CN102560168A - Preparation method of high-density neutron absorbing plate - Google Patents
Preparation method of high-density neutron absorbing plate Download PDFInfo
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- CN102560168A CN102560168A CN2010106025305A CN201010602530A CN102560168A CN 102560168 A CN102560168 A CN 102560168A CN 2010106025305 A CN2010106025305 A CN 2010106025305A CN 201010602530 A CN201010602530 A CN 201010602530A CN 102560168 A CN102560168 A CN 102560168A
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Abstract
The invention belongs to a preparation method of a neutron absorbing plate, and specifically relates to the preparation method of the high-density neutron absorbing plate, which comprises the following steps of: 1. preparing an aluminum alloy box; 2. charging; 3. vacuum sintering; 4. hot-rolling, including small lower rolling quantity of multi-pass rolling and large lower rolling quantity of multi-pass rolling; 5. hot-rolled annealing; 6. cold-rolling; 7. cold-rolled annealing, the annealing temperature being 350 DEG C to 440 DEG C, the annealing time is 30min to 70min, and naturally cooling to room temperature after the scheduled time is reached. The preparation method of the high-density neutron absorbing plate has the advantages that: the flow is simple, the required temperature in the whole process is relatively lower, the interface reaction can not be generated, and Al4C3 can not also be generated. The two surfaces of the neutron absorbing plate prepared by the invention are wrapped with the aluminum alloy material, so the wear resistance strength is high, and the neutron absorbing plate is more suitable for transporting and storing spent fuel.
Description
Technical field
The invention belongs to the preparation method of neutron absorber plate, be specifically related to a kind of preparation method of high-density neutron absorber plate.
Background technology
Neutron absorber plate is generally by B
4C-Al constitutes, and this material has good neutron absorptive character owing to contain the B element.Its remarkable advantage is corrosion-resistant, anti-irradiation, long service life, can improve the economy and the security of spent fuel storing greatly.B wherein
4C content can be up to 65wt%, and is very wide according to the adjustable extent of design demand, makes the design of spent fuel transportation and storage system more flexible, can realize more intensive storage.
In the prior art, this preparation methods has fusion casting, powder metallurgic method etc.Canada Alcan international corporation prepares B with casting
4C-Al neutron absorbing material; And the mixture that under molten state, stirs flow boron carbide particles and molten aluminum matrix has been described in its patent CN1708597A; So that matrix alloy soaks into boron carbide particles and makes size distribution in the whole volume of melt, cast this molten mixture then.Adopt smelting process often to have serious surface reaction, on norbide and aluminium interface, formed AlB
2, Al
4C
3, Al
4BC, AlB
24C
4Deng.These second phase materials are easy to combine the agglomerating inequality that causes boron to distribute, and have reduced the mechanical property of material simultaneously.CARDEN ROBIN A. has set forth a kind of casting-hot-extrusion method and has produced B in patent US5722033 (A)
4The C/Al material.This method is heated to 570 ℃ with the matrix material spindle, and the softening spindle of insulation is positioned over spindle in the hot extrusion chamber, at following remollescent spindle extrusion molding of certain pressure.Exist the serious problem of surface reaction equally.
Roll method with respect to casting, powder metallurgic method can be improved the distributing homogeneity of norbide greatly.Abenojar etc. are to the Al+50%B of powder metallurgic method preparation
4The mechanical property of the matrix material of C is studied.What in the preparation of material, adopt is technologies such as single shaft compacting, isostatic cool pressing, hot pressing, sintering.Complicated process of preparation, cost is high.US5700962 adds an amount of cakingagent to strengthen the cementability that powder particle is seen in the batch mixing process when preparing the neutron absorbing material with powder metallurgic method.Through to static pressure such as mixed powder, degasification, sintering, extrusion moulding then.In sintering process, sticker in the green compact and moisture can be removed.But often cakingagent is removed not exclusively, and it is unfavorable that this can bring for following process and use, for example in use can produce more hydrogen.Large diameter green compact once adopted long-time thermal cycling in order to remove sticker fully, but this has increased production cost again, and the decomposition condition at the control sticker also is that certain difficulty is arranged simultaneously.
The employing pressureless penetration legal systems such as Peng Kewu of China Northeastern University are equipped with B
4The C-Al matrix material, and studied B
4C and the chemical reaction of Al under hot conditions and composition mutually.The red strong grade of eating of Northeastern University has been described a kind of B in CN101215164A
4The preparation method of C matrix material: with an amount of MOX and boron carbide powder; At 100MPa～150MPa dip mold base, then precast billet is placed vacuum sintering furnace, be evacuated to 20Pa～100Pa; Be warming up to 1850 ℃～2060 ℃ with 5 ℃/min～8 ℃/min speed; Insulation 10min～60min obtains boron carbide-based porous sintered body, at last infiltration aluminium under vacuum condition.But when temperature surpassed 1000 ℃, aluminium and norbide can react and generate Al
4C
3Along with the continuation rising of temperature, Al
4C
3Can the be faster (Al of generating rate
4C
3Have water absorbability and very poor mechanical property).In a word, the temperature of pressureless penetration method infiltration is high, B
4C and Al surface reaction are serious, need especially skeleton presintering of complicated step before this technology infiltration, have had a strong impact on the preparation cycle of pressureless penetration.
Fan of Beijing Non-Ferrous Metal Research General Academy builds medium a kind of B that in CN1422970, described
4C, SiC, Al
2O
3, AlN particle enhanced aluminum matrix composite and method of manufacture thereof.Strengthen body granularity 0.1 μ m～1 μ m; Volume(tric)fraction 10%-60%; Its preparation method be with enhancing body powder and trace active metallic element join carry out high-energy ball milling in the ball grinding cylinder after, add the aluminum base alloy powder again and carry out the high speed high-energy ball milling, add micro-liquid surfactant ball milling in 15 ℃～80 ℃ scopes at last again; Composite powder behind the ball milling obtains billet through hot compacting, and billet makes finished product after through hot-work such as extruding, rolling, die forgings.Foreign matter content such as iron is high in this norbide-aluminum composite that utilizes the preparation of high-energy ball milling and hot-press method, complex process, and cost is high.
Summary of the invention
The objective of the invention is defective, provide a kind of preparation method simple, can not produce the preparation method of the high-density neutron absorber plate of surface reaction to prior art.
The present invention is achieved in that a kind of preparation method of high-density neutron absorber plate, comprises the steps:
Step 1: preparation duraluminum box
The duraluminum box of preparation is the rectangular parallelepiped that has top cover, on the sidewall of rectangular parallelepiped, has the plurality of rows pore;
Step 2: charging
With B
4C particle and Al powdered alloy are even according to predefined mixed, fill up the duraluminum box for preparing in the step 1 uniformly with the raw material that mixes, and the top cover welding is fixing;
Step 3: vacuum sintering
To B is housed in the step 2
4The duraluminum box that has top cover of C particle and Al alloy powder mixture carries out vacuum sintering;
Step 4: hot rolling
Hot rolling comprises that the multi-pass of little volume under pressure multi-pass rolling and big volume under pressure is rolling;
Step 5: hot-roll annealing
The annealing temperature of this step is 350 ℃-440 ℃, and annealing time is 30min-70min, naturally cools to room temperature after the arrival scheduled time;
Step 6: cold rolling
Plate-like product is pressed into the thickness that meets size with cold-rolling process of the prior art;
Step 7: cold rolled annealed
The annealing temperature of this step is 350 ℃-440 ℃, and annealing time is 30min-70min, naturally cools to room temperature after the arrival scheduled time.
The preparation method of aforesaid a kind of high-density neutron absorber plate, wherein, B in the described step 2
4C particle and the predefined ratio of Al powdered alloy are B
4The C granular mass accounts for B
45%～65% of C particle and Al alloy powder mixture quality.
The preparation method of aforesaid a kind of high-density neutron absorber plate, wherein, described B
4C particulate granularity is 5 μ m～150 μ m; The granularity of Al powdered alloy is 35 μ m～60 μ m.
The preparation method of aforesaid a kind of high-density neutron absorber plate, wherein, described vacuum tightness is 10
-2-10
-3Pa, sintering temperature is 350 ℃-540 ℃, sintering time is 5 hours-20 hours.
The preparation method of aforesaid a kind of high-density neutron absorber plate, wherein, what the little volume under pressure in the described step 4 rolling was the deflection scope at 5%-15% is rolling.
The preparation method of aforesaid a kind of high-density neutron absorber plate, wherein, what the big volume under pressure in the described step 4 rolling was the deflection scope at 20%-50% is rolling.
The preparation method of aforesaid a kind of high-density neutron absorber plate, wherein, the rolling rolling pass of the little volume under pressure in the described step 4 in 5 roads between 10 roads.
Advantage of the present invention is: the method flow that the present invention adopts is simple, and whole process is temperature required relatively low, can not produce surface reaction.And the neutron absorber plate that manufacturing of the present invention is come out all wraps up aluminum alloy materials on the two sides of sheet material, so abrasive wear resistance is big, is suitable for the spent fuel transportation more and stores.
Embodiment
A kind of preparation method of high-density neutron absorber plate comprises the steps:
Step 1: preparation duraluminum box
The duraluminum box of preparation is the rectangular parallelepiped that has top cover, on the sidewall of rectangular parallelepiped, has the plurality of rows pore.The size decision of the high-density neutron absorber plate that the size of duraluminum box prepares as required.Used duraluminum can be commercially available any aluminum alloy materials.Described venting hole can be according to the design of the frame size of reality, available comparatively dense arrange than small de-air hole or arrange the large-size venting hole of dredging, be as the criterion then in the follow-up operation of rolling, can discharge gas smoothly.
Step 2: charging
With B
4C particle and Al powdered alloy are even according to predefined mixed.Above-mentioned B
4The C particle is accomplished with using mixer mixing of Al powdered alloy.Raw material with mixing fills up the duraluminum box for preparing in the step 1 uniformly, and top cover is built.
Described B
4C particle and Al powdered alloy are the commercially available prod.Described B
4The C granular mass accounts for B
45%～65% of C particle and Al alloy powder mixture quality.B
4C particulate granularity is 5 μ m～150 μ m; The granularity of Al powdered alloy is 35 μ m～60 μ m.
Because the B element what the effect of the final intercept neutrons of neutron absorber plate depends on, get final product if therefore want to improve the assimilation effect of neutron absorber plate and only need increase the content of B element.
Step 3: vacuum sintering
To B is housed in the step 2
4The duraluminum box that has top cover of C particle and Al alloy powder mixture carries out vacuum sintering.Promptly at first utilize vacuum extractor to vacuumize processing, when vacuum tightness is 10
-2-10
-3Can think during Pa to have reached and vacuumize requirement.The duraluminum box sintering that with sintering oven this quilt is vacuumized then, sintering temperature are 350 ℃-540 ℃, and sintering time is 5 hours-20 hours.
Step 4: hot rolling
Hot rolling comprises that the multi-pass of little volume under pressure multi-pass rolling and big volume under pressure is rolling.
The product that sinters in the step 3 is carried out rolling (be also referred to as press down in a small amount) of multi-pass small deformation amount earlier, and the small deformation amount is meant that the deflection scope is at 5%-15%.The effect that presses down in a small amount is with the air emptying in the duraluminum box that sinters, and makes it reach closely knit state.Generally speaking, be pressed in 5 roads between 10 roads under a small amount of.
Press down in a small amount rolling (be also referred to as in a large number and press down) of carrying out aximal deformation value after the completion, aximal deformation value is meant that deflection is at 20%-50%.The effect that presses down in a large number is with evacuation of air and has been pressed into tabular product and continues to be pressed onto the size near finished product.Because hot rolling technology can not accurately controlled rolling size, so this step can only be roughly be pressed onto roughly the size near finished product with plate-like product.
Step 5: hot-roll annealing
The annealing temperature of this step is 350 ℃-440 ℃, and annealing time is 30min-70min, naturally cools to room temperature after the arrival scheduled time.
Step 6: cold rolling
Plate-like product is pressed into the thickness that meets size with cold-rolling process of the prior art.
Step 7: cold rolled annealed
The annealing temperature of this step is 350 ℃-440 ℃, and annealing time is 30min-70min, naturally cools to room temperature after the arrival scheduled time.
For further the present invention will be described, following embodiment is provided:
Embodiment 1
The massfraction of each component of present embodiment material is: B
4C particle 10%, mean particle size 100 μ m, Al matrix powder 90%, mean particle size 60 μ m.Even batch mixing in mixer is inserted in the Al alloy framework after the encapsulation, and the core base is 10 in vacuum tightness
-3510 ℃ of sintering are 10 hours in the vacuum oven of Pa, carry out continuous multiple tracks hot rolling system, and preceding 5 is 10% to draught, and follow-up draught is about 40%, after its thickness is 2.9mm after the hot rolling, and cool to room temperature, cold rolling aligning is size 4600mm * 650mm * 2.7mm to the end.
Record neutron absorber plate density 97.5% under this preparation condition (theoretical density 97.5%) with the hydrostatics method.Tensile property table 1 in this processing condition lower plate.
Table 1
Described ys is the parameter of beginning plastic deformation; Described tension is by force the parameter that plastic deformation finishes the neutron absorber plate fracture, and unit elongation is the ratio of preceding maximum length of this neutron absorber plate fracture and original length.
Instance 2:
The component of present embodiment material and massfraction thereof: B
4C particle 26%, mean particle size 35 μ m, Al powder matrix 74%, mean particle size 60 μ m.Even batch mixing in mixer is inserted in the Al alloy framework after the encapsulation, and the core base is 10 in vacuum tightness
-3540 ℃ of sintering are 6 hours in the vacuum oven of Pa, multiple tracks hot rolling system continuously then, and preceding 6 is 6% to draught, follow-up draught is about 35%, after suppressing thickness and being 2.9mm, cool to room temperature, cold rolling aligning is size 4600mm * 650mm * 2.0mm to the end.Record neutron absorber plate density 98.2% under this preparation condition with the hydrostatics method.Tensile property table 2 in this processing condition lower plate.
Table 2
Instance 3
The component of present embodiment material and massfraction thereof: B
4C particle 35%, mean particle size 25 μ m, Al powder matrix 65%, mean particle size 45 μ m.Even batch mixing in mixer is inserted in the Al alloy framework after the encapsulation, and the core base is 10 in vacuum tightness
-3480 ℃ of sintering are 15 hours in the vacuum oven of Pa, multiple tracks hot rolling system continuously then, and preceding 6 is 8% to draught, follow-up draught is about 30%, after suppressing thickness and being 2.9mm, cool to room temperature, cold rolling aligning is size 4600mm * 650mm * 2.3mm to the end.Record neutron absorber plate density 99.2% under this preparation condition with the hydrostatics method.Tensile property table 3 in this processing condition lower plate.
Table 3
Instance 4
The component of present embodiment material and massfraction thereof: B
4C particle 50%, mean particle size 60 μ m, Al powder matrix 50%, mean particle size 60 μ m.Even batch mixing in mixer is inserted in the Al alloy framework after the encapsulation, and the core base is 10 in vacuum tightness
-3350 ℃ of sintering are 20 hours in the vacuum oven of Pa, multiple tracks hot rolling system continuously then, and preceding 5 is 12% to draught, follow-up draught is about 45%, after suppressing thickness and being 2.9mm, cool to room temperature, cold rolling aligning is size 4600mm * 650mm * 2.5mm to the end.The neutron absorber plate density 98.5% that under this condition, prepares.
Tensile property table 4 in this processing condition lower plate.
Table 4
Instance 5
The component of present embodiment material and massfraction thereof: B
4C particle 65%, mean particle size 60 μ m, Al powder matrix 35%, mean particle size 35 μ m.Even batch mixing in mixer is inserted in the Al alloy framework after the encapsulation, and the core base is 10 in vacuum tightness
-2350 ℃ of sintering are 20 hours in the vacuum oven of Pa, multiple tracks hot rolling system continuously then, and preceding 5 is 13% to draught, follow-up draught is about 30%, after suppressing thickness and being 2.9mm, cool to room temperature, cold rolling aligning is size 4600mm * 650mm * 3.2mm to the end.The neutron absorber plate density 97.8% that under this condition, prepares.
Tensile property in this processing condition lower plate is seen table 5.
Table 5
Claims (7)
1. the preparation method of a high-density neutron absorber plate is characterized in that: comprise the steps:
Step 1: preparation duraluminum box
The duraluminum box of preparation is the rectangular parallelepiped that has top cover, on the sidewall of rectangular parallelepiped, has the plurality of rows pore;
Step 2: charging
With B
4C particle and Al powdered alloy are even according to predefined mixed, fill up the duraluminum box for preparing in the step 1 uniformly with the raw material that mixes, and the top cover welding is fixing;
Step 3: vacuum sintering
To B is housed in the step 2
4The duraluminum box that has top cover of C particle and Al alloy powder mixture carries out vacuum sintering;
Step 4: hot rolling
Hot rolling comprises that the multi-pass of little volume under pressure multi-pass rolling and big volume under pressure is rolling;
Step 5: hot-roll annealing
The annealing temperature of this step is 350 ℃-440 ℃, and annealing time is 30min-70min, naturally cools to room temperature after the arrival scheduled time;
Step 6: cold rolling
Plate-like product is pressed into the thickness that meets size with cold-rolling process of the prior art;
Step 7: cold rolled annealed
The annealing temperature of this step is 350 ℃-440 ℃, and annealing time is 30min-70min, naturally cools to room temperature after the arrival scheduled time.
2. the preparation method of a kind of high-density neutron absorber plate as claimed in claim 1 is characterized in that: B in the described step 2
4C particle and the predefined ratio of Al powdered alloy are B
4The C granular mass accounts for B
45%～65% of C particle and Al alloy powder mixture quality.
3. the preparation method of a kind of high-density neutron absorber plate as claimed in claim 2 is characterized in that: described B
4C particulate granularity is 5 μ m～150 μ m; The granularity of Al powdered alloy is 35 μ m～60 μ m.
4. like the preparation method of claim 1 or 3 described a kind of high-density neutron absorber plates, it is characterized in that: described vacuum tightness is 10
-2-10
-3Pa, sintering temperature is 350 ℃-540 ℃, sintering time is 5 hours-20 hours.
5. like the preparation method of claim 1 or 4 described a kind of high-density neutron absorber plates, it is characterized in that: what the little volume under pressure in the described step 4 rolling was the deflection scope at 5%-15% is rolling.
6. like the preparation method of claim 1 or 4 described a kind of high-density neutron absorber plates, it is characterized in that: what the big volume under pressure in the described step 4 rolling was the deflection scope at 20%-50% is rolling.
7. like the preparation method of claim 1 or 5 described a kind of high-density neutron absorber plates, it is characterized in that: the rolling rolling pass of the little volume under pressure in the described step 4 in 5 roads between 10 roads.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103614584A (en) * | 2013-11-07 | 2014-03-05 | 海龙核材科技（江苏）有限公司 | Preparation method of aluminium matrix composite with high B4C content |
| CN103962547A (en) * | 2014-05-07 | 2014-08-06 | 镇江市纽科利核能新材料科技有限公司 | Aluminum matrix composite material high in boron carbide content |
| CN104308161A (en) * | 2014-10-16 | 2015-01-28 | 中国工程物理研究院材料研究所 | Preparation method of low-cost boron carbide/aluminum composite board |
| CN105671373A (en) * | 2016-03-11 | 2016-06-15 | 江苏海龙核科技股份有限公司 | Preparing method for neutron absorption plate with high B4C content |
| CN110153187A (en) * | 2017-12-06 | 2019-08-23 | 安徽应流久源核能新材料科技有限公司 | A kind of milling method of aluminum-based boron carbide composite shielding material |
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|---|---|---|---|---|
| US4027377A (en) * | 1975-06-25 | 1977-06-07 | Brooks & Perkins, Incorporated | Production of neutron shielding material |
| JP2001042089A (en) * | 1999-05-27 | 2001-02-16 | Mitsubishi Heavy Ind Ltd | Aluminum composite with neutron absorption power and its manufacture |
| US20090104470A1 (en) * | 2007-10-23 | 2009-04-23 | Hideki Suzuki | Production method for metal matrix composite material |
-
2010
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4027377A (en) * | 1975-06-25 | 1977-06-07 | Brooks & Perkins, Incorporated | Production of neutron shielding material |
| JP2001042089A (en) * | 1999-05-27 | 2001-02-16 | Mitsubishi Heavy Ind Ltd | Aluminum composite with neutron absorption power and its manufacture |
| US20090104470A1 (en) * | 2007-10-23 | 2009-04-23 | Hideki Suzuki | Production method for metal matrix composite material |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103614584A (en) * | 2013-11-07 | 2014-03-05 | 海龙核材科技（江苏）有限公司 | Preparation method of aluminium matrix composite with high B4C content |
| CN103962547A (en) * | 2014-05-07 | 2014-08-06 | 镇江市纽科利核能新材料科技有限公司 | Aluminum matrix composite material high in boron carbide content |
| CN103962547B (en) * | 2014-05-07 | 2016-04-20 | 镇江市纽科利核能新材料科技有限公司 | A kind of aluminum matrix composite of high carbonization Boron contents |
| CN104308161A (en) * | 2014-10-16 | 2015-01-28 | 中国工程物理研究院材料研究所 | Preparation method of low-cost boron carbide/aluminum composite board |
| CN104308161B (en) * | 2014-10-16 | 2017-02-01 | 中国工程物理研究院材料研究所 | Preparation method of boron carbide/aluminum composite board |
| CN105671373A (en) * | 2016-03-11 | 2016-06-15 | 江苏海龙核科技股份有限公司 | Preparing method for neutron absorption plate with high B4C content |
| CN110153187A (en) * | 2017-12-06 | 2019-08-23 | 安徽应流久源核能新材料科技有限公司 | A kind of milling method of aluminum-based boron carbide composite shielding material |
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Application publication date: 20120711 |