CN114724759A - Armored signal cable for self-powered neutron detector and preparation method thereof - Google Patents
Armored signal cable for self-powered neutron detector and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
- H01B7/29—Protection against damage caused by extremes of temperature or by flame
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/22—Polishing of heavy metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/06—Insulating conductors or cables
- H01B13/065—Insulating conductors with lacquers or enamels
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/02—Disposition of insulation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
- H01B7/28—Protection against damage caused by moisture, corrosion, chemical attack or weather
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
- H01B7/28—Protection against damage caused by moisture, corrosion, chemical attack or weather
- H01B7/2806—Protection against damage caused by corrosion
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses an armored signal cable for a self-powered neutron detector and a preparation method thereof. The self-powered neutron detectionThe armored signal cable comprises a sleeve, an insulating porcelain column and a conductor signal core wire; the insulating knob insulator wraps the outer side of the conductor signal core wire, and the sleeve is sleeved on the outer side of the insulating knob insulator; the sleeve and the conductor signal core wire are made of Inconel 600 alloy, and the insulating knob insulator is made of high-purity electric melting MgO powder. The wire diameter of the armored signal cable is 1.00-1.50 mm, the surface roughness is not more than Ra1.6 mu m, and the room-temperature insulation resistance is more than 1.20 multiplied by 1013Omega.m, 400 ℃ insulation resistance > 2.50 x 108Omega.m, the length of a single branch is 80-120 m, and the using requirements of the armored signal cable for the self-powered neutron detector in the high-temperature and irradiation environment of the nuclear reactor are met.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to an armored signal cable for a self-powered neutron detector and a preparation method thereof.
Background
The self-powered neutron detector is a main detection element for on-line monitoring of the neutron fluence rate of a nuclear reactor and is used for measuring strong neutrons in the reactor. The on-line reactor core power density and distribution are generated by generating signal current, thereby ensuring the safe and effective operation of the nuclear reactor. The armored signal cable is a key component of a self-powered neutron detector, and the main structure of the armored signal cable is composed of a sleeve, an insulating layer and a conductor signal core wire. Under the working conditions of high temperature and high pressure of a reactor core, irradiation and corrosion, the armored signal cable is required to have higher insulation resistance and high temperature stability.
At present, the room temperature insulation resistance of an armored signal cable imported from foreign countries reaches more than or equal to 1013Omega, m, 400 ℃ insulation resistance is more than or equal to 108Omega, m; the length of the single cable is required to be 80-200 m; the cable wire diameter is required to be 1.00-1.50 mm, and the precision is biasedThe difference is +/-0.01 mm; the surface roughness requirement is less than or equal to Ra1.6 mu m. Compared with the armored signal cable for the self-powered neutron detector produced in China and imported from abroad, the armored signal cable for the self-powered neutron detector still has gaps in insulation resistance, high temperature resistance, irradiation resistance, single-branch length, size precision and sleeve integrity, and particularly, the insulation resistance of the armored signal cable in China is 1-2 orders of magnitude lower than that of the armored signal cable in China and the advanced level in the foreign country. Due to the difference, the armored signal cable produced in China cannot well meet the use scene of the self-powered neutron detector, and needs to be imported from abroad, so that the development of the armored signal cable technology for the self-powered neutron detector is restricted.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to solve the problems that the insulation resistance, the single-branch length, the dimensional accuracy, the surface roughness and the like of the existing armored signal cable for the self-powered neutron detector cannot meet the use requirements and need to be imported from foreign countries, and provides the armored signal cable for the self-powered neutron detector and the preparation method thereof.
In order to solve the technical problem, the invention adopts the following technical scheme:
an armored signal cable for a self-powered neutron detector comprises a sleeve, an insulating knob insulator and a conductor signal core wire; the insulating knob insulator wraps the outer side of the conductor signal core wire, and the sleeve is sleeved on the outer side of the insulating knob insulator; the sleeve and the conductor signal core wire are made of Inconel 600 alloy, and the insulating knob insulator is made of high-purity electric melting MgO powder.
The Inconel 600 alloy comprises main alloy elements of Ni, Cr and Fe, small materials of C, Mn, Al and Si, and inevitable impurity elements of Cu, S and P; the components are as follows by weight:
ni: more than or equal to 72 parts;
cr: 14.0-17.0 parts;
fe: 6.0-10.0 parts;
the small materials C, Mn, Al and Si are less than or equal to 1.0 part;
the inevitable impurity Cu + S + P is less than or equal to 0.05 part.
Further, the small materials and inevitable impurities comprise the following components in parts by weight:
c: less than or equal to 0.05 portion;
mn: less than or equal to 1.0 portion;
al: less than or equal to 0.30 portion;
si: less than or equal to 0.50 portion;
cu: less than or equal to 0.05 portion;
s: less than or equal to 0.015 part;
p: less than or equal to 0.015 portion.
In the high-purity electric melting MgO powder, the content of MgO is more than 99.8 percent.
The invention also provides a preparation method of the armored signal cable for the self-powered neutron detector, which comprises the following steps,
s1, selecting an Inconel 600 alloy sleeve with the diameter of 8-10 mm, the wall thickness of 2mm and the length of 5 m; selecting Inconel 600 alloy wires with the wire diameter of phi 2-phi 2.5mm as conductor signal core wires, and performing cleaning pretreatment on the sleeve and the conductor signal core wires for later use.
S2, preparing the insulating porcelain column by adopting high-purity electric melting MgO powder.
S3, assembling in a closed ultra-clean room, wherein the grade of the clean room is hundred thousand grade, the temperature is controlled to be 18-26 ℃, and the relative humidity is controlled to be 20-28%; sleeving an insulating knob insulator on a conductor signal core wire, and then putting the insulating knob insulator into a sleeve to assemble a cable; the grade of the clean room is of a hundred thousand grade, namely, particles in each cubic meter of the clean room are controlled within 10 ten thousand, so that the assembly process is ensured to be clean, and the influence of excessive impurities on the performance of the cable is avoided.
S4, performing cold drawing on the assembled cable, performing repeated drawing and intermediate annealing, drawing to obtain an armored signal cable with the diameter of 1.00-1.50 mm, and sealing the end of the armored signal cable by using epoxy resin glue after drawing.
S5, carrying out continuous electrolytic polishing cleaning in a NaOH solution with the concentration of 5-12% by weight, and drying to obtain the armored signal cable for the self-powered neutron detector.
Further, in step S1, the cleaning pretreatment is performed by using 5% HF and 15% HNO3The mixed solution of (a) is subjected to acid washing, wherein, HF: HNO3The volume ratio of (A) to (B) is 2: 8; after acid washing, carrying out alkali washing neutralization by using 5-12% NaOH solution, and then using high pressureWashing with deionized water; after the washing is finished, the inner wall and the outer wall of the sleeve and the conductor signal core wire are scrubbed by dipping alcohol on cotton gauze until the gauze is not obviously black.
Further, the preparation of the Inconel 600 alloy sleeve comprises the following steps,
vacuum induction melting: the main alloy elements are put into a crucible and then placed in vacuum induction melting, and the crucible is vacuumized to be better than 10 DEG- 1Opening the vacuum induction furnace after Pa, and refining for 15-30 min after main alloy elements are completely melted; then adding small materials to be completely melted, and refining for 10-15 min; and (3) standing the melt after refining, adjusting the temperature to 1500-1560 ℃, casting the melt into a round bar, cooling to room temperature, and taking out.
Vacuum consumable remelting: remelting the round bar serving as an electrode bar; the smelting vacuum degree is 0.10-2.0 Pa, the voltage is 20-40V, the current is 3000-9000A, the smelting rate is 2.5-4.8 kg/min, and the cooling water pressure is 6000-8000 MPa; and (4) enabling the molten liquid drops of the electrode rod to flow into the crucible for recrystallization to obtain the alloy ingot.
Forging and cogging: and (3) deforming, forging and cogging the alloy ingot by using a forging press, heating the alloy ingot at 1080-1150 ℃, keeping the temperature for 60-90 min, starting forging at a temperature of not less than 1080 ℃, finishing forging at a temperature of not less than 950 ℃, and processing the alloy ingot into an alloy rod with a diameter of 60-75 mm.
Hot rolling and pipe penetrating: heating the alloy rod and then penetrating the alloy rod into a hollow thick-wall pipe on a puncher; heating at 1000-1150 deg.c for 60-90 min; after the pipe is penetrated, hot rolling the hollow thick-wall pipe to a hollow thin-wall pipe with the diameter of 35-40 mm multiplied by 3.0mm on a continuous pipe rolling unit; wherein the continuous rolling speed is 5-7 m/min, the roller rotating speed is 80-120 r/mim, and the final rolling temperature is more than or equal to 850 ℃.
Cold rolling and cold drawing: controlling the cold rolling speed at 3-5 m/min, processing to phi 18-20 mm multiplied by 2.0mm, annealing for 25-35 min at 1050-1100 ℃ by using a mesh belt type annealing furnace, continuously drawing to phi 8-10 mm multiplied by 1.0mm, and annealing for 25-35 min at 1050-1100 ℃ by using the mesh belt type annealing furnace to obtain the cold-processed pipe.
Surface finishing: comprises straightening and polishing the inner wall and the outer wall; straightening the cold-processed pipe by a six-roller straightening machine at a straightening speed of 0.5-1 m/min,the straightening precision is less than or equal to 1.0 mm/m; performing inner and outer wall polishing on the pipe by adopting electrochemical polishing at the temperature of 60-85 ℃ and using phosphoric acid and sulfuric acid as electrolyte, wherein the concentration of the phosphoric acid is 35%, the concentration of the sulfuric acid is 40%, the volume ratio of the phosphoric acid to the sulfuric acid is 7:3, and the current density is 25-45A/dm2And polishing for 10-20 min to obtain the Inconel 600 alloy casing.
The preparation of the Inconel 600 alloy wire comprises the following steps,
vacuum induction melting: the main alloy elements are put into a crucible and then placed in vacuum induction melting, and the crucible is vacuumized to be better than 10 DEG- 1Opening the vacuum induction furnace after Pa, and refining for 15-30 min after main alloy elements are completely melted; then adding small materials to be completely melted, and refining for 10-15 min; and (3) standing the melt after refining, adjusting the temperature to 1500-1560 ℃, casting the melt into a round bar, cooling to room temperature, and taking out.
Vacuum consumable remelting: remelting the round bar serving as an electrode bar; the smelting vacuum degree is 0.10-2.0 Pa, the voltage is 20-40V, the current is 3000-9000A, the smelting rate is 2.5-4.8 kg/min, and the cooling water pressure is 6000-8000 MPa; and (4) enabling the molten liquid drops of the electrode rod to flow into the crucible for recrystallization to obtain the alloy ingot. The purpose of vacuum consumable remelting is to effectively remove trace elements such as gas (oxygen, nitrogen and hydrogen) and impurities P, S in the alloy, and simultaneously improve the cooling strength of a molten pool by controlling the cooling water pressure, so that the grain refining effect of the alloy is better, the grain size is reduced, the number is increased, the distribution of alloy elements is homogenized, the processability of the alloy is improved, and the influence on subsequent forging is avoided.
Forging and cogging: and (3) deforming, forging and cogging the alloy ingot by using a forging press, heating the alloy ingot at 1080-1150 ℃, keeping the temperature for 60-90 min, starting forging at a temperature of not less than 1080 ℃, finishing forging at a temperature of not less than 950 ℃, and processing the alloy ingot into an alloy rod with a diameter of 60-75 mm.
Hot rolling: heating the alloy bar, and then carrying out hot rolling in a hot rolling mill, wherein the single-pass deformation processing rate is 15-25%, the heating temperature is 1000-1150 ℃, and the heat preservation time is 60-90 min; processing the alloy bar with the diameter of 60-75 mm to the diameter of 8-10 mm, wherein the finishing temperature is more than or equal to 850 ℃.
Drawing the wire: and (3) drawing the alloy bar with the diameter of 8-10 mm into alloy wires with the diameter of 2-2.5 mm, carrying out intermediate annealing once when the drawing speed is 8-10 m/min and the pass accumulated deformation reaches 55-75%, and annealing for 25-35 min at 1050-1100 ℃ by adopting a mesh belt type annealing furnace in the intermediate annealing to obtain the processed alloy wires with the diameter of 2-2.5 mm.
Surface polishing and cleaning: and (3) continuously carrying out electrolytic polishing and cleaning on alloy wires with the diameter of 2-2.5 mm, carrying out electrolytic current of 5A-10A, carrying out NaOH solution with the alkali liquor concentration of 5-10 wt%, and carrying out wire winding at the speed of 10-15 m/min to obtain the alloy wires serving as conductor signal core wires.
Further, in step S2, the method for preparing the insulating porcelain post includes,
(1) high-energy ball milling: adding high-purity fused MgO powder into a ball milling tank, wherein the weight ratio of material balls is 1: 0.25-0.5, the ball milling speed is 1200-1800 r/min, and the ball milling time is 6-10 h.
(2) Precision molding: adding the forming agent into high-purity electric melting MgO powder, stirring and mixing uniformly, then putting into a die, and preparing the insulating knob insulator in an oil pressure forming mode; wherein the pressing pressure is 50-120 MPa, the pressure maintaining time is 10-15 s, the outer diameter of the prepared insulating porcelain cylinder blank is phi 5.5-phi 7.5mm in size, the inner diameter is phi 2.5-phi 3.0mm, and the length is 50 mm; the forming agent is prepared from absolute ethyl alcohol and glycerol according to the volume of 1:1, and the weight ratio of the high-purity electric melting MgO powder to the forming agent is 1: 0.01-0.05.
(3) And (3) vacuum sintering: putting the prepared insulating porcelain cylinder blank into a vacuum sintering furnace for sintering; wherein the vacuum degree is more than or equal to 1.0 multiplied by 10 < -2 > Pa; preserving heat for 2-3 h at 400-500 ℃, and preserving heat for 4-6 h at 1200-1300 ℃, wherein the temperature rise speed is 5-9 ℃/min; and after heating, cooling to room temperature along with the furnace, taking out to obtain the insulating knob insulator, and putting the insulating knob insulator into an oven at the temperature of 45-65 ℃ for later use.
Further, in step S3, a polycrystalline die is used as the wire-drawing die, and chlorinated paraffin is used as the lubricant; the single-pass deformation processing amount is 10-15%, when the pass accumulated deformation amount reaches 40-55%, intermediate annealing treatment is carried out, the annealing temperature is 900-1100 ℃, and the annealing time is 30-40 min; the surface of the cable was cleaned of the lubricant with alcohol before annealing.
Further, in step S4, the electrolytic current is 6-12A, the filament winding speed is 4-7 m/S, and the drying temperature is 50-60 ℃.
Compared with the prior art, the invention has the following advantages:
1. according to the armored signal cable for the self-powered neutron detector, the sleeve and the conductor signal core wire are made of Inconel 600 alloy, and the armored signal cable has high temperature corrosion resistance, irradiation resistance and oxidation resistance; the insulating ceramic columns are made of high-purity electric melting MgO powder, have high insulating resistance and are suitable for high-temperature and irradiation environments in a nuclear reactor. The wire diameter of the armored signal cable is 1.00-1.50 mm, the surface roughness is not more than Ra1.6 mu m, and the room-temperature insulation resistance is more than 1.20 multiplied by 1013Omega.m, 400 ℃ insulation resistance > 2.50 x 108Omega.m, the length of a single branch is 80-120 m, the performance index of the armored signal cable imported from foreign countries is achieved, and the using requirement of the armored signal cable for the self-powered neutron detector in a high-temperature and irradiation environment of a nuclear reactor can be met.
2. In the preparation method provided by the invention, the sleeve and the conductor signal core wire are subjected to cleaning treatment by adopting a chemical and physical combined method, so that the surfaces of the sleeve and the conductor signal core wire are ensured to be in a clean state, and the pollution of metal oxide skin and residual ions is avoided. The insulating ceramic column is prepared from the high-purity electro-melting MgO powder in the modes of precision forming, mold precision control and high-temperature calcination, the coaxiality and the density of the insulating layer are improved, the structural size of the insulating ceramic column is easy to control, and the high-temperature insulating property of the MgO insulating ceramic column is exerted to the maximum extent. The assembly process is completely carried out in a closed clean room, the temperature and the humidity in the clean room are strictly controlled, the phenomenon that water vapor is adsorbed on MgO insulating knob insulator due to overlarge humidity is avoided, the oxidation of the inner wall surfaces of the sleeve and the conductor signal core wire is brought in the subsequent annealing process, and the surfaces of the sleeve and the conductor signal core wire are ensured to be in a clean state. Therefore, the prepared armored signal cable for the self-powered neutron detector has high insulation resistance and high-temperature stability, and can meet the use requirements of the armored signal cable for the self-powered neutron detector in the high-temperature and irradiation environment of a nuclear reactor.
Drawings
Fig. 1 is a schematic structural diagram of an armored signal cable for a self-powered neutron detector according to the invention.
Detailed Description
The invention will be further explained with reference to the drawings and the embodiments.
Example 1
A preparation method of an armored signal cable for a self-powered neutron detector comprises the following steps,
s1, selecting an Inconel 600 alloy sleeve with the diameter of 8mm, the wall thickness of 2mm and the length of 5m as the sleeve. The conductor signal core wire is made of an Inconel 600 alloy wire with the diameter of 2.3 mm. The surfaces of the sleeve and the conductor signal core wire are required to be smooth and have no defects such as cracks, burrs and the like. Cleaning and pretreating the sleeve and the conductor signal core wire by a chemical and physical combined method, and firstly, acid cleaning (with the concentration of 5 percent HF and 15 percent HNO)3A mixed liquor, wherein HF: HNO3The volume ratio of the conducting wire to the conducting wire is 2: 8), after acid washing is finished, alkali washing neutralization (NaOH solution with the concentration of 5%) is carried out, then high-pressure deionized water is used for washing, after washing is finished, cotton gauze is used for dipping alcohol to scrub the inner wall and the outer wall of the sleeve and the conductor signal core wire until the gauze is not obviously black.
The components and the mixture ratio of the Inconel 600 alloy casing are shown in Table 1, and the preparation method comprises the following steps,
vacuum induction melting: smelting the alloy by adopting a 500kg vacuum induction smelting furnace, loading large Ni, Fe and Cr materials into a crucible, loading small C, Mn, Al and Si materials into a charging hopper, vacuumizing to 0.6Pa and 35kw, carrying out primary refining for 25min, slowly transmitting power from small to large until the alloy is completely melted, then adding the small C, Mn, Al and Si materials, carrying out secondary refining for 12min, fully and electromagnetically stirring in the refining process, standing molten steel, regulating the temperature to about 1530 ℃, casting into a round bar, cooling the temperature to room temperature, taking out the round bar, and taking the smelted round bar as an electrode bar for vacuum consumable remelting.
Vacuum consumable remelting: remelting the round bar by adopting a vacuum consumable arc furnace, controlling the smelting vacuum degree to be 0.3Pa, electrifying and arcing the electrode bar, controlling the voltage to be 32V and the current to be 7500A, slowly melting the electrode bar, and enabling the melted liquid drops to flow into a crucible for recrystallization to obtain the Inconel 600 alloy ingot.
Forging and cogging: and (3) forging and cogging the consumable remelting alloy ingot in a large deformation mode by using a forging press, heating to 1100 ℃, keeping the temperature for 80min, beginning forging to 1100 ℃, and finishing forging to 950 ℃, and processing the alloy ingot into the Inconel 600 alloy rod with the diameter of 60 mm. Through ultrasonic flaw detection (UT) nondestructive testing, the alloy ingot after forging and cogging has no cracks on the surface and no defects inside, and meets the requirements of subsequent processing.
Hot rolling and pipe penetrating: and (3) heating the forged Inconel 600 alloy rod, and then penetrating the heated Inconel 600 alloy rod into a hollow thick-wall pipe on a perforating machine, wherein the heating temperature is 1100 ℃, and the heat preservation time is 80 min. After the pipe is penetrated, the hollow thick-wall pipe is hot-rolled to a hollow thin-wall pipe with the diameter of 35mm multiplied by 3.0mm on a continuous pipe rolling unit, the continuous rolling speed is 5m/min, the roller rotating speed is 90r/mim, and the final rolling temperature is 850 ℃.
Cold rolling and cold drawing: cold working the hollow thin-wall pipe by rolling and drawing on a cold rolling cold-drawing unit, controlling the cold rolling speed at 4m/min, degreasing and deoiling by using a hydrocarbon cleaning agent when the pipe is machined to phi 18mm multiplied by 2.0mm, and then annealing by using a mesh belt type annealing furnace, wherein the annealing temperature is controlled at 1050 ℃ and the annealing time is 35 min. Continuously drawing until the diameter is 8mm multiplied by 1.0mm, degreasing and deoiling by using a hydrocarbon cleaning agent, and finally annealing by using a mesh belt type annealing furnace, wherein the annealing temperature is controlled at 1050 ℃ and the annealing time is 35 min.
Surface finishing: and (3) straightening the cold-processed pipe by adopting a six-roller straightening machine, wherein the straightening speed is 0.6m/min, and the straightening precision is 1.0 mm/m. Adopting electrochemical polishing to polish the inner wall and the outer wall of the pipe, wherein the temperature is 80 ℃, the electrolyte is phosphoric acid and sulfuric acid, the concentration of the adopted phosphoric acid is 35 percent, the concentration of the sulfuric acid is 40 percent, the volume ratio is 7:3, and the current density is 45A/dm2And polishing time is 15 min. And after polishing, immersing the sleeve into prepared deionized water to remove electrolyte remained on the surface, treating the sleeve in an ultrasonic cleaning instrument for 12min, and then putting the sleeve into a drying oven to carry out drying treatment to obtain the sleeve for the self-powered neutron detector.
The prepared sleeve is detected: the total content of O + N + H elements in the chemical composition of the sleeve is 87 ppm. The sleeve dimensions were measured to be 8mm x 1.0 mm. The surface of the sleeve has no cracks and white spots. The quality grade of the internal defects of the casing is A grade. And no leakage is detected by helium mass spectrum pressurization of the sleeve. The tensile strength of the sleeve is 648MPa, the yield strength is 285MPa, the elongation is 54.7%, the grain size grade G is 3.0, and the surface roughness is Ra1.2 mu m.
The Inconel 600 alloy wire is prepared by the steps of vacuum induction melting, vacuum consumable remelting, forging cogging, hot rolling, wire drawing and surface polishing and cleaning as shown in Table 1. Wherein, in the preparation process of the Inconel 600 alloy wire, the three steps of vacuum induction melting, vacuum consumable remelting and forging cogging are consistent with the preparation of the Inconel 600 alloy sleeve, and the hot rolling, wire drawing and surface polishing cleaning are specifically,
hot rolling: heating the alloy bar, and then carrying out hot rolling in a hot rolling mill, wherein the single-pass deformation processing rate is 15%, the heating temperature is 1150 ℃, and the heat preservation time is 60 min; the alloy bar with the diameter of 75mm is processed to the diameter of 10mm, and the finishing temperature is 850 ℃.
Drawing the wire: drawing the alloy bar with the diameter of 10mm into alloy wire with the diameter of 2.3mm, carrying out intermediate annealing once when the wire drawing speed is 8m/min and the pass accumulated deformation reaches 55%, and annealing for 35min at 1100 ℃ by adopting a mesh belt type annealing furnace to obtain the processed alloy wire with the diameter of 2.3 mm.
Surface polishing and cleaning: alloy wires with the diameter of 2.3mm are cleaned by continuous electrolytic polishing, the electrolytic current is 5A, the concentration of alkali liquor is 5 percent by weight of NaOH solution, and the wire collecting speed is 12 m/min.
S2, preparing the insulating ceramic column by adopting high-purity electric melting MgO powder, wherein the components and the mixture ratio of the high-purity electric melting MgO powder are shown in Table 2. The preparation method comprises the following steps of,
(1) high-energy ball milling: weighing 8kg of high-purity electric melting MgO powder, adding the high-purity electric melting MgO powder into a ball milling tank, wherein the weight ratio of material balls is 1:0.25, the weight of grinding balls is 2kg, the ball milling speed is 1200r/min, the ball milling time is 8h, and taking out the high-purity electric melting MgO powder after the ball milling is finished.
(2) Precision molding: adding a forming agent prepared in advance into high-purity electric melting MgO powder, wherein the forming agent is prepared from absolute ethyl alcohol and glycerol according to the volume of 1:1, the weight ratio of the MgO powder to the forming agent is 1:0.02, putting the uniformly mixed high-purity electric melting MgO powder into a precision die, preparing an insulating knob insulator in an oil pressure forming mode, pressing at 80MPa for 15s, and keeping the pressure for 15s, wherein the size of the prepared insulating knob insulator is phi 5.5mm in outer diameter, phi 2.5mm in inner diameter and 50mm in length.
(3) And (3) vacuum sintering: and (3) sintering the prepared insulating knob insulator in a vacuum sintering furnace, wherein the sintering system is as follows: the vacuum degree is 2.2X 10-2Pa, keeping the temperature at 400 ℃ for 2h, keeping the temperature at 1250 ℃ for 6h, keeping the temperature rise rate at 5 ℃/min, taking out after the heating is finished and cooling to the room temperature along with the furnace, and putting the furnace into an oven for standby, wherein the temperature of the oven is 60 ℃.
S3, assembling the armored signal cable in a closed ultra-clean room, wherein the grade of the clean room is hundred thousand grade, the temperature is controlled at 22 ℃, and the relative humidity is controlled at 24%. The insulating porcelain column 2 is sleeved on the conductor signal core wire 3 and then is arranged in the sleeve 1 to assemble the cable, and the structure of the cable is shown in figure 1.
S4, cold drawing is adopted for the assembled armored signal cable, a polycrystalline die is used as a wire drawing die, chlorinated paraffin is used as a lubricant, the single-pass deformation processing amount is 12%, when the pass accumulated deformation amount reaches 45%, intermediate annealing treatment is carried out, the annealing temperature is 1020 ℃, the annealing time is 40min, and the lubricant on the surface of the armored signal cable is cleaned by alcohol before annealing. Repeatedly drawing and intermediate annealing treatment, drawing to form a fine armored signal cable with the diameter of 1.10mm, and sealing the end by using epoxy resin glue after drawing.
S5, continuously carrying out electrolytic polishing and cleaning on the cable, and carrying out electrolytic current of 8A in NaOH solution with alkali liquor concentration of 7% by weight, wherein the filament winding speed is 6m/S, and the drying temperature is 55 ℃ to obtain the finished cable.
TABLE 1 Inconel 600 alloy chemistry in parts by weight
| Ni | Cr | Fe | Cu | Mn | C | Si | P | S | Cu |
| 75 | 16 | 8 | 0.05 | 0.40 | 0.2 | 0.35 | ≤0.015 | ≤0.015 | ≤0.05 |
TABLE 2 chemical composition of high purity electro-fused MgO powder in mass percent
| MgO | Fe | Mn | B | Cd | S | C |
| ≥99.8 | ≤0.001 | ≤0.001 | ≤0.001 | ≤0.001 | ≤0.005 | ≤0.02 |
The performance indexes of the armored signal cable prepared in the embodiment are as follows:
the wire diameter is 1.10mm measured by a micrometer, the surface roughness is Ra0.6 μm measured by a surface roughness measuring instrument, and the room temperature insulation resistance is 2.32 × 10 measured by a high resistance meter13Omega, m, 400 ℃ insulation resistance of 2.74 multiplied by 108And omega, m, measuring the length of the single armored signal cable to be 102m through a meter wheel.
Example 2
A preparation method of an armored signal cable for a self-powered neutron detector comprises the following steps,
s1, selecting an Inconel 600 alloy sleeve with the diameter of 10mm, the wall thickness of 2mm and the length of 5 m. The conductor signal core wire is made of an Inconel 600 alloy wire with the diameter of 2.5 mm. The surfaces of the sleeve and the conductor signal core wire are required to be smooth and have no defects such as cracks, burrs and the like. Cleaning and pretreating the sleeve and the conductor signal core wire by a chemical and physical combined method, and firstly, acid cleaning (with the concentration of 5 percent HF and 15 percent HNO)3A mixed liquor, wherein HF: HNO3The volume ratio of (2: 8), after the acid cleaning is finished, alkali cleaning neutralization (5% NaOH solution) is carried out, then high-pressure deionized water is used for washing, and the washing is carried outAfter the completion, the inner and outer walls of the sleeve and the conductor signal core wires are scrubbed by dipping alcohol on cotton gauze until the gauze is not obviously black. The Inconel 600 alloy sleeve and the Inconel 600 alloy wire were prepared in the same manner as in example 1.
S2, preparing the insulating porcelain column by adopting high-purity electric melting MgO powder,
(1) high-energy ball milling: weighing 12kg of high-purity electric melting MgO powder, adding the high-purity electric melting MgO powder into a ball milling tank, wherein the weight ratio of material balls to material balls is 1:0.30, the weight of grinding balls is 3.6kg, the ball milling speed is 1600r/min, the ball milling time is 6h, and taking out the high-purity electric melting MgO powder after the ball milling is finished. (2) Precision molding: adding a forming agent prepared in advance into high-purity electric melting MgO powder, wherein the forming agent is prepared from absolute ethyl alcohol and glycerol according to the volume of 1:1, the weight ratio of the MgO powder to the forming agent is 1:0.03, putting the uniformly mixed high-purity electric melting MgO powder into a precision die, preparing an insulating knob insulator in an oil pressure forming mode, pressing at 60MPa for 15s, and keeping the pressure for 15s, wherein the size of the prepared insulating knob insulator is phi 7.5mm in outer diameter, phi 2.7mm in inner diameter and 50mm in length.
(3) And (3) vacuum sintering: and (3) sintering the prepared insulating knob insulator in a vacuum sintering furnace, wherein the sintering system is as follows: vacuum degree of 1.9X 10-2Pa, keeping the temperature at 400 ℃ for 2h, keeping the temperature at 1300 ℃ for 5h, and keeping the temperature at 5 ℃/min, taking out after the heating is finished and cooling to the room temperature along with the furnace, and putting the furnace into an oven for standby, wherein the temperature of the oven is 55 ℃.
S3, assembling the armored signal cable in a closed ultra-clean room, wherein the grade of the clean room is hundred thousand grade, the temperature is controlled at 24 ℃, and the relative humidity is controlled at 22%. And (4) sleeving the insulating porcelain cylinder on a conductor signal core wire, then putting the conductor signal core wire into the sleeve, and assembling the cable.
S4, cold drawing is adopted for the assembled armored signal cable, a polycrystalline die is used as a wire drawing die, chlorinated paraffin is used as a lubricant, the single-pass deformation processing amount is 15%, when the pass accumulated deformation amount reaches 55%, intermediate annealing treatment is carried out, the annealing temperature is 1050 ℃, the annealing time is 35min, and the lubricant on the surface of the armored signal cable is cleaned by alcohol before annealing. Repeatedly drawing and intermediate annealing treatment, drawing to form a fine armored signal cable with the diameter of 1.50mm, and sealing the end by using epoxy resin glue after drawing.
S5, continuously performing electrolytic polishing and cleaning, and electrolyzing in NaOH solution with the alkali liquor concentration of 5 percent by weight at the current of 6A, the filament winding speed of 4m/S and the drying temperature of 60 ℃ to obtain the finished cable.
The performance indexes of the armored signal cable prepared in the embodiment are as follows:
the wire diameter was measured by a micrometer to be 1.50mm, the surface roughness was measured by a surface roughness measuring instrument to be Ra 0.8 μm, and the room-temperature insulation resistance was measured by a high resistance meter to be 2.85X 1013Omega m, insulation resistance at 400 ℃ of 5.47 x 108And omega.m, the length of the single armored signal cable is measured to be 96m by a meter wheel.
Therefore, the wire diameter of the armored signal cable is 1.00-1.50 mm, the surface roughness is not more than Ra1.6 mu m, and the room-temperature insulation resistance is more than 1.20 multiplied by 1013Omega.m, 400 ℃ insulation resistance > 2.50 x 108Omega.m, the length of a single branch is 80-120 m, and the using requirements of the armored signal cable for the self-powered neutron detector in the high-temperature and irradiation environment of the nuclear reactor are met. The performance index of the armored signal cable imported from foreign countries is achieved.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the technical solutions, and those skilled in the art should understand that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all that should be covered by the claims of the present invention.
Claims (10)
1. An armored signal cable for a self-powered neutron detector is characterized by comprising a sleeve, an insulating knob insulator and a conductor signal core wire; the insulating knob insulator wraps the outer side of the conductor signal core wire, and the sleeve is sleeved on the outer side of the insulating knob insulator; the sleeve and the conductor signal core wire are made of Inconel 600 alloy, and the insulating knob insulator is made of high-purity electric melting MgO powder.
2. The armored signal cable for the self-powered neutron detector of claim 1, wherein the Inconel 600 alloy comprises the main alloying elements Ni, Cr, Fe, minor elements C, Mn, Al, Si, and unavoidable impurity elements Cu, S, P; the components are as follows by weight:
ni: more than or equal to 72 parts;
cr: 14.0-17.0 parts;
fe: 6.0-10.0 parts;
the small materials C, Mn, Al and Si are less than or equal to 1.0 part;
the inevitable impurity Cu + S + P is less than or equal to 0.05 part.
3. The armored signal cable for the self-powered neutron detector of claim 2, wherein the small materials and inevitable impurities comprise, in parts by weight:
c: less than or equal to 0.05 portion;
mn: less than or equal to 1.0 portion;
al: less than or equal to 0.30 portion;
si: less than or equal to 0.50 portion;
cu: less than or equal to 0.05 portion;
s: less than or equal to 0.015 part;
p: less than or equal to 0.015 portion.
4. The armored signal cable for the self-powered neutron detector of claim 1, wherein the high purity electro-fused MgO powder has an MgO content of greater than 99.8%.
5. A preparation method of an armored signal cable for a self-powered neutron detector is characterized by comprising the following steps,
s1, selecting an Inconel 600 alloy sleeve with the diameter of 8-10 mm, the wall thickness of 2mm and the length of 5 m; selecting an Inconel 600 alloy wire with the wire diameter of phi 2-phi 2.5mm as a conductor signal core wire, and performing cleaning pretreatment on the sleeve and the conductor signal core wire for later use;
s2, preparing an insulating knob insulator by adopting high-purity electric melting MgO powder;
s3, assembling in a closed ultra-clean room, wherein the grade of the clean room is hundred thousand grade, the temperature is controlled to be 18-26 ℃, and the relative humidity is controlled to be 20-28%; sleeving an insulating knob insulator on a conductor signal core wire, and then putting the insulating knob insulator into a sleeve to assemble a cable;
s4, cold drawing the assembled cable, repeatedly drawing and performing intermediate annealing, drawing to an armored signal cable with the diameter of 1.00-1.50 mm, and sealing the end of the armored signal cable with epoxy resin glue after drawing;
s5, carrying out continuous electrolytic polishing cleaning in a NaOH solution with the concentration of 5-12% by weight, and drying to obtain the armored signal cable for the self-powered neutron detector as claimed in claim 1.
6. The method for preparing the armored signal cable for the self-powered neutron detector of claim 5, wherein in step S1, the cleaning pretreatment is to use HF with a concentration of 5% and HNO with a concentration of 15%3The mixed solution of (a) is subjected to acid washing, wherein, HF: HNO3The volume ratio of (A) to (B) is 2: 8; after acid washing, carrying out alkali washing neutralization by using a 5-12% NaOH solution, and then washing by using high-pressure deionized water; after the washing is finished, the inner wall and the outer wall of the sleeve and the conductor signal core wire are scrubbed by dipping alcohol on cotton gauze until the gauze is not obviously black.
7. The method for preparing an armored signal cable for a self-powered neutron detector of claim 5, wherein the preparation of the Inconel 600 alloy sleeve in step S1 comprises the following steps,
vacuum induction melting: the main alloy elements are put into a crucible and then placed in vacuum induction melting, and the crucible is vacuumized to be better than 10 DEG-1Opening the vacuum induction furnace after Pa, and refining for 15-30 min after main alloy elements are completely melted; then adding small materials to be completely melted, and refining for 10-15 min; standing the melt after refining, adjusting the temperature to 1500-1560 ℃, casting the melt into a round bar, cooling to room temperature, and taking out;
vacuum consumable remelting: remelting the round bar serving as an electrode bar; the smelting vacuum degree is 0.10-2.0 Pa, the voltage is 20-40V, the current is 3000-9000A, the smelting rate is 2.5-4.8 kg/min, and the cooling water pressure is 6000-8000 MPa; the liquid drops melted by the electrode bar flow into the crucible for recrystallization to obtain an alloy ingot;
forging and cogging: performing deformation forging cogging on the alloy ingot by using a forging press, heating the alloy ingot at 1080-1150 ℃, keeping the temperature for 60-90 min, performing initial forging at a temperature of not less than 1080 ℃, and performing final forging at a temperature of not less than 950 ℃, and processing the alloy ingot into an alloy rod with a diameter of 60-75 mm;
hot rolling and pipe penetrating: heating the alloy rod and then penetrating the alloy rod into a hollow thick-wall pipe on a puncher; heating at 1000-1150 deg.c for 60-90 min; after the pipe is penetrated, hot rolling the hollow thick-wall pipe to a hollow thin-wall pipe with the diameter of 35-40 mm multiplied by 3.0mm on a continuous pipe rolling unit; wherein the continuous rolling speed is 5-7 m/min, the roller rotating speed is 80-120 r/mim, and the final rolling temperature is more than or equal to 850 ℃;
cold rolling and cold drawing: controlling the cold rolling speed at 3-5 m/min, processing to phi 18-20 mm multiplied by 2.0mm, annealing for 25-35 min at 1050-1100 ℃ by using a mesh belt type annealing furnace, then continuously drawing to phi 8-10 mm multiplied by 1.0mm, and annealing for 25-35 min at 1050-1100 ℃ by using the mesh belt type annealing furnace to obtain a cold-processed pipe;
surface finishing: comprises straightening and polishing the inner wall and the outer wall; straightening the cold-processed pipe by using a six-roller straightening machine, wherein the straightening speed is 0.5-1 m/min, and the straightening precision is less than or equal to 1.0 mm/m; performing inner and outer wall polishing on the pipe by adopting electrochemical polishing at the temperature of 60-85 ℃ and using phosphoric acid and sulfuric acid as electrolyte, wherein the concentration of the phosphoric acid is 35%, the concentration of the sulfuric acid is 40%, the volume ratio of the phosphoric acid to the sulfuric acid is 7:3, and the current density is 25-45A/dm2And polishing for 10-20 min.
8. The method for preparing a armored signal cable for a self-powered neutron detector as recited in claim 5, wherein in step S2, the insulating knob is prepared by,
(1) high-energy ball milling: adding high-purity fused MgO powder into a ball milling tank, wherein the weight ratio of material balls is 1: 0.25-0.5, the ball milling speed is 1200-1800 r/min, and the ball milling time is 6-10 h;
(2) precision molding: adding the forming agent into high-purity electric melting MgO powder, stirring and mixing uniformly, then putting into a die, and preparing the insulating knob insulator in an oil pressure forming mode; wherein the pressing pressure is 50-120 MPa, the pressure maintaining time is 10-15 s, the outer diameter of the prepared insulating porcelain cylinder blank is phi 5.5-phi 7.5mm in size, the inner diameter is phi 2.5-phi 3.0mm, and the length is 50 mm; wherein the forming agent is prepared from absolute ethyl alcohol and glycerol according to the volume of 1:1, and the weight ratio of the high-purity electric melting MgO powder to the forming agent is 1: 0.01-0.05;
(3) and (3) vacuum sintering: putting the prepared insulating porcelain cylinder blank into a vacuum sintering furnace for sintering; wherein the vacuum degree is more than or equal to 1.0 multiplied by 10-2Pa; preserving heat for 2-3 h at 400-500 ℃, and preserving heat for 4-6 h at 1200-1300 ℃, wherein the temperature rise speed is 5-9 ℃/min; and after heating, cooling to room temperature along with the furnace, taking out to obtain the insulating knob insulator, and putting the insulating knob insulator into an oven at the temperature of 45-65 ℃ for later use.
9. The method for preparing a armored signal cable for a self-powered neutron detector as claimed in claim 5, wherein in step S3, the wire-drawing die uses a polycrystalline die, and the lubricant uses chlorinated paraffin; the single-pass deformation processing amount is 10-15%, when the pass accumulated deformation amount reaches 40-55%, intermediate annealing treatment is carried out, the annealing temperature is 900-1100 ℃, and the annealing time is 30-40 min; the surface of the cable was cleaned of lubricant with alcohol before annealing.
10. The method for preparing the armored signal cable for the self-powered neutron detector as claimed in claim 5, wherein in step S4, the electrolysis current is 6-12A, the filament winding speed is 4-7 m/S, and the drying temperature is 50-60 ℃.
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