CN108724893B - Preparation method of zirconium steel composite board - Google Patents
Preparation method of zirconium steel composite board Download PDFInfo
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- CN108724893B CN108724893B CN201710339710.0A CN201710339710A CN108724893B CN 108724893 B CN108724893 B CN 108724893B CN 201710339710 A CN201710339710 A CN 201710339710A CN 108724893 B CN108724893 B CN 108724893B
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/16—Drying; Softening; Cleaning
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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Abstract
The invention discloses a preparation method of a zirconium steel composite plate, which comprises the following steps: 1) selecting pure aluminum or aluminum alloy as an intermediate layer of zirconium alloy and low-carbon steel; 2) placing the aluminum intermediate layer between the zirconium plate and the steel plate, assembling the aluminum intermediate layer between two pieces of heat-resistant stainless steel, placing the aluminum intermediate layer in a vacuum hot-pressing sintering furnace, and pre-applying pressure of 0.1-3 MPa; 3) vacuumizing the hot-pressing sintering furnace, wherein when the vacuum degree is more than 10‑3Heating at the MPa, keeping the axial pressure at 0.5-6MPa and keeping the temperature for 0.5-10h when the temperature reaches 450-650 ℃; the axial pressure is unloaded and the furnace is cooled to less than 50 ℃. The method can solve the problem of realizing high-quality welding of zirconium and steel at low temperature in the prior welding technology, wherein the interface of the diffusion layer is smooth, the reaction product is single, and the welded zirconium steel composite plate has the advantages of small deformation, no oxidation, low residual stress and the like, and can be suitable for the fields of chemical reaction vessels and the like.
Description
Technical Field
The invention belongs to the technical field of metal material processing, and particularly relates to a preparation method of a zirconium steel composite plate.
Background
Diffusion welding is a method of applying a temperature lower than the melting point of the base metal in a solid state, maintaining axial pressure, and adding or not adding an intermediate layer to cause micro deformation of the base metal without damaging the overall performance, and finally achieving a certain bonding strength. However, the mechanical properties of the composite material depend on the microstructure of the area of the bonding surface. Therefore, the thickness and the type of the intermetallic compound generated on the bonding surface (diffusion layer) can be accurately controlled by adjusting the experimental parameters, and the key factors influencing the material performance can be found in the process. The same or different materials, such as metal to metal, metal to ceramic, can be joined together using diffusion welding methods.
Zirconium is a rare metal and has the advantages of easy processing, good corrosion resistance, low thermal neutron absorption cross section and the like. In recent years, zirconium has better corrosion resistance than stainless steel, titanium and nickel alloy, and is increasingly applied to industries such as petroleum, chemical engineering and the like. But is limited by the price of zirconium, so that the zirconium steel composite plate can be used for manufacturing the pressure container instead of pure zirconium, thereby not only reducing the manufacturing cost, but also greatly saving the zirconium resource.
The use of diffusion welding to weld zirconium and steel together is a very promising idea. However, the connection of zirconium alloys to steel presents certain difficulties, which are mainly due to two aspects: firstly, the formation of brittle intermetallic compounds reduces the mechanical strength and corrosion resistance of the joint; secondly, the thermal expansion coefficients of the two materials have great difference, and great internal stress is caused after connection. Therefore, in foreign countries, many researchers will employ the addition of an intermediate layer to relieve internal stresses caused by two different materials and to prevent the formation of intermetallic compounds.
The literature "Aboudi D, Lebaili S, Taouinet M, et al. MicroStructure evaluation of differentiation compared 304L/Zircaloy 4, with coater interlayer [ J ]].Materials&Design,2017,116: 386-394 ", reports that pure copper is used as an intermediate layer to connect stainless steel and Zr4 alloy, and the result shows that the copper can effectively prevent the mutual interaction of Fe and Zr and the crack propagation in a diffusion layer at 900 ℃; however, at 1050 ℃, copper reacts with zirconium violently to form a local liquid phase, and then forms brittle and hard C after contacting with Fe element36-Fe2The Laves phase of Zr, etc., affects the joint performance.
The document "Chen H, Long C, Wei T, et al. Effect of Ni interlayer on partial phase bonding of Zr-Sn-Nb alloy and 304 stainless steel[J].Materials&Design,2014,60(60):358-2When the phase is brittle, the reaction layer is thin and cracks are formed; however, the joint with the nickel intermediate layer has the reaction layer with the thickness of 135um, no crack appears and the bonding strength is obviously improved.
The intermediate layers mentioned in the above documents all belong to pure noble metals and the diffusion temperatures have exceeded 900 ℃, which belong to medium-high temperature diffusion welding. In the current examined documents, no case of success of the zirconium alloy and the low-carbon steel at the diffusion welding temperature lower than 650 ℃ is found.
Disclosure of Invention
The invention aims to solve the problems that in the prior art, a large amount of noble metal is required to be used in the preparation process of a zirconium steel composite plate, so that the cost is high, and the preparation process needs high temperature of over 900 ℃, and provides a preparation method of the zirconium steel composite plate. The invention further expands the industrial production of the zirconium steel composite board and improves the economic benefit, and the invention provides a method for successfully welding the zirconium alloy and the low-carbon steel together by using the aluminum intermediate layer by using the solid state diffusion welding principle under the condition that the diffusion temperature is lower than 650 ℃.
The invention realizes the aim through the following technical scheme, and the preparation method of the zirconium steel composite plate comprises the following steps:
1) selecting pure aluminum or low-melting-point aluminum alloy as an intermediate layer for preparing the zirconium steel composite plate, and removing oxides and mechanical impurities on the surfaces of a low-carbon steel plate, a zirconium plate, the aluminum or the low-melting-point aluminum alloy for welding;
2) placing aluminum or low-melting-point aluminum alloy between a zirconium plate and a low-carbon steel plate to obtain a workpiece, wherein the zirconium plate is arranged on the upper layer, and the low-carbon steel plate is arranged on the lowermost layer; then assembling the workpiece between two pieces of heat-resistant stainless steel, placing the workpiece in a vacuum hot-pressing sintering furnace, and pre-applying a pressure of 0.5-2MPa on a nickel-based high-temperature alloy pressure head of the vacuum hot-pressing sintering furnace to enable the workpiece to be in close contact with the nickel-based high-temperature alloy pressure head;
3) to vacuum heatThe pressure sintering furnace is vacuumized, and when the vacuum degree is more than 10-3Heating at the temperature of 8-12 ℃/s under MPa, keeping the axial pressure of the nickel-based high-temperature alloy pressure head of the vacuum hot-pressing sintering furnace at 0.5-6MPa when the preset temperature of 450-650 ℃, and keeping the heat preservation time at 0.5-10 h; after the heat preservation time is over, stopping heating, unloading the axial pressure and keeping the vacuum degree in the hot-pressing sintering furnace; the temperature of the hot-pressing sintering furnace is lower than 150 ℃, the vacuum pumping is closed, and the furnace cooling is lower than 50 ℃.
Preferably, the thickness of the middle layer of the pure aluminum or the low-melting-point aluminum alloy is 0.5mm-1 mm;
preferably, the purity of the pure aluminum is more than 99.9%, and the low-melting-point aluminum alloy is aluminum-silicon alloy.
Preferably, the aluminum-silicon alloy is Al12Si、Al8Si or Al4Si。
Preferably, the zirconium plate is pure zirconium or zirconium alloy; the steel plate is pure iron, low-carbon steel or alloy steel;
compared with the prior art, the invention has the following advantages:
the aluminum or aluminum-silicon alloy is creatively adopted as the intermediate layer diffusion layer, and the purpose is to reduce the cost of selecting the intermediate layer; secondly, the diffusion temperature is low, and the industrial energy consumption is reduced; the three aluminum foils do not need special treatment, and the production process is simplified. The results show that the aluminum interlayer effectively prevents the reaction between Fe and Zr, thereby avoiding ZrFe2，ZrFe3And ZrFe4The formation of brittle intermetallic compounds; formation of Al at the Fe-Al side interface5Fe2While Al is formed at the interface on the Zr-Al side3Zr; the integral characteristics are as follows: the bonding surface is flat and smooth, the reaction product is single, the hardness is moderate, and the shearing strength of the composite plate exceeds 23 MPa.
Drawings
FIG. 1 is a metallographic photograph of a zirconium steel composite plate according to example 1 using pure aluminum as the intermediate layer;
fig. 2 is a shear strength graph of the zirconium steel composite plate of example 1 using pure aluminum as the intermediate layer.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention.
EXAMPLE 1.0.5mm composite Panel of pure zirconium alloy with aluminum as the intermediate layer and Low carbon Steel
The invention steps of this case are as follows:
1) pretreatment of a workpiece: aluminum is selected as an intermediate layer for connecting pure zirconium alloy and low-carbon steel, the purity of the aluminum foil is 99.9 percent, the thickness of the aluminum foil is 0.5mm, the purity of the zirconium alloy is 99 percent, the thickness of the zirconium alloy is 1.5mm, the mark of the low-carbon steel is Q345, the thickness of the low-carbon steel is 6mm, and the length and the width of the aluminum foil and the zirconium alloy are both 100 x 50 mm. 1 hour before welding, the oxide on the surface of the aluminum foil is polished clean by using industrial scouring pad. And (3) grinding the pure zirconium alloy plate and the low-carbon steel plate to a certain degree of finish by using a mechanical grinding machine, then sequentially grinding and polishing by using 800#, 1000#, 1500# and 2000# metallographic abrasive paper, cleaning by using water and drying by blowing. And finally, putting the aluminum foil, the pure zirconium alloy plate and the low-carbon steel plate together into ultrasonic waves by using absolute alcohol, cleaning for 20min, and then drying for later use.
2) Assembling a workpiece:
firstly, an aluminum foil is placed between a pure zirconium alloy plate and a low-carbon steel plate, the low-carbon steel plate is placed at the bottommost layer, then an aluminum middle layer is placed, a zirconium alloy plate is placed at the topmost layer, and the aluminum foil, the low-carbon steel plate and the aluminum middle layer are adjusted to keep the pure zirconium alloy plate, the low-carbon steel plate and the zirconium alloy. And then placing the assembled workpiece between two pieces of heat-resistant stainless steel, wherein the heat-resistant stainless steel is used for keeping the vertical parallelism consistent, and then placing the assembled workpiece and the heat-resistant steel into a vacuum hot-pressing sintering furnace. And finally, applying a pre-pressure of 1MPa between the nickel-based high-temperature alloy pressing heads to enable the workpieces to be in close contact, and closing the furnace door.
3) Heating, heat preservation and discharging of the workpiece:
firstly, vacuumizing a vacuum hot-pressing sintering furnace with an assembled workpiece, and compiling parameters such as heating temperature, heat preservation time, pressure and the like. When the vacuum degree is more than 10-3Heating at MPa, and keeping the heating rate at 10 deg.C/min until the temperature reachesAnd (3) applying axial pressure of 3MPa to the nickel-based high-temperature alloy pressure head at 545 ℃, and then carrying out heat preservation reaction for 3 h. After the incubation reaction was complete, heating was stopped and the axial pressure was relieved, but continued at 10 deg.f-3The vacuum degree of MPa, so that the furnace is cooled. The vacuum pumping can be closed until the temperature is lower than 150 ℃, and finally, the sample is taken out at the temperature of not higher than 50 ℃.
The results show that: in FIG. 1, steel and Al are sequentially arranged from left to right5Fe2Aluminum, Al3Zr and zirconium. The diffusion between metals belongs to bulk diffusion, which is mainly carried out through vacancy movement, wherein the vacancy movement requires thermal activation energy, the activation energy is larger when the melting point of the metal is higher, and the temperature required by solid phase diffusion is generally 0.5-0.8Tm (Tm is the melting point of the metal) of the metal. The melting point of Al is about 660 ℃, the activation energy required by Al atom diffusion is met at 545 ℃, and Al is respectively formed by mutual diffusion reaction between Fe/Al and Zr/Al5Fe2And Al3Zr. In the shear test (see FIG. 2), the shear strength of the interface reached 23.1 MPa.
Example 2.0.5mmAl12Composite board of pure zirconium alloy and low-carbon steel with Si as intermediate layer
The invention steps of this case are as follows:
1) pretreatment of a workpiece: selecting 0.5mmAl12Si is used as an intermediate layer for connecting the pure zirconium alloy and the low-carbon steel, and the components of the aluminum-silicon intermediate layer are Al: 88%, Si: 12 percent of zirconium alloy with the thickness of 0.5mm, the purity of the zirconium alloy with the thickness of 99 percent of 1.5mm, the mark of low-carbon steel Q345 with the thickness of 6mm, and the length and the width of the zirconium alloy are both 100 x 50 mm. 1 hour before welding, the oxide on the surface of the aluminum foil is polished clean by using industrial scouring pad. And (3) grinding the pure zirconium alloy plate and the low-carbon steel plate to a certain degree of finish by using a mechanical grinding machine, then sequentially grinding and polishing by using 800#, 1000#, 1500# and 2000# metallographic abrasive paper, cleaning by using water and drying by blowing. And finally, putting the aluminum foil, the pure zirconium alloy plate and the low-carbon steel plate together into ultrasonic waves by using absolute alcohol, cleaning for 20min, and then drying for later use.
2) Assembling a workpiece:
firstly, an aluminum foil is placed between a pure zirconium alloy plate and a low-carbon steel plate, the low-carbon steel plate is placed at the bottommost layer, then an aluminum middle layer is placed, a zirconium alloy plate is placed at the topmost layer, and the aluminum foil, the low-carbon steel plate and the aluminum middle layer are adjusted to keep the pure zirconium alloy plate, the low-carbon steel plate and the zirconium alloy. And then placing the assembled workpiece between two pieces of heat-resistant stainless steel, wherein the heat-resistant stainless steel is used for keeping the upper parallelism and the lower parallelism consistent, and carefully placing the assembled workpiece and the heat-resistant steel into a vacuum hot-pressing sintering furnace. And finally, applying 0.5MPa of pre-pressure between the nickel-based high-temperature alloy pressing heads to enable the workpieces to be in close contact, and closing the furnace door.
3) Heating, heat preservation and discharging of the workpiece:
firstly, vacuumizing a vacuum hot-pressing sintering furnace with an assembled workpiece, and compiling parameters such as heating temperature, heat preservation time, pressure and the like. When the vacuum degree is more than 10-3Heating at the temperature of 600 ℃ at the temperature of 10 ℃/min all the time when the temperature is MPa, applying axial pressure of 3MPa, and then keeping the temperature for reaction for 40 min. After the incubation reaction was complete, heating was stopped and the axial pressure was relieved, but continued at 10 deg.f-3The vacuum degree of MPa, so that the furnace is cooled. The vacuum pumping can be closed until the temperature is lower than 150 ℃, and finally, the sample is taken out at the temperature of not higher than 50 ℃.
Example 3.0.5mmAl12Composite board of pure zirconium alloy and low-carbon steel with Si as intermediate layer
The invention steps of this case are as follows:
1) pretreatment of a workpiece: selecting 0.5mmAl12Si is used as an intermediate layer for connecting the pure zirconium alloy and the low-carbon steel, and the components of the aluminum-silicon intermediate layer are Al: 88%, Si: 12 percent of zirconium alloy with the thickness of 0.5mm, the purity of the zirconium alloy with the thickness of 99 percent of 1.5mm, the mark of low-carbon steel Q345 with the thickness of 6mm, and the length and the width of the zirconium alloy are both 100 x 50 mm. 1 hour before welding, the oxide on the surface of the aluminum foil is polished clean by using industrial scouring pad. And (3) grinding the pure zirconium alloy plate and the low-carbon steel plate to a certain degree of finish by using a mechanical grinding machine, then sequentially grinding and polishing by using 800#, 1000#, 1500# and 2000# metallographic abrasive paper, cleaning by using water and drying by blowing. And finally, putting the aluminum foil, the pure zirconium alloy plate and the low-carbon steel plate together into ultrasonic waves by using absolute alcohol, cleaning for 20min, and then drying for later use.
2) Assembling a workpiece:
firstly, an aluminum foil is placed between a pure zirconium alloy plate and a low-carbon steel plate, the low-carbon steel plate is placed at the bottommost layer, then an aluminum middle layer is placed, a zirconium alloy plate is placed at the topmost layer, and the aluminum foil, the low-carbon steel plate and the aluminum middle layer are adjusted to keep the pure zirconium alloy plate, the low-carbon steel plate and the zirconium alloy. And then placing the assembled workpiece between two pieces of heat-resistant stainless steel, wherein the heat-resistant stainless steel is used for keeping the upper parallelism and the lower parallelism consistent, and carefully placing the assembled workpiece and the heat-resistant steel into a vacuum hot-pressing sintering furnace. And finally, applying 2MPa of pre-pressure between the nickel-based high-temperature alloy pressing heads to enable the workpieces to be in close contact, and closing the furnace door.
3) Heating, heat preservation and discharging of the workpiece:
firstly, vacuumizing a vacuum hot-pressing sintering furnace with an assembled workpiece, and compiling parameters such as heating temperature, heat preservation time, pressure and the like. When the vacuum degree is more than 10-3Heating is started when the pressure is MPa, the heating rate is always kept at 10 ℃/min until the temperature reaches 460 ℃, the axial pressure is applied to be 3MPa, and then the reaction is carried out for 3h under the condition of heat preservation. After the incubation reaction was complete, heating was stopped and the axial pressure was relieved, but continued at 10 deg.f-3The vacuum degree of MPa, so that the furnace is cooled. The vacuum pumping can be closed until the temperature is lower than 150 ℃, and finally, the sample is taken out at the temperature of not higher than 50 ℃.
Although the embodiments of the present invention have been described in detail, it should be understood that various changes, substitutions, and alterations can be made hereto without departing from the spirit and scope of the invention.
Claims (4)
1. The preparation method of the zirconium steel composite plate is characterized by comprising the following steps of: comprises the following steps of (a) carrying out,
1) selecting pure aluminum or low-melting-point aluminum alloy as an intermediate layer for preparing the zirconium steel composite plate, and removing oxides and mechanical impurities on the surfaces of the low-carbon steel plate, the zirconium plate, the pure aluminum or the low-melting-point aluminum alloy for welding;
2) placing the pure aluminum or the low-melting-point aluminum alloy treated in the step 1) between a zirconium plate and a low-carbon steel plate to obtain a workpiece, wherein the zirconium plate is arranged on the upper layer, and the low-carbon steel plate is arranged on the lower layer; then assembling the workpiece between two pieces of heat-resistant stainless steel, placing the workpiece in a vacuum hot-pressing sintering furnace, and pre-applying pressure of 0.5-2MPa on a nickel-based high-temperature alloy pressure head of the vacuum hot-pressing sintering furnace to reduce gaps among the zirconium plate, the middle layer and the low-carbon steel plate;
3) vacuumizing the vacuum hot-pressing sintering furnace, wherein when the vacuum degree is more than 10-3Heating at the temperature of 8-12 ℃/s under MPa, keeping the axial pressure of the nickel-based high-temperature alloy pressure head of the vacuum hot-pressing sintering furnace at 0.5-6MPa when the preset temperature of 450-650 ℃, and keeping the temperature for 0.5-10 h; after the heat preservation is finished, stopping heating, unloading the axial pressure and keeping the vacuum degree in the hot-pressing sintering furnace; the temperature of the hot-pressing sintering furnace is lower than 150 ℃, the vacuum pumping is closed, and the furnace cooling is lower than 50 ℃.
2. The method of claim 1, wherein: the thickness of the pure aluminum or the low-melting-point aluminum alloy is 0.5mm-1 mm.
3. The method of claim 1, wherein: the purity of the pure aluminum is more than 99.9 percent, and the low-melting-point aluminum alloy is aluminum-silicon alloy.
4. The production method according to claim 3, characterized in that: the aluminum-silicon alloy is Al12Si、Al8Si or Al4Si。
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| CN104827241A (en) * | 2014-02-12 | 2015-08-12 | 上海却尘科技有限公司 | Manufacturing method of blanks for producing steel-zirconium composite boards |
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| CN201009489Y (en) * | 2007-02-07 | 2008-01-23 | 南京宝泰特种材料有限公司 | Zirconium steel composite board |
| CN101985190A (en) * | 2010-12-08 | 2011-03-16 | 西安优耐特容器制造有限公司 | Method for welding steel substrate layers of zirconium steel compound slabs |
| KR20140102469A (en) * | 2013-02-14 | 2014-08-22 | 충남대학교산학협력단 | Cu/al hybrid alloy with enhanced reliability through the control of diffusion and reaction kinetics of cu and al and method for manufacturing the same |
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