CN108724894B - Method for preparing zirconium steel composite board by using copper as intermediate layer - Google Patents
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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
- 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
- B32B37/1009—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 using vacuum and fluid pressure
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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
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/013—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium
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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
- B32B15/00—Layered products comprising a layer of metal
- B32B15/18—Layered products comprising a layer of metal comprising iron or steel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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Abstract
The invention provides a method for preparing a zirconium steel composite plate by using copper as an intermediate layer, which comprises the following steps: 1) selecting a copper foil as an intermediate layer of the zirconium steel composite board; 2) cleaning a sample and assembling the sample in a vacuum hot-pressing sintering furnace; 3) when the hot-pressing sintering furnace reaches a certain vacuum degree, the heating rate is 8-12 ℃/s to reach the preset temperature of 550-. The zirconium steel composite board after vacuum diffusion welding has bright surface without oxidation and strong interface cutting strength over 60 MPa. The invention effectively solves the problem of huge internal stress generated during welding due to large difference of linear expansion coefficients of zirconium and steel by presetting the copper interlayer through a vacuum diffusion welding technology, and prevents Zr and Fe from reacting to generate ZrFe2，ZrFe3And ZrFe4And the like brittle intermetallic compounds.
Description
Technical Field
The invention belongs to the technical field of metal material processing, and particularly relates to a method for preparing a zirconium steel composite plate by using copper as an intermediate layer.
Background
Zirconium is a rare metal, has the advantages of easy processing, good corrosion resistance, low thermal neutron absorption cross section and the like, and is widely applied to the nuclear industry. However, in recent years, zirconium has been found to have better corrosion resistance than stainless steel, titanium and nickel alloy, so that zirconium is increasingly applied to industries such as petroleum, chemical engineering and the like. The zirconium steel composite board can replace pure zirconium to be used for manufacturing the pressure container, so that the manufacturing cost is reduced, and the zirconium resource is greatly saved. Therefore, the connection of zirconium and steel is an important technology in engineering, and no satisfactory method is found at present. The connection of zirconium alloys to steel presents certain difficulties, mainly for two reasons: 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. At present, the zirconium steel composite plate is mainly prepared by means of explosive welding at home, and the zirconium and steel composite plate is researched by using the diffusion welding technology at home and abroad.
Patent document CN 201510178398.2 provides a method for preparing zirconium/steel composite board. The method comprises the steps of firstly preparing a zirconium-titanium splice plate, and preparing the zirconium-steel composite plate with the shear strength not less than 190MPa by using steel as a base and zirconium-titanium as a composite layer through an explosive welding method.
The documents "Lee S U, Song H O, Lee W, et al, characterization of the interfacial bonding of zirconium-4 and stainless steel [ J]Physics Procedia,2009,2(3):1231-1239 ", reported a vacuum diffusion welding method of Zr-4 and 304L stainless steel at 850 ℃ -1020 ℃ without the use of an intermediate layer. Three different diffusion regions appeared, 120um wide, of which Zr (Fe, Cr)2The phase hardness is up to 1370 HV.
In the two methods for preparing the zirconium steel composite plate, the process is very complex, the operation is difficult and dangerous, and the thickness and the components of the bonding layer are difficult to control in the explosive welding; and the diffusion temperature of the middle layer which is not adopted in the diffusion connection is higher than 850 ℃, and a plurality of intermetallic compounds with extremely high hardness appear in the diffusion area.
Disclosure of Invention
The invention aims to overcome the defect that in the prior art, in the preparation process of a zirconium-steel composite plate, a huge internal expansion coefficient is generated when the zirconium and the steel are welded with large linear expansion coefficient differenceStress, and Zr reacts with Fe to form ZrFe2，ZrFe3And ZrFe4And the like, which are disadvantages of brittle intermetallic compounds. Provides a method for preparing a zirconium steel composite plate by using copper as an intermediate layer. The invention effectively solves the problem of huge internal stress generated during welding due to large difference of linear expansion coefficients of zirconium and steel by presetting the copper interlayer through a vacuum diffusion welding technology, and prevents Zr and Fe from reacting to generate ZrFe2，ZrFe3And ZrFe4And the brittle intermetallic compounds are used, so that the industrial production of the zirconium steel composite plate is expanded, and the economic benefit is improved.
The invention realizes the purpose by the following technical scheme, and a method for preparing a zirconium steel composite plate by using copper as an intermediate layer comprises the following steps:
1) selecting a copper foil as an intermediate layer of the zirconium-steel composite board, mechanically polishing, and cleaning oxides, pollutants and grease on the surfaces of the steel plate, the zirconium plate and the copper foil in an acetone solution by using ultrasonic waves for welding;
2) placing a copper foil between a zirconium plate and a steel plate to obtain a workpiece, wherein the zirconium plate is arranged on the upper layer, and the 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 a pressure of 0.3-1MPa on a nickel-based high-temperature alloy pressure head in the vacuum hot-pressing sintering furnace to reduce gaps among the zirconium plate, the copper foil and the steel plate;
3) vacuumizing the vacuum hot-pressing sintering furnace, starting heating when the vacuum degree is more than 10-3MPa, wherein the heating rate is 8-12 ℃/s, keeping the axial pressure of the nickel-based high-temperature alloy pressure head in the vacuum hot-pressing sintering furnace at 0.5-10MPa and preserving heat for 0.5-10h when the preset temperature of 550-; after the heat preservation is finished, stopping heating, unloading the axial pressure of the nickel-based superalloy pressure head, and keeping the vacuum degree in the hot-pressing sintering furnace; the temperature of the vacuum hot-pressing sintering furnace is lower than 150 ℃, the vacuumizing is closed, and the cooling is lower than 50 ℃.
Preferably, the zirconium plate is pure zirconium or zirconium alloy; the steel plate is pure iron, low-carbon steel or alloy steel;
preferably, the thickness of the copper foil as the intermediate layer of the zirconium steel composite plate is 0.01mm-0.5mm, and more preferably 0.06 mm; the copper foil comprises, by atomic percentage, 5.4% of Ni, 10% of Sn, 7% of P and the balance of Cu.
The temperature of the solid phase diffusion welding without adding the intermediate layer is generally selected to be 0.5-0.8Tm(TmAs the melting temperature of the base metal), the melting point of zirconium is 1852 ℃, and the melting point of iron is 1538 ℃. In the method, the following effects are obtained by presetting the copper intermediate layer:
1) reducing the vacuum diffusion welding temperature to below 750 ℃;
2) the prepared zirconium steel composite board does not find that Fe diffuses into Zr, and the copper foil effectively prevents the reaction of Fe and Zr;
3) the flexibility of the copper foil effectively relieves the internal stress caused by the thermal expansion difference, and the interface shear strength exceeds 60 MPa.
Drawings
Fig. 1 is a SEM backscattered electron photograph of a zirconium steel composite plate prepared using a 0.03mm thick copper foil according to example 1.
Fig. 2 is a SEM backscattered electron photograph of a zirconium steel composite plate prepared using a 0.06mm thick copper foil of example 1.
FIG. 3 is a SEM backscattered electron photograph of a zirconium steel composite panel prepared using a 0.09mm thick copper foil of example 1.
Fig. 4 is a graph comparing shear strength for composite panels prepared in examples 1, 2 and 3.
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.
Composite board of pure zirconium alloy and low carbon steel using copper foil with thickness of 10.03 mm as intermediate layer
1) Pretreatment of a workpiece: selecting copper foil as an intermediate layer for connecting pure zirconium alloy and low-carbon steel, wherein the copper foil has a smooth surface and comprises 5.4% of Ni, 10% of Sn, 7% of P and the balance of Cu (at%), the thickness is 0.03mm, the width is 20mm, and 1 layer is used; the purity of the zirconium alloy is 99%, the thickness of the zirconium alloy is 1.5mm, the mark of the low-carbon steel is Q345, the thickness of the zirconium alloy is 6mm, and the length and the width of the zirconium alloy are 100 x 100 mm. 1 hour before welding, the oxide on the surface of the copper foil is polished clean by using an 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 copper foil, the pure zirconium alloy plate and the low-carbon steel plate together into an acetone solution, cleaning for 20min by ultrasonic waves, and then drying for later use.
2) Assembling a workpiece:
firstly, a copper 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 a copper middle layer is placed, the zirconium alloy plate is placed at the topmost layer, and the copper foil, the pure zirconium alloy plate and the low-carbon steel plate are adjusted to be parallel. 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 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 the temperature of 700 ℃ at the temperature of 10 ℃/min all the time when the temperature is MPa, applying axial pressure of 3MPa, and then preserving heat for 3 h. After the reaction was complete, heating was stopped and the pressure was relieved, but was kept at 10 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 20.06 mm copper foil as intermediate layer composite sheet of pure zirconium alloy and Low carbon Steel
1) Pretreatment of a workpiece: selecting copper foil as an intermediate layer for connecting pure zirconium alloy and low-carbon steel, wherein the copper foil has a smooth surface and comprises 5.4% of Ni, 10% of Sn, 7% of P and the balance of Cu (at%), the thickness is 0.03mm, the width is 20mm, and 2 layers are used; the purity of the zirconium alloy is 99%, the thickness of the zirconium alloy is 1.5mm, the mark of the low-carbon steel is Q345, the thickness of the zirconium alloy is 6mm, and the length and the width of the zirconium alloy are 100 x 100 mm. 1 hour before welding, the oxide on the surface of the copper foil is polished clean by using an 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 copper foil, the pure zirconium alloy plate and the low-carbon steel plate together into an acetone solution, cleaning for 20min by ultrasonic waves, and then drying for later use.
2) Assembling a workpiece:
firstly, a copper 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 a copper middle layer is placed, the zirconium alloy plate is placed at the topmost layer, and the copper foil, the pure zirconium alloy plate and the low-carbon steel plate are adjusted to be parallel. 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 0.6MPa 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 700 ℃ at the temperature of 10 ℃/min all the time when the temperature is MPa, applying axial pressure of 3MPa, and then preserving heat for 3 h. After the reaction was complete, heating was stopped and the pressure was relieved, but was kept at 10 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 30.09 composite sheet of pure zirconium alloy with Low carbon Steel having copper foil as intermediate layer
1) Pretreatment of a workpiece: selecting copper foil as an intermediate layer for connecting pure zirconium alloy and low-carbon steel, wherein the copper foil has a smooth surface and comprises 5.4% of Ni, 10% of Sn, 7% of P and the balance of Cu (at%), the thickness is 0.03mm, the width is 20mm, and 3 layers are used; the purity of the zirconium alloy is 99%, the thickness of the zirconium alloy is 1.5mm, the mark of the low-carbon steel is Q345, the thickness of the zirconium alloy is 6mm, and the length and the width of the zirconium alloy are 100 x 100 mm. 1 hour before welding, the oxide on the surface of the copper foil is polished clean by using an 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 copper foil, the pure zirconium alloy plate and the low-carbon steel plate together into an acetone solution, cleaning for 20min by ultrasonic waves, and then drying for later use.
2) Assembling a workpiece:
firstly, a copper 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 a copper middle layer is placed, the zirconium alloy plate is placed at the topmost layer, and the copper foil, the pure zirconium alloy plate and the low-carbon steel plate are adjusted to be parallel. 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 0.3MPa 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 700 ℃ at the temperature of 10 ℃/min all the time when the temperature is MPa, applying axial pressure of 3MPa, and then preserving heat for 3 h. After the reaction was complete, heating was stopped and the pressure was relieved, but was kept at 10 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: zirconium steel clad steel sheets of different shear strengths were successfully obtained using copper as the intermediate layer (see fig. 4). The copper intermediate layer and the base material were reacted at 700 ℃ to obtain a diffusion layer having a multilayer structure. As can be seen from the SEM photographs (see fig. 1-3), Q345, the reaction layer and zirconium, the copper intermediate layer reacted more strongly with zirconium,the reaction layer is wider, while the reaction layer obtained by reacting the copper intermediate layer with the steel is thinner. As can be seen from the Fe-Cu binary phase diagram, the solubility of Fe in Cu is low, and the reaction is very limited; in the Zr-Cu binary phase diagram, Zr reacts with Cu to obtain ZrCu and Zr2Cu and Zr3Cu8And the like. When the intermediate layer is 0.03mm, obvious cracks appear in the reaction layer shown in figure 1, and the shear strength of the zirconium steel composite plate is only 36.7 MPa. When the intermediate layer is 0.06mm and 0.09mm, the reaction layer as in fig. 2 and 3 is flat and smooth, and no obvious cracks are formed; the maximum shearing strength of the zirconium steel composite plate is 61.4MPa, and the bonding strength of the zirconium steel composite plate can be obviously improved by increasing the thickness of the middle layer.
In a word, the melting point of pure copper is about 1083 ℃, and the copper foil adopted by the method greatly reduces the temperature required by diffusion, shortens the time required by diffusion and simultaneously maintains higher shear strength while no large amount of noble metal is added.
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 (5)
1. A method for preparing a zirconium steel composite plate by using copper as an intermediate layer comprises the following steps:
1) selecting a copper foil as an intermediate layer of the zirconium-steel composite board, mechanically polishing, and cleaning oxides, pollutants and grease on the surfaces of the steel plate, the zirconium plate and the copper foil in an acetone solution by using ultrasonic waves for welding;
2) placing a copper foil between a zirconium plate and a steel plate to obtain a workpiece, wherein the zirconium plate is arranged on the upper layer, and the 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 a pressure of 0.3-1MPa on a nickel-based high-temperature alloy pressure head in the vacuum hot-pressing sintering furnace to reduce gaps among the zirconium plate, the copper foil and the steel plate;
3) vacuumizing the vacuum hot-pressing sintering furnace, wherein when the vacuum degree is more than 10-3Heating at a heating rate of 8-12 deg.C/s under MPaWhen the preset temperature is 550-750 ℃, keeping the axial pressure of the nickel-based high-temperature alloy pressure head in the vacuum hot-pressing sintering furnace at 0.5-10MPa, and preserving the heat for 0.5-10 h; after the heat preservation is finished, stopping heating, unloading the axial pressure of the nickel-based superalloy pressure head, and keeping the vacuum degree in the hot-pressing sintering furnace; and (3) closing the vacuum-pumping and cooling when the temperature of the vacuum hot-pressing sintering furnace is lower than 150 ℃ to obtain the zirconium steel composite plate, wherein the temperature is lower than 50 ℃.
2. The method of claim 1, wherein: the interface shear strength of the prepared zirconium steel composite plate is more than 60 MPa.
3. The method of claim 1, wherein: the zirconium plate is pure zirconium or zirconium alloy; the steel plate is pure iron, low-carbon steel or alloy steel.
4. The method of claim 1, wherein: the thickness of the copper foil is 0.01mm-0.5 mm; the copper foil comprises, by atomic percentage, 5.4% of Ni, 10% of Sn, 7% of P and the balance of Cu.
5. The method of claim 4, wherein: the thickness of the copper foil is 0.06 mm.
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| CN109808258B (en) * | 2019-03-13 | 2023-12-26 | 哈尔滨工程大学烟台研究院 | Diamond layer copper-laid base high-heat-conductivity composite material and preparation method thereof |
| CN110216364B (en) * | 2019-06-28 | 2021-11-12 | 南京佑天金属科技有限公司 | Ultrasonic consolidation forming method for zirconium steel layered composite material |
| CN110744266A (en) * | 2019-10-14 | 2020-02-04 | 西安理工大学 | Method for preparing high-chromium cast iron-low-carbon steel layered bimetallic material |
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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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