CN108447770A - The preparation method of silica membrane - Google Patents
The preparation method of silica membrane Download PDFInfo
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- CN108447770A CN108447770A CN201810190973.4A CN201810190973A CN108447770A CN 108447770 A CN108447770 A CN 108447770A CN 201810190973 A CN201810190973 A CN 201810190973A CN 108447770 A CN108447770 A CN 108447770A
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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
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
- H01L21/02164—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material being a silicon oxide, e.g. SiO2
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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- C23C16/401—Oxides containing silicon
- C23C16/402—Silicon dioxide
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4407—Cleaning of reactor or reactor parts by using wet or mechanical methods
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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
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/02227—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process
- H01L21/0223—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate
- H01L21/02233—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer
- H01L21/02236—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer group IV semiconductor
- H01L21/02238—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer group IV semiconductor silicon in uncombined form, i.e. pure silicon
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Abstract
The present invention provides a kind of silica membrane preparation method.First, a silicon substrate is provided.Secondly, the silicon substrate is put into oxidation furnace, the temperature in the oxidation furnace is 1000 DEG C 1200 DEG C.Then, oxygen is passed through into the oxidation furnace, the oxygen flow is 9slm/min 10slm/min.After being passed through oxygen 4min 6min into the oxidation furnace, it is passed through hydrogen into the oxidation furnace and lights a fire, the flow of the hydrogen is 14slm/min 14.6slm/min, and the first silicon dioxide layer is formed in the surface of silicon.
Description
Technical field
The present invention relates to a kind of electronic semi-conductor's techniques, more particularly to the preparation method of silica membrane.
Background technology
In semiconductor fabrication, the preparation method of film mostly uses oxidation and chemical vapor deposition (CVD).Thermal oxide
Method is the method for making silicon chip surface form silicon dioxide film at high temperature.The purpose of thermal oxide is that certain matter is produced on silicon chip
The effects that measuring desired silicon dioxide film, protection, passivation, insulation, buffer medium risen to silicon chip or device.
In existing process for fabrication of semiconductor device, wet oxygen technique is commonly used, i.e., carries high-temperature vapor in silicon with oxygen
Grown silicon dioxide film.In wet oxygen technique, the purity of high-temperature vapor there is great influence, water to steam processing quality
The purity of vapour is not high to cause silicon dioxide film impurity content height, film quality bad.For improve water purity, frequently with hydrogen with
The mode of oxygen combustion (hydrogen-oxygen synthesis) generates the water of high-purity.In addition, in silica membrane preparation process, oxygen
Flow and hydrogen flow for silica membrane generating rate and silica membrane uniformity also have weight
The influence wanted.
Invention content
Based on this, it is necessary to be directed to the problem of improving silicon dioxide film growth rate and uniformity of film, provide one
The preparation method of kind silica membrane.
The present invention provides a kind of preparation method of silica membrane, the method includes：
S100 provides a silicon substrate；
The silicon substrate is put into oxidation furnace by S200, and the temperature in the oxidation furnace is warming up to reaction temperature, described
Reaction temperature is 1000 DEG C -1200 DEG C；
S300 is passed through oxygen into the oxidation furnace, and the flow of the oxygen is 9slm/min-10slm/min；And
S400 after being passed through oxygen 4min-6min into the oxidation furnace, hydrogen is passed through into the oxidation furnace and is lighted a fire,
The flow of the hydrogen is 14slm/min-14.6slm/min, and the first silicon dioxide layer is formed in the surface of silicon.
The S400 includes in one of the embodiments,：
S410 after being passed through oxygen 4min-6min into the oxidation furnace, starts to be passed through hydrogen into the oxidation furnace, institute
The flow for stating hydrogen is 4slm/min-8slm/min；
S420, after hydrogen 0.5min-1.5min is passed through into the oxidation furnace, the flow-rate adjustment by the hydrogen is
14slm/min-14.6slm/min forms the first silicon dioxide layer in the surface of silicon.
In one of the embodiments, in the S300, the oxygen flow is 9.53slm/min.
In one of the embodiments, in the S400, the hydrogen flowing quantity is 14.3slm/min.
The S200 includes in one of the embodiments,：
The S200 includes：
S210 provides an oxidation furnace, is heated to pretreatment temperature to the oxidation furnace, the pretreatment temperature is
800℃-900℃；
After the oxidation furnace is warming up to the pretreatment temperature, the silicon substrate is put into the oxidation furnace simultaneously by S220
It is passed through nitrogen into the oxidation furnace；
S230, after keeping the pretreatment temperature 20min-40min, disconnect nitrogen and by the temperature in the oxidation furnace by
Pretreatment temperature rises to reaction temperature, and the reaction temperature is 1000 DEG C -1200 DEG C.
The S300 includes in one of the embodiments,：
S310, between temperature in the oxidation furnace rises to the reaction temperature by the pretreatment temperature, to described
Oxidation furnace is passed through oxygen, and the flow of the oxygen is 10slm/min-15slm/min；
S320, the temperature in the oxidation furnace are increased to after the reaction temperature, and the flow of the oxygen is adjusted
For 9slm/min-10slm/min, the second silicon dioxide layer is formed in the surface of silicon, second silicon dioxide layer is set
It is placed between first silicon oxide layer and the silicon substrate.
Further include in one of the embodiments, S500 after the S400, disconnects hydrogen, continue to lead into the oxidation furnace
Enter oxygen, the flow of the oxygen is 9slm/min-10slm/min, in first silicon dioxide layer far from the silicon substrate
Surface formed third silicon dioxide layer.
Further include in one of the embodiments, S110 after the S100, the silicon substrate is cleaned with cleaning solution.
The cleaning solution is H in one of the embodiments,2SO4\H2O2Mixed solution, NH4OH\H2O2\H2O mixing is molten
Liquid, HCL H2O2\H2It is one or more in O mixed solutions and HF solution.
Further include S600 in one of the embodiments, after the completion of prepared by first silicon dioxide layer, by the oxidation
Temperature in stove is down to 800 DEG C -900 DEG C, temperature fall time 60min-70min.
In the preparation method of silica membrane provided by the present invention, under 1000 DEG C -1200 DEG C of reaction temperature,
The oxygen for being 9slm/min-10slm/min by flow reacts generation with the hydrogen that flow is 14slm/min-14.6slm/min
The vapor of high-purity.The vapor reaches the surface of the silicon substrate by way of diffusion, with the surface of silicon
Silicon quickly react generate the first silicon dioxide layer.The hydrogen is in flow 14slm/min-14.6slm/min, the oxygen
When gas is in flow 9slm/min-10slm/min, the flow velocity size of the hydrogen and oxygen is suitable, has in the oxidation furnace
One preferable reaction atmosphere, so as to fast and efficiently prepare the first silicon dioxide layer, and described prepared
The uniformity of one silicon dioxide layer is greatly improved.
Description of the drawings
Fig. 1 is the flow chart for the silica membrane preparation method that one embodiment of the invention provides；
Fig. 2 is the technological reaction schematic diagram for the silica membrane preparation method that one embodiment of the invention provides；
Fig. 3 is the technological reaction schematic diagram for the silica membrane preparation method that another embodiment of the present invention provides；
The technological reaction schematic diagram for the silica membrane preparation method that Fig. 4 one embodiment of the invention provides；
The technological reaction schematic diagram for the silica membrane preparation method that Fig. 5 one embodiment of the invention provides；
The temperature course schematic diagram of the preparation method for the silica membrane that Fig. 6 one embodiment of the invention provides.
Reference sign
110：Silicon substrate
120：First silicon dioxide layer
130：Second silicon dioxide layer
140：Third silicon dioxide layer
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, by the following examples, it and combines attached
The preparation method of the silica membrane of the present invention is further elaborated in figure.It should be appreciated that tool described herein
Body embodiment only to explain the present invention, is not intended to limit the present invention.
Below in conjunction with the preparation method of the silica membrane of attached drawing the present invention will be described in detail embodiment.
Attached drawing 1 and attached drawing 2 are referred to, one embodiment of the invention provides a kind of silica membrane preparation method comprising
Following steps：
S100 provides a silicon substrate 110；
The silicon substrate 110 is put into oxidation furnace by S200, and the temperature in the oxidation furnace is warming up to reaction temperature,
The reaction temperature is 1000 DEG C -1200 DEG C；
S300 is passed through oxygen into the oxidation furnace, and the flow of the oxygen is 9slm/min-10slm/min；And
S400 after being passed through oxygen 4min-6min into the oxidation furnace, hydrogen is passed through into the oxidation furnace and is lighted a fire,
The flow of the hydrogen is 14slm/min-14.6slm/min, and the first silicon dioxide layer is formed on 110 surface of the silicon substrate
120。
In the S100, the silicon substrate 110 can be P-type wafer or N-type silicon chip.The silicon substrate 110 it is big
Small, thickness and shape are unlimited, can select according to actual needs.In one embodiment, 110 thickness of the silicon substrate is
400um-600um。
In the S200, the oxidation furnace is a kind of device for being used to prepare silica membrane.The oxidation furnace packet
Include ignition furnace, burning torch, synthesis chamber and thermocouple group.The main body of the synthesis chamber is built in ignition furnace, the synthesis chamber
Outlet side extends to outside the ignition furnace and is connected to quartz ampoule.The inlet end of the synthesis chamber extends to outside ignition furnace simultaneously
It is set with burning torch, burning torch inlet end is equipped with hydrogen gas pipe.The inlet end of synthesis chamber is equipped with oxygen intake pipe, thermocouple group
It is divided on ignition furnace and burning torch.
In the S200, the silicon substrate 110 is put into the oxidation furnace.Temperature in oxidation furnace is reaction temperature
Degree, the reaction temperature are 1000 DEG C -1200 DEG C, preferably 1050 DEG C.Reaction temperature increases, and reaction speed is accelerated, and can be improved two
The throughput rate of silicon oxide film.
In the S400, first silicon dioxide layer 120 is that hydrogen-oxygen synthetic method prepares the wet of silica membrane
Oxygen layer.After being passed through oxygen 4min-6min into the oxidation furnace, show for measuring the measurement of meter of the oxygen flow
After number tends towards stability, it is passed through hydrogen into the oxidation furnace and lights a fire, the flow of the hydrogen is 4slm/min-8slm/min.
When can avoid enabling due to flowmeter moment in this way, flow measurement is inaccurate and causes hydrogen and oxygen proportion excessive and quick-fried
It is fried, so as to ensure that the preparation process of silica membrane has higher safety.
In the present embodiment, the silica membrane preparation method is led under 1000 DEG C -1200 DEG C of reaction temperature
It is high that the oxygen that inflow-rate of water turbine is 9slm/min-10slm/min reacts generation with the hydrogen that flow is 14slm/min-14.6slm/min
The vapor of purity.The vapor can diffuse to the surface of the silicon substrate 110 and pasc reaction forms the first silica
Layer 120.When the hydrogen flow be 14slm/min-14.6slm/min, and the flow of the oxygen be 9slm/min-
When 10slm/min, the hydrogen can be reacted with the oxygen generates more vapor, in this way can be in the oxidation furnace
A stable water vapor atmosphere is quickly formed, so as to efficiently prepare preferable first silicon dioxide layer of uniformity
120, and the uniformity for the silica membrane prepared is greatly improved.
In one embodiment, the S400 includes：
S410 after being passed through oxygen 4min-6min into the oxidation furnace, starts to be passed through hydrogen into the oxidation furnace, institute
The flow for stating hydrogen is 4slm/min-8slm/min；And
S420, after hydrogen 0.5min-1.5min is passed through into the oxidation furnace, the flow-rate adjustment by the hydrogen is
14slm/min-14.6slm/min forming the first silicon dioxide layer 120 on 110 surface of the silicon substrate.
In the present embodiment, it is first passed through oxygen, the flow of the oxygen is 9slm/min-10slm/min, described being passed through
After oxygen 4min-6min, start to be passed through hydrogen.The hydrogen is reacted with the oxygen generates vapor, the water vapor diffusion
The first silicon dioxide layer 120 is formed to 110 surface of the silicon substrate and pasc reaction.The flow of the hydrogen is 4slm/min-
8slm/min, after being passed through the hydrogen 0.5min-1.5min that flow is 4slm/min-8slm/min, the measurement registration of flowmeter
It is 14slm/min-14.6slm/min by the flow-rate adjustment of the hydrogen after stabilization.Flowmeter moment can be effectively avoided in this way
When enabling, flow measurement is inaccurate and leads to that hydrogen is excessive with oxygen proportion and explodes, so as to ensure first dioxy
The preparation process of SiClx layer 120 has higher safety.
In one embodiment, in the S300, the oxygen flow is 9.53slm/min.
In the present embodiment, the flow of the oxygen is 9.53slm/min, and the flow of the hydrogen is 14slm/min-
14.6slm/min, preferably 14.3slm/min.The flow velocity of the hydrogen and oxygen is suitable, and the hydrogen and oxygen can react
More vapor is generated, one stable water vapor atmosphere of formation that can be quickly in the oxidation furnace described in this way, to make
It is standby go out preferable first silicon dioxide layer of uniformity 120.
In one embodiment, in the S400, the flow of the hydrogen is 14.3slm/min.
In the present embodiment, the flow of the oxygen is optimal flux 9.53slm/min, and the flow of the hydrogen is optimal
Flow 14.3slm/min.The hydrogen and the oxygen, which can react, generates a large amount of vapor, can be fast in the oxidation furnace
The water vapor atmosphere of the formation stabilization of speed, to prepare the preferable silica membrane of uniformity, the silica membrane
Uniformity can reach within ± 2%.
Table 1 is please referred to, is 9.53slm/min in the flow of oxygen, the flow of the hydrogen is in one embodiment
Under the conditions of 14.3slm/min, can grow thickness by 37.5min and 20min isWithSilica
Film.Data can be seen that in hydrogen flowing quantity be 14.3slm/min from table 1, and oxygen flow is 9.53slm/min conditions
The uniformity of the silica membrane of lower preparation is preferable, is attained by within ± 2%.
The technological parameter and uniformity of the silica membrane of table 1 37.5min and 20min growth
| Time | Temperature (DEG C) | H2Flow | O2Flow | Uniformity in piece | Uniformity between piece |
| 37.5min | 1050 | 14.3 | 9.53 | ≤ ± 0.97% | ± 0.34% |
| 20min | 1050 | 14.3 | 9.53 | ≤ ± 1.35% | ± 0.7% |
In one embodiment, the S200 includes：
S210 provides an oxidation furnace, is heated to pretreatment temperature to the oxidation furnace, the pretreatment temperature is
800℃-900℃；
After the oxidation furnace is warming up to the pretreatment temperature, the silicon substrate 110 is put into the oxidation furnace by S220
And it is passed through nitrogen into the oxidation furnace；And
S230, after keeping the pretreatment temperature 20min-40min, disconnect nitrogen and by the temperature in the oxidation furnace by
Pretreatment temperature rises to reaction temperature, and the reaction temperature is 1000 DEG C -1200 DEG C.
In the present embodiment, the oxidation furnace is warming up to 800 DEG C -900 DEG C of pretreatment temperature, it in this way can be in production two
Reaction efficiency is improved when silicon oxide film.The silicon substrate 110 is put into the oxidation furnace, nitrogen is passed through in the oxidation furnace
Gas can also be passed through other inert gases, not limit herein.The nitrogen is going out the impurities purging in the oxidation furnace
It goes, to ensure the high-purity of silica membrane.The oxidation furnace keeps described 800 DEG C -900 DEG C about 20min- of pretreatment temperature
40min waits for that the temperature in stove is constant, and after reaching stable state, reaction temperature, the reaction temperature are risen to the oxidation stove heat
Degree is 1000 DEG C -1200 DEG C.When temperature in the oxidation furnace is risen to 1000 DEG C -1200 DEG C of the reaction temperature, Neng Goubao
Card carries out the preparation of second silicon dioxide layer 130 in preferably temperature range, described in ensureing quickly to prepare
Second silicon dioxide layer 130.
In one embodiment, the S300 includes：
S310, between temperature in the oxidation furnace rises to the reaction temperature by the pretreatment temperature, to described
Oxidation furnace is passed through oxygen, and the flow of the oxygen is 10slm/min-15slm/min；
S320, the temperature in the oxidation furnace are increased to after the reaction temperature, and the flow of the oxygen is adjusted
For 9slm/min-10slm/min, the second silicon dioxide layer 130, second titanium dioxide are formed on 110 surface of the silicon substrate
Silicon layer 130 is set between first silicon oxide layer 120 and the silicon substrate 110.
Attached drawing 3, attached drawing 4 are referred to, in the present embodiment, waits for temperature in the oxidation furnace by 800 DEG C of pretreatment temperature-
900 DEG C when rising to 1000 DEG C -1200 DEG C of reaction temperature, lead to during rising to the reaction temperature by the pretreatment temperature
Enter oxygen, to carry out the building-up process of the second silicon dioxide layer 130.Second silicon dioxide layer 130 is that silica is thin
First dry oxygen layer of film.The surface that the oxygen diffuses to the silicon substrate 110 is reacted with silicon, to generate the second dioxy
SiClx layer 130.In the present embodiment, the silica membrane can be entirely to diffuse to 110 table of the silicon substrate by oxygen
Prepared by face and pasc reaction, the second silicon dioxide layer 130 constituted, and can also be by the first silicon dioxide layer 120 and the second dioxy
SiClx layer 130 collectively forms, and does not limit herein.
In the present embodiment, the oxygen flow for preparing second silicon dioxide layer 130 is 10slm/min-15slm/
min.There are one relatively stable oxygen atmospheres for tool in the oxidation furnace described in this way, can carry out the second silicon dioxide layer 130 very well
Synthetic reaction, to prepare second silicon dioxide layer 130 with preferable uniformity.When in the oxidation furnace
Temperature rise to after the reaction temperature, the flow of the oxygen is adjusted to 9slm/min-10slm/min.In this way can
Ensure that the oxygen is reacted under the flow condition of 1000 DEG C -1200 DEG C more excellent temperature and 9slm/min-10slm/min
The first silicon dioxide layer 120 is prepared, the preparation time of first silicon dioxide layer 120 greatly shortens, and prepares the dioxy of gained
There has also been larger raisings for the uniformity of SiClx film.
In one embodiment, further include S500, disconnect hydrogen, continue to be passed through oxygen, the oxygen into the oxidation furnace
The flow of gas is 9slm/min-10slm/min, in surface shape of first silicon dioxide layer 120 far from the silicon substrate 110
At third silicon dioxide layer 140.
Fig. 5 and Fig. 6 are referred to, in the present embodiment, after the preparation for completing first silicon dioxide layer 120, is disconnected
The hydrogen continues to be passed through the oxygen, carries out the preparation of third silicon dioxide layer 140, and the third silicon dioxide layer 140 is
Second dry oxygen layer of silica membrane.
In one embodiment, the silica membrane of the method acquisition is dry-wet-dry layer structure.Described two
Silicon oxide film is collectively formed by the first silicon dioxide layer 120, the second silicon dioxide layer 130 and third silicon dioxide layer 140.Institute
The compactness of the silica membrane can be increased by stating the first dry oxygen layer 130 and the second dry oxygen layer 140.The first dry oxygen layer
130 and second dry oxygen layer 140 growth rate it is slower relative to the growth rate of wet oxygen layer 120, it is contemplated that silica is thin
The thickness of the manufacturing cost of film, the second dry oxygen layer 140 and the first dry oxygen layer 130 is no more than 700 angstroms.Therefore, when
The thickness of the second dry oxygen layer 140 and the first dry oxygen layer 130 is no more than 700 angstroms, then the silica membrane has
Preferable compactness, and the manufacturing cost of the silica membrane is relatively low.
In the present embodiment, the oxygen flow for preparing the third silicon dioxide layer 140 is 9slm/min-10slm/min,
Preferably 9.53slm/min.Continue the preparation of third silicon dioxide layer 140 on 120 surface of the first silicon dioxide layer,
The compactness of the silica membrane can be increased in this way.
In one embodiment, further include S110 after the S100, the silicon substrate 110 is cleaned with cleaning solution.
110 surface of the silicon substrate there may be pollution impurity, including organic matter and inorganic matter.These impurity are with atom
State, ionic condition, form of film or particle form are present in 110 surface of the silicon substrate.Thoroughly to understand these impurity, with
The silica membrane for generating high-purity, in the present embodiment cleans the silicon substrate 110 using cleaning solution.
In one embodiment, the cleaning solution includes H2SO4\H2O2Mixed solution, NH4OH\H2O2\H2O mixing is molten
Liquid, HCL H2O2\H2It is one or more in O mixed solutions and HF solution.
In the present embodiment, the selection of the cleaning solution is selected according to different types of impurity is removed.H2SO4\
H2O2Mixed solution can be used for removing weight organic impurities.NH4OH\H2O2\H2O mixed solutions can be used for removing organic
Object, inorganic matter, metal ion.HCL\H2O2\H2O mixed solutions can be used for removing the metal ions such as aluminium, iron, sodium.HF solution can
For removing metal ion and natural oxidizing layer.
It in one embodiment,, will be in the oxidation furnace after the completion of prepared by the silica membrane after the S600
Temperature be down to 800 DEG C -900 DEG C, time 60min-70min.
Attached drawing 6 is referred to, in the present embodiment, after the S600, after the completion of prepared by the silica membrane, by institute
The temperature stated in oxidation furnace is down to 800 DEG C -900 DEG C for 1000 DEG C -1200 DEG C by reaction temperature.By 1000 DEG C of reaction temperature-
1200 DEG C are down to during 800 DEG C -900 DEG C, can be passed through nitrogen and be cooled down, can also be passed through other inert gases, herein
It does not limit.By reducing the temperature in the oxidation furnace, the temperature in reacting furnace can be avoided too high and caused by safety it is hidden
Suffer from.
Each technical characteristic of embodiment described above can carry out arbitrary combination, to keep description clean and tidy, not to above-mentioned implementation
The all possible combination of each technical characteristic in example is all described, as long as however, the combination of these technical characteristics is not present
Contradiction is all considered to be the range of this specification record.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of silica membrane preparation method, including：
S100 provides a silicon substrate (110)；
S200, the silicon substrate (110) is put into oxidation furnace, the temperature in the oxidation furnace is warming up to reaction temperature, institute
It is 1000 DEG C -1200 DEG C to state reaction temperature；
S300 is passed through oxygen into the oxidation furnace, and the flow of the oxygen is 9slm/min-10slm/min；And
S400 after being passed through oxygen 4min-6min into the oxidation furnace, hydrogen is passed through into the oxidation furnace and is lighted a fire, described
The flow of hydrogen is 14slm/min-14.6slm/min, and the first silicon dioxide layer is formed on the silicon substrate (110) surface
(120)。
2. silica membrane preparation method as described in claim 1, which is characterized in that the S400 includes：
S410 after being passed through oxygen 4min-6min into the oxidation furnace, starts to be passed through hydrogen into the oxidation furnace, the hydrogen
The flow of gas is 4slm/min-8slm/min；
The flow-rate adjustment of the hydrogen is 14slm/ after being passed through hydrogen 0.5min-1.5min into the oxidation furnace by S420
Min-14.6slm/min forms the first silicon dioxide layer (120) on the silicon substrate (110) surface.
3. silica membrane preparation method as described in claim 1, which is characterized in that in the S300, the oxygen
Flow is 9.53slm/min.
4. silica membrane preparation method as claimed in claim 3, which is characterized in that in the S400, the hydrogen
Flow is 14.3slm/min.
5. silica membrane preparation method as described in claim 1, which is characterized in that the S200 includes：
S210 provides an oxidation furnace, and pretreatment temperature is heated to the oxidation furnace, and the pretreatment temperature is 800 DEG C-
900℃；
After the oxidation furnace is warming up to the pretreatment temperature, the silicon substrate (110) is put into the oxidation furnace simultaneously by S220
It is passed through nitrogen into the oxidation furnace；
S230 after keeping the pretreatment temperature 20min-40min, disconnects nitrogen and by the temperature in the oxidation furnace by advance
Reason temperature rises to reaction temperature, and the reaction temperature is 1000 DEG C -1200 DEG C.
6. silica membrane preparation method as described in claim 1, which is characterized in that the S300 includes：
S310, between temperature in the oxidation furnace rises to the reaction temperature by the pretreatment temperature, to the oxidation
Stove is passed through oxygen, and the flow of the oxygen is 10slm/min-15slm/min；
S320, the temperature in the oxidation furnace are increased to after the reaction temperature, and the flow of the oxygen is adjusted to
9slm/min-10slm/min forms the second silicon dioxide layer (130), second dioxy on the silicon substrate (110) surface
SiClx layer (130) is set between first silicon oxide layer (120) and the silicon substrate (110).
7. the preparation method of silica membrane as described in claim 1, which is characterized in that further include：S500 disconnects hydrogen
Gas continues to be passed through oxygen into the oxidation furnace, and the flow of the oxygen is 9slm/min-10slm/min, the described 1st
Surface of the silicon oxide layer (120) far from the silicon substrate (110) forms third silicon dioxide layer (140).
8. the preparation method of silica membrane as described in claim 1, which is characterized in that further include after the S100,
S110 cleans the silicon substrate (110) with cleaning solution.
9. the preparation method of silica membrane as claimed in claim 8, which is characterized in that the cleaning solution is H2SO4\H2O2
Mixed solution, NH4OH\H2O2\H2O mixed solutions, HCL H2O2\H2It is one or more in O mixed solutions and HF solution.
10. such as the preparation method of claim 1-9 any one of them silica membranes, which is characterized in that further include：
Temperature in the oxidation furnace after the completion of prepared by first silicon dioxide layer, is down to 800 DEG C -900 DEG C, drop by S600
The warm time is 60min-70min.
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