CN110331382A - The pouring-in vacuum vapor deposition apparatus of liquid reaction solution miniflow and method - Google Patents
The pouring-in vacuum vapor deposition apparatus of liquid reaction solution miniflow and method Download PDFInfo
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- CN110331382A CN110331382A CN201910597400.8A CN201910597400A CN110331382A CN 110331382 A CN110331382 A CN 110331382A CN 201910597400 A CN201910597400 A CN 201910597400A CN 110331382 A CN110331382 A CN 110331382A
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- reaction solution
- vacuum chamber
- pouring
- vapor deposition
- miniflow
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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
- C23C16/448—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
- C23C16/4485—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 evaporation without using carrier gas in contact with the source material
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses the pouring-in vacuum vapor deposition apparatus of liquid reaction solution miniflow and method, device includes closed container, vacuum chamber, microflow controllers, heating and heat-insulating device equipped with reaction solution, and the gas cylinder equipped with nonreactive gas；Closed container is connect by pipeline with vacuum chamber, below the liquid level of pipeline intercalation reaction solution；Closed container is connect by tracheae with gas cylinder；Microflow controllers and heating and heat-insulating device are installed on the pipeline that closed container is connect with vacuum chamber, the reaction solution that microflow controllers are used to control tiny flow quantity enters vacuum chamber, heating and heat-insulating device is placed between microflow controllers and vacuum chamber, for the reaction solution of tiny flow quantity to gasify.The present invention can be realized the injection and gasification of small quantity of fluid, to realize the optimization deposition of function film.The device of the invention and method can be widely applied to inorganic or organic functional thin film material the deposition of various micro-nano devices under vacuum condition.
Description
Technical field
The present invention relates to technical field of film preparation, in particular to a kind of pouring-in vacuum gas-phase of liquid reaction solution miniflow
Precipitation equipment and method.
Background technique
Currently, various inorganic or organic functional thin film is prepared using vacuum technique, such as metal organic-matter chemical gas
Mutually deposition (MOCVD), atomic layer deposition (ALD), low-pressure chemical vapor deposition (LPCVD), plasma-enhanced CVD are heavy
Product (PECVD), hot-wire chemical gas-phase deposition or catalytic chemical gaseous phase deposition (HWCVD, Cat-CVD) cause chemical vapor deposition
The first chances vacuum such as product (iCVD), oxidation chemistry vapor deposition (oCVD), molecular-layer deposition (MLD), vapor deposition dimerization (VDP) are thin
Film deposition technique.All these vacuum film deposition technologies require to carry out film preparation using gaseous raw material, thus real
Now uniform, fine and close, smooth, conformal deposition and thickness are controllable etc., obtain excellent film material property.
Nevertheless, depositing for specific film, raw material are for example organic metallorganic material of liquid or have
Machine monomer material or inorganic liquid such as water etc..It, usually can be with if necessary to which these liquid raw materials are become gaseous starting materials
Using following two technologies: 1. pairs of materials carry out heating and are vaporized；2. using inert gas as argon gas or non-reaction
Liquid gaseous state is loaded into vacuum chamber by the mode that gas such as nitrogen carrier gas transports.Furthermore, it is possible to be realized in conjunction with above two technology
It the gasification of better liquid raw material and transports.
For certain reaction solution raw material, carrier gas transfer ways can not be passed through due to its excessively high viscosity property
Realize gaseous state input, and it is organic that liquid starting material such as metal is likely to cause if being vaporized using excessively high heating temperature
The decomposition of object or the polymerization of organic monomer material.Therefore, how to realize the gasification of this kind of material and realize in vacuum chamber
The homogeneous film formation in portion is an important technical problem.
Summary of the invention
It is an object of the invention to overcome the deficiencies of existing technologies and insufficient, a kind of liquid reaction solution miniflow injection is provided
Formula vacuum vapor deposition apparatus, the device can be realized the injection and gasification of small quantity of fluid, to realize function film most
Optimization deposition.
It is another object of the present invention to provide a kind of pouring-in vacuum vapor deposition method of liquid reaction solution miniflow,
It can be realized the preparation of excellent film material with function.
The purpose of the present invention can be achieved through the following technical solutions:
The pouring-in vacuum vapor deposition apparatus of liquid reaction solution miniflow, including the closed container, true equipped with reaction solution
Plenum chamber, microflow controllers, heating and heat-insulating device, and the gas cylinder equipped with nonreactive gas；The closed container passes through pipeline
It is connect with vacuum chamber, below the liquid level of the pipeline intercalation reaction solution；The closed container is connect by tracheae with gas cylinder；
Microflow controllers and heating and heat-insulating device, the microflow controllers are installed on the pipeline that closed container is connect with vacuum chamber
Reaction solution for controlling tiny flow quantity enters vacuum chamber, and the heating and heat-insulating device is placed in the microflow controllers and institute
It states between vacuum chamber, for the reaction solution of tiny flow quantity to gasify.
The microflow controllers include capillary device and pressure valve device as a preferred technical solution,.
As a preferred technical solution, the pressure valve device using manually control, pneumatic control or Electronic control mode control
The opening degree of system pressure valve.
The pressure valve device is connect with electromagnetic induction coil as a preferred technical solution, electromagnetic induction coil successively with
Voltage controlling components and control software connection, control software are connect by signal connecting line with the indoor barometer of vacuum chamber.Electricity
Magnetic induction coil and barometer and control software form close loop control circuit, can be real using the air pressure value of feedback that barometer measures
When regulate and control pressure valve opening degree, realize automatically control.
Voltage is changed using constant pressure, linear increment, square-wave voltage variation or triangle wave voltage as a preferred technical solution,
Control mode controls the magnetic field strength of electromagnetic induction coil, to control the opening degree of pressure valve.
Heated filament and sample stage are installed as a preferred technical solution, the heated filament is fixed on heat in the vacuum chamber
On guide frame, sample substrate is installed on the sample stage.
The reaction solution is metallorganic, organic matter or inorganic liquid as a preferred technical solution,.Inorganic liquid
The liquid such as including water.
The nonreactive gas is inert gas as a preferred technical solution,.Nonreactive gas can be inert gas
Or any gas reacted does not occur with reaction solution for general gas flow etc..
The heating and heat-insulating device is heated baking band, resistive heater or infrared heating as a preferred technical solution,
Fluorescent tube.Heating and heat-insulating device makes micro-reaction vaporizer, and guarantees that gas does not condense under cryogenic.
Another object of the present invention can be achieved through the following technical solutions: the pouring-in vacuum of liquid reaction solution miniflow
Vapor deposition method includes the following steps: for reaction solution to be packed into closed container, and nonreactive gas is packed into gas cylinder；It controls non-anti-
Gas is answered to enter the gas flow of closed container to control the output quantity of reaction solution；The microflow controllers being installed on pipeline
The reaction solution of control tiny flow quantity enters vacuum chamber；Before the reaction solution of tiny flow quantity enters vacuum chamber, by heating
Attemperator gasification；Reaction solution after gasification is vapor-deposited in vacuum chamber forms film.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the present invention realizes the injection and gasification of small quantity reaction solution, solution using microflow controllers and heating and heat-insulating device
It has determined to use in the prior art and has been heated at high temperature the problem of causing liquid reaction solution to decompose or polymerize.
2. deposition apparatus design of the present invention is simple, and can be controlled in closed container by pressure reducing valve, gas flowmeter
Pressure controls the output quantity of reaction solution by microflow controllers, to realize reaction solution flow and vacuum chamber room pressure
Accurate control.
Detailed description of the invention
Fig. 1 is the pouring-in vacuum vapor deposition apparatus structural schematic diagram of liquid reaction solution miniflow in the embodiment of the present invention.
Wherein: 101: closed container 102: pipeline, 103: reaction solution, 104: gas cylinder, 105: nonreactive gas, 106: valve
Door, 107: pressure reducing valve, 108: gas flowmeter, 109: microflow controllers, 110: capillary device, 111: pressure valve device, 112:
Voltage controlling components, 113: electromagnetic induction coil, 114: even device of air, 115: slide valve, 116: turbomolecular pump, 117: mechanical
Pump, 118: solenoid valve, 119: pump-line, 120: sample stage, 121: sample substrate, 122: tracheae, 123: vacuum chamber, 124:
Heating and heat-insulating device, 125: barometer, 126: control connecting line, 127: control software, 128: signal connecting line, 129: heated filament,
130: heated filament frame, 131: heating power supply connecting line.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
The pouring-in vacuum vapor deposition apparatus of liquid reaction solution miniflow, including closed container, vacuum chamber, microfluidic control
Device, heating and heat-insulating device and gas cylinder.Closed container for containing reaction solution, by pipeline and tracheae respectively with vacuum chamber
It is connected with gas cylinder.Pipeline needs intercalation reaction liquid level of solution or less.Gas cylinder is for containing the non-reaction such as inert gas or general gas flow
With reaction solution any react does not occur for gas, nonreactive gas.Valve, pressure reducing valve and gas flow are installed on tracheae
Meter, valve are used to guarantee the switch and safety of gas cylinder and closed container, pressure reducing valve and gas flowmeter for controlling closed container
Interior pressure.
Microflow controllers and heating and heat-insulating device are sequentially installed on the pipeline that closed container is connect with vacuum chamber.It is micro-
Stream controller includes capillary device and pressure valve device, and capillary device can pass through setting capillary dimensions, quantity and arrangement
The output quantity of equal state modulators reaction solution.Using the unlatching journey of electromagnetic induction coil control pressure valve in pressure valve device the present embodiment
Degree controls electromagnetic induction coil by voltage controlling components, to control pressure valve device.It is automatically controlled to realize, it is settable
Software is controlled, is connect by control connecting line with voltage controlling components, control software passes through signal connecting line and vacuum chamber simultaneously
Indoor barometer connection, forms close loop control circuit.The atmospheric pressure value feedback that barometer measures, can be automatic into control software
Regulate and control the voltage of electromagnetic induction coil, to automatically control the opening degree of pressure valve device, realizes reaction solution tiny flow quantity
Real-time monitoring.Electromagnetic induction coil can pass through the voltages such as constant pressure, linear increment, square-wave voltage variation or triangle wave voltage variation
Control mode controls the magnetic field strength of electromagnetic induction coil, to control the opening degree of pressure valve.In addition to electric control method,
It can also be true with the entrance for controlling reaction solution small quantity using manually controlling or the modes such as pneumatic control control pressure valve device
Plenum chamber.
Heating and heat-insulating device can be the devices such as heated baking band, resistive heater or infrared heating fluorescent tube, to small stream
The reaction solution of amount carries out heating and thermal insulation, makes the micro-reaction vaporizer sprayed, and guarantee that gas is not cold under cryogenic
It is solidifying.
Vacuum chamber is vacuumized by vacuum suction device, and vacuum suction device includes turbomolecular pump and mechanical pump, is passed through
Pump-line is connect with vacuum chamber, and slide valve can isolate vacuum chamber and turbomolecular pump, and solenoid valve is for controlling pumping
The switch of pipeline.Heated filament and sample stage are installed, heated filament is fixed on heated filament frame, and sample is equipped on sample stage inside vacuum chamber
Product substrate, sample stage have heating and refrigerating function.Heated filament is connect by heating power supply connecting line with external power supply, external power supply
Heated filament can be heated.It is also equipped with even device of air in vacuum chamber, is even compression ring or uniform gas board etc., into vacuum chamber
Gas by even device of air realize gas it is uniform diffusion and be distributed.Reaction solution after the gasification gas phase in vacuum chamber is heavy
Product forms film.
Embodiment one
Poly (glycidyl methacrylate) (Polyglycidyl is prepared using gas phase thermal polymerization depositing operation
Methacrylate, PGMA).Glycidyl methacrylate (GMA) monomer is packed into closed container, pipeline is inserted into GMA liquid
Below face.Tracheae connects gas cylinder and closed container, and gas cylinder internal is equipped with high pressure argon gas.Argon flow inside closed container and
Pressure can be adjusted by pressure reducing valve and gas flowmeter.GMA monomer enters pipeline under the action of closed container internal pressure,
Microflow controllers are reached simultaneously.Microflow controllers control the output of reaction solution by internal capillary device and pressure valve device
Amount, pressure valve device adjust the opening degree of pressure valve under the action of electromagnetic induction coil.In close loop control circuit, software is controlled
It can be according to the opening degree for the atmospheric pressure value real-time monitoring pressure valve that barometer measures.Pass through by the GMA monomer of microflow controllers
Heating and heat-insulating device heating sublimation, the gas after distillation pass through the even gas of even device of air of vacuum chamber.GMA monomer is using NiCr warm
Silk heating realizes that GMA heat causes and polymerize, so that PGAM film be prepared.
Embodiment two
ZnO film is prepared using low-pressure chemical vapor deposition (LPCVD) mode, wherein reaction solution uses diethyl zinc
(Dimethylzinc, DEZ) and water (H2O).Wherein DEZ and water can be using microfluidic controls shown in precipitation equipment of the present invention
Device carries out being filled with for reaction solution, (130-250 DEG C) is heated to sample substrate by sample stage, to realize ZnO film
Preparation.Water can also carry out gas input in such a way that carrier gas transports or heats.It is pointed out that heated filament and heated filament
Frame and the connecting line for connecting heating power supply no longer need in LPCVD deposition process.The present embodiment does not refer to part with implementation
Example one.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot 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 guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. the pouring-in vacuum vapor deposition apparatus of liquid reaction solution miniflow, which is characterized in that including close equipped with reaction solution
Close container, vacuum chamber, microflow controllers, heating and heat-insulating device, and the gas cylinder equipped with nonreactive gas；The closed container
It is connect by pipeline with vacuum chamber, below the liquid level of the pipeline intercalation reaction solution；The closed container by tracheae with
Gas cylinder connection；Microflow controllers and heating and heat-insulating device are installed on the pipeline that closed container is connect with vacuum chamber, it is described
The reaction solution that microflow controllers are used to control tiny flow quantity enters vacuum chamber, and the heating and heat-insulating device is placed in the miniflow
Between controller and the vacuum chamber, for the reaction solution of tiny flow quantity to be gasified.
2. the pouring-in vacuum vapor deposition apparatus of liquid reaction solution miniflow according to claim 1, which is characterized in that institute
Stating microflow controllers includes capillary device and pressure valve device.
3. the pouring-in vacuum vapor deposition apparatus of liquid reaction solution miniflow according to claim 2, which is characterized in that institute
State pressure valve device using manually control, pneumatic control or Electronic control mode control the opening degree of pressure valve.
4. the pouring-in vacuum vapor deposition apparatus of liquid reaction solution miniflow according to claim 2, which is characterized in that institute
It states pressure valve device to connect with electromagnetic induction coil, electromagnetic induction coil is successively connect with voltage controlling components and control software, is controlled
Software processed is connect by signal connecting line with the indoor barometer of vacuum chamber.
5. the pouring-in vacuum vapor deposition apparatus of liquid reaction solution miniflow according to claim 4, which is characterized in that adopt
With the magnetic of constant pressure, linear increment, square-wave voltage variation or triangle wave voltage variation voltage control mode control electromagnetic induction coil
Field intensity, to control the opening degree of pressure valve.
6. the pouring-in vacuum vapor deposition apparatus of liquid reaction solution miniflow according to claim 1, which is characterized in that institute
It states and heated filament and sample stage is installed in vacuum chamber, the heated filament is fixed on heated filament frame, is equipped with sample on the sample stage
Substrate.
7. the pouring-in vacuum vapor deposition apparatus of liquid reaction solution miniflow according to claim 1, which is characterized in that institute
Stating reaction solution is metallorganic, organic matter or inorganic liquid.
8. the pouring-in vacuum vapor deposition apparatus of liquid reaction solution miniflow according to claim 1, which is characterized in that institute
Stating nonreactive gas is inert gas.
9. the pouring-in vacuum vapor deposition apparatus of liquid reaction solution miniflow according to claim 1, which is characterized in that institute
Stating heating and heat-insulating device is heated baking band, resistive heater or infrared heating fluorescent tube.
10. the method for preparing film using the described in any item precipitation equipments of claim 1 to 9, which is characterized in that including as follows
Step:
Reaction solution is packed into closed container, nonreactive gas is packed into gas cylinder；Control nonreactive gas enters the gas of closed container
Body flow is to control the output quantity of reaction solution；It is installed on the reaction solution of the microflow controllers control tiny flow quantity on pipeline
Into vacuum chamber；Before the reaction solution of tiny flow quantity enters vacuum chamber, gasify by heating and heat-insulating device；It is anti-after gasification
It answers solution to be vapor-deposited in vacuum chamber and forms film.
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Application publication date: 20191015 |