CN114717448A - Sleeve for self-powered neutron detector - Google Patents
Sleeve for self-powered neutron detector Download PDFInfo
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- CN114717448A CN114717448A CN202210232422.6A CN202210232422A CN114717448A CN 114717448 A CN114717448 A CN 114717448A CN 202210232422 A CN202210232422 A CN 202210232422A CN 114717448 A CN114717448 A CN 114717448A
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- 229910045601 alloy Inorganic materials 0.000 claims abstract description 72
- 239000000956 alloy Substances 0.000 claims abstract description 72
- 238000005242 forging Methods 0.000 claims abstract description 37
- 229910001055 inconels 600 Inorganic materials 0.000 claims abstract description 25
- 230000006698 induction Effects 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 21
- 238000005097 cold rolling Methods 0.000 claims abstract description 20
- 238000002844 melting Methods 0.000 claims abstract description 19
- 230000008018 melting Effects 0.000 claims abstract description 19
- 238000010622 cold drawing Methods 0.000 claims abstract description 16
- 238000005098 hot rolling Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 9
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 9
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 9
- 230000035515 penetration Effects 0.000 claims abstract description 6
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 5
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 5
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 5
- 229910052802 copper Inorganic materials 0.000 claims abstract description 3
- 238000005275 alloying Methods 0.000 claims abstract 2
- 238000000137 annealing Methods 0.000 claims description 26
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- 238000005498 polishing Methods 0.000 claims description 20
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- 238000003723 Smelting Methods 0.000 claims description 13
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- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 10
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- 230000007547 defect Effects 0.000 claims description 8
- 230000000149 penetrating effect Effects 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- 239000004215 Carbon black (E152) Substances 0.000 claims description 6
- 239000012459 cleaning agent Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000005238 degreasing Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229930195733 hydrocarbon Natural products 0.000 claims description 6
- 150000002430 hydrocarbons Chemical class 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000009659 non-destructive testing Methods 0.000 claims description 5
- 238000005266 casting Methods 0.000 claims description 4
- 239000000498 cooling water Substances 0.000 claims description 4
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- 238000001953 recrystallisation Methods 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 239000000470 constituent Substances 0.000 claims 1
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 13
- 230000001276 controlling effect Effects 0.000 description 8
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- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
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- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 229910001026 inconel Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- 230000001105 regulatory effect Effects 0.000 description 2
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- 238000005482 strain hardening Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 1
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- 238000009616 inductively coupled plasma Methods 0.000 description 1
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Images
Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B19/00—Tube-rolling by rollers arranged outside the work and having their axes not perpendicular to the axis of the work
- B21B19/02—Tube-rolling by rollers arranged outside the work and having their axes not perpendicular to the axis of the work the axes of the rollers being arranged essentially diagonally to the axis of the work, e.g. "cross" tube-rolling ; Diescher mills, Stiefel disc piercers or Stiefel rotary piercers
- B21B19/04—Rolling basic material of solid, i.e. non-hollow, structure; Piercing, e.g. rotary piercing mills
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B37/00—Control devices or methods specially adapted for metal-rolling mills or the work produced thereby
- B21B37/46—Roll speed or drive motor control
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B37/00—Control devices or methods specially adapted for metal-rolling mills or the work produced thereby
- B21B37/74—Temperature control, e.g. by cooling or heating the rolls or the product
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C1/00—Manufacture of metal sheets, metal wire, metal rods, metal tubes by drawing
- B21C1/16—Metal drawing by machines or apparatus in which the drawing action is effected by other means than drums, e.g. by a longitudinally-moved carriage pulling or pushing the work or stock for making metal sheets, bars, or tubes
- B21C1/22—Metal drawing by machines or apparatus in which the drawing action is effected by other means than drums, e.g. by a longitudinally-moved carriage pulling or pushing the work or stock for making metal sheets, bars, or tubes specially adapted for making tubular articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/06—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of tubes or metal hoses; Combined procedures for making tubes, e.g. for making multi-wall tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21D—WORKING OR PROCESSING OF SHEET METAL OR METAL TUBES, RODS OR PROFILES WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21D3/00—Straightening or restoring form of metal rods, metal tubes, metal profiles, or specific articles made therefrom, whether or not in combination with sheet metal parts
- B21D3/02—Straightening or restoring form of metal rods, metal tubes, metal profiles, or specific articles made therefrom, whether or not in combination with sheet metal parts by rollers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J1/00—Preparing metal stock or similar ancillary operations prior, during or post forging, e.g. heating or cooling
- B21J1/04—Shaping in the rough solely by forging or pressing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J1/00—Preparing metal stock or similar ancillary operations prior, during or post forging, e.g. heating or cooling
- B21J1/06—Heating or cooling methods or arrangements specially adapted for performing forging or pressing operations
-
- 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
-
- 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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- 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
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a sleeve for a self-powered neutron detector, which is prepared from Inconel 600 alloy through the working procedures of vacuum induction melting, vacuum consumable remelting, forging cogging, hot rolling tube penetration, cold rolling cold drawing and surface finishing; wherein the Inconel 600 alloy comprises: main alloying elements of Ni, Cr and Fe, small materials of C, Mn, Al and Si, and inevitable impurity elements of Cu, S and P. The surface of the sleeve provided by the invention has no cracks and white spots; judging the quality grade to be A grade by adopting ultrasonic flaw detection (UT); the sleeve has no leakage; the tensile strength is more than or equal to 630MPa, the yield strength is more than or equal to 240MPa, the elongation is more than or equal to 30%, and the average grain size G is 2.0-3.5; the surface roughness is less than or equal to Ra1.6 mu m, and the use requirement of the self-powered neutron detector can be met.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to a sleeve for a self-powered neutron detector.
Background
The self-powered neutron detector is packaged in the reactor core instrument assembly and used for monitoring the neutron fluence rate of the reactor core of the nuclear reactor and generating online reactor core power distribution information by generating signal current, so that the safe and effective operation of the nuclear reactor is ensured. The sleeve is a key material of a shell of the self-powered neutron detector, not only has the functions of fixing and supporting the self-powered neutron detector, but also plays a role in protection and signal current collection. Thus, the performance of the sleeve material will directly affect the service life of the self-powered neutron detector and the accuracy of the measurement. Under complex working conditions of high temperature, high pressure, irradiation and the like of a reactor core, the sleeve material is required to have strong corrosion resistance and oxidation resistance, low thermal conductivity and electric conductivity, large linear expansion coefficient and high breaking strength at high temperature.
At present, the sleeve material for the foreign self-powered neutron detector mainly adopts nickel-based alloy such as Inconnel 600. Although development of nickel-based alloy pipes such as domestic Inconnel 600 and the like has been advanced to a certain extent in recent years, the performance stability is different from that of foreign countries, so that the sleeve material for the self-powered neutron detector still depends on import.
Therefore, it is the research direction of those skilled in the art to provide a sleeve capable of satisfying the use requirement of a self-powered neutron detector.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to solve the problems that the existing domestic Inconnel 600 nickel-based alloy has poor performance and cannot meet the use requirement of a sleeve for a self-powered neutron detector, and provides the sleeve for the self-powered neutron detector.
In order to solve the technical problem, the invention adopts the following technical scheme:
the sleeve is prepared from Inconel 600 alloy through the working procedures of vacuum induction melting, vacuum consumable remelting, forging cogging, hot rolling pipe penetration, cold rolling cold drawing and surface finishing.
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.
Further, the procedures of vacuum induction melting, vacuum consumable remelting, forging and cogging, hot rolling and pipe penetrating, cold rolling and cold drawing and surface finishing are as follows:
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: the alloy ingot is subjected to deformation forging cogging by adopting a forging press, the heating temperature is 1080-1150 ℃, the heat preservation time is 60-90 min, the initial forging temperature is not less than 1080 ℃, the final forging temperature is not less than 950 ℃, and the alloy ingot is processed into an alloy rod with the diameter of 60-75 mm.
Hot rolling and tube threading: 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 adopting 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/dm2Polishing for 10-20 min; and after polishing, immersing the sleeve into prepared deionized water to remove electrolyte remained on the surface, and then carrying out ultrasonic cleaning and drying to obtain the sleeve for the self-powered neutron detector.
Preferably, in the vacuum induction melting, the melt is electromagnetically stirred during the refining.
Preferably, the alloy ingot after forging and cogging is subjected to nondestructive testing by using ultrasonic waves, and the alloy ingot after forging and cogging, which has no surface cracks, no defect inside and uniform forging structure, is selected and processed into an alloy rod. Thus, the subsequent processing requirements can be met.
Preferably, in cold-rolling and cold-drawing, degreasing and deoiling are carried out by using a hydrocarbon cleaning agent before each annealing.
Preferably, after the electrochemical polishing is finished, the pipe is immersed in deionized water to remove electrolyte remaining on the surface, and then the pipe is treated in an ultrasonic cleaner for 10-15 min and then dried.
Compared with the prior art, the invention has the following advantages:
1. the Inconel 600 nickel-based alloy adopted by the sleeve for the self-powered neutron detector provided by the invention has high standard potential of nickel in electrochemistry, has good corrosion resistance and cold and hot processing performances, is easy to form a solid solution with some elements with excellent corrosion resistance, and can work in an oxidizing atmosphere at the temperature of more than 1000 ℃ for a long time compared with the performance of a stainless steel material. Therefore, the requirement of the self-powered neutron detector on the service performance of the sleeve is met.
2. The sleeve provided by the invention is prepared by the processes of vacuum induction melting, vacuum consumable remelting, forging cogging, hot rolling pipe penetration, cold rolling and cold drawing and surface finishing. Due to the adoption of a combined process of duplex vacuum induction melting and vacuum consumable remelting, the strict control of alloy components is realized, gases (oxygen, nitrogen and hydrogen) in the Inconel 600 alloy and trace impurity elements such as P, S are effectively removed, the purity of the alloy is high, alloy grains are refined by controlling the cooling strength, and the distribution of the alloy elements is homogenized. Meanwhile, the two-combined process has the characteristic of short smelting process, and the production cost is reduced compared with a multi-combined smelting process. The chemical components of the Inconel 600 alloy are detected by an inductively coupled plasma mass spectrometer and an oxygen-nitrogen-hydrogen analyzer, the Inconel 600 alloy component requirement is met, the total content of O + N + H elements is less than or equal to 100ppm, and the processability of the Inconel 600 alloy is improved.
3. The size of the sleeve provided by the invention is measured by a vernier caliper as follows: phi is 8-10 mm multiplied by 1.0 mm; the surface quality of the sleeve is subjected to nondestructive testing by adopting eddy current inspection (ET), and the surface of the sleeve has no cracks and white spots; judging the quality grade of the internal defects of the sleeve to be A grade by adopting ultrasonic flaw detection (UT); the integrity of the sleeve is detected by a helium mass spectrometer leak detector in a pressurizing way, and the sleeve has no leakage; the mechanical property of the sleeve is tested by adopting a CMT microcomputer control electronic universal tester, the tensile strength of the pipe is more than or equal to 630MPa, the yield strength is more than or equal to 240MPa, the elongation is more than or equal to 30 percent, and the grain size is detected by adopting a metallographic microscope to have the microscopic average grain size grade G of 2.0-3.5; the surface roughness is measured by a roughness measuring instrument to be less than or equal to Ra1.6 mu m.
Drawings
FIG. 1 is a flow chart of the present invention for manufacturing a sleeve for a self-powered neutron detector.
Fig. 2 is a pictorial view of a cannula made in example 1 of the present invention.
Detailed Description
The invention will be further explained with reference to the drawings and the embodiments.
Example 1
The sleeve for the self-powered neutron detector is prepared from Inconel 600 alloy through the working procedures of vacuum induction melting, vacuum consumable remelting, forging cogging, hot rolling pipe penetration, cold rolling cold drawing and surface finishing. Wherein the Inconel 600 alloy composition is shown in Table 1.
TABLE 1
Ni | Cr | Fe | C | Mn | Al | Si | P | S | Cu |
74 | 16 | 9 | 0.05 | 0.5 | 0.25 | 0.2 | ≤0.015 | ≤0.015 | ≤0.05 |
The preparation method of the sleeve comprises the following steps:
the alloy formulation shown in table 1 was 300kg of Inconel 600 alloy. The preparation process is shown in figure 1.
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 0.4Pa and 40kw, carrying out primary refining for 30min, 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 15min, fully and electromagnetically stirring in the refining process, standing molten steel, casting into round bars when the temperature is regulated to about 1550 ℃, cooling to room temperature, taking out the round bars, and taking the smelted round bars as vacuum consumable remelting electrode bars.
Vacuum consumable remelting: remelting the round bar by using a vacuum consumable arc furnace, wherein the smelting vacuum degree is 0.65Pa, electrifying the electrode bar for arcing, controlling the voltage to be 30V and the current to be 8000A, the smelting speed to be 3.8kg/min, and the cooling water pressure to be 7600 MPa. And slowly melting the electrode rod, and enabling the molten liquid drops to flow into the 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, wherein the heating temperature is 1150 ℃, the heat preservation time is 60min, the initial forging temperature is 1150 ℃, the final forging temperature is 950 ℃, and the alloy ingot is processed into the Inconel 600 alloy rod with the diameter of 75 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 1150 ℃, and the heat preservation time is 60 min. After the pipe is penetrated, the hollow thick-wall pipe is hot-rolled to a hollow thin-wall pipe with the diameter of 40mm multiplied by 3.0mm on a continuous pipe rolling unit, the continuous rolling speed is 7m/min, the roller rotating speed is 120r/mim, and the final rolling temperature is 850 ℃.
Cold rolling and cold drawing: cold working the hollow thin-walled tube by rolling and drawing on a cold rolling and drawing unit, controlling the cold rolling speed at 5m/min, degreasing and deoiling by using a hydrocarbon cleaning agent when the tube is machined to be phi 20mm multiplied by 2.0mm, and then annealing by using a mesh belt type annealing furnace, wherein the annealing temperature is controlled at 1080 ℃ and the annealing time is 30 min. Continuously drawing until the diameter is 10mm 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 30 min.
Surface finishing: including straightening and inner and outer wall polishing. And (3) straightening the cold-processed pipe by adopting a six-roller straightening machine, wherein the straightening speed is 0.8m/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 40A/dm2And polishing time is 20 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 15min, 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 cannula prepared in this example is shown in figure 2.
The casing provided by the embodiment is detected as follows: the total content of O + N + H elements in the chemical composition of the sleeve is 92 ppm. The cannula dimensions were measured as phi 10mm 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 655MPa, the yield strength is 278MPa, the elongation is 46.2 percent, the grain size grade G is 2.5, and the surface roughness is Ra0.7 mu m.
Example 2
The sleeve for the self-powered neutron detector is prepared from Inconel 600 alloy through the working procedures of vacuum induction melting, vacuum consumable remelting, forging cogging, hot rolling pipe penetration, cold rolling cold drawing and surface finishing. Wherein the Inconel 600 alloy composition is shown in Table 2.
TABLE 2
Ni | Cr | Fe | C | Mn | Al | Si | P | S | Cu |
75 | 16 | 8 | 0.05 | 0.40 | 0.2 | 0.35 | ≤0.015 | ≤0.015 | ≤0.05 |
The preparation method of the sleeve comprises the following steps:
the alloy proportioning of 200kg Inconel 600 alloy is shown in Table 2.
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 remelted alloy ingot in a large deformation manner by adopting a forging press, wherein the heating temperature is 1100 ℃, the heat preservation time is 80min, the initial forging temperature is 1100 ℃, the final forging temperature is 950 ℃, and the alloy ingot is processed 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 tube threading: 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-walled tube by rolling and drawing on a cold rolling and drawing unit, controlling the cold rolling speed at 4m/min, degreasing and deoiling by using a hydrocarbon cleaning agent when the tube 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: including straightening and inner and outer wall polishing. 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 casing provided by the embodiment is detected as follows: the total content of O + N + H elements in the chemical composition of the sleeve is 87 ppm. The cannula dimensions were measured to 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.
Therefore, the sleeve provided by the invention has the advantages of small caliber, good mechanical property and surface quality stability, and can meet the requirement of a self-powered neutron detector on the use performance of the sleeve.
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 (8)
1. The sleeve for the self-powered neutron detector is characterized by being prepared from Inconel 600 alloy through the working procedures of vacuum induction melting, vacuum consumable remelting, forging cogging, hot rolling pipe penetration, cold rolling, cold drawing and surface finishing.
2. The thimble for a self-powered neutron detector of claim 1, wherein the Inconel 600 alloy includes the major alloying elements Ni, Cr, Fe, minor constituents 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 sleeve 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 sleeve for a self-powered neutron detector of claim 1, wherein the vacuum induction melting, vacuum consumable remelting, forging cogging, hot rolling tube threading, cold rolling cold drawing and surface finishing processes are as follows:
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 all main alloy elements are 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/dm2Polishing for 10-20 min; and after polishing, immersing the sleeve into prepared deionized water to remove electrolyte remained on the surface, and then carrying out ultrasonic cleaning and drying to obtain the sleeve for the self-powered neutron detector.
5. The bushing for a self-powered neutron detector of claim 4, wherein the melt is electromagnetically stirred during refining in vacuum induction melting.
6. The bushing for a self-powered neutron detector of claim 4, wherein the alloy ingot after forging and cogging is subjected to nondestructive testing by using ultrasonic waves during forging and the alloy ingot after forging and cogging having no surface cracks, no defect inside and uniform forged structure is selected and processed into an alloy rod.
7. The sleeve for the self-powered neutron detector of claim 4, wherein in cold rolling and cold drawing, degreasing is performed with a hydrocarbon cleaning agent before each annealing.
8. The bushing for the self-powered neutron detector of claim 4, wherein after the electrochemical polishing is finished, the pipe is immersed in deionized water to remove electrolyte remaining on the surface, and then is dried after being treated in an ultrasonic cleaner for 10-15 min.
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CN103962411A (en) * | 2013-01-31 | 2014-08-06 | 宝钢特钢有限公司 | GH3600 alloy fine thin-walled seamless pipe manufacturing method |
CN108456807A (en) * | 2017-12-19 | 2018-08-28 | 重庆材料研究院有限公司 | A kind of nickel material of high temperature resistant molten caustic (soda) corrosion |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN103962411A (en) * | 2013-01-31 | 2014-08-06 | 宝钢特钢有限公司 | GH3600 alloy fine thin-walled seamless pipe manufacturing method |
CN108456807A (en) * | 2017-12-19 | 2018-08-28 | 重庆材料研究院有限公司 | A kind of nickel material of high temperature resistant molten caustic (soda) corrosion |
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Title |
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