CN106756245B - A kind of alloy material and preparation method thereof for nuclear field liquid waste processing tankage - Google Patents
A kind of alloy material and preparation method thereof for nuclear field liquid waste processing tankage Download PDFInfo
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- CN106756245B CN106756245B CN201610968170.8A CN201610968170A CN106756245B CN 106756245 B CN106756245 B CN 106756245B CN 201610968170 A CN201610968170 A CN 201610968170A CN 106756245 B CN106756245 B CN 106756245B
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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
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/053—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 30% but less than 40%
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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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Abstract
The present invention relates to a kind of alloy material for nuclear field liquid waste processing tankage, the mass percent of the material each component is：Cr：30.0~32.0%；Mo：3.0~5.0%；W：1.0~2.0%；Nb：0.8~2.0%；Fe：5.5~8.5%；Ce：≤ 0.05%；C：≤ 0.02%；Si：≤ 0.5%；Mn：≤ 1.0%；S：≤ 0.01%；P：≤ 0.01%；Ti：≤ 0.1%；Co:≤ 0.01%；Al：≤ 0.04%；Remaining is Ni.The material has excellent resistance to corrosion in nuclear field waste liquid environment, and the replacement frequency of tankage can be greatly reduced, and improves working efficiency.
Description
Technical field
The present invention relates to a kind of metal materials, specifically a kind of alloy material for nuclear field liquid waste processing tankage
Material and preparation method.
Background technology
The processing of nuclear field waste liquid is all the key that all the time a ring in nuclear industry, is related to environment and to human health
Great influence.Radioactive element production tech uses and improves technological process, radioactivity of the flow in processing line terminal
Waste liquid needs to handle.According to the regulation of International Atomic Energy Agency (IAEA), radioactive liquid waste is according to the size of its radioactive activity
Level Four can be divided into：1st grade of radioactive activity≤3.7 × 102Bq/L is weak radioactive waste liquid；Section II grade radioactive activity>3.7×
102Bq/L ,≤3.7 × 105Bq/L are low radioactive waste liquid；Section III grade radioactive activity>3.7 × 105Bq/L ,≤3.7 ×
109Bq/L is intermediate level liquid waste；IVth grade of radioactive activity>3.7 × 109Bq/L is high activity liquid waste.Radioactive liquid waste concentration point
Include evaporation, chemical precipitation method, ion-exchange, membrane separation process and electrochemical process etc. from method, is handled and radiated with evaporation
Property waste liquid efficiency it is relatively high, when containing only the waste liquid of fixedness radioactive pollutant, single effect evaporator can reach l0 for processing4
Above decontamination factor, and using multi-effect evaporator and the evaporator with deentrainment device can then reach 106~l08Decontamination
Coefficient, the method is mainly for the treatment of some high activity liquid wastes.In addition, evaporation need not use other substances substantially, it will not be as it
His method generates the pollutant of other forms because of the transfer of pollutant, thus evaporation use it is more.
All the time, nuclear field liquid waste processing material generally uses stainless steel, but there are one very big for the use of such material
The drawbacks of, i.e., it needs replacing every 1-2, must be replaced less than 1 year in the case of utilization rate height every year.To find out its cause, mainly
Because in the waste liquid of the specific composition environment, the corrosion rate of active service stainless steel material is too fast, with the development of nuclear industry, makes
It is higher and higher with frequency, rate also higher is replaced, the corresponding research and production demand of nuclear industry cannot be met.Therefore, it is necessary to change
In generation, upgrades the novel evaporator material with more high-corrosion resistance, and the application to meet the corresponding technological process of nuclear industry is wanted
It asks, under same high frequency service condition, largely reduces replacement frequency.
At present in actual production process, the group of typical radioactive liquid waste becomes：HNO36mol/L, MoO3 -10mmol/L,
MnO3 -10mmol/L, F-300mg/L,Zr4+300mg/L.Radioactive liquid waste is concentrated by evaporation 10 times or so to recycle nitric acid, and emphasis is
Reduce waste liquid volume, then carries out glass solidification and cement solidification respectively.Especially high activity liquid waste must be by being concentrated by evaporation back
Nitric acid process is received, the areas control Chuan Gaochuan cycle prevents tritium in reprocessing plant extensive diffusive, influences personnel and Environmental security.It is existing
The stainless steel makings of 316L are used with evaporator, corrosion resistance is poor, is just needed replacing using 1 year, generates a large amount of secondary solid
Body waste, causes production process to be interrupted, and influences production capacity, safety and efficiency.
Therefore, the corrosion resistance in specific nuclear field waste liquid environment, and preparation easy to process are greatly improved, exploitation rises
Grade nuclear field liquid waste processing of new generation is of great significance with evaporator material.
Invention content
The invention aims to provide a kind of alloy material and preparation method for nuclear field liquid waste processing tankage,
The material has excellent resistance to corrosion in nuclear field waste liquid environment, and the replacement frequency of tankage can be greatly reduced
Rate improves working efficiency.
To achieve the above object, the technical solution adopted by the present invention is：
Mass percent for the alloy material of nuclear field liquid waste processing tankage, the material each component is：
Cr：30.0~32.0%；Mo：3.0~5.0%；W：1.0~2.0%；Nb：0.8~2.0%；Fe：5.5~
8.5%；Ce：≤ 0.05%；C：≤ 0.02%；Si：≤ 0.5%；Mn：≤ 1.0%；S：≤ 0.01%；P：≤ 0.01%；Ti：
≤ 0.1%；Co:≤ 0.01%；Al：≤ 0.04%；Remaining is Ni.
Preferable technical solution is used for the alloy material of nuclear field liquid waste processing tankage, the quality of the material each component
Percentage is：
Cr：30.5~31.51%；Mo：3.95~4.80%；W：1.2~1.7%；Nb：1.02~1.67%；Fe：5.99
~7.52%；Ce：<0.01%；C：0.007~0.010%；Si：0.05~0.10%；Mn：0.53~0.80%；S：≤
0.001%；P：0.001~0.003%；Ti：0.05~0.08%；Co:0.003~0.005%；Al：0.01~0.03%；Its
Remaining is Ni.
The preparation method of the above-mentioned alloy material for nuclear field liquid waste processing tankage, there is following steps：
1) melting：Take the component of above-mentioned material, melting under vacuum refines 1500 DEG C~1550 DEG C, refining period vacuum degree>
1Pa, 1450 DEG C~1480 DEG C of pouring temperature, obtains vacuum ingot, then ternary slag system is used to protect electroslag remelting, obtains surface quality light
Sliding ESR ingot；
2) Homogenization Treatments：Step 1) the ESR ingot homogenizes heat treatment 4~6 hours at 1100~1180 DEG C；
3) it forges：Forge 1150~1180 DEG C of initial temperature, final forging temperature>980 DEG C, forge slab；
4) hot rolling：Forging stock is heated to 1150~1180 DEG C, hot rolling at thickness 8mm~20mm plank or Φ 12mm
~Φ 20mm bars, are air-cooled to room temperature；
5) cold rolling cold drawing：By bar plate cold rolling at cold-reduced sheet with materials, or by bar cold drawing at wire rod.
6) annealing heat-treats temperature：1050 DEG C × (25~60) minute.
Ternary slag system described in step 1) is CaF2+Al2O3+ CaO, mass percent 50%CaF2+ 20%Al2O3+
30%CaO.
When step 5) cold rolling cold drawing, processing hardening is eliminated using 1040 DEG C~1080 DEG C annealing.
The above-mentioned alloy material for nuclear field liquid waste processing tankage can be used for preparing the various appearances of nuclear field liquid waste processing
Device.
The effect of each element of material of the present invention is as follows,
Ni：Matrix element has excellent corrosion resisting property, has intensity height, plasticity and toughness good by the alloy of matrix of nickel, can
With hot and cold deformation and processing and forming, various good comprehensive performances such as weldability is good.
Cr：Chromium is a kind of oxidation resistant element, and chromium promotes Nickel-based Corrosion-resistance Materials to form surface passivated membrane in an oxygen-containing environment,
Confrontation homogeneous corrosion has good effect.
Mo：Mo is apparent to the anti-anti-corrosion effect of reproducibility acid, can improve corrosion resistance of the corrosion resistant alloy in reproducibility acid, right
Anti- homogeneous corrosion, intercrystalline corrosion etc. have preferable effect.
W：The carbide of tungsten has prevention intergranular stress corrosion in addition to playing invigoration effect in the adventitious deposit of crystal boundary
There is good effect.
Mn：The alloying element for manufacturing the scaling loss of beneficial element in welding process for compensating material evaporator and adding, with
Ensure the chemical composition and performance of weld metal.
Fe：Not influencing to improve processability under the premise of its is corrosion proof.
Nb：Resistance to spot corrosion and crevice corrosion behavior are improved, anti intercrystalline corrosion is improved.
Al：Harmful element in abros will increase the depth of Intergranular stress corrosion cracking, especially work as content
In 0.05%~0.14% range, content is higher, and corrosion cracking is more serious, therefore controls below 0.04%.
Ti：Micro Ti has certain effect to melt deoxidation in the melting middle and later periods, and the compound of formation can play crystal boundary
To pinning effect, but Ti high may cause metallurgy to be mingled with, and be used as impurity element control below 0.04% herein.
Ce：Improve inclusion morphology, distribution and property, and improves the weldability, toughness and cold-forming property of material.
Si：Silicon is beneficial under high corrosion current potential, but the position for forming field trash easy tos produce spot corrosion, influences alloy
Corrosion resisting property.Therefore, the control of Si contents is below 0.5%.
S、P：The two seriously affects the processing performance of alloy, can be made to the performance of welding performance especially welding heat affected zone
At serious damage.S, the content of P controls below 0.01%.
C：Carbon content raising is very big on the influence of the performance of welding heat affected zone, and the carbide of formation will influence seam organization
Mechanical property, corrosion resisting property, cause welding degenerate.But a small amount of Nb, Ti can fix residual carbon point, can play carbon
The invigoration effect of compound.Therefore, carbon content general control is below 0.02%.
Co：Waste liquid has certain radiation property, and Co members, which are known as longer half-life period, to be controlled.Therefore, Co≤0.1%.
In preparation process, the formulation and effect of special parameter are as follows：
For the features such as alloying component is complicated, ingot shape is coarse, using Homogenization Treatments, it is therefore intended that improve W, Mo, Nb, Fe
The distributing homogeneity of equal elements wherein, simultaneously because solid solution element is more, therefore more a height of 1150 DEG C~1180 DEG C of temperature, it should
Processing can reduce material in hot procedure because of situations such as being broken caused by the reasons such as element crystal boundary segregation, rolling the hair split
It is raw, improve the lumber recovery of material.
Hot rolling is to obtain the necessary process means of the various final product forms of the material, is provided for follow-up cold machining process necessary
Middle transition material forms, such as slab, bar stock.
Cold rolling cold drawing be in order to obtain various forms of finished materials, plank be in order to prepare the surrounding structure of container, and
Wire rod is then to pull structure in container accordingly to prepare.
Annealing is to allow anneal of material to make its recrystallization to eliminate the machining stress during cold working, improve material
The plasticity toughness of material ensures the smooth extension of material cold working.
Alloy material of the present invention can ensure to improve safety, stability and the economy of radioactive liquid waste processing, ensure
Evaporating concentration process safety, improves production capacity and efficiency, and material of the invention can greatly improve safety guarantee, and material
Processability, weldability etc. are excellent, can be used for the making of the various containers of nuclear field liquid waste processing, such as evaporator.
Specific implementation mode
Embodiment 1
Weight percent for nuclear field liquid waste processing tankage alloy material each component is shown in Table 1.
Table 1 is used for nuclear field liquid waste processing tankage alloy material chemical composition (wt%)
| Number | C | Si | Mn | Cr | W | Nb | Fe | Mo |
| 1 | 0.010 | 0.05 | 0.53 | 30.50 | 1.2 | 1.16 | 5.99 | 4.80 |
| 2 | 0.010 | 0.06 | 0.59 | 31.51 | 1.7 | 1.02 | 6.23 | 3.95 |
| 3 | 0.007 | 0.10 | 0.80 | 30.91 | 1.3 | 1.67 | 7.52 | 4.18 |
| Ti | Co | Al | Ce | P | S | Ni | ||
| 1 | 0.05 | 0.004 | 0.02 | 0.010 | 0.003 | ＜ 0.001 | Surplus | |
| 2 | 0.05 | 0.005 | 0.01 | 0.015 | 0.001 | 0.001 | Surplus | |
| 3 | 0.04 | 0.003 | 0.03 | 0.020 | 0.001 | 0.001 | Surplus |
Embodiment 2
Each component is taken according to table 1, is prepared with following method of the present invention for nuclear field liquid waste processing tankage alloy
Material.
Alloy of the present invention is refined using vacuum induction furnace smelting and electroslag furnace, forged, hot rolling, heat treatment, cold rolling
Etc. processes, be processed into the anti-corrosive alloy material of different product form, processing and heat treatment process are as follows：
Melting：Using vacuum induction smelt and electroslag furnace remelting refining, vacuum induction smelt when 1500 DEG C of refining temperature~
1550 DEG C, refining period vacuum degree is better than 2Pa, and 1450 DEG C~1480 DEG C of pouring temperature obtains vacuum ingot, then protects electroslag with slag system
Remelting obtains the more smooth ESR ingot of surface quality；Homogenization Treatments：It is heat-treated 4~6 hours at 1100~1180 DEG C, so
Hammer cogging afterwards；Forging：1150~1180 DEG C of initial temperature is forged, final forging temperature is not less than 980 DEG C, can be swaged into breaking down as required
Slab or bar stock；Hot rolling：Forging stock is heated to 1150~1180 DEG C, hot rolling at thickness 8mm~20mm plank or Φ
12mm~Φ 20mm bars, are air-cooled to room temperature；Cold rolling cold drawing：By bar plate cold rolling at the cold-reduced sheet with materials of required specification, by bar
Cold drawing can carry out 1050 DEG C × (25~60) min annealing eliminations and add at the wire rod of required specification in cold rolling cold drawing process
Work is hardened.
Chemical composition ranges set by the present invention, on vaccum sensitive stove melting obtain three stove corrosion resistant alloy materials,
The alloy material of required form is obtained after electroslag remelting, forging, rolling, drawing.
3 experimental result of embodiment
1. the performance test of material
Chemical composition sample drilling cuttings on ESR ingot samples, remaining all test sample is sampled along machine direction, is measured
Chemical composition it is as shown in table 1, mechanical property is as shown in table 2.
Alloy material mechanical property prepared by 2 present invention of table
2. the environmental experiment of material
Above-described embodiment material, according to the use temperature range of room temperature to 110 DEG C, and evaporator process needs to use
To welding procedure, by simulating the corrosion-resistant experimental verification of nuclear field waste liquid environment, corrosion resistance is outstanding, year corrosion rate such as table
Shown in 3.
The corrosion resistance of alloy prepared by table 3 in nuclear field waste liquid environment
Claims (6)
1. a kind of alloy material for nuclear field liquid waste processing tankage, which is characterized in that the quality hundred of the material each component
Point ratio is：Cr：30.0~32.0%；Mo：3.0~5.0%；W：1.0~2.0%；Nb：0.8~2.0%；Fe：5.5~8.5%；
Ce：≤0.05%；C：≤0.02%；Si：≤0.5%；Mn：≤1.0%；S：≤0.01%； P：≤0.01%；Ti： ≤0.1%；Co:
≤0.01%；Al：≤0.04%；Remaining is Ni, which is made using following methods：
1）Melting：Take above-mentioned material each component, melting under vacuum, 1500 DEG C~1550 DEG C of refining temperature, refining period vacuum degree>
1Pa, 1450 DEG C~1480 DEG C of pouring temperature, obtains vacuum ingot, then ternary slag system is used to protect electroslag remelting, obtains surface quality light
Sliding ESR ingot；
2）Homogenization Treatments：Step 1）The ESR ingot homogenizes heat treatment 4~6 hours at 1100~1180 DEG C；
3）Forging：Forge 1150~1180 DEG C of initial temperature, final forging temperature>980 DEG C, it is forged into slab；
4）Hot rolling：The forging stock obtained after forging is heated to 1150~1180 DEG C, hot rolling at thickness 8mm~20mm plank
Or Φ 12mm~Φ 20mm bars, it is air-cooled to room temperature；
5）Cold rolling cold drawing：Plank is cold rolled to cold-rolled plate and strip, or by bar cold drawing at wire rod；
6）Annealing heat-treats temperature and time：1050℃×（25~60）Minute.
2. material according to claim 1, which is characterized in that the mass percent of each component is：Cr：30.5~
31.51%；Mo：3.95~4.80%；W：1.2~1.7%；Nb：1.02~1.67%；Fe：5.99~7.52%；Ce<0.05%；C：
0.007~0.010%；Si：0.05~0.10%；Mn：0. 53~0.80%；S：≤0.001%； P：0.001~0.003%；Ti：
0.05~0.08%；Co:0.003~0.005%；Al：0.01~0.03%；Remaining is Ni.
3. the method for preparing any alloy materials for nuclear field liquid waste processing tankage of claim 1-2, special
Sign is there are following steps：
1）Melting：Take each component of any materials of claim 1-2, melting under vacuum, refining temperature 1500 DEG C~1550
DEG C, refining period vacuum degree>1Pa, 1450 DEG C~1480 DEG C of pouring temperature, obtains vacuum ingot, then ternary slag system is used to protect electroslag weight
It is molten, obtain the smooth ESR ingot of surface quality；
2）Homogenization Treatments：Step 1）The ESR ingot homogenizes heat treatment 4~6 hours at 1100~1180 DEG C；
3）Forging：Forge 1150~1180 DEG C of initial temperature, final forging temperature>980 DEG C, it is forged into slab；
4）Hot rolling：The forging stock obtained after forging is heated to 1150~1180 DEG C, hot rolling at thickness 8mm~20mm plank
Or Φ 12mm~Φ 20mm bars, it is air-cooled to room temperature；
5）Cold rolling cold drawing：Plank is cold rolled to cold-rolled plate and strip, or by bar cold drawing at wire rod；
6）Annealing heat-treats temperature and time：1050℃×（25~60）Minute.
4. according to the method described in claim 3, it is characterized in that：Step 1）The ternary slag system is CaF2+Al2O3+ CaO,
Its mass percent is 50%CaF2+20%Al2O3+30%CaO。
5. according to the method described in claim 3, it is characterized in that：Step 5）When cold rolling cold drawing, using 1040 DEG C~1080 DEG C
Processing hardening is eliminated in annealing.
6. any alloy materials for nuclear field liquid waste processing tankage of claim 1-2 are preparing nuclear field liquid waste processing
Application in various containers.
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| US3574612A (en) * | 1969-02-03 | 1971-04-13 | Atomic Energy Commission | Nickel-chromium alloy |
| JPS6050134A (en) * | 1983-08-29 | 1985-03-19 | Sumitomo Metal Ind Ltd | Alloy for heat exchanger tube |
| DE19723491C1 (en) * | 1997-06-05 | 1998-12-03 | Krupp Vdm Gmbh | Use of a nickel-chromium-molybdenum alloy |
| CN103556003A (en) * | 2013-09-27 | 2014-02-05 | 贵州航天新力铸锻有限责任公司 | Preparation method for nickel-based alloy used for nuclear power station equipment parts |
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