CN109848501B - High-strength brazing method for molybdenum-copper alloy and stainless steel - Google Patents
High-strength brazing method for molybdenum-copper alloy and stainless steel Download PDFInfo
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Abstract
The invention discloses a high-strength brazing method for molybdenum-copper alloy and stainless steel, which comprises the following steps: (1) surface cleaning treatment, (2) surface modification treatment, (3) brazing filler metal preparation, (4) material clamping treatment, and (5) welding treatment. The invention carries out special optimization and improvement treatment on the brazing method, has simple process, reasonable collocation of the steps, convenient popularization and application, high strength and strong stability of the treated welded joint, lower welding temperature, production cost saving, powerful technical support for the production of high-quality workpieces and strong market competitiveness.
Description
Technical Field
The invention belongs to the technical field of alloy processing, and particularly relates to a high-strength brazing method for molybdenum-copper alloy and stainless steel.
Background
The molybdenum-copper alloy is a high-temperature material prepared from molybdenum and copper by powder metallurgy, infiltration and other technologies, has the characteristics of high strength, high hardness, low thermal expansion coefficient and the like of molybdenum and the characteristics of high plasticity, high electric conductivity and thermal conductivity and the like of copper, has excellent comprehensive performance, and is widely applied to electric contact materials, heat dissipation materials, electronic packaging materials and the like. In actual use, the molybdenum-copper alloy needs to be welded with stainless steel and other materials, but the linear expansion coefficient and the heat conductivity of the molybdenum-copper alloy are greatly different, so that the joint is easy to generate large stress, further cracking is caused, and the service quality and the service life are finally influenced.
The welding mode is various, such as solid phase welding, liquid phase welding and the like, brazing belongs to solid phase welding and is a common welding mode, most of weldments are integrally heated or large-area and uniform heating is carried out around a brazing seam during welding treatment, so that the deformation of workpieces and the residual stress of brazed joints are much smaller than those of fusion welding, and the precision size of the workpieces is easy to guarantee. Molybdenum-manganese metallization and nickel-plating brazing method adopted by institute of electronics of Chinese academy of sciences for welding molybdenum-copper alloy and Al2O3And (3) obtaining the sealing joint with good air tightness by using ceramic. But before welding, the molybdenum-copper alloy needs to be plated with nickel, and Al needs to be plated with nickel2O3The ceramic is metallized and nickel-plated, and the welding process is more, which is not beneficial to popularization and application. In response to this problem, a number of brazing methods have been developed, such as the following: CN201110429990.7 discloses a vacuum active brazing process of molybdenum-copper alloy and stainless steel, which comprises the steps of brazing molybdenum with active brazing filler metal under vacuum conditionThe complex physical and chemical reaction between the copper alloy and the stainless steel realizes the sealing connection between the molybdenum-copper alloy and the stainless steel, and although the welding fastness is obviously improved, the mode also needs further optimization and improvement along with the continuous improvement of the product performance, the service life and the like of the market.
Disclosure of Invention
The invention aims to solve the existing problems and provides a high-strength brazing method for molybdenum-copper alloy and stainless steel.
The invention is realized by the following technical scheme:
a high-strength brazing method for molybdenum-copper alloy and stainless steel comprises the following steps:
(1) surface cleaning treatment:
respectively putting the molybdenum-copper alloy and the stainless steel into degreasing liquid for soaking and degreasing treatment, taking out after 10-15 min, then putting into a drying box for drying treatment, taking out after 20-25 min, and finally polishing with abrasive paper for later use;
(2) surface modification treatment:
placing the molybdenum-copper alloy and the stainless steel treated in the step (1) into an ultraviolet irradiation box for irradiation treatment, and taking out for later use after 30-40 min;
(3) preparing a brazing filler metal:
a. immersing attapulgite in a sulfuric acid solution for soaking for 4-6 min, taking out the attapulgite, immersing the attapulgite in a sodium hydroxide solution for soaking for 5-8 min, and finally taking out the attapulgite and washing the attapulgite with deionized water for later use;
b. b, placing the attapulgite treated in the operation a into a calcining furnace for calcining, controlling the calcining temperature to be 700-750 ℃, and taking out for later use after heat preservation and calcination for 1-2 hours;
c. b, immersing the attapulgite treated in the operation b into a silane coupling agent solution for soaking for 20-25 min, taking out and drying for later use;
d. mixing the attapulgite, the aluminum phosphate, the polyethylene glycol, the polyurea formaldehyde and the zinc stearate which are treated in the operation c according to a weight ratio of 6-8: 18-22: 5-7: 2-5: 0.2-0.4, then putting the mixture into a temperature changing box for temperature changing treatment, firstly heating the temperature changing box to 110-120 ℃, carrying out heat preservation treatment for 3-5 min, then heating the temperature changing box to 180-200 ℃, carrying out heat preservation treatment for 15-20 min, then heating the temperature changing box to 690-720 ℃, carrying out heat preservation treatment for 20-25 min, and finally taking out and naturally cooling to room temperature to obtain a reactant A for later use;
e. weighing the following substances in parts by weight for later use: 80-85 parts of silver, 13-17 parts of copper, 1-3 parts of titanium, 2-4 parts of reactant A prepared in the operation d, 0.1-0.2 part of rare earth nitrate salt and 0.3-0.6 part of disodium ethylene diamine tetraacetate;
f. mixing the silver, the copper and the titanium weighed in the operation e together, putting the mixture into a vacuum smelting furnace, heating the mixture to keep the temperature in the vacuum smelting furnace at 1150-1180 ℃, carrying out heat preservation treatment for 35-40 min, then carrying out vacuum gas atomization for powder preparation, and taking out the powder to obtain a mixture B for later use;
g. putting the mixture B prepared in the operation f and the reactant A prepared in the operation d, the rare earth nitrate and the disodium ethylene diamine tetraacetate, which are weighed in the operation e, into a ball mill together for ball milling and crushing, taking out after 30-35 min, and finally preparing the brazing filler metal for later use through pressure sintering, heat treatment, calendaring and intermediate annealing;
(4) material clamping treatment:
placing the brazing filler metal prepared in the step (3) between the molybdenum-copper alloy treated in the step (2) and the to-be-welded surface of the stainless steel, and then assembling by using a clamp, wherein the sealing pressure is controlled to be 1-1.4 MPa, so that a to-be-welded part is obtained for later use;
(5) welding treatment:
and (5) putting the to-be-welded piece treated in the step (4) into vacuum brazing equipment for welding treatment, and taking out the to-be-welded piece after the welding treatment is finished and naturally cooling the to-be-welded piece to room temperature.
Further, the deoiling liquid in the step (1) is an acetone solution with the mass fraction of 10-15%; and during drying treatment, the temperature in the drying oven is controlled to be 70-75 ℃.
Further, during the irradiation treatment in the step (2), the irradiation power in the ultraviolet irradiation box is controlled to be 1200-1400W, and the wavelength of ultraviolet rays is 300-320 nm.
Further, the mass fraction of the sulfuric acid solution in the operation a in the step (3) is 7-10%; the mass fraction of the sodium hydroxide solution is 12-14%.
Further, the mass fraction of the silane coupling agent solution in the operation c of the step (3) is 25-30%; the silane coupling agent is any one of a silane coupling agent kh550, a silane coupling agent kh560 and a silane coupling agent kh 570.
Further, the rare earth nitrate salt in the operation e of the step (3) is any one of lanthanum nitrate, cerium nitrate and yttrium nitrate.
Further, in the step (3), the atomizing gas used in the powder preparation by vacuum gas atomization in operation f is nitrogen.
Further, in the step (3), the pressure sintering treatment is carried out under the conditions that the pressure is controlled to be 62-66 MPa and the sintering temperature is controlled to be 650-680 ℃; the heat treatment is to carry out homogenization heat treatment on the material, the temperature of the heat treatment is controlled to be 550-580 ℃, and the time duration is 10-12 hours; the rolling processing and the intermediate annealing treatment are to roll the heat-treated material for multiple times, and the intermediate annealing treatment is carried out between two times of rolling, wherein the temperature is controlled to be 530-560 ℃ during annealing, and the time duration is 1-3 h.
Further, the vacuum degree in the vacuum brazing equipment is controlled to be 1-3 multiplied by 10 during the welding treatment in the step (5)-4Pa, the brazing temperature is 880-920 ℃, and the heat preservation time is 12-16 min.
In the prior art, the performances such as the welding strength of a weldment are not strong enough, so that the manufacturing and application of a high-quality and high-performance original part are poor. The invention optimizes and improves the welding process method, obviously improves the welding quality, ensures the welding quality and lays a foundation for higher-quality application. The surface of the workpiece to be welded is subjected to surface cleaning treatment, oil stains, impurities and the like on the surface are removed, a surface oxidation film layer is removed, a foundation is laid for subsequent processing, then surface modification treatment is carried out, the surface of the workpiece to be welded is subjected to irradiation treatment by ultraviolet irradiation, the activity of the surface of the workpiece to be welded is well activated, and subsequent welding reaction is facilitated; then the preparation of the brazing filler metal is carried out, the bonding and fusion capacity between the existing brazing filler metal and a part to be welded is not strong, and unstable cracking at a welding point is easy to cause, so the preparation of the brazing filler metal is carried out again, the attapulgite is firstly subjected to acid-base soaking and calcining treatment, the specific surface area and the adsorption property of the attapulgite are effectively improved, then the silane coupling agent soaking treatment is carried out, the silanization treatment is carried out on the surface of the attapulgite, the fusion reaction capacity between the attapulgite and other components is improved, then the attapulgite, the aluminum phosphate, the polyethylene glycol, the polyurea formaldehyde and the zinc stearate are mixed to prepare a reactant A, the reactant A is an inorganic composite particle component with the particle size of about 400nm and the pore size of about 150nm, the component can be immersed by molten metal liquid during subsequent welding, the riveting and fastening effects are achieved, and the bonding strength among tissues can be enhanced, the brazing filler metal can be filled to improve the compactness of the structure, can be crystallized around particles, promotes certain lattice distortion of brazing filler metal crystal grains, prevents grain boundary scratch and deformation under the action of external force, improves the external force resistance and the creep resistance, further improves the structure quality, and then is mixed with silver, copper, titanium, rare earth nitrate, disodium ethylene diamine tetraacetate and the like to be processed into the brazing filler metal.
Compared with the prior art, the invention has the following advantages:
the invention carries out special optimization and improvement treatment on the brazing method, has simple process, reasonable collocation of the steps, convenient popularization and application, high strength and strong stability of the treated welded joint, lower welding temperature, production cost saving, powerful technical support for the production of high-quality workpieces and strong market competitiveness.
Detailed Description
Example 1
A high-strength brazing method for molybdenum-copper alloy and stainless steel comprises the following steps:
(1) surface cleaning treatment:
respectively putting the molybdenum-copper alloy and the stainless steel into degreasing liquid for soaking and degreasing treatment, taking out after 10min, then putting into a drying oven for drying treatment, taking out after 20min, and finally polishing with abrasive paper for later use;
(2) surface modification treatment:
placing the molybdenum-copper alloy and the stainless steel treated in the step (1) into an ultraviolet irradiation box for irradiation treatment, and taking out for later use after 30 min;
(3) preparing a brazing filler metal:
a. immersing attapulgite in a sulfuric acid solution for soaking for 4min, taking out the attapulgite, immersing the attapulgite in a sodium hydroxide solution for soaking for 5min, and finally taking out the attapulgite and washing the attapulgite with deionized water for one time for later use;
b. b, putting the attapulgite treated in the operation a into a calcining furnace for calcining, controlling the calcining temperature to be 700 ℃, keeping the temperature for calcining for 1h, and taking out for later use;
c. b, immersing the attapulgite treated in the operation b into a silane coupling agent solution for soaking for 20min, taking out and drying for later use;
d. mixing the attapulgite, the aluminum phosphate, the polyethylene glycol, the polyurea formaldehyde and the zinc stearate which are treated in the operation c correspondingly according to the weight ratio of 6:18:5:2:0.2, then putting the mixture into a temperature change box for temperature change treatment, firstly heating the temperature change box to 110 ℃, carrying out heat preservation treatment for 3min, then heating the temperature change box to 180 ℃, carrying out heat preservation treatment for 15min, then heating the temperature change box to 690 ℃, carrying out heat preservation treatment for 20min, and finally taking out the mixture and naturally cooling the mixture to room temperature to obtain a reactant A for later use;
e. weighing the following substances in parts by weight for later use: 80 parts of silver, 13 parts of copper, 1 part of titanium, 2 parts of the reactant A prepared in the operation d, 0.1 part of nitric acid rare earth salt and 0.3 part of ethylene diamine tetraacetic acid disodium;
f. mixing the silver, the copper and the titanium weighed in the operation e together, putting the mixture into a vacuum smelting furnace, heating the mixture to keep the temperature in the vacuum smelting furnace at 1150 ℃, carrying out heat preservation treatment for 35min, then carrying out vacuum gas atomization for powder preparation, and taking out the mixture to obtain a mixture B for later use;
g. putting the mixture B prepared in the operation f and the reactant A prepared in the operation d, the rare earth nitrate and the disodium ethylene diamine tetraacetate, which are weighed in the operation e, into a ball mill together for ball milling and crushing treatment, taking out after 30min, and finally preparing the brazing filler metal for later use through pressure sintering, heat treatment, calendaring and intermediate annealing;
(4) material clamping treatment:
placing the brazing filler metal prepared in the step (3) between the molybdenum-copper alloy treated in the step (2) and the to-be-welded surface of the stainless steel, assembling by using a clamp, controlling the sealing pressure to be 1MPa during the assembly, and obtaining a to-be-welded part for later use;
(5) welding treatment:
and (5) putting the to-be-welded piece treated in the step (4) into vacuum brazing equipment for welding treatment, and taking out the to-be-welded piece after the welding treatment is finished and naturally cooling the to-be-welded piece to room temperature.
Further, the deoiling liquid in the step (1) is an acetone solution with the mass fraction of 10%; the temperature in the drying oven is controlled to be 70 ℃ during the drying treatment.
Further, during the irradiation treatment in the step (2), the irradiation power in the ultraviolet irradiation box is controlled to be 1200W, and the wavelength of ultraviolet rays is 300-320 nm.
Further, the mass fraction of the sulfuric acid solution in the operation a in the step (3) is 7%; the mass fraction of the sodium hydroxide solution is 12%.
Further, the mass fraction of the silane coupling agent solution in the operation c of the step (3) is 25%; the silane coupling agent is a silane coupling agent kh 550.
Further, the rare earth nitrate salt in the operation e of the step (3) is lanthanum nitrate.
Further, in the step (3), the atomizing gas used in the powder preparation by vacuum gas atomization in operation f is nitrogen.
Further, in the pressure sintering treatment in the operation g of the step (3), the pressure is controlled to be 62MPa, and the sintering temperature is 650 ℃; the heat treatment is to carry out homogenization heat treatment on the material, the temperature of the treatment is controlled to be 550 ℃, and the time duration is 10 hours; the rolling processing and the intermediate annealing treatment are to roll the heat-treated material for multiple times, and the intermediate annealing treatment is carried out between two times of rolling, wherein the temperature is controlled to be 530 ℃ during annealing, and the time duration is 1 h.
Further, the vacuum degree in the vacuum brazing equipment is controlled to be 1-3 multiplied by 10 during the welding treatment in the step (5)-4Pa, the brazing temperature is 880 ℃, and the heat preservation time is 12 min.
Example 2
A high-strength brazing method for molybdenum-copper alloy and stainless steel comprises the following steps:
(1) surface cleaning treatment:
respectively putting the molybdenum-copper alloy and the stainless steel into degreasing liquid for soaking and degreasing treatment, taking out after 13min, then putting into a drying oven for drying treatment, taking out after 22min, and finally polishing with abrasive paper for later use;
(2) surface modification treatment:
placing the molybdenum-copper alloy and the stainless steel treated in the step (1) into an ultraviolet irradiation box for irradiation treatment, and taking out for later use after 35 min;
(3) preparing a brazing filler metal:
a. immersing attapulgite in a sulfuric acid solution for soaking for 5min, taking out the attapulgite, immersing the attapulgite in a sodium hydroxide solution for soaking for 7min, and finally taking out the attapulgite and washing the attapulgite with deionized water for one time for later use;
b. b, putting the attapulgite treated in the operation a into a calcining furnace for calcining, controlling the calcining temperature to be 730 ℃, keeping the temperature for calcining for 1.5h, and taking out for later use;
c. b, immersing the attapulgite treated in the operation b into a silane coupling agent solution for soaking for 22min, taking out and drying for later use;
d. mixing the attapulgite, the aluminum phosphate, the polyethylene glycol, the polyurea formaldehyde and the zinc stearate which are treated in the operation c correspondingly according to the weight ratio of 7:20:6:4:0.3, then putting the mixture into a temperature change box for temperature change treatment, firstly heating the temperature change box to 115 ℃, carrying out heat preservation treatment for 4min, then heating the temperature change box to 190 ℃, carrying out heat preservation treatment for 17min, then heating the temperature change box to 710 ℃, carrying out heat preservation treatment for 22min, and finally taking out the mixture and naturally cooling the mixture to room temperature to obtain a reactant A for later use;
e. weighing the following substances in parts by weight for later use: 83 parts of silver, 16 parts of copper, 2 parts of titanium, 3 parts of the reactant A prepared in the operation d, 0.15 part of nitric acid rare earth salt and 0.5 part of ethylene diamine tetraacetic acid disodium;
f. mixing the silver, the copper and the titanium weighed in the operation e together, putting the mixture into a vacuum smelting furnace, heating to keep the temperature in the vacuum smelting furnace at 1170 ℃, carrying out heat preservation treatment for 38min, then carrying out vacuum gas atomization for powder preparation, and taking out the mixture B for later use;
g. putting the mixture B prepared in the operation f and the reactant A prepared in the operation d, the rare earth nitrate and the disodium ethylene diamine tetraacetate, which are weighed in the operation e, into a ball mill together for ball milling and crushing treatment, taking out after 33min, and finally preparing the brazing filler metal for later use through pressure sintering, heat treatment, calendaring and intermediate annealing;
(4) material clamping treatment:
placing the brazing filler metal prepared in the step (3) between the molybdenum-copper alloy treated in the step (2) and the to-be-welded surface of the stainless steel, assembling by using a clamp, controlling the sealing pressure to be 1.2MPa during the assembly, and obtaining a to-be-welded part for later use;
(5) welding treatment:
and (5) putting the to-be-welded piece treated in the step (4) into vacuum brazing equipment for welding treatment, and taking out the to-be-welded piece after the welding treatment is finished and naturally cooling the to-be-welded piece to room temperature.
Further, the deoiling liquid in the step (1) is an acetone solution with the mass fraction of 13%; and during the drying treatment, the temperature in the drying oven is controlled to be 72 ℃.
Further, during the irradiation treatment in the step (2), the irradiation power in the ultraviolet irradiation box is controlled to be 1300W, and the wavelength of ultraviolet rays is 300-320 nm.
Further, the mass fraction of the sulfuric acid solution in the operation a in the step (3) is 9%; the mass fraction of the sodium hydroxide solution is 13%.
Further, the mass fraction of the silane coupling agent solution in the operation c of the step (3) is 28%; the silane coupling agent is a silane coupling agent kh 560.
Further, the rare earth nitrate salt in the operation e of the step (3) is cerium nitrate.
Further, in the step (3), the atomizing gas used in the powder preparation by vacuum gas atomization in operation f is nitrogen.
Further, in the pressure sintering treatment in the operation g of the step (3), the pressure is controlled to be 64MPa, and the sintering temperature is 670 ℃; the heat treatment is to carry out homogenization heat treatment on the material, the temperature of the treatment is controlled to be 560 ℃, and the time duration is 11 hours; the rolling processing and the intermediate annealing treatment are to roll the heat-treated material for multiple times, and the intermediate annealing treatment is carried out between two times of rolling, wherein the temperature is controlled to be 550 ℃ during annealing, and the time duration is 2 hours.
Further, the vacuum degree in the vacuum brazing equipment is controlled to be 1-3 multiplied by 10 during the welding treatment in the step (5)-4Pa, the brazing temperature is 900 ℃, and the heat preservation time is 14 min.
Example 3
A high-strength brazing method for molybdenum-copper alloy and stainless steel comprises the following steps:
(1) surface cleaning treatment:
respectively putting the molybdenum-copper alloy and the stainless steel into degreasing liquid for soaking and degreasing, taking out after 15min, then putting into a drying oven for drying, taking out after 25min, and finally polishing with abrasive paper for later use;
(2) surface modification treatment:
placing the molybdenum-copper alloy and the stainless steel treated in the step (1) into an ultraviolet irradiation box for irradiation treatment, and taking out for later use after 40 min;
(3) preparing a brazing filler metal:
a. immersing attapulgite in a sulfuric acid solution for soaking for 6min, taking out the attapulgite, immersing the attapulgite in a sodium hydroxide solution for soaking for 8min, and finally taking out the attapulgite and washing the attapulgite with deionized water for one time for later use;
b. b, putting the attapulgite treated in the operation a into a calcining furnace for calcining, controlling the calcining temperature to be 750 ℃, keeping the temperature for calcining for 2 hours, and taking out for later use;
c. b, immersing the attapulgite treated in the operation b into a silane coupling agent solution for soaking for 25min, taking out and drying for later use;
d. mixing the attapulgite, the aluminum phosphate, the polyethylene glycol, the polyurea formaldehyde and the zinc stearate which are treated in the operation c correspondingly according to the weight ratio of 8:22:7:5:0.4, then putting the mixture into a temperature change box for temperature change treatment, firstly heating the temperature change box to 120 ℃, carrying out heat preservation treatment for 5min, then heating the temperature change box to 200 ℃, carrying out heat preservation treatment for 20min, then heating the temperature change box to 720 ℃, carrying out heat preservation treatment for 25min, and finally taking out the mixture and naturally cooling the mixture to room temperature to obtain a reactant A for later use;
e. weighing the following substances in parts by weight for later use: 85 parts of silver, 17 parts of copper, 3 parts of titanium, 4 parts of the reactant A prepared in the operation d, 0.2 part of nitric acid rare earth salt and 0.6 part of ethylene diamine tetraacetic acid disodium;
f. mixing the silver, the copper and the titanium weighed in the operation e together, putting the mixture into a vacuum smelting furnace, heating to keep the temperature in the vacuum smelting furnace at 1180 ℃, carrying out heat preservation treatment for 40min, then carrying out vacuum gas atomization for powder preparation, and taking out the mixture B for later use;
g. putting the mixture B prepared in the operation f and the reactant A prepared in the operation d, the rare earth nitrate and the disodium ethylene diamine tetraacetate, which are weighed in the operation e, into a ball mill together for ball milling and crushing, taking out after 35min, and finally preparing the brazing filler metal for later use through pressure sintering, heat treatment, calendaring and intermediate annealing;
(4) material clamping treatment:
placing the brazing filler metal prepared in the step (3) between the molybdenum-copper alloy treated in the step (2) and the to-be-welded surface of the stainless steel, assembling by using a clamp, controlling the sealing pressure to be 1.4MPa during the assembly, and obtaining a to-be-welded part for later use;
(5) welding treatment:
and (5) putting the to-be-welded piece treated in the step (4) into vacuum brazing equipment for welding treatment, and taking out the to-be-welded piece after the welding treatment is finished and naturally cooling the to-be-welded piece to room temperature.
Further, the deoiling liquid in the step (1) is an acetone solution with the mass fraction of 15%; and during the drying treatment, the temperature in the drying oven is controlled to be 75 ℃.
Further, during the irradiation treatment in the step (2), the irradiation power in the ultraviolet irradiation box is controlled to be 1400W, and the wavelength of ultraviolet rays is 300-320 nm.
Further, the mass fraction of the sulfuric acid solution in the operation a in the step (3) is 10%; the mass fraction of the sodium hydroxide solution is 14%.
Further, the mass fraction of the silane coupling agent solution in the operation c of the step (3) is 30%; the silane coupling agent is a silane coupling agent kh 570.
Further, the rare earth nitrate salt in the operation e of the step (3) is yttrium nitrate.
Further, in the step (3), the atomizing gas used in the powder preparation by vacuum gas atomization in operation f is nitrogen.
Further, in the pressure sintering treatment in the operation g of the step (3), the pressure is controlled to be 66MPa, and the sintering temperature is 680 ℃; the heat treatment is to carry out homogenization heat treatment on the material, the temperature of the treatment is controlled to be 580 ℃, and the time duration is 12 hours; the rolling processing and the intermediate annealing treatment are to roll the heat-treated material for multiple times, and the intermediate annealing treatment is carried out between two times of rolling, wherein the temperature is controlled to be 560 ℃ during annealing, and the time duration is 3 hours.
Further, the vacuum degree in the vacuum brazing equipment is controlled to be 1-3 multiplied by 10 during the welding treatment in the step (5)-4Pa, the brazing temperature is 920 ℃, and the heat preservation time is 16 min.
Comparative example 1
This comparative example 1 compares to example 2 in the step (3) solder preparation, the manufacture and use of the reactant a component obtained in operation d is omitted except that the process steps are the same.
Comparative example 2
Compared with the example 2, in the step (3), the use of rare earth nitrate and disodium ethylene diamine tetraacetate is omitted in the preparation of the brazing filler metal of the comparative example 2, except that the steps of the method are the same.
Control group
The application numbers are: CN201110429990.7 discloses a vacuum active brazing process of molybdenum-copper alloy and stainless steel.
In order to compare the effects of the invention, molybdenum-copper alloy with molybdenum mass fraction of 60% and copper mass fraction of 40% and 1Cr18Ni9Ti stainless steel are selected as experimental objects, and the length, width and thickness of the materials are controlled as follows: 30mm × 10mm × 3mm, then welding treatment is performed by the method corresponding to the above example 2, comparative example 1, comparative example 2 and control group, and finally performance test is performed on the welded parts after each group of treatment, wherein the specific comparative data are shown in the following table 1:
TABLE 1
Note: the weld performance tests described in table 1 above were all performed with reference to industry standards.
As can be seen from the above table 1, the welding treatment method of the invention can obviously improve the welding strength quality between the molybdenum-copper alloy and the stainless steel, obviously improve the welding stability and service life, and has great market competitiveness and popularization and application value.
Claims (9)
1. A high-strength brazing method for molybdenum-copper alloy and stainless steel is characterized by comprising the following steps:
(1) surface cleaning treatment:
respectively putting the molybdenum-copper alloy and the stainless steel into degreasing liquid for soaking and degreasing treatment, taking out after 10-15 min, then putting into a drying box for drying treatment, taking out after 20-25 min, and finally polishing with abrasive paper for later use;
(2) surface modification treatment:
placing the molybdenum-copper alloy and the stainless steel treated in the step (1) into an ultraviolet irradiation box for irradiation treatment, and taking out for later use after 30-40 min;
(3) preparing a brazing filler metal:
a. immersing attapulgite in a sulfuric acid solution for soaking for 4-6 min, taking out the attapulgite, immersing the attapulgite in a sodium hydroxide solution for soaking for 5-8 min, and finally taking out the attapulgite and washing the attapulgite with deionized water for later use;
b. b, placing the attapulgite treated in the operation a into a calcining furnace for calcining, controlling the calcining temperature to be 700-750 ℃, and taking out for later use after heat preservation and calcination for 1-2 hours;
c. b, immersing the attapulgite treated in the operation b into a silane coupling agent solution for soaking for 20-25 min, taking out and drying for later use;
d. mixing the attapulgite, the aluminum phosphate, the polyethylene glycol, the polyurea formaldehyde and the zinc stearate which are treated in the operation c according to a weight ratio of 6-8: 18-22: 5-7: 2-5: 0.2-0.4, then putting the mixture into a temperature changing box for temperature changing treatment, firstly heating the temperature changing box to 110-120 ℃, carrying out heat preservation treatment for 3-5 min, then heating the temperature changing box to 180-200 ℃, carrying out heat preservation treatment for 15-20 min, then heating the temperature changing box to 690-720 ℃, carrying out heat preservation treatment for 20-25 min, and finally taking out and naturally cooling to room temperature to obtain a reactant A for later use;
e. weighing the following substances in parts by weight for later use: 80-85 parts of silver, 13-17 parts of copper, 1-3 parts of titanium, 2-4 parts of reactant A prepared in the operation d, 0.1-0.2 part of rare earth nitrate salt and 0.3-0.6 part of disodium ethylene diamine tetraacetate;
f. mixing the silver, the copper and the titanium weighed in the operation e together, putting the mixture into a vacuum smelting furnace, heating the mixture to keep the temperature in the vacuum smelting furnace at 1150-1180 ℃, carrying out heat preservation treatment for 35-40 min, then carrying out vacuum gas atomization for powder preparation, and taking out the powder to obtain a mixture B for later use;
g. putting the mixture B prepared in the operation f and the reactant A prepared in the operation d, the rare earth nitrate and the disodium ethylene diamine tetraacetate, which are weighed in the operation e, into a ball mill together for ball milling and crushing, taking out after 30-35 min, and finally preparing the brazing filler metal for later use through pressure sintering, heat treatment, calendaring and intermediate annealing;
(4) material clamping treatment:
placing the brazing filler metal prepared in the step (3) between the molybdenum-copper alloy treated in the step (2) and the to-be-welded surface of the stainless steel, and then assembling by using a clamp, wherein the sealing pressure is controlled to be 1-1.4 MPa, so that a to-be-welded part is obtained for later use;
(5) welding treatment:
and (5) putting the to-be-welded piece treated in the step (4) into vacuum brazing equipment for welding treatment, and taking out the to-be-welded piece after the welding treatment is finished and naturally cooling the to-be-welded piece to room temperature.
2. The high-strength brazing method for the molybdenum-copper alloy and the stainless steel according to claim 1, wherein the degreasing liquid in the step (1) is an acetone solution with the mass fraction of 10-15%; and during drying treatment, the temperature in the drying oven is controlled to be 70-75 ℃.
3. The high-strength brazing method for the molybdenum-copper alloy and the stainless steel according to claim 1, wherein the irradiation power in the ultraviolet irradiation box is controlled to be 1200-1400W during the irradiation treatment in the step (2), and the wavelength of the ultraviolet is controlled to be 300-320 nm.
4. The high-strength brazing method for the molybdenum-copper alloy and the stainless steel according to claim 1, wherein the mass fraction of the sulfuric acid solution in the operation a in the step (3) is 7-10%; the mass fraction of the sodium hydroxide solution is 12-14%.
5. The high-strength brazing method for the molybdenum-copper alloy and the stainless steel according to claim 1, wherein the silane coupling agent solution in the operation c of the step (3) is 25-30% by mass; the silane coupling agent is any one of a silane coupling agent kh550, a silane coupling agent kh560 and a silane coupling agent kh 570.
6. The high-strength brazing method for the molybdenum-copper alloy and the stainless steel according to claim 1, wherein the rare earth nitrate in the operation e in the step (3) is any one of lanthanum nitrate, cerium nitrate and yttrium nitrate.
7. The method for brazing Mo-Cu alloy and stainless steel with high strength as claimed in claim 1, wherein the atomizing gas used in step (3) is nitrogen gas.
8. The high-strength brazing method for the molybdenum-copper alloy and the stainless steel according to claim 1, wherein the pressure sintering treatment in the operation g of the step (3) is carried out under the conditions that the pressure is controlled to be 62-66 MPa and the sintering temperature is 650-680 ℃; the heat treatment is to carry out homogenization heat treatment on the material, the temperature of the heat treatment is controlled to be 550-580 ℃, and the time duration is 10-12 hours; the rolling processing and the intermediate annealing treatment are to roll the heat-treated material for multiple times, and the intermediate annealing treatment is carried out between two times of rolling, wherein the temperature is controlled to be 530-560 ℃ during the intermediate annealing, and the time duration is 1-3 h.
9. The high-strength brazing method for Mo-Cu alloy and stainless steel as claimed in claim 1, wherein the degree of vacuum in the vacuum brazing apparatus is controlled to be 1-3X 10 during the welding process in step (5)-4Pa, the brazing temperature is 880-920 ℃, and the heat preservation time is 12-16 min.
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