CN108796473A - A kind of thermal decomposition preparation method of film - Google Patents
A kind of thermal decomposition preparation method of film Download PDFInfo
- Publication number
- CN108796473A CN108796473A CN201810722203.XA CN201810722203A CN108796473A CN 108796473 A CN108796473 A CN 108796473A CN 201810722203 A CN201810722203 A CN 201810722203A CN 108796473 A CN108796473 A CN 108796473A
- Authority
- CN
- China
- Prior art keywords
- quartz ampoule
- substrate
- catch
- pyrolytic reaction
- film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- C23C16/48—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 by irradiation, e.g. photolysis, radiolysis, particle radiation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C16/4409—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber characterised by sealing means
-
- 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
- C23C16/4412—Details relating to the exhausts, e.g. pumps, filters, scrubbers, particle traps
-
- 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
- C23C16/448—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 characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4486—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 characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by producing an aerosol and subsequent evaporation of the droplets or particles
-
- 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
- C23C16/455—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 characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45587—Mechanical means for changing the gas flow
- C23C16/45591—Fixed means, e.g. wings, baffles
Abstract
The present invention discloses a kind of thermal decomposition preparation method of film, it is characterised in that includes the following steps：Step a：Design a equipment for producing thin film；Step b：The input end of compressed pipe is connected to the aerosol output end of atomizer, and the precursor liquid for waiting for pyrolytic reaction is added in atomizer；Step c：First start atomizer, after precursor liquid is atomized and generates aerosol；Step d：It can pass through the response situation inside quartz ampoule and upper cover plate observation when pyrolytic reaction；Step e：It waits for a period of time and takes out substrate after substrate cooling.The deposition boat for being horizontally arranged substrate is arranged in the Preparation equipment of this preparation method, the deposition boat has pyrolytic reaction chamber, and coordinate the necking of the first and second thermal resistance piece and compressed pipe that the flow field of pyrolytic reaction chamber, temperature field can be allowed constant, to make substrate near surface airflow field, temperature field constant, it is final to ensure being smoothed out for pyrolytic reaction, greatly improve the quality of forming film of film.
Description
Technical field
The invention belongs to field of film preparation more particularly to a kind of thermal decomposition preparation methods of film.
Background technology
In the industrial production, it is often necessary in substrate surface plated film.Existing thin film preparation process is mainly using thermal decomposition
Mode, a kind of thermal decomposition manner is using tube furnace to the silicon in quartz ampoule, axis parallel of the substrate along quartz ampoule
It is arranged or is obliquely installed, so that in substrate near surface pyrolytic reaction occurs for precursor gas colloidal sol species, in substrate surface
Adhere to film.Also, pyrolysis carries out under normal pressure or low pressure and vacuum environment.
The defect of existing thermal decomposition process is as follows：1, we have found that existing thermal decomposition process can not make high quality always
Film, however the reaction mechanism that pyrolysis prepares film is very complicated, and all not yet research is clear so far by those skilled in the art
Chu.Present preliminary analysis film quality is related with the gentle even flow field degree in the temperature field of substrate near surface, and existing substrate
Arrangement is open, can not ensure the gentle even flow field in the temperature field of substrate near surface, constant.Also, the quality of film
Also related with precursor gas colloidal sol species " activity ", we also want to " activity " of precursor gas colloidal sol species when preparing film
It is high as much as possible.
In addition, existing pyrolysis carries out under low pressure, vacuum environment, resulted in this way to equipment requirement height, if
It is standby expensive.Also, carry out pyrolytic reaction in very pressure, must be requested that the environment of a relative closure results in this way
Carry out continuous production needs to pay more costs, and equipment complexity also results in the raising of failure rate.
Invention content
Technical problem to be solved by the present invention lies in providing a kind of thermal decomposition preparation method of film, film to be improved
Quality of forming film.
Technical scheme is as follows：A kind of thermal decomposition preparation method of film, it is characterised in that include the following steps：
Step a：A equipment for producing thin film is designed, which includes quartz ampoule (1), the heat point of the quartz ampoule
Solution part is located in the furnace chamber of tube furnace (2), the inside of quartz ampoule (1) input end be coaxially provided with one it is molten for precursor gas
Glue by compressed pipe (3), sealed between the input end of the input end and quartz ampoule (1) of the compressed pipe, pressed by sealing structure
The outlet end necking of the draw (3), and it is cased with interior cooling tube (4) on compressed pipe (3) outer wall；Compressed pipe (3) outlet end
Outside is installed with the first thermal resistance piece (5), which fixes and seal with the inner wall of the quartz ampoule (1) simultaneously；It is described
Sealing shroud (6) is equipped at quartz ampoule (1) outlet end, which is connected with exhaust collection cooling component, and goes out in quartz ampoule (1)
Mouth is cased with outer cooling tube (7) outside end；The inside of quartz ampoule (1) outlet end is coaxially provided with the second thermal resistance piece (8), this second
Thermal resistance piece is fixed with quartz ampoule (1) and seals, and the quartz ampoule (1) between the second thermal resistance piece (8) and first thermal resistance piece (5)
Interior to be equipped with deposition boat (C), the deposition boat is for installing substrate, and the position of deposition boat (C) corresponds to the stove of the tube furnace (2)
Chamber；
The deposition boat (C) includes catch (9) and gear air parcel (16), and wherein catch (9) number is two panels, this two panels catch
(9) along the axial direction setting of the quartz ampoule (1), and it is connected by intermediate axial connecting rod (10)；Catch described in two panels (9) phase
Back to surface it is respectively coaxially fixed there are one fixed ring (11), same axis clamping between the fixed ring and corresponding catch (9)
There are multiple opening gaskets (12), these opening gaskets circumferentially mutual dislocation, and be open gasket (12) and the quartz ampoule (1)
Inner wall is in close contact, and there are gaps between catch (9) and fixed ring (11) and quartz ampoule (1) inner wall；Catch described in two panels
(9) notch there are one opening is corresponded at center, and upper cover plate (13) and lower cover (14) are fitted between the two notches；On described,
The both sides of lower cover (13,14) are respectively equipped with a height adjustment pad item (15), axis of the height adjustment pad item along quartz ampoule (1)
To setting, and the pyrolytic reaction of a rectangular-shape is formed between the above, the lower lid (13,14) and two height adjustment pad items (15)
Chamber, and substrate is placed on the lower cover (14) upper surface；The gear air parcel (16) is made of bar shaped interconnecting piece and occlusion part,
Middle occlusion part is n shape structures, is fixed with bar shaped interconnecting piece bottom end at the top of the connection side of occlusion part, on the bar shaped interconnecting piece
Locking nut (17) is equipped in strip-shaped hole, on a locking nut catch (9) installed therein, so as to adjust gear gas
The height of block (16)；The gear air parcel (16) is located at the inlet end of deposition boat (C), and can be connected by keeping off the occlusion part of air parcel (16)
Edge fit blocks the gap between upper cover plate (13) and corresponding catch (9) notch, to prevent precursor gas colloidal sol from the gap
Leakage；Light loading hole (2a) there are one being opened on the bell of the tube furnace (2), and the material of the upper cover plate (13) is transparent
Quartz material, to make, the short wavelength light of load passes through light loading hole (2a) and upper cover plate (13) is irradiated to lower cover (14)
On substrate；It remains electrically isolated between the above, the lower lid (13,14), and is connected respectively with an electrode, the two electrodes
Polarity is opposite；
Step b：The input end of compressed pipe (3) is connected to the aerosol output end of atomizer, and is added in atomizer
It waits for the precursor liquid of pyrolytic reaction, and substrate is horizontally arranged in lower cover (14) upper surface, described in the position face of the substrate
Light loading hole (2a)；
Step c：First start atomizer, after precursor liquid is atomized and generates aerosol, starts the film preparation and set
Standby and tube furnace (2), and short wavelength light is loaded, simultaneously or separately two electrodes can also be given to be powered；
Step d：It can pass through the response situation inside quartz ampoule (1) and upper cover plate (13) observation when pyrolytic reaction, reach pre-
Atomizer is closed after determining sedimentation time, the time required further according to concrete technology closes tube furnace (2) and equipment for producing thin film；
Step e：It waits for a period of time, takes out substrate after substrate cooling.
In the above preparation method, compressed pipe (3) input end is connected with atomizer, to the presoma for making atomizer generate
Precursor gas colloidal sol enters in compressed pipe, and interior cooling tube (4) can first cool down to the presoma precursor gas colloidal sol of high temperature, prevent
Only because temperature is excessively high pyrolytic reaction occurs in advance for presoma precursor gas colloidal sol, to ensure presoma precursor gas colloidal sol
Pyrolytic reaction just occurs at pyrolytic reaction chamber.The outlet end necking of compressed pipe (3), thus can be to the presoma forerunner of output
Aerosol is compressed, and output pressure is improved, and ensures that presoma precursor gas colloidal sol is moved along the axial line of quartz ampoule as possible
It is dynamic, to ensure the axial line presoma precursor gas colloidal sol even flow field along quartz ampoule as possible.Meanwhile tube furnace (2) is to stone
English pipe (1) heats, to allow the presoma precursor gas colloidal sol in quartz ampoule to heat up, and the first thermal resistance piece (5) and the second thermal resistance
The organic cooperation of piece can effectively carry out thermal resistance, prevent heat from running helter-skelter, and by heat " lock " in the first thermal resistance piece (5) and the second thermal resistance
Region between piece, and make the temperature field at deposition boat (C) constant, to ensure being smoothed out for pyrolytic reaction, and then improve
The quality of forming film of film.Also, substrate level is arranged, and is located at narrow pyrolytic reaction intracavitary, high temperature presoma precursor gas
Colloidal sol aggregation, be oppressed by the way that pyrolytic reaction occurs when narrow pyrolytic reaction chamber, narrow pyrolytic reaction intracavitary flow field,
Temperature field is stablized relatively, and then ensures that substrate near surface flow field, temperature field are stablized relatively.Meanwhile the wavelength of short wavelength light exists
356nm is hereinafter, such as ultraviolet light.The effect of short wavelength light is to improve precursor gas sol particle " activity ", to ensure
Pyrolytic reaction be smoothed out and the extent of reaction, and then improve film quality of forming film.This process is in the above, the lower lid
Between (13,14) formed an electric field, to allow by precursor gas colloidal sol electrification, and then reach excitation precursor gas colloidal sol
The purpose of " activity ", ensure pyrolytic reaction be smoothed out and the extent of reaction, finally further increase the quality of forming film of film, this
Measure is organically combined with load short wavelength light, and the effect of 1+1 > 2 can be played for improving forming thin film quality.Specific
In implementation process, the above, the lower lid (13,14) determines according to actual conditions polarity.Using above-mentioned technical proposal, this preparation side
Method can effectively improve the quality of forming film of film.
In the present case, the exhaust collection cooling component includes exhaust gas collecting pipe (18) and cover board (21), and wherein tail gas is received
Collector (18) inlet end is connected with the centre bore of the sealing shroud (6), the outlet side of the exhaust gas collecting pipe and U-tube (19) into
Gas end is connected, and the outlet side of the U-tube is connected with exhaust collection device；The U-tube (19) is located in water-cooled cylinder (20), the water cooling
It is open by the cover board (21) closing at the top of cylinder (20).
Using the above structure, tail gas can be cooled down well, adverse current interferes substrate after preventing exhaust temperature excessively high
The pyrolytic reaction at place is smoothed out, so as to improve the performance of the present invention.
In order to further improve thermal resistance effect, the number of first thermal resistance piece (5) and the second thermal resistance piece (8) is respectively two
Piece.
The height adjustment pad item (15) of different height can be replaced for different precursor liquids as preferred design,
Pyrolytic reaction occurs in the pyrolytic reaction intracavitary of suitable size after being atomized so as to precursor liquid.
Preferably, when preparing, can also by importing diluent gas and/or protective gas at deposition boat (C),
Middle diluent gas effect is that the concentration for adjusting precursor gas colloidal sol or the chemical atmosphere for adjusting deposition region, protective gas are made
With being the chemical change for preventing sample from may occur after atomization.
Advantageous effect：The deposition boat for being horizontally arranged substrate, deposition boat tool is arranged in the Preparation equipment of this preparation method
There is pyrolytic reaction chamber, and coordinates the necking of the first and second thermal resistance piece and compressed pipe that the flow field of pyrolytic reaction chamber, temperature field can be allowed permanent
It is fixed, to make substrate near surface airflow field, temperature field constant, while being carried further through the mode of load short wavelength light and added electric field
" activity " of high presoma precursor gas colloidal sol, it is final to ensure being smoothed out for pyrolytic reaction, greatly improve film at film quality
Amount, preparation method have apparent substantive distinguishing features and significant technological progress with the prior art.
Description of the drawings
Fig. 1 is the structural schematic diagram of equipment for producing thin film of the present invention.
Fig. 2 is the internal structure schematic diagram of Fig. 1 quartz ampoules.
Fig. 3 is the schematic diagram of deposition boat in Fig. 2.
Specific implementation mode
The invention will be further described with reference to the accompanying drawings and examples：
A kind of thermal decomposition preparation method of film, it is characterised in that include the following steps：
Step a：A equipment for producing thin film is designed, such as Fig. 1 -- shown in 3, which includes mainly quartz ampoule
1, the compositions such as tube furnace 2, compressed pipe 3, interior cooling tube 4 and first thermal resistance piece 5.Wherein, the thermal decomposition part of quartz ampoule 1 is located at pipe
In the furnace chamber of formula stove 2, which is outsourcing piece, for being heated to quartz ampoule.In the present case, it is provided on the bell of tube furnace 2
One light loading hole 2a, light loading hole 2a run through the top and bottom of bell, and light loading hole 2a can allow short wavelength
Light passes through.
1 input end of quartz ampoule is connected when using with atomizer, to the presoma precursor gas colloidal sol for allowing atomizer to occur
Into in quartz ampoule 1.The inside of 1 input end of quartz ampoule be coaxially provided with one for precursor gas colloidal sol by compressed pipe 3, the pressure
It is sealed by sealing structure between the input end and the input end of quartz ampoule 1 of the draw 3.In the present case, sealing structure is by input end
Sealing shroud 22 and input end seal cover board 23 form, and wherein input end sealing shroud 22 is solidly set on 1 input end of quartz ampoule, the input end
The annular portion of sealing shroud 22 and input end seal cover board 23 are coaxially connected, and the compressed pipe 3 and input end seal cover board 23 1
Body structure, and the input end of compressed pipe 3 is coaxially fixed with 23 inner plate surface of input end seal cover board.In being cased on 3 outer wall of compressed pipe
Cooling tube 4, the interior cooling tube 4 are cooled down using water-cooling pattern, and the effect of interior cooling tube 4 comes to atomizer conveying
High temperature precursor gas colloidal sol is cooled down, and prevents high temperature precursor gas colloidal sol from not reaching substrate also and pyrolysis just occurs, from
And ensures pyrolysis and be happened at substrate.The outlet end necking of compressed pipe 3 can thus increase the output of precursor gas colloidal sol
Air pressure when compressed pipe 3, to utmostly ensure that precursor gas colloidal sol is moved along the axial line of quartz ampoule 1, before final guarantee
Aerosol is driven in 1 axis line location even flow field of quartz ampoule.
Such as Fig. 1 -- shown in 3, the first thermal resistance piece 5 is installed with outside 3 outlet end of the compressed pipe, first thermal resistance piece is same
When fix and seal with the inner wall of the quartz ampoule 1.In the present case, 5 number of the first thermal resistance piece is two panels, this first thermal resistance of two panels
It is spaced 3-10mm between piece 5, thus can utmostly prevent hot gas toward the input end reverse flow of quartz ampoule 1, thermal resistance effect
It is good.Sealing shroud 6 is equipped at 1 outlet end of quartz ampoule, which is connected with exhaust collection cooling component, and is exported in quartz ampoule 1
End outside is cased with outer cooling tube 7, which uses water-cooling pattern, and effect is to prevent exhaust temperature excessively high, to avoid
The tail gas of high temperature ensures being smoothed out for pyrolytic reaction toward the reverse flow of pyrolytic reaction region.Exhaust collection cooling component
Including exhaust gas collecting pipe 18 and cover board 21, wherein 18 inlet end of exhaust gas collecting pipe is connected with the centre bore of the sealing shroud 6, the tail
The outlet side of gas collecting pipe 18 is connected with the inlet end of U-tube 19, and the outlet side of the U-tube is connected with exhaust collection device；The U
Shape pipe 19 is located in water-cooled cylinder 20, and the opening at 20 top of water-cooled cylinder is closed by the cover board 21.
The inside of 1 outlet end of quartz ampoule is coaxially provided with the second thermal resistance piece 8, and second thermal resistance piece and quartz ampoule 1 are fixed and close
Envelope, in the present case, the number of the second thermal resistance piece 8 are two panels, and the spacing between this second thermal resistance piece of two panels 8 is 5-20mm, and two
The centre bore of the second thermal resistance piece of piece 8 is concentric, and with the axial line of quartz ampoule 1 on same straight line.Second thermal resistance piece 8 and first
Deposition boat C is equipped in quartz ampoule 1 between thermal resistance piece 5, deposition boat C is for installing substrate, and the position respective tube of deposition boat C
The furnace chamber of formula stove 2.
Such as Fig. 1 -- shown in 3, deposition boat C includes catch 9 and gear air parcel 16, and wherein 9 number of catch is two panels, this two panels gear
Piece 9 is arranged along the axial direction of quartz ampoule 1, and is connected by intermediate 3 axial connecting rods 10, this 3 axial distributions of connecting rods 10
On the same circumference.9 opposite facing surface of two panels catch is respectively coaxially fixed there are one fixed ring 11, the fixed ring 11 with it is right
There are multiple opening gaskets 12 with axis clamping between the catch 9 answered, these circumferentially mutual dislocations of gaskets 12 that are open.In this case
In, there are 2 opening gaskets 12, the gap position of this 2 opening gaskets 12 with axis clamping between fixed ring 11 and corresponding catch 9
Relatively.Be open gasket 12 and 1 inner wall of quartz ampoule is in close contact, between catch 9 and fixed ring 11 and 1 inner wall of quartz ampoule there are
Gap prevents presoma leakage of aerosol to realize sealing by the gasket 12 that is open.This case has bullet using opening gasket 12
The characteristics of property, is sealed, to solve the defect that can not be effectively sealed between rigid catch 9, fixed ring 11 and quartz ampoule 1.
Notch (unmarked in figure) there are one opening is corresponded at 9 center of two panels catch, and one piece is fitted between the two notches
Upper cover plate 13 and one piece of lower cover 14, this two cover plates are horizontal positioned.The both sides of upper cover plate 13 and lower cover 14 are respectively equipped with one
Root height adjustment pad item 15, axial direction setting of the height adjustment pad item 15 along quartz ampoule 1.Upper cover plate 13, lower cover 14 and two
The pyrolytic reaction chamber of a rectangular-shape is formed between height adjustment pad item 15, which is slit, and pyrolytic reaction
The height of chamber can be realized by replacing different height adjustment pad items 15, to make different presomas in most suitable space
Pyrolytic reaction occurs in the pyrolytic reaction chamber of size.Before pyrolytic reaction, substrate level is placed on to the upper surface of lower cover 14.
Gear air parcel 16 is made of bar shaped interconnecting piece and occlusion part, and wherein occlusion part is n shape structures, the connection side top of occlusion part and bar shaped
Interconnecting piece bottom end is fixed, and is equipped with locking nut 17 in the strip-shaped hole on the bar shaped interconnecting piece, the locking nut is installed therein
On one catch 9, so as to adjust the height of gear air parcel 16.Gear air parcel 16 is located at the inlet end of deposition boat C, and can pass through gear
The occlusion part connection side bumper of air parcel 16 lives in the gap between cover board 13 and 9 notch of corresponding catch, to prevent precursor gas molten
Glue is revealed from the gap.In addition, the outlet side of deposition boat C is set, there are one pull block 30, the pull block 30 and two above-mentioned axis
It is fixed to 10 end of connecting rod, and pull block 30 is used to that deposition boat C to be pulled out or is pumped into out of quartz ampoule 1, so as to demolition, installation
Deposition boat C.
Such as Fig. 1 -- shown in 3, the material of upper cover plate 13 is suprasil material, to make the short wavelength light of load pass through
Light loading hole 2a and upper cover plate 13 are irradiated to the substrate on lower cover 14.Meanwhile electricity is kept between upper cover plate 13, lower cover 14
Insulation, and be connected respectively with an electrode, the polarity of the two electrodes is opposite.In addition, deposition boat C, compressed pipe 3, the second thermal resistance
Piece 8 and 5 axial line of the first thermal resistance piece are and conllinear with the axial line of quartz ampoule 1 on same straight line.
Step b：The input end of compressed pipe 3 is connected to the aerosol output end of atomizer, and is added and waits in atomizer
The precursor liquid of pyrolytic reaction, and it is horizontally arranged substrate, the position face light load of the substrate in 14 upper surface of lower cover
Hole 2a；
Step c：First start atomizer, after precursor liquid be atomized generate aerosol after, start equipment for producing thin film and
Tube furnace 2, and short wavelength light is loaded, simultaneously or separately two electrodes can also be given to be powered；Preferably, when preparing, also
It can be by the way that importing diluent gas and/or protective gas at deposition boat C, wherein diluent gas effect be to adjust precursor gas
The concentration of colloidal sol or the chemical atmosphere for adjusting deposition region, protective gas effect are to prevent sample may after atomization
The chemical change of generation.Importing diluent gas and/or protective gas can be imported by atomizer, can also be set using other
It is standby.
Step d：It can pass through quartz ampoule 1 when pyrolytic reaction and upper cover plate 13 observe internal response situation, reach predetermined heavy
Atomizer is closed after the product time, the time required further according to concrete technology closes tube furnace 2 and equipment for producing thin film；
Step e：It waits for a period of time, takes out substrate after substrate cooling.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not limitation, all essences in the present invention with the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (5)
1. a kind of thermal decomposition preparation method of film, it is characterised in that include the following steps：
Step a：A equipment for producing thin film is designed, which includes quartz ampoule (1), the thermal decomposition portion of the quartz ampoule
Divide in the furnace chamber of tube furnace (2), the inside of quartz ampoule (1) input end is coaxially provided with one and leads to for precursor gas colloidal sol
The compressed pipe (3) crossed is sealed between the input end of the input end and quartz ampoule (1) of the compressed pipe, compressed pipe by sealing structure
(3) outlet end necking, and it is cased with interior cooling tube (4) on compressed pipe (3) outer wall；The outside of compressed pipe (3) outlet end
It is installed with the first thermal resistance piece (5), which fixes and seal with the inner wall of the quartz ampoule (1) simultaneously；The quartz
It manages and is equipped with sealing shroud (6) at (1) outlet end, which is connected with exhaust collection cooling component, and in quartz ampoule (1) outlet end
Outside is cased with outer cooling tube (7)；The inside of quartz ampoule (1) outlet end is coaxially provided with the second thermal resistance piece (8), second thermal resistance
Piece is fixed with quartz ampoule (1) and seals, and is set in the quartz ampoule (1) between the second thermal resistance piece (8) and first thermal resistance piece (5)
There is deposition boat (C), the deposition boat is for installing substrate, and the position of deposition boat (C) corresponds to the furnace chamber of the tube furnace (2)；
The deposition boat (C) includes catch (9) and gear air parcel (16), and wherein catch (9) number is two panels, this two panels catch (9)
Along the axial direction setting of the quartz ampoule (1), and it is connected by intermediate axial connecting rod (10)；Catch described in two panels (9) is opposite
To surface it is respectively coaxially fixed there are one fixed rings (11), have with axis clamping between the fixed ring and corresponding catch (9)
Multiple opening gaskets (12), these gaskets circumferentially mutual dislocations that are open, and the gasket (12) that is open is interior with the quartz ampoule (1)
Wall is in close contact, and there are gaps between catch (9) and fixed ring (11) and quartz ampoule (1) inner wall；Catch described in two panels (9)
Notch there are one opening is corresponded at center, and upper cover plate (13) and lower cover (14) are fitted between the two notches；The upper and lower cover
The both sides of plate (13,14) are respectively equipped with a height adjustment pad item (15), which sets along the axial direction of quartz ampoule (1)
It sets, and forms the pyrolytic reaction chamber of a rectangular-shape between the above, the lower lid (13,14) and two height adjustment pad items (15),
And substrate is placed on the lower cover (14) upper surface；The gear air parcel (16) is made of bar shaped interconnecting piece and occlusion part, wherein
Occlusion part is n shape structures, is fixed with bar shaped interconnecting piece bottom end at the top of the connection side of occlusion part, the item on the bar shaped interconnecting piece
Locking nut (17) is equipped in shape hole, on a locking nut catch (9) installed therein, so as to adjust gear air parcel
(16) height；The gear air parcel (16) is located at the inlet end of deposition boat (C), and can be connected by keeping off the occlusion part of air parcel (16)
Side bumper lives in the gap between cover board (13) and corresponding catch (9) notch, to prevent precursor gas colloidal sol from being let out from the gap
Dew；Light loading hole (2a) there are one being opened on the bell of the tube furnace (2), and the material of the upper cover plate (13) is transparent stone
English material, to make, the short wavelength light of load passes through light loading hole (2a) and upper cover plate (13) is irradiated on lower cover (14)
Substrate；It remains electrically isolated between the above, the lower lid (13,14), and is connected respectively with an electrode, the pole of the two electrodes
Property is opposite；
Step b：The input end of compressed pipe (3) is connected to the aerosol output end of atomizer, and is added in atomizer and waits for heat
The precursor liquid of reaction is solved, and substrate is horizontally arranged in lower cover (14) upper surface, light described in the position face of the substrate
Loading hole (2a)；
Step c：First start atomizer, after precursor liquid be atomized generate aerosol after, start the equipment for producing thin film and
Tube furnace (2), and short wavelength light is loaded, simultaneously or separately two electrodes can also be given to be powered；
Step d：It can pass through the response situation inside quartz ampoule (1) and upper cover plate (13) observation when pyrolytic reaction, reach predetermined heavy
Atomizer is closed after the product time, the time required further according to concrete technology closes tube furnace (2) and equipment for producing thin film；
Step e：It waits for a period of time, takes out substrate after substrate cooling.
2. the thermal decomposition preparation method of film according to claim 1, it is characterised in that：The exhaust collection cooling component
Including exhaust gas collecting pipe (18) and cover board (21), the wherein centre bore of exhaust gas collecting pipe (18) inlet end and the sealing shroud (6)
It is connected, the outlet side of the exhaust gas collecting pipe is connected with the inlet end of U-tube (19), outlet side and the exhaust collection device of the U-tube
It is connected；The U-tube (19) is located in water-cooled cylinder (20), open by the cover board (21) closing at the top of the water-cooled cylinder (20).
3. the thermal decomposition preparation method of film according to claim 1, it is characterised in that：First thermal resistance piece (5) and
The number of second thermal resistance piece (8) is respectively two panels.
4. the thermal decomposition preparation method of film according to claim 1, it is characterised in that：For different precursor liquids
Body can replace the height adjustment pad item (15) of different height, and the pyrolysis after being atomized so as to precursor liquid in suitable size is anti-
Answer intracavitary that pyrolytic reaction occurs.
5. the thermal decomposition preparation method of film according to claim 1, it is characterised in that：When preparation, can also pass through to
Diluent gas and/or protective gas are imported at deposition boat (C), wherein diluent gas effect is the dense of adjusting precursor gas colloidal sol
Degree or the chemical atmosphere for adjusting deposition region, protective gas effect is the change for preventing sample from may occur after atomization
Learn variation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810722203.XA CN108796473B (en) | 2018-06-26 | 2018-06-26 | Thermal decomposition preparation method of film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810722203.XA CN108796473B (en) | 2018-06-26 | 2018-06-26 | Thermal decomposition preparation method of film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108796473A true CN108796473A (en) | 2018-11-13 |
| CN108796473B CN108796473B (en) | 2020-03-31 |
Family
ID=64074484
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810722203.XA Active CN108796473B (en) | 2018-06-26 | 2018-06-26 | Thermal decomposition preparation method of film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108796473B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109440083A (en) * | 2018-12-25 | 2019-03-08 | 重庆理工大学 | It is atomized assisted CVD membrane deposition method |
| CN114774883A (en) * | 2022-04-14 | 2022-07-22 | 重庆理工大学 | Compact atomizing auxiliary CVD film preparation device |
| CN114892144A (en) * | 2022-04-14 | 2022-08-12 | 重庆理工大学 | Atomization-assisted CVD reaction cavity |
| CN114918087A (en) * | 2022-04-14 | 2022-08-19 | 重庆理工大学 | Circular tube outer wall coating device |
| CN114990522A (en) * | 2022-04-14 | 2022-09-02 | 重庆理工大学 | Thermal decomposition film preparation device |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007324318A (en) * | 2006-05-31 | 2007-12-13 | Tsukishima Kikai Co Ltd | Substrate treating apparatus and substrate treatment method |
| CN101245453A (en) * | 2007-12-27 | 2008-08-20 | 北京石油化工学院 | Equipment for producing thin film with whirl coating atomizing thermal decomposition |
| JP2012204694A (en) * | 2011-03-25 | 2012-10-22 | Hitachi Kokusai Electric Inc | Manufacturing method of semiconductor device and substrate processing device |
| CN103834931A (en) * | 2014-03-13 | 2014-06-04 | 华延芯光（北京）科技有限公司 | Equipment for carrying out chemical vapor deposition process |
-
2018
- 2018-06-26 CN CN201810722203.XA patent/CN108796473B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007324318A (en) * | 2006-05-31 | 2007-12-13 | Tsukishima Kikai Co Ltd | Substrate treating apparatus and substrate treatment method |
| CN101245453A (en) * | 2007-12-27 | 2008-08-20 | 北京石油化工学院 | Equipment for producing thin film with whirl coating atomizing thermal decomposition |
| JP2012204694A (en) * | 2011-03-25 | 2012-10-22 | Hitachi Kokusai Electric Inc | Manufacturing method of semiconductor device and substrate processing device |
| CN103834931A (en) * | 2014-03-13 | 2014-06-04 | 华延芯光（北京）科技有限公司 | Equipment for carrying out chemical vapor deposition process |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109440083A (en) * | 2018-12-25 | 2019-03-08 | 重庆理工大学 | It is atomized assisted CVD membrane deposition method |
| CN109440083B (en) * | 2018-12-25 | 2020-09-25 | 重庆理工大学 | Atomization-assisted CVD film deposition method |
| CN114774883A (en) * | 2022-04-14 | 2022-07-22 | 重庆理工大学 | Compact atomizing auxiliary CVD film preparation device |
| CN114892144A (en) * | 2022-04-14 | 2022-08-12 | 重庆理工大学 | Atomization-assisted CVD reaction cavity |
| CN114918087A (en) * | 2022-04-14 | 2022-08-19 | 重庆理工大学 | Circular tube outer wall coating device |
| CN114990522A (en) * | 2022-04-14 | 2022-09-02 | 重庆理工大学 | Thermal decomposition film preparation device |
| CN114918087B (en) * | 2022-04-14 | 2023-01-20 | 重庆理工大学 | Coating device for outer wall of circular tube |
| CN114892144B (en) * | 2022-04-14 | 2023-08-08 | 重庆理工大学 | Atomization-assisted CVD reaction cavity |
| CN114990522B (en) * | 2022-04-14 | 2023-08-08 | 重庆理工大学 | Thermal decomposition film preparation device |
| CN114774883B (en) * | 2022-04-14 | 2023-10-31 | 重庆理工大学 | Compact atomizing auxiliary CVD film preparation device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108796473B (en) | 2020-03-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108796473A (en) | A kind of thermal decomposition preparation method of film | |
| US11236421B2 (en) | Atomic layer deposition device for massively coating micro-nano particles | |
| WO2020124544A1 (en) | Vacuum degreasing and sintering furnace and usage method therefor | |
| CN109440083A (en) | It is atomized assisted CVD membrane deposition method | |
| CN104498891A (en) | Carbon/carbon composite component chemical vapor infiltration device | |
| CN102320606B (en) | Method for growing nanocrystalline silicon powder | |
| CN213708459U (en) | Surface carburization treatment device for production and processing of carbon steel self-tapping screw | |
| CN101298693A (en) | Double-layer airflow quartz fairing reaction chamber apparatus for MOCVD system | |
| CN108588682A (en) | A kind of thermal decomposition film preparation reaction unit | |
| CN202066356U (en) | Vertical open tubular furnace | |
| CN208328102U (en) | Thermally decompose film preparation reaction unit | |
| CN107601515A (en) | A kind of device for preparing SiO powder | |
| CN208901908U (en) | A kind of water cooling equipment for Czochralski furnace | |
| CN214276520U (en) | Rotary bell jar furnace | |
| CN108588821A (en) | Microwave plasma CVD device and leak source detection method | |
| CN209307486U (en) | It is atomized assisted CVD film deposition apparatus | |
| CN102320603B (en) | Heat-conducting oil silicon-core jacketed-type small bell cover for polycrystalline-silicon silane-decomposing furnace | |
| CN109338338B (en) | Atomization-assisted CVD film deposition device | |
| CN106929825B (en) | A kind of device and method being quickly cooled down depositing homogeneous metal oxide film | |
| CN206986325U (en) | A kind of anti-deposition structure of single-crystal furnace guide shell | |
| CN207109038U (en) | A kind of high-speed steel circulator bath annealing pipe | |
| CN205907045U (en) | Acid dip pickle is used in production of carbonization silica flour | |
| CN216115403U (en) | Device with function of accurately adjusting sintering atmosphere of ultra-high-temperature sintering furnace | |
| CN209307485U (en) | Reaction chamber | |
| CN218893766U (en) | Silane collecting device applied to silicon carbide film forming device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20221118 Address after: 230000 B-1015, wo Yuan Garden, 81 Ganquan Road, Shushan District, Hefei, Anhui. Patentee after: HEFEI MINGLONG ELECTRONIC TECHNOLOGY Co.,Ltd. Address before: No.69 Hongguang Avenue, Banan District, Chongqing Patentee before: Chongqing University of Technology |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20221219 Address after: No. 313, Donghai Avenue, Dongdao, Zhanjiang, Guangdong 524000 Patentee after: GUANGDONG GUANHAO HIGH-TECH CO.,LTD. Address before: 230000 B-1015, wo Yuan Garden, 81 Ganquan Road, Shushan District, Hefei, Anhui. Patentee before: HEFEI MINGLONG ELECTRONIC TECHNOLOGY Co.,Ltd. |
|
| TR01 | Transfer of patent right |