SiON composite membrane boiling water is without change Change, the phenomenon that absorbs water does not occur, water vapor performance is good.
3, SiON film layers and Si3N4The thickness proportion of film layer is to Si3N4The stress in thin film of/SiON composite membranes plays crucial Effect, therefore, the application is also to SiON film layers and Si3N4The thickness proportion and Si of film layer3N4The film layer of/SiON composite membranes is answered Relationship between power is studied, and obtains thickness proportion-stress in thin film relational graph, as shown in Fig. 10.By attached drawing 10 as it can be seen that with SiON film layers and Si3N4The gradual increase of the thickness proportion of film layer, Si3N4The stress in thin film of/SiON composite membranes first reduces to be increased afterwards Add.It can be learnt by attached thickness proportion shown in Fig. 10-stress in thin film relational graph as a result, as SiON film layers and Si3N4Film layer Thickness proportion be 3.33 when, Si3N4The stress in thin film of/SiON composite membranes is minimum.
It is required that those skilled in the art can be understood that the technology in the embodiment of the present invention can add by software The mode of general hardware platform realize.Based on this understanding, the technical solution in the embodiment of the present invention substantially or Say that the part that contributes to existing technology can be expressed in the form of software products, which can deposit Storage is in storage medium, such as ROM/RAM, magnetic disc, CD, including some instructions are used so that computer equipment (can be with Be personal computer, server either network equipment etc.) execute certain part institutes of each embodiment of the present invention or embodiment The method stated.
Invention described above embodiment is not intended to limit the scope of the present invention..
Those skilled in the art will readily occur to its of the present invention after considering specification and putting into practice the disclosure invented here Its embodiment.This application is intended to cover the present invention any variations, uses, or adaptations, these modifications, purposes or Person's adaptive change follows the general principle of the present invention and includes undocumented common knowledge in the art of the invention Or conventional techniques.The description and examples are only to be considered as illustrative, and true scope and spirit of the invention are by following Claim is pointed out.
It should be understood that the invention is not limited in the precision architectures for being described above and being shown in the accompanying drawings, and And various modifications and changes may be made without departing from the scope thereof.The scope of the present invention is limited only by the attached claims.

Claims (10)

1. a kind of Si3N4/ SiON composite membranes, which is characterized in that the SiON film layers that are formed including deposition reaction and be deposited on described Si in SiON film layers3N4The Si that film layer or deposition reaction are formed3N4Film layer and it is deposited on the Si3N4SiON in film layer Film layer.
2. Si according to claim 13N4/ SiON composite membranes, which is characterized in that N2O、SiH4And NH3Deposition reaction generates The SiON film layers, the N2O, the SiH4With the NH3Volume flow ratio be 40:1:2.
3. Si according to claim 13N4/ SiON composite membranes, which is characterized in that SiH4And NH3Described in deposition reaction generates Si3N4Film layer, the SiH4With the NH3Volume flow ratio be 1:2.
4. a kind of Si3N4The preparation method of/SiON composite membranes, which is characterized in that including：
PECVD chambers are vacuumized, and set temperature is 280 DEG C；
After the PECVD chamber temps reach set temperature, Ar, N are passed through into the PECVD chambers2, He and N2O, so that institute It states PECVD cavity indoor pressures and reaches default operating pressure；
After the PECVD cavity indoor pressures are stablized, SiH is passed through into the PECVD chambers4And NH3；
Under conditions of radio-frequency power supply power is 50W, reaction generates SiON film layers；
Stopping is passed through N2O、SiH4And NH3, keep Ar, N2It is constant with the volume flow of He；
Under the radio-frequency power supply effect that power is 80W, it is passed through SiH again into the PECVD chambers4And NH3, reaction generation Si3N4Film layer obtains Si3N4/ SiON composite membranes.
5. Si according to claim 43N4The preparation method of/SiON composite membranes, which is characterized in that the Ar, the N2、 The He and N2The volume flow ratio of O is 1:15:1:4.
6. Si according to claim 43N4The preparation method of/SiON composite membranes, which is characterized in that the default work pressure Power is 1300mTorr.
7. Si according to claim 43N4The preparation method of/SiON composite membranes, which is characterized in that the method further includes：
Stopping is passed through SiH4And NH3, keep Ar, N2It is constant with the volume flow of He；
Stopping is passed through N2And He, keep the volume flow of Ar constant；Finally stop being passed through Ar.
8. a kind of chip of laser, which is characterized in that including wafer and the Si being deposited on the wafer3N4/ SiON is compound Film, the Si3N4/ SiON composite membranes are any one composite membrane or the Si in claim 1-33N4/ SiON composite membranes are pressed It is prepared according to any one method in claim 4-7.
9. a kind of preparation method of chip of laser, which is characterized in that including：
Wafer sulfuric acid cleaned, drying are placed in PECVD chambers；
PECVD chambers are vacuumized, and set temperature is 280 DEG C；
After the PECVD chamber temps reach set temperature, Ar, N are passed through into the PECVD chambers2, He and N2O, so that institute It states PECVD cavity indoor pressures and reaches default operating pressure；
After the PECVD cavity indoor pressures are stablized, power is used to remove the oxidation of the crystal column surface for the radio-frequency power supply of 50W Layer；
It is passed through SiH into the PECVD chambers4And NH3, deposited in the crystal column surface and generate SiON film layers；
Stopping is passed through N2O、SiH4And NH3, keep Ar, N2It is constant with the volume flow of He；
Under the radio-frequency power supply effect that power is 80W, it is passed through SiH again into the PECVD chambers4And NH3, in the SiON Film surface deposition generates Si3N4Film layer obtains Si3N4The chip of laser of/SiON composite membranes encapsulation.
10. the preparation method of chip of laser according to claim 9, which is characterized in that described that wafer sulfuric acid is clear Wash bags include first impregnates 3min in concentrated sulfuric acid, is then rinsed with water 10min.
CN201810317772.6A 2018-04-10 2018-04-10 A kind of Si3N4/ SiON composite membranes, chip of laser and preparation method Pending CN108493760A (en)

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