CN110261256A - A method of the measurement intrinsic deposition rate of CVD/CVI technique presoma - Google Patents
A method of the measurement intrinsic deposition rate of CVD/CVI technique presoma Download PDFInfo
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- CN110261256A CN110261256A CN201910502911.7A CN201910502911A CN110261256A CN 110261256 A CN110261256 A CN 110261256A CN 201910502911 A CN201910502911 A CN 201910502911A CN 110261256 A CN110261256 A CN 110261256A
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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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/02—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
Abstract
The present invention discloses a kind of method for measuring the intrinsic deposition rate of CVD/CVI technique presoma, the intrinsic deposition rate that the present invention measures is unrelated with gas phase intermediate product, what is represented is the deposition rate of source gas itself, the size of deposition rate is at low cost by of poor quality the determining of experiment front and back porous ceramic chip.The intrinsic deposition rate of presoma can be obtained by simple data processing, it is easy to operate, quickly and efficiently.
Description
Technical field
The present invention relates to a kind of methods for measuring the intrinsic deposition rate of CVD/CVI technique presoma.
Background technique
Chemical vapor deposition/infiltration (CVD/CVI) technique is to prepare high-performance coating material, carbon-based and ceramic base composite wood
The main method of material.However it is there are long preparation period, the problems such as high production cost, limits coating material, carbon-based and ceramic
The extensive industry application of based composites.The pyrolysis and sedimentation mechanism for studying different presomas, measure its deposition rate, favorably
In advanced optimizing for CVD/CVI depositing operation.
The homogeneous reaction that CVD/CVI process is related to a variety of pyrolysis intermediate products in gas phase is being deposited with various thermal decomposition products
The heterogeneous reaction of substrate surface.The method of currently used measurement deposition rate includes optical method, microbalance method and electricity
Method.However optical method and electrical method are all difficult to fit in CVD/CVI technique the deposition rate for using, and measuring and represent
Be a variety of gas phase intermediate products mixed deposit rate.It can be integrated into CVD/CVI technique, survey on microbalance law theory
The intrinsic deposition rate of source gas out, but to realize that the cost of this purpose is very high, it is difficult to it is applied to Practical Project.
Summary of the invention
Above of the existing technology to solve the problems, such as, the present invention proposes that a kind of measurement CVD/CVI technique presoma is intrinsic
The method of deposition rate, the intrinsic deposition rate measured is unrelated with gas phase intermediate product, and representative is the heavy of source gas itself
Product rate.
The present invention can be achieved by the following technical programs:
A method of measurement CVD/CVI technique is pyrolyzed the intrinsic deposition rate of carbon matrix precursor, comprising the following steps:
1) deposition substrate prepares: preparing muti-piece cylindrical porous potsherd, number 1,2,3,4 ... ... simultaneously weighs respectively
Its mass M11, M12, M13, M14... ...；
2) mold assembles: the muti-piece cylindrical porous potsherd being vertically loaded into graphite jig in order, is organized die-filling
Tool；
3) CVD/CVI is deposited: the mold being packed into constant temperature zone in cvd furnace, is passed through inert gas as protective gas
Heating is controlled by vacuum pump to specified pressure after reaching assigned temperature, is controlled source gas in the residence time of isothermal region, is carried out
CVD/CVI deposition；
4) deposition substrate is weighed: after deposition, being passed through inert gas makes deposition furnace pressure revert to normal pressure, to temperature
Stop being passed through inert gas after being cooled to room temperature, the mold is taken out out of cvd furnace, weighs to obtain the muti-piece cylinder in mold
Shape porous ceramic chip mass M21, M22, M23, M24... ...；
5) it calculates deposition rate: according to the of poor quality of the muti-piece cylindrical porous potsherd measured, calculating the source
Deposition rate of the gas at each numbered positions；
6) draw along journey deposition rate curve: by each number porous ceramic chip by with a distance from isothermal region air inlet by
Proximal and distal sequence is drawn out so that, as abscissa, deposition rate is ordinate with a distance from air inlet along journey deposition rate curve
Figure；
7) calculate intrinsic deposition rate: will reversely be extended down to outside along journey deposition rate curve is 0 with a distance from isothermal region air inlet
Place, the deposition rate obtained herein is exactly intrinsic deposition rate of the source gas under present technological conditions.
It is of the present invention measurement the intrinsic deposition rate of CVD/CVI technique presoma method, the graphite grinding tool into
Port is bellmouth, and the lower end of bellmouth is connected to a cylindrical hole by gas passage；The diameter of the cylindrical hole is greater than institute
State the diameter of gas passage, the diameter of the diameter of the gas passage and the bellmouth inlet face is equal.
The method of the measurement intrinsic deposition rate of CVD/CVI technique presoma of the present invention, the assigned temperature are lower than
1200℃。
The method of the measurement intrinsic deposition rate of CVD/CVI technique presoma of the present invention, the specified pressure are less than
10kPa。
The method of the measurement CVD/CVI technique pyrolysis intrinsic deposition rate of carbon matrix precursor of the present invention, the source gas
For small molecule hydrocarbon gas or other small molecule vaporous precursors.
It is of the present invention measurement CVD/CVI technique pyrolysis the intrinsic deposition rate of carbon matrix precursor method, it is described specify it is stagnant
Stay the time less than 1 second.
Beneficial effect
The size of deposition rate of the present invention is at low cost by of poor quality the determining of experiment front and back porous ceramic chip.Pass through
Simple data processing can obtain the intrinsic deposition rate of presoma, easy to operate, quickly and efficiently.
Detailed description of the invention
Fig. 1 is flow chart of the invention；
Fig. 2 is porous ceramic chip top view of the present invention；
Fig. 3-1,3-2 are respectively graphite jig air inlet assembly side view and top view；
Fig. 4 is along journey deposition rate curve graph；
Fig. 5 is deposition rate with residence time change curve.
Specific embodiment
Illustrate embodiments of the present invention below by way of particular specific embodiment, those skilled in the art can be by this theory
The bright revealed content of book is understood other advantages and efficacy of the present invention easily.
As shown in Figure 1, a kind of method of the intrinsic deposition rate of measurement CVD/CVI technique presoma of the invention, including with
Lower step:
1) deposition substrate prepares: preparing muti-piece cylindrical porous potsherd (as shown in Figure 2), number 1,2,3,4 ... ... is simultaneously
Its mass M is weighed to obtain respectively11, M12, M13, M14... ...；
2) mold assembles: muti-piece cylindrical porous potsherd being vertically loaded into graphite jig in order, assembly mold；
3) CVD/CVI is deposited: mold being packed into constant temperature zone in cvd furnace, is passed through inert gas (nitrogen or argon gas or helium
Gas) as protective gas heating, after reaching the specified isothermal temperature lower than 1200 DEG C, by vacuum pump control to lower than 10kPa
Specified pressure, be passed through small molecule hydrocarbon gas or other small molecule vaporous precursors and carry out CVD/CVI deposition；
4) deposition substrate is weighed: after deposition, being passed through inert gas makes deposition furnace pressure revert to normal pressure, to temperature
Stop being passed through inert gas after being cooled to room temperature, the mold is taken out out of cvd furnace, weighs to obtain the muti-piece cylinder in mold
Shape porous ceramic chip mass M21, M22, M23, M24... ...；
5) it calculates deposition rate: according to the of poor quality of the muti-piece cylindrical porous potsherd measured, calculating the small molecule
The deposition rate of hydrocarbon gas or other small molecule vaporous precursors at each numbered positions；
6) it draws along journey deposition rate curve: each number porous ceramic chip is arranged from the near to the distant as with a distance from air inlet
Sequence is drawn out so that, as abscissa, deposition rate is ordinate with a distance from air inlet along journey deposition rate curve graph；
7) it calculates intrinsic deposition rate: will be reversely extended down to outside along journey deposition rate curve with a distance from air inlet at for 0, herein
Obtained deposition rate is exactly intrinsic deposition rate of the source gas under present technological conditions.
Such as Fig. 3-1, shown in 3-2, the air inlet of graphite grinding tool is bellmouth A, and the lower end of bellmouth A is connected by gas passage
A logical cylindrical hole C；The diameter of cylindrical hole is greater than the diameter of gas passage B, the diameter and bellmouth A entrance of gas passage B
The diameter in face is equal.
Embodiment 1
A method of measurement CVD/CVI technique is pyrolyzed the intrinsic deposition rate of carbon matrix precursor, comprising the following steps:
1) deposition substrate prepares: 7 blocks of cylindrical porous potsherds of preparation, number 1,2, and 3,4,5,6,7, and weigh to obtain its matter
Measure 2.6288g, 2.5583g, 2.5301g, 2.5613g, 2.5823g, 2.5672g, 2.5980g；
2) mold assembles: 7 pieces of porous ceramic chips being vertically loaded into graphite jig in order, assembly mold；
3) CVD/CVI is deposited: mold being packed into constant temperature zone in cvd furnace, nitrogen is passed through and heats up as protective gas, reach
It is controlled by vacuum pump to 5kPa after to 950 DEG C, is passed through propylene and carries out CVD/CVI deposition；
4) deposition substrate is weighed: after deposition, being passed through nitrogen to make to deposit furnace pressure and reply is normal pressure, cooling to temperature
Stop being passed through nitrogen after to room temperature, mold taken out out of cvd furnace, weighs to obtain porous ceramics tablet quality 2.6506g in mold,
2.5829g, 2.5574g, 2.5895g, 2.6114g, 2.5966g, 2.6290g；
5) deposition rate is calculated: according to 0.0218g, 0.0246g, the 0.0273g of poor quality of the porous ceramic chip measured,
0.0282g, 0.0291g, 0.0294g, 0.031g calculate deposition rate of the propylene at each numbered positions；
6) it draws along journey deposition rate curve: each number porous ceramic chip is arranged from the near to the distant as with a distance from air inlet
Sequence is drawn out so that, as abscissa, deposition rate is ordinate with a distance from air inlet along journey deposition rate curve graph (Fig. 4)；
7) calculate intrinsic deposition rate: will reversely be extended down to outside along journey deposition rate curve is 0 with a distance from isothermal region air inlet
Place, the deposition rate obtained herein is exactly intrinsic deposition rate of the propylene under present technological conditions.
It can be replaced with the residence time with a distance from air inlet, drawing can be fast with deposition is drawn along journey deposition rate curve
Rate is replaced with residence time change curve, and by the curve, reversely the outer also available intrinsic deposition rate that is extended down at 0s is detained
Time illustrates.
Embodiment 2
A method of measurement CVD/CVI technique is pyrolyzed the intrinsic deposition rate of carbon matrix precursor, comprising the following steps:
1) deposition substrate prepares: preparing 1 block of cylindrical porous potsherd, and weighs to obtain its quality 2.9867g；
2) mold assembles: potsherd being fitted into graphite jig, assembly mold；
3) CVD/CVI is deposited: mold being packed into constant temperature zone in cvd furnace, the control residence time is 0.125s, is passed through nitrogen
Gas heats up as protective gas, is controlled by vacuum pump to 5kPa after reaching 975 DEG C, is passed through propylene and carries out CVD/CVI deposition；
4) deposition substrate is weighed: after deposition, being passed through nitrogen to make to deposit furnace pressure and reply is normal pressure, cooling to temperature
Stop being passed through nitrogen after to room temperature, mold is taken out out of cvd furnace, weighs to obtain porous ceramics tablet quality 3.0195g in mold；
5) it repeats step 1-4 totally 6 times.Porous ceramic chip in replacement step 1 every time, and weigh to obtain its quality
(2.8967g, 3.0096g, 2.9575g, 2.9092g, 2.8936g, 2.9374g), when corresponding the delay in change step 3
Between (0.25s, 0.375s, 0.5s, 0.625s, 0.75s, 0.875s), obtain post-depositional porous ceramics tablet quality in step 4
(2.9305g, 3.0458g, 2.9946g, 2.9474g, 2.9333g, 2.9791g)
6) calculate deposition rate: according to the porous ceramic chip measured it is of poor quality (0.0328g, 0.0338g, 0.0362g,
0.0371g, 0.0382g, 0.0397g, 0.0417g), calculate deposition rate of the propylene under each residence time；
7) draw deposition rate with residence time change curve: using the residence time as abscissa, deposition rate is ordinate,
Deposition rate is drawn out with residence time change curve, shown in Fig. 5；
8) calculate intrinsic deposition rate: by deposition rate, with residence time change curve, reversely outer to be extended down to the residence time be 0
Second, the deposition rate obtained herein is exactly intrinsic deposition rate of the propylene under present technological conditions.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (6)
1. a kind of method for measuring the intrinsic deposition rate of CVD/CVI technique presoma, which comprises the following steps:
1) deposition substrate prepares: preparing muti-piece cylindrical porous potsherd, number 1,2,3,4 ... ..., and weighs to obtain its matter respectively
Measure M11, M12, M13, M14... ...；
2) mold assembles: the muti-piece cylindrical porous potsherd being vertically loaded into graphite jig in order, assembly mold；
3) CVD/CVI is deposited: the mold being packed into constant temperature zone in cvd furnace, is passed through inert gas as protective gas liter
Temperature is controlled by vacuum pump to specified pressure after reaching assigned temperature, is controlled source gas in the residence time of isothermal region, is carried out
CVD/CVI deposition；
4) deposition substrate is weighed: after deposition, being passed through inert gas makes deposition furnace pressure revert to normal pressure, cooling to temperature
Stop being passed through inert gas after to room temperature, the mold taken out out of cvd furnace, weigh in mold the muti-piece it is cylindrical more
Hole potsherd mass M21, M22, M23, M24... ...；
5) it calculates deposition rate: according to the of poor quality of the muti-piece cylindrical porous potsherd measured, calculating the source gas
Deposition rate at each numbered positions；
6) it draws along journey deposition rate curve: each number porous ceramic chip is arranged from the near to the distant as with a distance from air inlet
Sequence is drawn out so that, as abscissa, deposition rate is ordinate with a distance from isothermal region air inlet along journey deposition rate curve graph；
7) it calculates intrinsic deposition rate: will be reversely extended down to outside along journey deposition rate curve with a distance from isothermal region air inlet at for 0, this
The deposition rate that place obtains is exactly intrinsic deposition rate of the source gas under present technological conditions.
2. the method for the measurement intrinsic deposition rate of CVD/CVI technique presoma according to claim 1, which is characterized in that
The air inlet of the graphite grinding tool is bellmouth, and the lower end of bellmouth is connected to a cylindrical hole by gas passage；The cylinder
The diameter in shape hole is greater than the diameter of the gas passage, the diameter phase of the diameter of the gas passage and the bellmouth inlet face
Deng.
3. the method for the measurement intrinsic deposition rate of CVD/CVI technique presoma according to claim 1, which is characterized in that
The assigned temperature is lower than 1200 DEG C.
4. the method for the measurement intrinsic deposition rate of CVD/CVI technique presoma according to claim 1, which is characterized in that
The specified pressure is lower than 10kPa.
5. the method for the measurement intrinsic deposition rate of CVD/CVI technique presoma according to claim 1, which is characterized in that
The source gas is small molecule hydrocarbon gas or other small molecule vaporous precursors.
6. the method for the measurement intrinsic deposition rate of CVD/CVI technique presoma according to claim 1, which is characterized in that
The designated gas residence time is lower than 1 second.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP4345185A1 (en) * | 2022-09-30 | 2024-04-03 | RTX Corporation | Minimization of chemical vapor infiltration tooling hole length through counterbores |
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