CN109055915A - TiN coating chemical vapor deposition unit and preparation method based on electric current heating - Google Patents
TiN coating chemical vapor deposition unit and preparation method based on electric current heating Download PDFInfo
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- CN109055915A CN109055915A CN201811273697.4A CN201811273697A CN109055915A CN 109055915 A CN109055915 A CN 109055915A CN 201811273697 A CN201811273697 A CN 201811273697A CN 109055915 A CN109055915 A CN 109055915A
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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
- C23C16/34—Nitrides
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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
- C23C16/04—Coating on selected surface areas, e.g. using masks
- C23C16/045—Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
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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
- C23C16/46—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 heating the substrate
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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
- C23C16/52—Controlling or regulating the coating process
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The present invention provides a kind of TiN coating chemical vapor deposition unit and preparation method based on electric current heating, the device includes air supply system, the source Ti system and depositing system, the air supply system provides carrier gas, carrier gas and nitrogen, the depositing system includes preheating section, conversion zone, the preheating section, conversion zone pass through electric current and are heated, the outlet side of the air supply system is connect with the inlet end of the source Ti system, the outlet side of the source Ti system and the inlet end of preheating section connect, and the outlet side of preheating section and the inlet end of conversion zone connect.The present invention realizes long-range microchannel list inner wall deposition；And during the deposition process: energy consumption is relatively low, and film forming speed is fast, and coating purity is high, coating surface even compact；And whole device occupied space is smaller.
Description
Technical field
The invention belongs to material surface processing and coating technology fields, more particularly, to a kind of TiN based on electric current heating
Coating chemical vapor deposition unit and preparation method.
Background technique
For future aircraft in high-speed flight, indoor combustion reaction of burning generates amount of heat, so that the wall of combustion chamber
Face temperature is up to 3000K, and carrying out active cooling using Endothermic Hydrocarbon Fuel becomes the effective scheme of solution heat management problems.But
It is that Endothermic Hydrocarbon Fuel, can be with the metals member such as Fe, Ni in pipeline basis material while being cracked to form small molecule product
Surface catalysis coking reaction occurs for element contact.Inhibit metal surface catalytic coking can be using surface covering modification technology come real
It is existing, currently, preparing various inert coatings using chemical vapor deposition method becomes the research direction of emphasis.
In comparison, TiN coating is close with basis material in terms of density, coefficient of thermal expansion and heating conduction, possesses excellent
Different property.But there are some disadvantages by traditional chemical vapor deposition method preparation TiN, in the deposition for being directed to microchannel interior walls face
Aspect, using the depositional mode of large-size horizontal furnace or vertical heater radiant heating there are power consumptions it is high, single wall coating is difficult the problems such as,
Also have much room for improvement in terms of crystal film forming speed.It is external it has been reported that Michael E.A.Warwick et al. has been carried out about adopting
With the experiment of electric field assistant chemical vapor deposition prepares coating, it is greatly improved as the result is shown to the property of coating.Electric field
Auxiliary can change the surface microstructure of film, including crystallite dimension, surface area, influence wettability and the growth side of film
To.The increase of electric field strength leads to the film growth of preparation faster, and the thickness of film increases, and the average grain diameter of crystal becomes smaller, together
When also result in film surface area and porosity improve.The coating of electric field-assisted chemical vapor deposition preparation is due to its high surface
Long-pending performance has in fields such as chemical sensor, energy and material, glass system and catalysis to be widely applied very much.But the country is to this
That studies is fewer, and especially the coating of preparation is applied to inhibit coking direction.
Therefore, we use for reference the method that traditional chemical vapor deposition prepares TiN, the microchannel interior walls heated using electric current
Face TiN coating chemical vapor deposition unit and preparation method realize the coating treatment technology of microchannel inner surface.
Summary of the invention
It is an object of the invention to: provide it is a kind of based on electric current heating TiN coating chemical vapor deposition unit and preparation
Method, single inner wall deposition and large scale industry heating furnace heating speed can not be carried out to long-range microchannel by solving in traditional handicraft device
Slow problem is spent, the uniform coating in microchannel interior walls face TiN coating is realized.
Goal of the invention of the invention is achieved through the following technical solutions:
A kind of TiN coating chemical vapor deposition unit based on electric current heating, which includes air supply system, the source Ti system
And depositing system, it includes preheating section, conversion zone, institute that the air supply system, which provides carrier gas, carrier gas and nitrogen, the depositing system,
It states preheating section, conversion zone and passes through electric current and heated, the outlet side of the air supply system is connect with the inlet end of the source Ti system,
The outlet side of the source Ti system and the inlet end of preheating section connect, and the outlet side of preheating section and the inlet end of conversion zone connect.
Preferably, the air supply system includes dilution gas tank, carrier gas tank, N2Tank and three groups of feeding pneumatics, every group of gas supply gas
Road includes sequentially connected drying tube, pressure reducing valve and mass flowmenter, and the dilution gas tank connects the dry of one group of feeding pneumatic
Dry pipe, the carrier gas tank connect the drying tube of another group of feeding pneumatic, the N2The drying tube of tank connection third group feeding pneumatic.
Preferably, the source Ti system includes heating tape, mixed gas tank and TiCl4Tank, with the tank connected gas supply gas of carrier gas
Road is connected to mixed gas tank, with N2Tank connected feeding pneumatic is connected to mixed gas tank, is connected to the tank connected feeding pneumatic of carrier gas
TiCl4Tank, TiCl4Tank connects mixed gas tank by pipeline, and the mixed gas tank is connected to the preheating section of depositing system, institute by pipeline
State TiCl4Connecting pipe between tank, mixed gas tank and mixed gas tank and preheating section is placed in heating tape.
Preferably, with the tank connected feeding pneumatic of carrier gas and TiCl4It is equipped with ball valve between tank, mixes gas tank and TiCl4The company of tank
Adapter tube road is equipped with ball valve, and the connecting pipe mixed between gas tank and preheating section is equipped with ball valve.
Preferably, the pipeline of three groups of feeding pneumatics is polyfluortetraethylene pipe, TiCl4The inlet and outlet of tank are 316L type Φ
6.35mm stainless steel tube, mixing the connecting pipe between gas tank and preheating section is 316L type Φ 6.35mm stainless steel tube.
Preferably, the outer wall of the preheating section and conversion zone is equipped with thermocouple, and 5cm is divided between neighboring thermocouple, heat
The data of galvanic couple are acquired by data collection system.
Preferably, which further includes exhaust treatment system, which connects conversion zone by ball valve.
A kind of preparation method preparing TiN coating, the method comprising the steps of:
(1) cleaning pretreatment is carried out to stainless steel sample；
(2) import of coating exemplar is connected to the rear end of preheating section, electric current heating equipment is docked to preheating section respectively
With the coating exemplar of conversion zone；
(3) before heating up, nitrogen purging is carried out by air supply system, removes the air in whole device；Open air supply system
Nitrogen and carrier gas, and the source Ti, preheating section and conversion zone are heated respectively, control Ti source temperature is 120 DEG C, and control is pre-
Hot arc temperature is 750 DEG C, and control conversion zone temperature is 850 DEG C；The carrier gas of air supply system is opened, TiCl is taken in carrier gas out of4Steam with
Nitrogen and carrier gas enter preheating section after mixing, enter back into conversion zone and carry out deposition reaction, prepare TiN coating.
Compared with prior art, the invention has the following advantages that
1, long-range microchannel list inner wall deposition is realized, the coating of inside pipe wall is only carried out, will not have to the outer wall of pipeline and appoint
What is influenced.
2, whole device temperature control method is easier, and the coating under condition of different temperatures can be made, and heating rate is fast, energy consumption
It is relatively low.
3, film forming speed is fast, and coating purity is high, coating surface even compact.
4, occupied space is smaller, does not need using large-size horizontal furnace or vertical heater.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of apparatus of the present invention；
Fig. 2 is that electric current heats microchannel interior walls face CVD preparation TiN coating morphology (SEM)；
Fig. 3 is that electric current heats microchannel interior walls face CVD preparation TiN coating EDS spectrogram.
Description of symbols:
1- gas source；2- drying tube；3- pressure reducing valve；4- mass flowmenter；The heating tape 5-；6- mixes gas tank；7- ball valve；8- temperature control
Instrument；9-TiCl4Tank；10- transformer；11- preheating section；12- conversion zone；13- thermocouple；14- data collection system；15- tail gas
Absorb slot.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment
As shown in Figure 1, the present invention provides a kind of TiN coating chemical vapor deposition unit based on electric current heating, the device
Including the source air supply system I, Ti system II and depositing system III.Tail gas pollution in order to prevent, the present apparatus also have additional vent gas treatment
System IV.Air supply system provides carrier gas, carrier gas and nitrogen.Depositing system includes preheating section 11, conversion zone 12, preheating section 11,
Conversion zone 12 is heated by electric current.The outlet side of air supply system I is connect with the inlet end of the source Ti system II, the source Ti system
The outlet side of II is connect with the inlet end of preheating section 11, and the outlet side of preheating section 11 is connect with the inlet end of conversion zone 12.
Air supply system I includes dilution gas tank, carrier gas tank, N2Tank and three groups of feeding pneumatics.Wherein, dilute gas tank, carrier gas tank,
N2Tank is referred to as gas source 1.Every group of feeding pneumatic includes sequentially connected drying tube 2, pressure reducing valve 3 and mass flowmenter 4.Dilution
Gas tank connects the drying tube of one group of feeding pneumatic, and carrier gas tank connects the drying tube of another group of feeding pneumatic, N2Tank connects third group
The drying tube of feeding pneumatic.Using mass flowmenter control gas source flow, it is dried after gas source entered by pressure reducing valve
Next system.
The source Ti system II includes heating tape 5, mixed gas tank 6, ball valve 7, temperature controller 8 and TiCl4Tank 9.It is connect with dilution gas tank
Feeding pneumatic be connected to mixed gas tank, with N2Tank connected feeding pneumatic is connected to mixed gas tank, with the tank connected gas supply gas of carrier gas
Road is connected to TiCl4Tank.TiCl4Tank connects mixed gas tank by pipeline.Mixed gas tank is connected to the preheating of depositing system by pipeline
Section, conversion zone, conversion zone connect exhaust treatment system by pipeline.Thinning tank and carrier gas tank are all made of hydrogen.Pass through heating
Mode makes TiCl in evaporator4It in higher vapor pressure (28 DEG C), is brought into mixed gas tank by carrier gas, all reaction gas are uniformly mixed
Enter depositing system afterwards.
To prevent TiCl4It condenses before entry into the deposition chamber, TiCl4Company between tank, mixed gas tank and mixed gas tank and preheating section
Adapter tube road is placed in heating tape, carries out heating and thermal insulation.The pipeline of three groups of feeding pneumatics is polyfluortetraethylene pipe.Due to TiCl4
With very strong corrosivity, TiCl4The inlet and outlet of tank are 316L type Φ 6.35mm stainless steel tube, are mixed between gas tank and preheating section
Connecting pipe is 316L type Φ 6.35mm stainless steel tube.
In order to avoid reaction terminates, air is entered in device, with the tank connected feeding pneumatic of carrier gas and TiCl4Between tank
Equipped with ball valve, gas tank and TiCl are mixed4The connecting pipe of tank is equipped with ball valve, sets in the connecting pipe between mixed gas tank and preheating section
There is ball valve.Valve equally uses anti-corrosion type.
Depositing system III includes transformer 10, preheating section 11 and conversion zone 12.Preheating section and conversion zone (or chemical gas
Mutually deposition section) it is heated respectively by electric current, two pieces of copper sheets are fixed at conversion zone both ends, connect transformer (low-voltage, the work of high current
Make state) as heat source.Copper sheet one end is fixed on the right reaction channel exit, the other end, which moves to left to be fixed to, reacts logical
Road inlet, until copper sheet both ends keep experiment setting length.Preheating section and the outer wall of chemical vapor deposition section are equipped with thermoelectricity
Even 13,5cm is divided between neighboring thermocouple, and the data of thermocouple are acquired by data collection system 14.Whole device
Tail end connects a ball valve and closes ball valve after experiment terminates, and prevents air from entering in device.The pipe of whole device
Road connection is connected by nut cutting ferrule connector.
Exhaust treatment system IV includes tail gas absorption groove 15, mainly uses NaOH alkaline solution.Since this experiment tail gas contains
There are by-product HCl gas and unreacted TiCl4Acid tail gas can be absorbed using NaOH alkaline solution in residual gas.
In addition, the present invention also provides a kind of preparation method for preparing TiN coating using aforementioned device, this method be according to
Lower step carries out:
Step 1: the pretreatment of stainless steel sample:
Remove the dust and fine impurity in spot cleaning removal process；
Mass fraction is that 1~3% hydrochloric acid solution carries out pickling, removes the oxidation film and corrosion product of sample surfaces；
It is cleaned by ultrasonic using the high deionized water of degree of purity, removes surface residual debris；
Degreasing and other organic substances are removed using acetone ultrasonic cleaning；Scavenging period is 15~30min.It is put into baking oven
It is dried for standby at 120 DEG C.
Step 2: the assembly of coating exemplar:
The import of coating exemplar is connected to the rear end of preheating section, outlet is connected to before exhaust gas purification system.By temperature control
Two electricity folders of cabinet clip to the front-end and back-end of coating exemplar respectively, and the positive and negative anodes of coating exemplar and temperature control cabinet is made to constitute circuit.
K-type thermocouple is welded in preheating section and coating sample surface respectively, to measure the wall surface temperature of pipeline, to control the painting of coating
It covers.Temperature control cabinet mainly realizes that heating and temperature control, data collection system realizes the data acquisition of thermocouple, this belongs to existing normal
See technology, which is not described herein again.
Step 3: heating depositing operation:
High pure nitrogen purging is carried out before heating, flow 1L/min is purged whole system 10 minutes, in removing system
Air；High pure nitrogen and diluted in hydrogen gas are opened, heating tape, preheating section and conversion zone are heated respectively, controls heating tape
Temperature is 120 DEG C, controls electric current and voltage heats up to pipeline, and it is 750 DEG C that preheating section temperature is controlled by thermocouple, instead
Answering section temperature is 850 DEG C；After all temperature rise to laboratory set temperature, guarantee that gas flow temperature reaches a stationary value, after
After continuous heating 30min, carrier gas steel cylinder main valve and pressure reducing valve are opened, carrier gas flux meter needle valve is rotated, logical carrier gas enters
TiCl4In tank, TiCl is taken in carrier gas out of4Steam and reaction gas and carrier gas enter preheating section after mixing, enter back into conversion zone
Deposition reaction is carried out, exhaust treatment system is entered finally into；Reach the scheduled time wait test, closes TiCl4The inlet valve of tank
And outlet valve, stop being passed through carrier gas into reaction tube, purge 5min with diluted in hydrogen gas and high pure nitrogen, then adjusts protection gas
Flow 1L/min purges entire reaction system, after reaction system 30min is swept in air-blowing to be protected, closes protection gas and heating tape, allows
System Temperature fall.Gas flow is as shown in table 1 in entire deposition process.
1 electric current of table heating microchannel interior walls face chemical vapor deposition prepares the experiment condition of TiN coating
Step 4: exemplar takes out:
Room temperature is reduced to preheating section and conversion zone.Coating exemplar is disassembled from entire pipeline, obtains required painting
Layer sample.
In order to coating prepared by the present invention performance and pattern verify, the present invention also provides verification test,
Steps are as follows for specific experiment:
Experiment condition: decane, SS304# stainless steel tube Φ 3, ID2mm × 800mm divides two-part to heat.
(1) preparation of TiN coating: according to Fig. 1 connection experimental provision, controlling 850 DEG C of wall temperature of reaction tube, and the reaction time is
Carry out the coating of TiN coating within 2 hours.Conversion zone is finally obtained coating exemplar, welds k in preheating section and reaction section surface
Type thermocouple.Electric current by adjusting electric heating temperature control cabinet heats the inner wall of microchannel, and the registration for controlling thermocouple obtains most
Depositing temperature required for end.
(2) coking is tested: blank tube is respectively adopted and based on electric current heating microchannel interior walls face chemical vapor deposition preparation
TiN coating carry out coking experiment.Adjustment fuel flow is 76ml/min (1.0g/s), and standby pressure is 3.5Mpa, is stablized to system
After gradually increase electric current until outlet oil temperature is arrived of about 700 DEG C, stabling current voltage continues 30min at this time, monitors and heats segment difference
It presses Δ p and is distributed T along Cheng Biwenwall。
(3) coking measurement experiment: measurement carries out the coke content of coking experiment reaction tube.Reaction tube is cut into several 5cm
Long segment, is respectively put into porcelain boat.Each porcelain boat is 2400ml/min, quilt under conditions of 900 DEG C of temperature in oxygen flow
Oxidation.It aoxidizes obtained carbon dioxide and the complete carbon monoxide of a part of unreacted is transported to the oxidation furnace that temperature is 300 DEG C
It is oxidized again, final carbon dioxide is input in capnograph, obtains the quality of carbon dioxide.Finally calculate
The content of each section of reaction tube coke.The coking amount of table 3 is the amount of coke that reaction tube tail end 5cm is generated.
2 Elemental redistribution of table
The coking amount of the different pipelines of table 3
By the Elemental redistribution of 2 coating of the surface topography of analysis chart 2, the EDS spectrogram of Fig. 3 and table and the coking amount of table 3,
Electric current heating microchannel interior walls face CVD prepares the pattern of TiN coating and tradition CVD to prepare the pattern of TiN coating almost the same,
For Pentagram shape.It is analyzed by EDS, Ti, N element ratio are approximately 1:1, illustrate to heat microchannel interior walls face using electric current
The element composition that the coating and tradition CVD of CVD device preparation prepare TiN coating is almost identical.For coking situation, adopt
The microchannel interior walls face CVD preparation TiN coating heated with electric current can also effectively inhibit coking, reduce Filamentous carbon and formed.
To sum up interpretation of result, using the TiN coating and biography of the microchannel interior walls face chemical vapor deposition preparation of electric current heating
The TiN coating performance of chemical vapor deposition of uniting preparation is almost the same.But the microchannel interior walls face chemical vapor deposition of electric current heating
Device solves and can not carry out single inner wall deposition and large scale industry heating furnace heating speed in traditional handicraft device to long-range microchannel
Slow problem is spent, the uniform coating in stainless steel inner wall TiN coating is realized.The microchannel interior walls face of electric current heating simultaneously
Learning deposition method can control electric current, the coating under available condition of different temperatures, further to study.Prepares coating
During, the flow of required gas is relatively low, and only carries out the coating of inside pipe wall, will not have to the outer wall of pipeline any
It influences.Using the microchannel interior walls face TiN coating chemical vapor deposition unit and preparation method heated based on electric current compared to tradition
The method of the TiN coating of chemical vapor deposition method preparation has great progress.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, it is noted that all
Made any modifications, equivalent replacements, and improvements etc. within the spirit and principles in the present invention should be included in guarantor of the invention
Within the scope of shield.
Claims (8)
1. a kind of TiN coating chemical vapor deposition unit based on electric current heating, which is characterized in that the device includes gas supply system
System, the source Ti system and depositing system, the air supply system provide carrier gas, carrier gas and nitrogen, and the depositing system includes preheating
Section, conversion zone, the preheating section, conversion zone pass through electric current and are heated, the outlet side of the air supply system and the source Ti system
Inlet end connection, the inlet end of the outlet side of the source Ti system and preheating section connects, the outlet side of preheating section and conversion zone
Inlet end connection.
2. the TiN coating chemical vapor deposition unit according to claim 1 based on electric current heating, which is characterized in that institute
Stating air supply system includes dilution gas tank, carrier gas tank, N2Tank and three groups of feeding pneumatics, every group of feeding pneumatic include sequentially connected
Drying tube, pressure reducing valve and mass flowmenter, the dilution gas tank connect the drying tube of one group of feeding pneumatic, the carrier gas tank connection
The drying tube of another group of feeding pneumatic, the N2The drying tube of tank connection third group feeding pneumatic.
3. the TiN coating chemical vapor deposition unit according to claim 2 based on electric current heating, which is characterized in that institute
Stating the source Ti system includes heating tape, mixed gas tank and TiCl4Tank is connected to mixed gas tank with the tank connected feeding pneumatic of carrier gas, with N2
Tank connected feeding pneumatic is connected to mixed gas tank, is connected to TiCl with the tank connected feeding pneumatic of carrier gas4Tank, TiCl4Tank passes through pipe
Road connects mixed gas tank, and the mixed gas tank is connected to the preheating section of depositing system, the TiCl by pipeline4Tank, mixed gas tank and
Connecting pipe between mixed gas tank and preheating section is placed in heating tape.
4. the TiN coating chemical vapor deposition unit according to claim 3 based on electric current heating, which is characterized in that with
The tank connected feeding pneumatic of carrier gas and TiCl4Ball valve is equipped between tank, the connecting pipe for mixing gas tank and TiCl4 tank is equipped with ball
Valve, the connecting pipe mixed between gas tank and preheating section are equipped with ball valve.
5. the TiN coating chemical vapor deposition unit according to claim 3 based on electric current heating, which is characterized in that three
The pipeline of group feeding pneumatic is polyfluortetraethylene pipe, TiCl4The inlet and outlet of tank are 316L type Φ 6.35mm stainless steel tube, mix gas tank
Connecting pipe between preheating section is 316L type Φ 6.35mm stainless steel tube.
6. the TiN coating chemical vapor deposition unit according to claim 1 based on electric current heating, which is characterized in that institute
The outer wall for stating preheating section and conversion zone is equipped with thermocouple, and 5cm is divided between neighboring thermocouple, and the data of thermocouple pass through data
Acquisition system is acquired.
7. the TiN coating chemical vapor deposition unit according to claim 1 based on electric current heating, which is characterized in that should
Device further includes exhaust treatment system, which connects conversion zone by ball valve.
8. a kind of preparation method for preparing TiN coating using claim 1 described device, which is characterized in that this method includes step
It is rapid:
(1) cleaning pretreatment is carried out to stainless steel sample；
(2) import of coating exemplar is connected to the rear end of preheating section, electric current heating equipment is docked to preheating section and anti-respectively
Answer the coating exemplar of section；
(3) before heating up, nitrogen purging is carried out by air supply system, removes the air in whole device；Open the nitrogen of air supply system
Gas and carrier gas, and the source Ti, preheating section and conversion zone are heated respectively, control Ti source temperature is 120 DEG C, controls preheating section
Temperature is 750 DEG C, and control conversion zone temperature is 850 DEG C；The carrier gas of air supply system is opened, TiCl is taken in carrier gas out of4Steam and nitrogen
Enter preheating section after mixing with carrier gas, enters back into conversion zone and carry out deposition reaction, prepare TiN coating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811273697.4A CN109055915A (en) | 2018-10-30 | 2018-10-30 | TiN coating chemical vapor deposition unit and preparation method based on electric current heating |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811273697.4A CN109055915A (en) | 2018-10-30 | 2018-10-30 | TiN coating chemical vapor deposition unit and preparation method based on electric current heating |
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| CN109055915A true CN109055915A (en) | 2018-12-21 |
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| CN201811273697.4A Pending CN109055915A (en) | 2018-10-30 | 2018-10-30 | TiN coating chemical vapor deposition unit and preparation method based on electric current heating |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114059040A (en) * | 2021-11-24 | 2022-02-18 | 四川大学 | Deposition method and device for TiN coating on inner surface of pipe network |
| CN114150293A (en) * | 2021-11-25 | 2022-03-08 | 四川大学 | Deposition method and device for TiN and silicon dioxide double-layer coating |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104264126A (en) * | 2014-09-17 | 2015-01-07 | 四川大学 | Long-range micro-channel inner wall TiO2 coating chemical vapor deposition device and coating method |
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| CN114059040A (en) * | 2021-11-24 | 2022-02-18 | 四川大学 | Deposition method and device for TiN coating on inner surface of pipe network |
| CN114150293A (en) * | 2021-11-25 | 2022-03-08 | 四川大学 | Deposition method and device for TiN and silicon dioxide double-layer coating |
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