CN112481601A - Device and method for preparing tungsten-boron radiation-proof fiber by CVD method - Google Patents
Device and method for preparing tungsten-boron radiation-proof fiber by CVD method Download PDFInfo
- Publication number
- CN112481601A CN112481601A CN202011349520.5A CN202011349520A CN112481601A CN 112481601 A CN112481601 A CN 112481601A CN 202011349520 A CN202011349520 A CN 202011349520A CN 112481601 A CN112481601 A CN 112481601A
- Authority
- CN
- China
- Prior art keywords
- filament
- tungsten
- boron
- air inlet
- continuous cooling
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—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
- C23C16/28—Deposition of only one other non-metal element
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention belongs to the field of preparing continuous radiation-proof fibers by a chemical vapor deposition method, and particularly relates to a device and a method for preparing tungsten-boron radiation-proof fibers by a CVD method. The device comprises a filament unwinding device, a reactor and a filament winding device, wherein a tungsten filament is wound on the filament unwinding device, one end of the tungsten filament penetrates through the reactor and is connected to the filament winding device, and the reactor consists of an upper filament penetrating device, a reaction tube and a lower filament penetrating device. The chemical vapor deposition method is adopted, a tungsten wire with the diameter of 10-15 mu m passes through a reaction tube, the tungsten wire is heated by a direct current power supply, and the elemental boron with the thickness of 10-20 mu m is deposited on the surface of the tungsten wire. The invention can improve the mechanical property of the tungsten-boron fiber and reduce the defects in the fiber and on the surface, so that the fiber property is more stable, the residual stress in the tungsten/boron radiation-proof fiber is reduced, the tungsten-boron fiber has the knittability, and the W/B content can be adjusted according to the requirements of different radiation conditions.
Description
Technical Field
The invention belongs to the field of preparing continuous radiation-proof fibers by a chemical vapor deposition method, and particularly relates to a device and a method for preparing tungsten-boron radiation-proof fibers by a CVD method.
Background
Nuclear energy plays an important role in the world energy composition, and as an important link in nuclear fuel circulation, spent fuel aftertreatment receives more and more attention. Occupational personnel can be irradiated by neutron and gamma ray radiation when working in operation, cleaning, maintenance and the like in working environments and other environments with radiation, and the low-energy radiation brings great harm to the health of people. The radiation-proof clothes can effectively reduce the radiation dose of personnel when being worn, the most widely applied radiation-proof materials at present are polymer fibers containing light elements and heavy metal elements, and the fibers are knitted to prepare knitted fabrics, woven fabrics, non-woven fabrics and the like and have a certain radiation-proof function. However, the polymer fiber has low content of heavy metals and light elements with large cross sections (40 wt% -50 wt%), so that the absorption efficiency of neutrons is low, the requirement of people on neutron radiation protection is not met, the service life of a radiation protection product is greatly reduced due to the poor strength of the fiber, most of protective clothing shields single rays, and almost no protective clothing can comprehensively shield neutrons and gamma rays and has good durability. It is contemplated that boron can shield thermal neutrons and tungsten can shield low energy gamma rays. Therefore, the research and development of high-strength tungsten boron fiber with comprehensive protective effect becomes the focus of the research and development of radiation-proof products.
Disclosure of Invention
In order to solve the problems existing in the prior art, the invention aims to provide a device and a method for preparing tungsten-boron radiation-proof fibers by a CVD method, wherein the device has the characteristics of simple structure, small occupied space, convenience in operation, low cost and the like, the tungsten-boron fibers prepared by the method have knittability, and the W/B content can be adjusted according to different radiation condition requirements.
The technical scheme of the invention is as follows:
the utility model provides a CVD legal system preparation tungsten boron radiation protection fibrous device, includes filament unwinding device, reactor and receipts filament device, and the tungsten filament is convoluteed on filament unwinding device, and the one end of tungsten filament passes reactor and links to receiving filament device, and the reactor comprises last threading device, reaction tube and lower threading device, and the concrete structure is as follows:
the center of one end of the upper wire feeding device is provided with a wire feeding hole, the other end of the upper wire feeding device is connected with the upper end of the reaction tube through an upper conical grinding opening, and the side surface of the upper wire feeding device is provided with an air inlet of the upper wire feeding device; the center of one end of the lower wire penetrating device is provided with a lower wire penetrating hole, the other end of the lower wire penetrating device is connected with the lower end of the reaction tube through a lower conical ground, and the side surface of the lower wire penetrating device is provided with an air inlet of the lower wire penetrating device; the upper end and the lower end of the reaction tube are respectively an upper quartz grinding port communicated with the upper conical grinding port and a lower quartz grinding port communicated with the lower conical grinding port.
The CVD method preparation tungsten boron radiation protection fibrous device, the reaction tube comprises three reaction section, from top to bottom is tungsten filament cleaning section, boron deposit section and continuous cooling section in proper order, tungsten filament cleaning section, boron deposit section and continuous cooling section are quartz glass tube, the upper portion of boron deposit section is equipped with boron deposit section air inlet, the upper portion and the middle part of continuous cooling section are equipped with continuous cooling section air inlet, continuous cooling section air inlet down, the lower part of continuous cooling section is equipped with tail gas discharge port.
According to the device for preparing the tungsten-boron radiation-proof fiber by the CVD method, all the air inlets are formed by quartz glass tubes with spiral structures, all the air inlets are provided with flow regulating valves and gas filtering devices, the flow regulating valves are used for regulating the flow of gas, and the filtering devices are used for filtering gas and solid particles in raw material gas.
In the device for preparing the tungsten boron radiation-proof fiber by the CVD method, the upper wire-penetrating device is made of quartz glass, the center of one end of the upper wire-penetrating device is an upper wire-penetrating hole with the diameter of 0.5-1 mm, the length of the upper wire-penetrating hole is 20mm, and the other end of the upper wire-penetrating device is an upper conical ground with the length of 100 mm; the lower wire feeding device is made of quartz glass, a lower wire feeding hole with the diameter of 0.5-1 mm is arranged in the center of one end of the lower wire feeding device, the length of the lower wire feeding hole is 20mm, and a lower conical grinding opening with the length of 100mm is arranged at the other end of the lower wire feeding device.
According to the device for preparing the tungsten boron radiation-proof fiber by the CVD method, a reaction tube is made of a quartz glass tube with the length of 800mm, wherein: the inner diameter of the quartz glass tube at the tungsten filament cleaning section is 25mm, and the length of the quartz glass tube is 200-300 mm; the boron deposition section quartz glass tube has an inner diameter of 25mm and a length of 300-400 mm; the inner diameter of the continuous cooling section is 25mm, and the length of the continuous cooling section is 100-200 mm.
A method for preparing tungsten-boron radiation-proof fibers by a CVD method adopts a chemical vapor deposition method, a tungsten wire with the diameter of 10-15 mu m passes through a reaction tube, the tungsten wire is heated by a direct current power supply, and elemental boron with the thickness of 10-20 mu m is deposited on the surface of the tungsten wire.
The method for preparing the tungsten boron radiation-proof fiber by the CVD method comprises the following steps:
(1) connecting the reaction tube with an upper wire feeding device and a lower wire feeding device, wherein the upper wire feeding device and the lower wire feeding device are tightly connected with the reaction tube;
(2) fixing a tungsten filament disc on the filament releasing device, wherein one end of a tungsten filament enters from an upper filament passing hole and penetrates out from a lower filament passing hole and is bonded on the filament collecting device;
(3) introducing high-purity argon from an air inlet of the upper wire threading device and an air inlet of the lower wire threading device, emptying air in the reactor, wherein the flow of the introduced argon is 0.5-3L/min, and the introduction time is 8-15 min;
(4) after air in the reactor is exhausted, hydrogen is respectively introduced from an air inlet of the upper filament passing device and an air inlet of the lower filament passing device, the flow of the hydrogen introduced from the air inlet of the upper filament passing device is 0.1-0.5L/min, and the flow of the hydrogen introduced from the air inlet of the lower filament passing device is 0.1-0.2L/min;
(5) introducing mixed gas of boron trichloride, hydrogen and argon into an air inlet of the upper boron deposition section of the boron deposition section for boron deposition;
(6) hydrogen is respectively introduced into an upper continuous cooling section air inlet and a lower continuous cooling section air inlet of the continuous cooling section for realizing continuous cooling, the flow rate of the hydrogen introduced into the upper part of the continuous cooling section is 0.2-0.5L/min, and the flow rate of the hydrogen introduced into the middle part of the continuous cooling section is 0.5-1L/min;
(7) starting a filament collecting device, wherein the rotating speed of a filament collecting wheel of the filament collecting device is 3-10 rpm;
(8) starting a direct current power supply to heat the tungsten wire, controlling the temperature of a tungsten wire cleaning section to be 500-800 ℃, the temperature of a boron deposition section to be 1100-1350 ℃, and the temperature of a continuous cooling section to be 1250 +/-30-300 +/-30 ℃;
(9) and after the temperature of each section reaches a specified range for 5-15 min, formally starting to wind the filaments.
According to the method for preparing the tungsten boron radiation-proof fiber by the CVD method, in the mixed gas in the step (5), 30-40% of boron trichloride, 30-40% of hydrogen and the balance of argon are calculated according to volume percentage, and the flow rate of the mixed gas is 1.5-3L/min.
The design idea of the invention is as follows:
the invention provides a preparation method of radiation-proof fiber which is formed at high temperature and has continuously adjustable W/B content, wherein the purity of radiation-proof elements in the fiber can be improved by depositing a B coating on a pure tungsten core, and the element content can be continuously adjusted according to different radiation-proof requirements; the deposition at high temperature can improve the strength and durability of the fiber, so that the fiber has good knitting performance, the protection effect of the protective clothing can be improved, and the service life of the protective clothing can be prolonged.
The invention has the following advantages and beneficial effects:
1. the invention designs the air inlet form and structure of the continuous B fiber reaction vessel, so that all processes are carried out in the same quartz glass tube, the performance and stability of the fiber are improved, the preparation cost of the device is saved, the preparation difficulty of the reaction device is reduced, the preparation process flow is shortened, and the production efficiency is improved.
2. The tungsten boron radiation-proof fiber prepared by the process method has high mechanical property, stable performance and certain weaving performance.
3. The content of heavy metal elements and boron in the traditional polymer spinning fiber is about 40 wt% -50 wt%, while the tungsten core radiation-proof boron fiber prepared by the CVD method has the W/B radiation-proof fiber with only two W/B elements, the W/B content accounts for 100% of the fiber content, and the fiber has higher absorption efficiency for protecting thermal neutrons, fast neutrons or neutron streams with larger dose.
4. The tungsten core radiation-proof boron fiber prepared by the CVD method has adjustable W/B content according to radiation-proof requirements. The diameter of the W/B radiation-proof fiber is 40-50 μm, the fiber has higher strength, and the current fiber strength is 2600-3200 MPa.
Drawings
FIG. 1 is a schematic diagram of an apparatus for preparing a tungsten boron radiation-proof fiber by a CVD method.
Fig. 2 shows the microstructure of the surface (a) and cross section (b) of the anti-radiation fiber of tungsten boron.
In the figure: 1. the device comprises a filament discharging device, 2, a tungsten filament, 3, an upper filament feeding device, 31, an upper filament feeding hole, 32, an upper conical grinding opening, 4, an upper filament feeding device air inlet, 5, a reaction tube, 51, a tungsten filament cleaning section, 52, a boron deposition section, 53, a continuous cooling section, 54, an upper quartz grinding opening, 55, a lower quartz grinding opening, 6, a boron deposition section air inlet, 7, an upper continuous cooling section air inlet, 8, a lower continuous cooling section air inlet, 9, a tail gas discharge opening, 10, a lower filament feeding device, 101, a lower filament feeding hole, 102, a lower conical grinding opening, 11, a lower filament feeding device air inlet, 12 and a filament collecting device.
Detailed Description
As shown in fig. 1, the device for preparing tungsten-boron radiation-proof fiber by CVD method of the present invention mainly comprises a filament unwinding device 1, a reactor and a filament winding device 12, wherein a tungsten filament 2 is wound on the filament unwinding device 1, one end of the tungsten filament 2 passes through the reactor and is connected to the filament winding device 12, the reactor is composed of an upper filament passing device 3, a reaction tube 5 and a lower filament passing device 10, and the specific structure is as follows:
the upper wire feeding device 3 is made of quartz glass, an upper wire feeding hole 31 with the diameter of 0.5 mm-1 mm is arranged in the center of one end of the upper wire feeding device 3, the length of the upper wire feeding hole 31 is 20mm, an upper conical grinding opening 32 with the length of 100mm is arranged at the other end of the upper wire feeding device 3 and used for being connected with the reaction tube 5, and an upper wire feeding device air inlet 4 is arranged on the side surface of the upper wire feeding device 3. The lower wire feeding device 10 is made of quartz glass, a lower wire feeding hole 101 with the diameter of 0.5 mm-1 mm is formed in the center of one end of the lower wire feeding device, the length of the lower wire feeding hole 101 is 20mm, a lower conical grinding opening 102 with the length of 100mm is formed in the other end of the lower wire feeding device 10 and used for being connected with the reaction tube 5, and a lower wire feeding device air inlet 11 is formed in the side face of the lower wire feeding device 10.
The reaction tube 5 is made of a quartz glass tube with a length of 800mm, and the upper end and the lower end of the reaction tube are respectively provided with an upper quartz grinding port 54 communicated with the upper conical grinding port 32 and a lower quartz grinding port 55 communicated with the lower conical grinding port 102. The reaction tube 5 is composed of three reaction sections, and is tungsten filament cleaning section 51, boron deposition section 52 and continuous cooling section 53 from top to bottom in proper order, and tungsten filament cleaning section 51, boron deposition section 52 and continuous cooling section 53 are quartz glass tubes, wherein: the inner diameter of the quartz glass tube of the tungsten wire cleaning section 51 is 25mm, and the length of the quartz glass tube is 200-300 mm; the inner diameter of the quartz glass tube of the boron deposition section 52 is 25mm, the length of the quartz glass tube is 300-400 mm, and the upper part of the boron deposition section 52 is provided with a boron deposition section air inlet 6; the inner diameter of the continuous cooling section 53 is 25mm, the length is 100-200 mm, the upper part and the middle part of the continuous cooling section 53 are provided with an upper continuous cooling section air inlet 7 and a lower continuous cooling section air inlet 8, and the lower part of the continuous cooling section 53 is provided with a tail gas discharge port 9.
In the invention, all the air inlets are composed of quartz glass tubes with spiral structures, all the air inlets are provided with flow regulating valves and gas filtering devices, the flow regulating valves are used for regulating the flow of gas, and the filtering devices are used for filtering gas and small solid particles in raw material gas.
The present invention is further explained below with reference to examples and figures, which are intended to be illustrative only and should not be taken as limiting the scope of the invention.
Examples
As shown in fig. 1, in this embodiment, a tungsten filament with a diameter of 13 micrometers (μm) is passed through a reaction tube with a diameter of 25mm and a length of 800mm by a Chemical Vapor Deposition (CVD), the tungsten filament is heated by a direct current power supply, and after heating to a certain temperature, elemental boron is deposited on the surface of the tungsten filament, which includes the following specific steps:
(1) the reaction tube 5 is connected with the upper wire-threading device 3 and the lower wire-threading device 10, and the upper wire-threading device 3 and the lower wire-threading device 10 are tightly connected with the reaction tube 5.
(2) The tungsten filament plate is fixed on the filament releasing device 1, one end of the tungsten filament 2 enters from the upper filament passing hole 31, penetrates out from the lower filament passing hole 101 and is bonded on the filament collecting device 12.
(3) Introducing high-purity argon (with the volume purity of 99.999%) from an air inlet 4 of an upper wire threading device and an air inlet 11 of a lower wire threading device, and evacuating air in the reactor, wherein the flow of the introduced argon is 1.5L/min, and the introduction time is 10 min;
(4) after air in the reactor is exhausted, hydrogen is respectively introduced from the air inlet 4 of the upper wire threading device and the air inlet 11 of the lower wire threading device, the flow rate of the hydrogen introduced from the air inlet 4 of the upper wire threading device is 0.3L/min, and the flow rate of the hydrogen introduced from the air inlet 11 of the lower wire threading device is 0.15L/min.
(5) And introducing mixed gas of boron trichloride, hydrogen and argon into the upper boron deposition section gas inlet 6 of the boron deposition section 52, wherein the volume percentages of the boron trichloride, the hydrogen and the argon are respectively 30%, 30% and 40%, the mixed gas is used for B deposition, and the flow of the mixed gas introduced into the upper boron deposition section gas inlet 6 of the boron deposition section 52 is 1.8L/min.
(6) The upper continuous cooling section air inlet 7 and the lower continuous cooling section air inlet 8 of the continuous cooling section 53 are respectively filled with hydrogen for realizing continuous cooling, the flow rate of the hydrogen filled into the upper part of the continuous cooling section 53 is 0.27L/min, and the flow rate of the hydrogen filled into the middle part of the continuous cooling section 53 is 0.6L/min.
(7) The yarn collecting device 12 is started, and the rotating speed of a yarn collecting wheel of the yarn collecting device 12 is 5.5 rpm.
(8) Starting a direct current power supply to heat the tungsten wire 2, controlling the temperature of the tungsten wire cleaning section 51 at 750 +/-30 ℃, the temperature of the boron deposition section 52 at 1250 +/-30 ℃, and the temperature of the continuous cooling section 53 at 1250 +/-30-300 +/-30 ℃.
(9) After the temperature of each section reaches 10min, the obtained tungsten boron radiation-proof fiber is wound after the diameter of the tungsten boron radiation-proof fiber is stabilized at 50 mu m +/-2 mu m.
As shown in fig. 2(a) - (b), the microstructure of the surface and the cross section of the tungstoboron radiation-proof fiber, in this example, the performance indexes of the tungstoboron radiation-proof fiber are as follows: the tensile strength of the fiber at room temperature is more than 2950MPa, and the continuous length is more than 200 m.
The embodiment result shows that the method can improve the mechanical property of the tungsten-boron fiber, can reduce the defects in the fiber and on the surface of the fiber, enables the fiber property to be more stable, and reduces the residual stress in the tungsten/boron radiation-proof fiber.
Claims (8)
1. The device for preparing the tungsten-boron radiation-proof fiber by the CVD method is characterized by comprising a filament unwinding device, a reactor and a filament winding device, wherein a tungsten filament is wound on the filament unwinding device, one end of the tungsten filament penetrates through the reactor to be connected to the filament winding device, the reactor consists of an upper filament passing device, a reaction tube and a lower filament passing device, and the device has the following specific structure:
the center of one end of the upper wire feeding device is provided with a wire feeding hole, the other end of the upper wire feeding device is connected with the upper end of the reaction tube through an upper conical grinding opening, and the side surface of the upper wire feeding device is provided with an air inlet of the upper wire feeding device; the center of one end of the lower wire penetrating device is provided with a lower wire penetrating hole, the other end of the lower wire penetrating device is connected with the lower end of the reaction tube through a lower conical ground, and the side surface of the lower wire penetrating device is provided with an air inlet of the lower wire penetrating device; the upper end and the lower end of the reaction tube are respectively an upper quartz grinding port communicated with the upper conical grinding port and a lower quartz grinding port communicated with the lower conical grinding port.
2. The apparatus for preparing anti-radiation W-B fiber by CVD process as claimed in claim 1, wherein the reaction tube is composed of three reaction sections, which are a W filament cleaning section, a B deposition section and a continuous cooling section from top to bottom, the W filament cleaning section, the B deposition section and the continuous cooling section are all quartz glass tubes, the upper part of the B deposition section is provided with a B deposition section air inlet, the upper part and the middle part of the continuous cooling section are provided with an upper continuous cooling section air inlet and a lower continuous cooling section air inlet, and the lower part of the continuous cooling section is provided with a tail gas discharge outlet.
3. The apparatus for preparing anti-radiation fiber of tungsten and boron by CVD method as claimed in claim 2, wherein all the gas inlets are formed of quartz glass tubes having a spiral structure, and all the gas inlets are provided with a flow regulating valve for regulating the flow rate of gas and a gas filtering device for filtering solid particles in the gas and the raw material gas.
4. The apparatus for preparing W-B radiation-proof fiber by CVD method according to claim 1, wherein the upper threading device is made of quartz glass, the center of one end of the upper threading device is an upper threading hole with a diameter of 0.5mm to 1mm, the length of the upper threading hole is 20mm, and the other end of the upper threading device is an upper tapered ground with a length of 100 mm; the lower wire feeding device is made of quartz glass, a lower wire feeding hole with the diameter of 0.5-1 mm is arranged in the center of one end of the lower wire feeding device, the length of the lower wire feeding hole is 20mm, and a lower conical grinding opening with the length of 100mm is arranged at the other end of the lower wire feeding device.
5. An apparatus for manufacturing a tungstoboron radiation protective fiber by CVD method as claimed in claim 1, characterized in that the reaction tube is made of a quartz glass tube 800mm long, in which: the inner diameter of the quartz glass tube at the tungsten filament cleaning section is 25mm, and the length of the quartz glass tube is 200-300 mm; the boron deposition section quartz glass tube has an inner diameter of 25mm and a length of 300-400 mm; the inner diameter of the continuous cooling section is 25mm, and the length of the continuous cooling section is 100-200 mm.
6. A method for preparing a tungsten-boron radiation-proof fiber by using a CVD method of the device of any one of claims 1 to 5, characterized in that a tungsten wire with a diameter of 10 μm to 15 μm is passed through a reaction tube by a chemical vapor deposition method, and the tungsten wire is heated by a direct current power supply, and elemental boron with a thickness of 10 μm to 20 μm is deposited on the surface of the tungsten wire.
7. The method for preparing the tungsten boron radiation protective fiber by the CVD method according to claim 6, which is characterized by comprising the following steps:
(1) connecting the reaction tube with an upper wire feeding device and a lower wire feeding device, wherein the upper wire feeding device and the lower wire feeding device are tightly connected with the reaction tube;
(2) fixing a tungsten filament disc on the filament releasing device, wherein one end of a tungsten filament enters from an upper filament passing hole and penetrates out from a lower filament passing hole and is bonded on the filament collecting device;
(3) introducing high-purity argon from an air inlet of the upper wire threading device and an air inlet of the lower wire threading device, emptying air in the reactor, wherein the flow of the introduced argon is 0.5-3L/min, and the introduction time is 8-15 min;
(4) after air in the reactor is exhausted, hydrogen is respectively introduced from an air inlet of the upper filament passing device and an air inlet of the lower filament passing device, the flow of the hydrogen introduced from the air inlet of the upper filament passing device is 0.1-0.5L/min, and the flow of the hydrogen introduced from the air inlet of the lower filament passing device is 0.1-0.2L/min;
(5) introducing mixed gas of boron trichloride, hydrogen and argon into an air inlet of the upper boron deposition section of the boron deposition section for boron deposition;
(6) hydrogen is respectively introduced into an upper continuous cooling section air inlet and a lower continuous cooling section air inlet of the continuous cooling section for realizing continuous cooling, the flow rate of the hydrogen introduced into the upper part of the continuous cooling section is 0.2-0.5L/min, and the flow rate of the hydrogen introduced into the middle part of the continuous cooling section is 0.5-1L/min;
(7) starting a filament collecting device, wherein the rotating speed of a filament collecting wheel of the filament collecting device is 3-10 rpm;
(8) starting a direct current power supply to heat the tungsten wire, controlling the temperature of a tungsten wire cleaning section to be 500-800 ℃, the temperature of a boron deposition section to be 1100-1350 ℃, and the temperature of a continuous cooling section to be 1250 +/-30-300 +/-30 ℃;
(9) and after the temperature of each section reaches a specified range for 5-15 min, formally starting to wind the filaments.
8. The CVD method for preparing W-B radiation-proof fiber according to claim 7, wherein in the mixed gas in the step (5), by volume percentage, boron trichloride is 30-40%, hydrogen is 30-40%, and the balance is argon, and the flow rate of the mixed gas is 1.5-3L/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011349520.5A CN112481601A (en) | 2020-11-26 | 2020-11-26 | Device and method for preparing tungsten-boron radiation-proof fiber by CVD method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011349520.5A CN112481601A (en) | 2020-11-26 | 2020-11-26 | Device and method for preparing tungsten-boron radiation-proof fiber by CVD method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112481601A true CN112481601A (en) | 2021-03-12 |
Family
ID=74935258
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011349520.5A Pending CN112481601A (en) | 2020-11-26 | 2020-11-26 | Device and method for preparing tungsten-boron radiation-proof fiber by CVD method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112481601A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1071398A (en) * | 1991-10-05 | 1993-04-28 | 石家庄市电子加工技术研究所 | High-frequency thermal reactor for silicon carbide fibre |
| CN2283068Y (en) * | 1996-11-25 | 1998-06-03 | 中国科学院金属研究所 | Chemical vapour deposition silicon carbide fibre reactor |
| CN102180706A (en) * | 2011-03-03 | 2011-09-14 | 西北工业大学 | Method for preparing hexagonal boron nitride interface coating |
| CN106367849A (en) * | 2016-02-22 | 2017-02-01 | 河北陆元新材料科技有限公司 | Continuous silicon carbide fiber production system |
| CN106756873A (en) * | 2016-11-15 | 2017-05-31 | 中国科学院金属研究所 | A kind of DC heating method prepares the short route integrated apparatus and method of continuous tungsten core SiC fibers |
-
2020
- 2020-11-26 CN CN202011349520.5A patent/CN112481601A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1071398A (en) * | 1991-10-05 | 1993-04-28 | 石家庄市电子加工技术研究所 | High-frequency thermal reactor for silicon carbide fibre |
| CN2283068Y (en) * | 1996-11-25 | 1998-06-03 | 中国科学院金属研究所 | Chemical vapour deposition silicon carbide fibre reactor |
| CN102180706A (en) * | 2011-03-03 | 2011-09-14 | 西北工业大学 | Method for preparing hexagonal boron nitride interface coating |
| CN106367849A (en) * | 2016-02-22 | 2017-02-01 | 河北陆元新材料科技有限公司 | Continuous silicon carbide fiber production system |
| CN106756873A (en) * | 2016-11-15 | 2017-05-31 | 中国科学院金属研究所 | A kind of DC heating method prepares the short route integrated apparatus and method of continuous tungsten core SiC fibers |
Non-Patent Citations (1)
| Title |
|---|
| K.SINGHA ET AL.: ""硼纤维的研究概述"", 《国际纺织导报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103046165B (en) | Preparation method of continuous filament of asphalt-based carbon fiber | |
| US20020172316A1 (en) | Divertor filtering element for a tokamak nuclear fusion reactor; divertor employing the filtering element; and tokamak nuclear fusion reactor employing the divertor | |
| KR101526305B1 (en) | Multi-layered metal-ceramic composite nuclear fuel cladding tube | |
| CN112481601A (en) | Device and method for preparing tungsten-boron radiation-proof fiber by CVD method | |
| CN104844222B (en) | Method for preparing boron nitride fiber cloth by using precursor conversion | |
| CN112885518B (en) | Continuous alumina fiber reinforced aluminum-based cable core and preparation method and equipment thereof | |
| CN105271706B (en) | A kind of high pressure argon gas fibre drawing furnace | |
| CN101602107A (en) | The method of rare refractory metal of a kind of laser spheroidization and the non-spherical powder of carbide alloy | |
| EP3327729B1 (en) | System for continuously preparing coated particles in large scale | |
| US3867191A (en) | Carbon-boron surfaced carbon filament | |
| CN111479377A (en) | D-D neutron tube target film protective layer | |
| CN111231441A (en) | Multifunctional nuclear radiation protection double-layer fabric and preparation method thereof | |
| CN106120126A (en) | A kind of preparation method of gas burner metal fibre interlacement | |
| CN115538157A (en) | Method for producing carbon nano tube modified silicon carbide fiber by continuous vapor deposition method | |
| CN111916227B (en) | Metal-coated fuel and preparation method thereof | |
| CN102127830B (en) | Production process for 15000D high-modulus and high-strength terylene industrial interlaced yarn | |
| CN106399977B (en) | Production system of coating silicon carbide composite fiber | |
| CN211897250U (en) | Maintain convenient polyester fiber steam heating device | |
| CN103361592B (en) | A kind of method improving high-temperature corrosion resistance of zirconium alloy pipe | |
| CN1332082C (en) | Graphitization preparation process for carbon fiber by using radio frequency method and production system thereof | |
| CN106948031A (en) | The preparation method of ultra-fine tow silicon carbide fibre | |
| CN106747453B (en) | High-temperature cracking treatment method for SiC composite fiber winding cladding | |
| CN116446099B (en) | Production process of alloy steel cloth T-shirt | |
| WO2022103297A1 (en) | Method for manufacturing a fuel rod cladding tube | |
| CN206985689U (en) | A kind of funnel |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210312 |
|
| RJ01 | Rejection of invention patent application after publication |