CN117268270B - Real-time monitoring device and method for continuous chemical vapor deposition interface layer thickness - Google Patents
Real-time monitoring device and method for continuous chemical vapor deposition interface layer thickness Download PDFInfo
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- CN117268270B CN117268270B CN202311567301.8A CN202311567301A CN117268270B CN 117268270 B CN117268270 B CN 117268270B CN 202311567301 A CN202311567301 A CN 202311567301A CN 117268270 B CN117268270 B CN 117268270B
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- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 179
- 238000000034 method Methods 0.000 title claims abstract description 56
- 238000012806 monitoring device Methods 0.000 title claims abstract description 41
- 239000000835 fiber Substances 0.000 claims abstract description 138
- 238000001228 spectrum Methods 0.000 claims abstract description 54
- 239000006185 dispersion Substances 0.000 claims abstract description 39
- 238000012544 monitoring process Methods 0.000 claims abstract description 23
- 239000003086 colorant Substances 0.000 claims abstract description 9
- 230000001066 destructive effect Effects 0.000 claims abstract description 4
- 239000011521 glass Substances 0.000 claims description 38
- 230000008569 process Effects 0.000 claims description 29
- 238000002834 transmittance Methods 0.000 claims description 18
- 238000007789 sealing Methods 0.000 claims description 14
- 230000005540 biological transmission Effects 0.000 claims description 13
- 238000005286 illumination Methods 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- 238000004364 calculation method Methods 0.000 claims description 10
- 238000005260 corrosion Methods 0.000 claims description 8
- 230000007797 corrosion Effects 0.000 claims description 8
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical group N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 7
- 229910052582 BN Inorganic materials 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 5
- 230000004907 flux Effects 0.000 claims description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 5
- 238000004804 winding Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims 2
- 238000005070 sampling Methods 0.000 abstract description 6
- 230000003287 optical effect Effects 0.000 description 10
- 238000000576 coating method Methods 0.000 description 8
- 238000001514 detection method Methods 0.000 description 8
- 238000000151 deposition Methods 0.000 description 7
- 230000003595 spectral effect Effects 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 230000008021 deposition Effects 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000011153 ceramic matrix composite Substances 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011226 reinforced ceramic Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000005019 vapor deposition process Methods 0.000 description 1
Classifications
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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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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
- C04B35/62805—Oxide ceramics
- C04B35/62813—Alumina or aluminates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
- C04B35/62828—Non-oxide ceramics
- C04B35/62836—Nitrides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62884—Coating the powders or the macroscopic reinforcing agents by gas phase techniques
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/02—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
- G01B11/06—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material
- G01B11/0616—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material of coating
- G01B11/0675—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material of coating using interferometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/02—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
- G01B11/06—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material
- G01B11/0616—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material of coating
- G01B11/0683—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material of coating measurement during deposition or removal of the layer
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
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- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Length Measuring Devices By Optical Means (AREA)
Abstract
The invention discloses a real-time monitoring device and a method for the thickness of a continuous chemical vapor deposition interface layer, wherein the device comprises a light emitting component and a light collecting component, the light emitting component consists of a first closed shell, a full spectrum light source and a first reflecting mirror, and the light collecting component consists of a second closed shell, a dispersion prism, a spectrum screen, a second reflecting mirror and a third reflecting mirror. The method comprises the following steps: in the real-time monitoring process, light generated by a full-spectrum light source irradiates the continuous chemical vapor deposition fiber interface layer through a first reflecting mirror, and interference destructive interference and interference constructive phenomena occur; the light passes through the second reflector, the third reflector and the dispersion prism, and the dispersed light irradiates the spectrum projection screen board to present a dispersion spectrum with single color or different colors. The invention can monitor the thickness and the consistency of the interface layer prepared by continuous chemical vapor deposition in real time under the conditions of no furnace opening, no shutdown and no sampling.
Description
Technical Field
The invention belongs to the technical field of preparation and quality monitoring of ceramic matrix composite interface layers, and particularly relates to a real-time monitoring device and method for the thickness of a continuous chemical vapor deposition interface layer.
Background
In the fiber reinforced ceramic matrix composite, the interface coating is one of key components, and the interface coating covers the surface of the reinforced fiber and connects the reinforced fiber with the ceramic matrix, so that the functions of load transmission, load adjustment and crack deflection are achieved, and the advantages and disadvantages of the interface coating directly affect the performance of the composite.
Chemical Vapor Deposition (CVD) processes are the most commonly used processes for preparing boron nitride interface layers, and can be classified into static CVD processes and continuous CVD processes according to the positional state of the workpiece at the time of deposition. The static CVD process is the most common preparation method of the CVD interface coating, and is characterized in that a substrate workpiece is kept in a deposition chamber during deposition, and is heated up together with equipment, kept warm (deposited), and finally cooled and taken out. The continuous CVD process is an upgrade to a static CVD process in which a workpiece such as a fiber bundle or fiber tape is continuously transported through an effective reaction zone for deposition, thereby achieving higher production efficiency and thickness uniformity than static deposition. The thickness and uniformity of the interface layer (i.e., thickness uniformity) are one of the most important indicators of interest in the preparation of ceramic matrix composites, and there is a strong need for real-time monitoring of the interface layer produced during the continuous preparation of the interface layer.
In the prior art, the fiber to be detected needs to be sampled and sampled firstly, then the thickness of the interface layer is detected by detection means such as SEM, metallographic microscope or chemical analysis, the detection process is complex, the detection speed is low, the detection feedback time is as long as several hours or even days, the whole fiber can be destroyed by sampling, and the detection means can not monitor the thickness and the thickness consistency of the prepared interface layer in real time in the continuous chemical vapor deposition process.
In addition, for the film thickness covered on the surface of the planar workpiece, the existing film thickness analyzer is used for carrying out nondestructive detection on the film thickness by utilizing the diffraction and interference principles of light, and the nondestructive detection method has the following general problems: (1) The measurement data is required to be subjected to analysis and operation such as modeling, fitting and the like, so that the feedback is slower, and the detection result is difficult to feedback in real time; (2) The measuring equipment is used in the atmosphere environment, so that the negative pressure and corrosive environment required by continuous vapor deposition are difficult to adapt; (3) Continuous chemical vapor deposition produces an interfacial layer on the surface of the fiber, whereas existing equipment is generally directed to measuring the thickness of a planar film, and is not applicable to measuring the thickness of the interfacial layer on the surface of the fiber (tiny cylindrical surface, the diameter of the fiber is usually 5-12 μm); (4) The fiber used for continuous chemical vapor deposition is a fiber bundle or a fiber belt formed by a large number of monofilament fibers, and the thickness and uniformity of a large number of different interface layers are difficult to be measured simultaneously by the existing equipment; (5) With the existing equipment, the thickness can only be tested after the continuous chemical vapor deposition is finished by sampling and sampling, and the interface layer thickness can not be monitored in real time in the continuous vapor deposition process.
In the actual deposition process of the interface layer, the fiber bundles or fiber tapes with the interface layer can present various colors under illumination due to the difference of the thickness of the interface layer, the principle is that interference of electromagnetic waves is cancelled, namely, electromagnetic waves can be reflected and refracted simultaneously when irradiated to the surface with the film coating, when the optical path difference of the optical waves in the film is equal to odd times of half wavelength, extinction of the optical waves occurs, when the optical path difference of the optical waves in the film is equal to even times of wavelength, the optical waves are enhanced, and therefore, the thickness of the coating can be determined by observing the color of reflected light of the fiber with the coating under illumination.
The invention patent with application publication number of CN116817820A discloses a method for testing the thickness of a nitride interface layer of a continuous-strand silicon carbide fiber, which uses an oxygen-nitrogen analyzer to measure the content of nitrogen and oxygen elements of the fiber before and after depositing the nitride interface layer or the fiber with the interface layer, and calculates the thickness of the interface layer according to the bulk density and average diameter of the fiber and the bulk density of the interface layer material. According to the technical scheme, the thickness of the prepared continuous filament silicon carbide fiber nitride interface layer can be detected only, and the thickness consistency of the prepared interface layer can not be monitored in real time in the continuous deposition process.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a real-time monitoring device for the thickness of a continuous chemical vapor deposition interface layer, which is arranged at a position of a continuous chemical vapor deposition chamber close to the tail end of the continuous chemical vapor deposition chamber, wherein a first sealing flange and a second sealing flange are arranged at the top of the continuous chemical vapor deposition chamber, and the real-time monitoring device comprises a light emitting component and a light collecting component; the light emission component consists of a first closed shell, a full spectrum light source and a first reflecting mirror, wherein the full spectrum light source and the first reflecting mirror are respectively positioned at the top and the bottom of the first closed shell, and the bottom of the first closed shell is vertically inserted into the continuous chemical vapor deposition chamber through the first sealing flange; the light collection assembly is composed of a second airtight shell, a dispersion prism, a spectrum screen, a second reflecting mirror and a third reflecting mirror, wherein the second reflecting mirror and the third reflecting mirror are respectively arranged at the bottom and the top of the second airtight shell, the dispersion prism is arranged at the outer side of the top of the second airtight shell, the spectrum screen and the dispersion prism are oppositely arranged, the central axes of the spectrum screen and the dispersion prism are positioned on the same horizontal line, and the bottom of the second airtight shell is vertically inserted into the continuous chemical vapor deposition chamber through a second sealing flange.
Preferably, the first airtight housing and the second airtight housing are both cylindrical, and are disposed in parallel in a vertical direction.
In any of the above schemes, preferably, the bottom end of the first closed housing and the bottom end of the second closed housing are positioned on the same horizontal line, and are positioned above the continuous chemical vapor deposition fibers, and the distances between the bottom ends of the first closed housing and the continuous chemical vapor deposition fibers are equal.
In any of the above embodiments, preferably, a side of the bottom of the first airtight enclosure opposite to the first reflecting mirror is made of high light-transmitting glass, and the other parts are made of stainless steel or corrosion-resistant plastic; the side surface of the bottom of the second airtight shell, which is opposite to the second reflecting mirror, is made of high-light-transmittance glass, and the other parts are made of stainless steel or corrosion-resistant plastic.
In any of the above schemes, preferably, the continuous chemical vapor deposition chamber is arranged between the pay-off roller and the take-up roller, and the fiber sequentially passes through the pay-off roller, the continuous chemical vapor deposition chamber, the real-time monitoring device near the tail end part of the continuous chemical vapor deposition chamber and the take-up roller along the horizontal direction.
The invention also provides a real-time monitoring method for the thickness of the continuous chemical vapor deposition interface layer, which uses the real-time monitoring device for the thickness of the continuous chemical vapor deposition interface layer, and comprises the following steps in sequence:
step one: the real-time monitoring device is arranged at the tail end part of the continuous chemical vapor deposition chamber, the tightness and the connectivity are checked, and the real-time monitoring device can be ensured to be normally used;
step two: the fiber is arranged on a wire unwinding roller, the fiber head is pulled out to sequentially pass through a continuous chemical vapor deposition chamber and a real-time monitoring device near the tail end of the continuous chemical vapor deposition chamber along the horizontal direction, and is fixed on a wire winding roller, the angles of a first reflecting mirror, a second reflecting mirror and a third reflecting mirror are adjusted, and a full-spectrum light source is turned on;
step three: starting a pay-off roller and a take-up roller to convey fibers, enabling the fibers to continuously move sequentially through a continuous chemical vapor deposition chamber and a real-time monitoring device close to the tail end of the continuous chemical vapor deposition chamber, and monitoring the interface layer thickness of the prepared continuous chemical vapor deposition fibers in real time;
step four: in the real-time monitoring process, light generated by the full-spectrum light source irradiates on the first reflecting mirror, light irradiates on high-transmittance glass opposite to the first reflecting mirror through the first reflecting mirror, and light irradiates on an interface layer of the continuous chemical vapor deposition fiber through the high-transmittance glass, so that interference destructive and interference constructive phenomena occur, and mixed light with different colors is displayed;
step five: light reflected from the interface layer of the continuous chemical vapor deposition fiber is further irradiated onto high-transmittance glass opposite to the second reflector, the light passes through the high-transmittance glass to be sequentially irradiated onto the second reflector, the third reflector and the dispersion prism, dispersion occurs through the dispersion prism, the light after dispersion is irradiated onto the spectrum projection screen board, and further a dispersion spectrum of single color or different colors is displayed;
step six: and comparing the dispersion spectrum displayed on the spectrum screen throwing plate with the interface layer thickness range of the continuous chemical vapor deposition fiber, so that the interface layer thickness of the continuous chemical vapor deposition fiber can be monitored in real time.
Preferably, when the real-time monitoring device is installed and debugged, the horizontal distance between the central axis of the first closed shell and the central axis of the second closed shell is ensured to be 20-100cm, the horizontal distance between the center of the dispersion prism and the center of the spectrum screen panel is ensured to be 1-15cm, the wavelength of light waves generated by the full spectrum light source needs to be covered with 390-780nm, the illumination flux is 2000-5200Lm, and the illumination cross section area is 1-20cm 2 。
In any of the above embodiments, it is preferable that the incident angle of the light is 45 to 70 ° when the light is irradiated onto the interface layer of the continuous chemical vapor deposition fiber after passing through the first mirror and the high light transmission glass opposite to the first mirror.
In any of the above embodiments, it is preferable that the calculation formula of the thickness range of the interface layer of the continuous chemical vapor deposition fiber is as followsIn which, in the process,
-interfacial layer thickness in nm for continuous chemical vapor deposition fibers;
the light passes through the high light-transmission glass opposite to the first reflecting mirror and irradiates the light wave wavelength in nm when interference constructive occurs on the interface layer of the continuous chemical vapor deposition fiber;
-the light passes throughIncident angle of light ray irradiated onto interface layer of continuous chemical vapor deposition fiber after high light transmission glass opposite to first reflecting mirror, unit degree;
the interfacial layer refractive index of the continuous chemical vapor deposition fiber is dimensionless.
In the invention, the interfacial layer of the continuous chemical vapor deposition fiber is observed to present a certain color because the light wave of the color generates interference constructive phenomenon on the surface of the interfacial layer, and the condition that the reflected light generates interference constructive phenomenon on the surface of the interfacial layer is that the optical path difference is equal to even times of half wavelength, namelyWherein, the method comprises the steps of, wherein,
-optical path difference in nm of the light wave in the interface layer of the continuous chemical vapor deposition fiber;is determined by the incident angle, interface layer thickness and interface layer refractive index;
the light passes through the high light-transmission glass opposite to the first reflecting mirror and irradiates the light wave wavelength in nm when interference constructive occurs on the interface layer of the continuous chemical vapor deposition fiber;
-natural number.
A large number of experiments prove that when n=1, bright colored light is generated on the surface of the continuous chemical vapor deposition fiber, and when n is more than 1, no color is generated on the surface of the continuous chemical vapor deposition fiber, which means that no interface layer or too thick interface layer exists, so the invention sets the n value to be 1, namely。
The calculation formula of the interfacial layer refractive index of the continuous chemical vapor deposition fiber is as followsWherein, the method comprises the steps of, wherein,
the interfacial layer refractive index of the continuous chemical vapor deposition fiber, dimensionless,
-the incident angle of light rays onto the interfacial layer of the continuous chemical vapor deposition fiber after passing through the high light transmission glass opposite to the first mirror, in degrees;
the light passes through the high light transmission glass opposite to the first reflector and irradiates the light refraction angle of the interface layer of the continuous chemical vapor deposition fiber, and the unit degree is the unit degree;
wherein,in which, in the process,
-interfacial layer thickness in nm for continuous chemical vapor deposition fibers;
optical path difference of light wave in continuous chemical vapor deposition fiber interface layer, unit nm.
And (3) converting and substituting the formulas to obtain a calculation formula of the continuous chemical vapor deposition fiber interface layer thickness range.
The incident angle of the light is in the range of 45-70 deg.. The wavelength range of the light can be determined by the color of the reflected light. The interfacial layer refractive index of different chemical components can be obtained from physical and chemical properties of substances or the prior art, but the interfacial layers with the same chemical components prepared by different methods are still different in refractive index under the influence of the crystal structure and purity of the interfacial layers. The invention provides a partial continuous chemical vapor deposition fiber interfacial layer refractive index range suitable for the technical scheme of the invention through a plurality of experiments and combining theoretical basis, and the refractive index range is shown in table 1.
TABLE 1 continuous chemical vapor deposition fiber interfacial layer refractive index ranges
| Interfacial layer material | Preparation temperature (. Degree. C.) | Refractive index |
| Boron Nitride (BN) | 800-1100 | 1.72-1.73 |
| Silicon nitride (Si) 3 N 4 ） | 850-1400 | 1.85-1.88 |
| Alumina (Al) 2 O 3 ） | 600-1000 | 1.76-1.78 |
And under the condition that the light incidence angle range, the light wavelength range and the interface layer refractive index range are all determined, the interface layer thickness range can be calculated. Each interface layer thickness range corresponds to a reflected light color, and when the reflected light color is observed, the interface layer thickness range or thickness value can be directly read.
In the present invention, the fibers used are fiber bundles, fiber tapes, fiber cloths, or the like. Thickness uniformity, i.e., thickness uniformity, means that the thicknesses of the interface layer surface and the plurality of filament cladding coatings near the surface are equal, close or very different.
The real-time monitoring device can use some auxiliary components for assisting light reflection and light refraction, and the auxiliary components only adopt the traditional technology and are not particularly limited. The fragile components such as the light source, the reflector and the like can be physically separated from the vacuum and corrosion environment generated by continuous chemical vapor deposition by adopting a corrosion-resistant sealing ring, high-light-transmittance glass, a closed shell and the like.
The center of the first reflecting mirror and the center of the second reflecting mirror are positioned on the same horizontal line, the horizontal line is parallel to the continuous chemical vapor deposition fiber, and the distance between the horizontal line and the continuous chemical vapor deposition fiber is determined by the incident angle or needs to meet the requirement of the incident angle. The shape of the light spot projected by the light on the continuous chemical vapor deposition fiber can be designed into a round shape, a square shape, a long strip shape or the like according to the actual situation of the continuous chemical vapor deposition process.
For the spectrum screen throwing plate, the wavelength of light waves and the thickness of the interface layer can be combined for comparison, so that the thickness and the thickness distribution condition of the interface layer can be monitored in real time, the corresponding thickness of the interface layer can be visually compared and read out by observing the color of the scattered light on the spectrum screen throwing plate, and the thickness consistency or uniformity of the interface layer can be estimated by observing the dispersion condition of the scattered light.
The continuous chemical vapor deposition chamber, the matched components, the technological process, the technological parameters and the like which are used are all conventional technologies, the method is not particularly limited, the thickness and the thickness consistency of the interface layer of the prepared continuous chemical vapor deposition fiber can be directly monitored by using the real-time monitoring device, whether the former continuous chemical vapor deposition process meets the requirements can be judged through the thickness of the interface layer, and if the former continuous chemical vapor deposition process does not meet the requirements, the continuous chemical vapor deposition process can be adjusted in real time.
The real-time monitoring device and the method for the thickness of the continuous chemical vapor deposition interface layer can monitor the thickness and the consistency of the thickness of the interface layer prepared by the continuous chemical vapor deposition in real time under the conditions of no furnace opening, no shutdown and no sampling, and lay a foundation for the design and the quality control of the continuous chemical vapor deposition process.
Drawings
FIG. 1 is a schematic diagram of a real-time monitoring device for continuous chemical vapor deposition interface layer thickness according to a preferred embodiment of the present invention;
FIG. 2 is a schematic view of the overall structure of the continuous chemical vapor deposition chamber and the real-time monitoring apparatus in the embodiment shown in FIG. 1;
FIG. 3 is a photograph of a fiber bundle prior to continuous chemical vapor deposition in the embodiment of FIG. 1;
FIG. 4 is a photograph of a fiber bundle with a boron nitride interfacial layer after continuous chemical vapor deposition in the embodiment of FIG. 1, where the reflected light on the spectral projection screen is a single blue color;
FIG. 5 is a photograph of a fiber bundle with a silicon nitride interface layer after continuous chemical vapor deposition in accordance with another preferred embodiment of the apparatus and method for monitoring the thickness of an interface layer in accordance with the present invention, wherein the color of the reflected light on the spectral mask is single green;
FIG. 6 is a photograph of a fiber bundle with a silicon nitride interface layer after continuous chemical vapor deposition in the embodiment of FIG. 5, where the color of the reflected light on the spectral mask repeatedly changes between magenta, yellow and green;
fig. 7 is a photograph of a fiber bundle with a boron nitride interface layer after continuous chemical vapor deposition in accordance with another preferred embodiment of the apparatus and method for monitoring the thickness of an interface layer in accordance with the present invention, wherein the color of the reflected light on the spectral mask includes red, green, blue and violet.
The reference numerals in the drawings indicate:
the system comprises a 1-real-time monitoring device, a 11-light emission component, a 111-first closed shell, a 112-full spectrum light source, a 113-first reflecting mirror, a 12-light collection component, a 121-second closed shell, a 122-dispersion prism, a 123-spectrum projection screen, a 124-second reflecting mirror, a 125-third reflecting mirror and 13-high light-transmitting glass;
2-a continuous chemical vapor deposition chamber, 21-a first sealing flange, 22-a second sealing flange;
3-pay-off roll, 4-take-up roll, 5-fiber, 6-continuous chemical vapor deposition fiber;
a-light cross section, b-horizontal distance between the central axis of the first closed shell and the central axis of the second closed shell, c-vertical distance between the centers of the first reflecting mirror and the second reflecting mirror and the continuous chemical vapor deposition fiber, and horizontal distance between the center of the d-dispersion prism and the center of the spectrum screen throwing plate, wherein alpha-light passes through high-transmittance glass opposite to the first reflecting mirror and irradiates on the light incident angle of the interface layer of the continuous chemical vapor deposition fiber.
Detailed Description
For a further understanding of the present invention, the present invention will be described in detail with reference to the following examples.
Embodiment one:
as shown in fig. 1-2, according to a preferred embodiment of the apparatus for monitoring the thickness of an interfacial layer in continuous chemical vapor deposition of the present invention, the apparatus 1 is disposed at a position of a continuous chemical vapor deposition chamber 2 near the end thereof, a first sealing flange 21 and a second sealing flange 22 are disposed at the top of the continuous chemical vapor deposition chamber 2, and the apparatus 1 includes a light emitting component 11 and a light collecting component 12; the light emission component 11 is composed of a first closed shell 111, a full spectrum light source 112 and a first reflecting mirror 113, wherein the full spectrum light source 112 and the first reflecting mirror 113 are respectively positioned at the top and the bottom of the first closed shell 111, and the bottom of the first closed shell 111 is vertically inserted into the continuous chemical vapor deposition chamber 2 through the first sealing flange 21; the light collecting component 12 is composed of a second closed casing 121, a dispersion prism 122, a spectrum projection screen 123, a second reflecting mirror 124 and a third reflecting mirror 125, the second reflecting mirror 124 and the third reflecting mirror 125 are respectively arranged at the bottom and the top of the second closed casing 121, the dispersion prism 122 is arranged at the outer side of the top of the second closed casing 121, the spectrum projection screen 123 and the dispersion prism 122 are oppositely arranged, the central axes of the spectrum projection screen 123 and the dispersion prism 122 are positioned on the same horizontal line, and the bottom of the second closed casing 121 is vertically inserted into the interior of the continuous chemical vapor deposition chamber 2 through the second sealing flange 22.
The first airtight housing 111 and the second airtight housing 121 are both cylindrical, and are disposed in parallel in the vertical direction. The bottom ends of the first and second airtight housings 111 and 121 are on the same horizontal line, and are above the continuous chemical vapor deposition fibers 6, and the distances between the bottom ends of the two and the continuous chemical vapor deposition fibers 6 are equal.
The side of the bottom of the first airtight housing 111 opposite to the first reflecting mirror 113 is made of high light-transmitting glass 13, and the other parts are made of stainless steel or corrosion-resistant plastic; the side of the bottom of the second closed housing opposite to the second reflecting mirror is made of high light transmission glass 13, and the other parts are made of stainless steel or corrosion resistant plastic.
The continuous chemical vapor deposition chamber 2 is arranged between the paying-off roller 3 and the take-up roller 4, and the fiber 5 sequentially passes through the paying-off roller 3, the continuous chemical vapor deposition chamber 2, the real-time monitoring device 1 near the tail end part of the continuous chemical vapor deposition chamber and the take-up roller 4 along the horizontal direction.
The embodiment also provides a real-time monitoring method for the thickness of the continuous chemical vapor deposition interface layer, which comprises the following steps in sequence:
step one: the real-time monitoring device is arranged at the tail end part of the continuous chemical vapor deposition chamber, the tightness and the connectivity are checked, and the real-time monitoring device can be ensured to be normally used;
step two: the fiber is arranged on a wire unwinding roller, the fiber head is pulled out to sequentially pass through a continuous chemical vapor deposition chamber and a real-time monitoring device near the tail end of the continuous chemical vapor deposition chamber along the horizontal direction, and is fixed on a wire winding roller, the angles of a first reflecting mirror, a second reflecting mirror and a third reflecting mirror are adjusted, and a full-spectrum light source is turned on;
step three: starting a pay-off roller and a take-up roller to convey fibers, enabling the fibers to continuously move sequentially through a continuous chemical vapor deposition chamber and a real-time monitoring device close to the tail end of the continuous chemical vapor deposition chamber, and monitoring the interface layer thickness of the prepared continuous chemical vapor deposition fibers in real time;
step four: in the real-time monitoring process, light generated by the full-spectrum light source irradiates on the first reflecting mirror, light irradiates on high-transmittance glass opposite to the first reflecting mirror through the first reflecting mirror, and light irradiates on an interface layer of the continuous chemical vapor deposition fiber through the high-transmittance glass, so that interference destructive and interference constructive phenomena occur, and mixed light with different colors is displayed;
step five: light reflected from the interface layer of the continuous chemical vapor deposition fiber is further irradiated onto high-transmittance glass opposite to the second reflector, the light passes through the high-transmittance glass to be sequentially irradiated onto the second reflector, the third reflector and the dispersion prism, dispersion occurs through the dispersion prism, the light after dispersion is irradiated onto the spectrum projection screen board, and further a dispersion spectrum of single color or different colors is displayed;
step six: and comparing the dispersion spectrum displayed on the spectrum screen throwing plate with the interface layer thickness range of the continuous chemical vapor deposition fiber, so that the interface layer thickness of the continuous chemical vapor deposition fiber can be monitored in real time.
When the real-time monitoring device is installed and debugged, the horizontal distance between the central axis of the first closed shell and the central axis of the second closed shell is ensured to be 60cm, the horizontal distance between the center of the dispersion prism and the center of the spectrum screen throwing board is ensured to be 8cm, the wavelength of light waves generated by the full-spectrum light source needs to be covered by 390-780nm, the illumination flux is 3500Lm, and the illumination cross section area is 10cm 2 . When light passes through the first reflecting mirror and the high light transmission glass opposite to the first reflecting mirror and irradiates the interface layer of the continuous chemical vapor deposition fiber, the incident angle of the light is 45 degrees.
Continuous chemical vapor depositionThe calculation formula of the thickness range of the fiber interface layer is as followsIn which, in the process,
-interfacial layer thickness in nm for continuous chemical vapor deposition fibers;
the light passes through the high light-transmission glass opposite to the first reflecting mirror and irradiates the light wave wavelength in nm when interference constructive occurs on the interface layer of the continuous chemical vapor deposition fiber;
-the incident angle of light rays onto the interfacial layer of the continuous chemical vapor deposition fiber after passing through the high light transmission glass opposite to the first mirror, in degrees;
the interfacial layer refractive index of the continuous chemical vapor deposition fiber is dimensionless.
In this embodiment, it is observed that the interfacial layer of the continuous chemical vapor deposition fiber presents a certain color because the light waves of the color generate interference constructive phenomenon on the surface of the interfacial layer, and the condition that the reflected light generates interference constructive phenomenon on the surface of the interfacial layer is that the optical path difference is equal to even times of half wavelength, namelyWherein, the method comprises the steps of, wherein,
-optical path difference in nm of the light wave in the interface layer of the continuous chemical vapor deposition fiber;is determined by the incident angle, interface layer thickness and interface layer refractive index;
the light passes through the high light-transmission glass opposite to the first reflecting mirror and irradiates the light wave wavelength in nm when interference constructive occurs on the interface layer of the continuous chemical vapor deposition fiber;
-natural number.
The experiment in this example shows that when n=1, bright colored light is generated on the surface of the continuous chemical vapor deposition fiber, and when n > 1, no color is generated on the surface of the continuous chemical vapor deposition fiber, which means that no interface layer or interface layer is too thick, so the example sets the n value to 1, namely。
The calculation formula of the interfacial layer refractive index of the continuous chemical vapor deposition fiber is as followsWherein, the method comprises the steps of, wherein,
the interfacial layer refractive index of the continuous chemical vapor deposition fiber, dimensionless,
-the incident angle of light rays onto the interfacial layer of the continuous chemical vapor deposition fiber after passing through the high light transmission glass opposite to the first mirror, in degrees;
light rays irradiating the interface layer of the continuous chemical vapor deposition fiber after passing through the high light transmission glass opposite to the first reflectorAngle of refraction, unit °;
wherein,in which, in the process,
-interfacial layer thickness in nm for continuous chemical vapor deposition fibers;
optical path difference of light wave in continuous chemical vapor deposition fiber interface layer, unit nm.
And (3) converting and substituting the formulas to obtain a calculation formula of the continuous chemical vapor deposition fiber interface layer thickness range.
The wavelength range of the light can be determined by the color of the reflected light. The interfacial layer refractive index of different chemical components can be obtained from physical and chemical properties of substances or the prior art, but the interfacial layers with the same chemical components prepared by different methods are still different in refractive index under the influence of the crystal structure and purity of the interfacial layers. The present example provides a range of interfacial refractive indices of partially continuous chemical vapor deposited fibers suitable for the technical scheme of the present example through a number of experiments in combination with theoretical basis, as shown in table 1 of the foregoing part of the present invention. And under the condition that the light incidence angle range, the light wavelength range and the interface layer refractive index range are all determined, the interface layer thickness range can be calculated. Each interface layer thickness range corresponds to a reflected light color, and when the reflected light color is observed, the interface layer thickness range or thickness value can be directly read.
In this embodiment, a comparison table of the color of the reflected light and the thickness of the interface layer is obtained according to the calculation formula of the thickness of the interface layer, as shown in table 2.
TABLE 2 comparison of reflected light color and interface layer thickness
Fig. 3 is a photograph of a fiber bundle before continuous chemical vapor deposition, fig. 4 is a photograph of a fiber bundle with a boron nitride interface layer after continuous chemical vapor deposition, at this time, the color of scattered light is observed to be blue from a spectrum projection screen, and the thickness of the interface layer is about 214-233nm, as compared with table 2, and the thickness of the interface layer is relatively uniform.
In this embodiment, the fibers used are fiber bundles. Thickness uniformity, i.e., thickness uniformity, means that the thicknesses of the interface layer surface and the plurality of filament cladding coatings near the surface are equal, close or very different.
The real-time monitoring device can use some auxiliary components for assisting light reflection and light refraction, and the auxiliary components only adopt the traditional technology and are not particularly limited. The center of the first reflecting mirror and the center of the second reflecting mirror are positioned on the same horizontal line, the horizontal line is parallel to the continuous chemical vapor deposition fiber, and the distance between the horizontal line and the continuous chemical vapor deposition fiber is determined by the incident angle or needs to meet the requirement of the incident angle. The shape of the light spot projected by the light on the continuous chemical vapor deposition fiber can be designed into a round shape, a square shape, a long strip shape or the like according to the actual situation of the continuous chemical vapor deposition process.
For the spectrum screen throwing plate, the wavelength of light waves and the thickness of the interface layer can be combined for comparison, so that the thickness and the thickness distribution condition of the interface layer can be monitored in real time, the corresponding thickness of the interface layer can be visually compared and read out by observing the color of the scattered light on the spectrum screen throwing plate, and the thickness consistency or uniformity of the interface layer can be estimated by observing the dispersion condition of the scattered light.
The continuous chemical vapor deposition chamber, the matched components, the technological process, the technological parameters and the like which are used are all conventional technologies, the method is not particularly limited, the thickness and the thickness consistency of the interface layer of the prepared continuous chemical vapor deposition fiber can be directly monitored by using the real-time monitoring device, whether the former continuous chemical vapor deposition process meets the requirements can be judged through the thickness of the interface layer, and if the former continuous chemical vapor deposition process does not meet the requirements, the continuous chemical vapor deposition process can be adjusted in real time.
The real-time monitoring device and the method for the thickness of the continuous chemical vapor deposition interface layer can monitor the thickness and the thickness consistency of the interface layer prepared by the continuous chemical vapor deposition in real time under the conditions of no furnace opening, no shutdown and no sampling, and lay a foundation for the design and the quality control of the continuous chemical vapor deposition process.
Embodiment two:
according to another preferred embodiment of the continuous chemical vapor deposition interface layer thickness real-time monitoring device and the method thereof, the structure of the device, the connection relation among all the components, the real-time monitoring method, the technical principle, the beneficial effects and the like are basically the same as those of the first embodiment, except that:
when the real-time monitoring device is installed and debugged, the horizontal distance between the central axis of the first closed shell and the central axis of the second closed shell is ensured to be 100cm, the horizontal distance between the center of the dispersion prism and the center of the spectrum screen throwing board is ensured to be 15cm, the wavelength of light waves generated by the full-spectrum light source needs to be covered by 390-780nm, the illumination flux is 5200Lm, and the illumination cross section area is 20cm 2 . When light passes through the first mirror and the high light transmission glass opposite to the first mirror and irradiates the interface layer of the continuous chemical vapor deposition fiber, the incident angle of the light is 50 degrees.
In this embodiment, a comparison table of the color of the reflected light and the thickness of the interface layer is obtained according to the calculation formula of the thickness of the interface layer, as shown in table 3.
TABLE 3 comparison of reflected light color and interface layer thickness
The color of the scattered light on the spectral panel remained green throughout the first 10 hours and 15 minutes of continuous chemical vapor deposition, indicating that the interface layer thickness prepared during the first 10 hours and 15 remained stable and controlled at about 192-215nm for the fiber bundles deposited during this period of time as shown in fig. 5.
During the continuous chemical vapor deposition process, which was carried out for 10 hours 15 minutes to 10 hours 25 minutes, the color of the scattered light on the spectral mask was repeatedly changed between magenta, yellow and green, which means that the thickness of the interface layer obtained by the deposition during this period was no longer stable, and the thickness of the interface layer was continuously fluctuated in the range of 192-276nm, so that it was necessary to adjust the continuous chemical vapor deposition process in real time, and the fiber bundles deposited during this period were as shown in fig. 6.
Embodiment III:
according to another preferred embodiment of the continuous chemical vapor deposition interface layer thickness real-time monitoring device and the method thereof, the structure of the device, the connection relation among all the components, the real-time monitoring method, the technical principle, the beneficial effects and the like are basically the same as those of the first embodiment, except that:
when the real-time monitoring device is installed and debugged, the horizontal distance between the central axis of the first closed shell and the central axis of the second closed shell is ensured to be 20cm, the horizontal distance between the center of the dispersion prism and the center of the spectrum screen throwing board is ensured to be 1cm, the wavelength of light waves generated by the full-spectrum light source needs to be covered by 390-780nm, the illumination flux is 2000Lm, and the illumination cross section area is 1cm 2 . When light passes through the first mirror and the high light transmission glass opposite to the first mirror and irradiates the interface layer of the continuous chemical vapor deposition fiber, the incident angle of the light is 65 degrees.
In this embodiment, a comparison table of the color of the reflected light and the thickness of the interface layer is obtained according to the calculation formula of the thickness of the interface layer, as shown in table 4.
TABLE 4 comparison of reflected light color and interface layer thickness
Scattered light colors including red, green, blue and violet blue were observed from the spectral projection panel, which suggests that the resulting interface layer thickness range covered 185-306nm, and that the interface layer thickness uniformity was poor, thus requiring real-time adjustment of the continuous chemical vapor deposition process, where the deposited fiber bundles are as shown in fig. 7.
The specific description is as follows: the technical scheme of the invention relates to a plurality of parameters, and the beneficial effects and remarkable progress of the invention can be obtained by comprehensively considering the synergistic effect among the parameters. In addition, the value ranges of all the parameters in the technical scheme are obtained through a large number of tests, and aiming at each parameter and the mutual combination of all the parameters, the inventor records a large number of test data, and the specific test data are not disclosed herein for a long period of time.
It will be appreciated by those skilled in the art that the apparatus and method for monitoring the thickness of an interfacial layer in continuous chemical vapor deposition of the present invention includes any combination of the foregoing summary of the invention and the detailed description of the invention and the portions shown in the drawings, and is limited in scope and does not describe each of these combinations in any way for brevity. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. The utility model provides a real-time monitoring device of continuous chemical vapor deposition interface layer thickness, real-time monitoring device sets up the position that is close to its terminal at continuous chemical vapor deposition cavity, the top of continuous chemical vapor deposition cavity sets up first sealing flange and second sealing flange, its characterized in that: the real-time monitoring device comprises a light emitting component and a light collecting component; the light emission component consists of a first closed shell, a full spectrum light source and a first reflecting mirror, wherein the full spectrum light source and the first reflecting mirror are respectively positioned at the top and the bottom of the first closed shell, and the bottom of the first closed shell is vertically inserted into the continuous chemical vapor deposition chamber through the first sealing flange; the light collecting assembly consists of a second airtight shell, a dispersion prism, a spectrum screen throwing plate, a second reflecting mirror and a third reflecting mirror, wherein the second reflecting mirror and the third reflecting mirror are respectively arranged at the bottom and the top of the second airtight shell;
the method for monitoring the thickness of the continuous chemical vapor deposition interface layer in real time by using the real-time monitoring device comprises the following steps in sequence:
step one: the real-time monitoring device is arranged at the tail end part of the continuous chemical vapor deposition chamber, the tightness and the connectivity are checked, and the real-time monitoring device can be ensured to be normally used;
step two: the fiber is arranged on a wire unwinding roller, the fiber head is pulled out to sequentially pass through a continuous chemical vapor deposition chamber and a real-time monitoring device near the tail end of the continuous chemical vapor deposition chamber along the horizontal direction, and is fixed on a wire winding roller, the angles of a first reflecting mirror, a second reflecting mirror and a third reflecting mirror are adjusted, and a full-spectrum light source is turned on;
step three: starting a pay-off roller and a take-up roller to convey fibers, enabling the fibers to continuously move sequentially through a continuous chemical vapor deposition chamber and a real-time monitoring device close to the tail end of the continuous chemical vapor deposition chamber, and monitoring the interface layer thickness of the prepared continuous chemical vapor deposition fibers in real time;
step four: in the real-time monitoring process, light generated by the full-spectrum light source irradiates on the first reflecting mirror, light irradiates on high-transmittance glass opposite to the first reflecting mirror through the first reflecting mirror, and light irradiates on an interface layer of the continuous chemical vapor deposition fiber through the high-transmittance glass, so that interference destructive and interference constructive phenomena occur, and mixed light with different colors is displayed;
step five: light reflected from the interface layer of the continuous chemical vapor deposition fiber is further irradiated onto high-transmittance glass opposite to the second reflector, the light passes through the high-transmittance glass to be sequentially irradiated onto the second reflector, the third reflector and the dispersion prism, dispersion occurs through the dispersion prism, the light after dispersion is irradiated onto the spectrum projection screen board, and further a dispersion spectrum of single color or different colors is displayed;
step six: the dispersion spectrum displayed on the spectrum screen throwing plate is compared with the interface layer thickness range of the continuous chemical vapor deposition fiber, so that the interface layer thickness of the continuous chemical vapor deposition fiber can be monitored in real time;
when the real-time monitoring device is installed and debugged, the horizontal distance between the central axis of the first closed shell and the central axis of the second closed shell is ensured to be 20-100cm, the horizontal distance between the center of the dispersion prism and the center of the spectrum screen throwing plate is ensured to be 1-15cm, the wavelength of light waves generated by the full spectrum light source needs to be covered by 390-780nm, the illumination flux is 2000-5200Lm, and the illumination cross section area is 1-20cm 2 The method comprises the steps of carrying out a first treatment on the surface of the When the light passes through the first reflecting mirror and the high-transmittance glass opposite to the first reflecting mirror and irradiates the interface layer of the continuous chemical vapor deposition fiber, the incident angle of the light is 45-70 degrees;
the calculation formula of the thickness range of the interface layer of the continuous chemical vapor deposition fiber is as followsIn which, in the process,
-interfacial layer thickness in nm for continuous chemical vapor deposition fibers;
the light passes through the high light-transmission glass opposite to the first reflecting mirror and irradiates the light wave wavelength in nm when interference constructive occurs on the interface layer of the continuous chemical vapor deposition fiber;
-the incident angle of light rays onto the interfacial layer of the continuous chemical vapor deposition fiber after passing through the high light transmission glass opposite to the first mirror, in degrees;
-interfacial layer refractive index of continuous chemical vapor deposition fiber, dimensionless;
the fibers are fiber bundles, fiber belts or fiber cloths; when the interface layer substance is boron nitride and the chemical vapor deposition temperature is 800-1100 ℃, the refractive index of the boron nitride interface layer after correction is 1.72-1.73; when the interface layer material is silicon nitride and the chemical vapor deposition temperature is 850-1400 ℃, the refractive index of the silicon nitride interface layer after correction is 1.85-1.88; when the interface layer material is aluminum nitride and the chemical vapor deposition temperature is 600-1000 ℃, the refractive index of the aluminum nitride interface layer after correction is 1.76-1.78.
2. The apparatus for real-time monitoring of continuous chemical vapor deposition interface layer thickness according to claim 1, wherein: the first airtight shell and the second airtight shell are cylindrical and are arranged in parallel in the vertical direction.
3. The apparatus for real-time monitoring of continuous chemical vapor deposition interface layer thickness according to claim 2, wherein: the bottom end of the first closed shell and the bottom end of the second closed shell are positioned on the same horizontal line, are positioned above the continuous chemical vapor deposition fibers, and have the same distance with the continuous chemical vapor deposition fibers.
4. The apparatus for real-time monitoring of continuous chemical vapor deposition interface layer thickness according to claim 3, wherein: the side surface of the bottom of the first airtight shell, which is opposite to the first reflecting mirror, is made of high-light-transmittance glass, and the other parts are made of stainless steel or corrosion-resistant plastic; the side surface of the bottom of the second airtight shell, which is opposite to the second reflecting mirror, is made of high-light-transmittance glass, and the other parts are made of stainless steel or corrosion-resistant plastic.
5. The apparatus for real-time monitoring of continuous chemical vapor deposition interface layer thickness according to claim 4, wherein: the continuous chemical vapor deposition chamber is arranged between the wire unwinding roller and the wire winding roller, and the fiber sequentially passes through the wire unwinding roller, the continuous chemical vapor deposition chamber, the real-time monitoring device near the tail end part of the continuous chemical vapor deposition chamber and the wire winding roller along the horizontal direction.
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