CN109570669B - Preparation method of multilayer high-temperature-resistant composite anode - Google Patents
Preparation method of multilayer high-temperature-resistant composite anode Download PDFInfo
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- CN109570669B CN109570669B CN201811585145.7A CN201811585145A CN109570669B CN 109570669 B CN109570669 B CN 109570669B CN 201811585145 A CN201811585145 A CN 201811585145A CN 109570669 B CN109570669 B CN 109570669B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/0008—Soldering, e.g. brazing, or unsoldering specially adapted for particular articles or work
Abstract
The invention discloses a preparation method of a multilayer high-temperature-resistant composite anode, which comprises the following steps: respectively preparing a first metal layer, a second metal layer and a nonmetal layer according to a target product composite anode, and sequentially stacking from top to bottom; secondly, adding a first brazing filler metal between the stacking surfaces of the first metal layer and the second metal layer; thirdly, adding a second brazing filler metal between the non-metal layer and the stacking surface of the second metal added with the first brazing filler metal to obtain a composite anode pre-welded part; and fourthly, carrying out high-temperature vacuum hot-press welding on the composite anode prewelded part to form a transition layer between the second metal layer and the non-metal layer, and then processing to obtain the composite anode. The method comprises the steps of processing each layer of the composite anode, then sequentially stacking each layer, adding brazing filler metal between each layer, and carrying out vacuum hot-press welding to obtain the composite anode, wherein the interfaces of each layer are in regular transition and clear by utilizing high-temperature diffusion connection between each layer, so that the high-temperature resistance of the composite anode is ensured, and the dynamic balance deviation of the composite anode is reduced.
Description
Technical Field
The invention belongs to the technical field of preparation of anode materials, and particularly relates to a preparation method of a multilayer high-temperature-resistant composite anode.
Background
When the X-ray tube of the CT machine works, more than 98 percent of energy of the anode target is converted into heat energy while the anode target is bombarded by electrons to generate X-rays, and the heat is mainly concentrated on the anode. The heat is distributed on the rotating anode target surface with a certain inclination angle to form a circular ring-shaped heated area. Because the rotary anode is used in a vacuum environment and under the condition of alternating thermal load, the temperature of the whole anode target body can be increased to be very high when the load is continuously loaded, the environment temperature of the X-ray tube during working is above 1300 ℃, and the heat dissipation mainly depends on thermal radiation. The metal tungsten has the advantages of high melting point, low vapor pressure, large density, high atomic number and the like, can ensure that a large amount of X rays are generated under the bombardment of electron beams, and can be used as an anode material; however, pure tungsten has a small heat capacity and poor heat dissipation. Graphite has high heat capacity and heat dissipating capacity, and very high heat stress resistance. The W/Mo composite layer is connected with the three-high graphite with different thicknesses to form a whole, so that the volume and the weight of the anode can be reduced to a great extent, and the service life of the anode is prolonged.
In the aspect of X-ray anode preparation, little intellectual property rights and literature of related technologies are published at home and abroad, and CN101290852A is formed by one-step sintering at high temperature by using a powder metallurgy process and graphite; US4119879 adds rare earth elements between tungsten and molybdenum layers as transition layers; CN102124537A, CN103050357A and CN 104350574A all focus on the material and structure design of the substrate. In the aspect of the technology of connecting refractory metal molybdenum and molybdenum alloy with graphite, CN102240836B adds foil brazing filler metal and the method for increasing the roughness of the graphite surface is used for welding; the welding methods of molybdenum and its alloy and graphite involved in the foreign patents such as US2002/0085678a1, US2011/0103553a1, US2011/0103553a1, US2011/008059785B2, JP2010-140879a and the like are all used for brazing by adding different elements and different adding forms, including powder, foil, plating and the like.
The dynamic balance yield of the product obtained by the method is poor, and the introduction of new elements under high-temperature work inevitably causes the problems of product pollution, material high-temperature service life reduction and the like.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for preparing a multilayer high temperature resistant composite anode, aiming at the defects of the prior art. The method comprises the steps of processing all layers of the composite anode, then sequentially stacking all layers, adding brazing filler metal between all layers, and carrying out vacuum hot-press welding to obtain the composite anode finally.
In order to solve the technical problems, the invention adopts the technical scheme that: a preparation method of a multilayer high-temperature-resistant composite anode is characterized by comprising the following steps:
step one, respectively preparing a first metal layer, a second metal layer and a nonmetal layer according to a target product composite anode, and sequentially stacking from top to bottom; the first metal layer is made of tungsten or tungsten alloy, the second metal layer is made of molybdenum or molybdenum alloy, and the nonmetal layer is made of graphite;
step two, adding a first brazing filler metal between the stacking surfaces of the first metal layer and the second metal layer in the step one;
step three, adding a second brazing filler metal between the non-metal layer in the step one and the stacking surface of the second metal added with the first brazing filler metal in the step two to obtain a composite anode pre-welded part;
and step four, carrying out high-temperature vacuum hot-press welding on the composite anode prewelded part obtained in the step three, forming a transition layer between the second metal layer and the nonmetal layer after welding, and then processing to obtain the multi-layer high-temperature-resistant composite anode which is degassed at the high temperature of 1600 ℃ and has no abnormal volatilization.
According to the invention, each layer forming the composite anode is machined and formed according to a target product composite anode, then each layer is sequentially stacked, and brazing filler metal is added between each layer for vacuum hot-press welding, so that the composite anode is finally obtained.
The preparation method of the multilayer high-temperature-resistant composite anode is characterized in that in the step one, the surface roughness of the stacking surface of the first metal layer and the second metal layer, the surface roughness of the stacking surface of the second metal layer and the first metal layer, the surface roughness Ra of the stacking surface of the second metal layer and the non-metal layer is less than or equal to 1.6, and the surface roughness Ra of the stacking surface of the non-metal layer and the second metal layer is less than or equal to 3.2. By limiting the surface roughness of the stacking surfaces, the impurity gas entering in the subsequent welding process is effectively reduced, the atomic diffusion distance between the stacking surfaces of all layers is favorably reduced, and meanwhile, the bonding surface of a weldment is ensured not to generate pores.
The preparation method of the multilayer high-temperature-resistant composite anode is characterized in that in the second step, the first brazing filler metal is nano powder, the nano powder is nano tungsten powder or nano molybdenum powder, and the particle size of the nano powder is not more than 200 nm; the first brazing filler metal is added in a mode of brushing or pasting, and the thickness of the first brazing filler metal is not more than 0.1 mm. The nano powder as the brazing filler metal has the characteristic of high activity, and can realize solid-phase metallurgy at a lower temperature, thereby realizing the solid-phase connection of two matrixes. According to the invention, the nano tungsten powder or the nano molybdenum powder is used as the first brazing filler metal, so that the connection effect between the first metal layer and the second metal layer is effectively improved, meanwhile, impurity elements are prevented from being introduced, and the high-temperature cleanliness and the high-temperature working stability of the composite anode are ensured; the adoption is brushed or is scribbled the cream mode and is favorable to the even interpolation of first brazing filler metal, with the thickness control of first brazing filler metal for no more than 0.1mm, has both guaranteed the firm connection between first metal level and the second metal level, has avoided the metallurgical pore that first brazing filler metal excessively thick formed to be unfavorable for the connection between first metal level and the second metal level again.
The preparation method of the multilayer high-temperature-resistant composite anode is characterized in that in the third step, the second brazing filler metal is graphene or superfine graphite powder, and the particle size of the second brazing filler metal is not more than 1 micron; the second brazing filler metal is added in a spraying or paste coating mode, and the thickness of the second brazing filler metal is not more than 0.1 mm. According to the invention, graphene or superfine graphite powder with high activity is used as the second brazing filler metal, so that the diffusion activation energy is effectively reduced, a diffusion channel is opened, carbon elements in the non-metal layer are induced to be rapidly diffused to the second metal layer, and the stable connection between the second metal layer and the non-metal layer is promoted; the mode of spraying or pasting is favorable for uniformly adding the second brazing filler metal, and the thickness of the second brazing filler metal is controlled to be not more than 0.1mm, so that the stable connection between the nonmetal layer and the second metal layer is ensured, the phenomenon that the second brazing filler metal layer taking carbide as a main component is too thick and presents obvious brittleness characteristic is avoided, and the welding strength and the processing performance of the subsequent composite anode are adversely affected.
The preparation method of the multilayer high-temperature-resistant composite anode is characterized in that the vacuum degree of the high-temperature vacuum hot-press welding in the fourth step is not more than 10-1Pa, the pressure is 10 MPa-30 MPa, the temperature is 1700-2000 ℃, the heat preservation time is 1-3 h, the heating rate of the high-temperature vacuum hot-pressing welding is 5 ℃/min-10 ℃/min, and the cooling rate after heat preservation is not more than 15 ℃/min. The O, N existing in the welding line and the oxidizing gas generated by reaction in the high-temperature vacuum hot-pressing welding process are effectively discharged through the stricter vacuum degree requirement, and the quality of the composite anode is improved; the temperature and the pressure of the high-temperature vacuum hot-pressing welding ensure the diffusion effect between the first metal layer and the second metal layer and between the second metal layer and the nonmetal layer, and the welding temperature is far higher than the service temperature of the composite anode of 1300 ℃, so that the problems of liquid phase and phase change in the service process of the composite anode are effectively avoided; the vacuum degree, the pressure, the temperature, the heat preservation time and the temperature rising and falling speed of the high-temperature vacuum hot-pressing welding are matched with each other, and finally the smooth proceeding of the high-temperature vacuum hot-pressing welding process is realized.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, each layer forming the composite anode is machined and formed according to a target product composite anode, then each layer is sequentially stacked, and brazing filler metal is added between each layer for vacuum hot-press welding, so that the composite anode is finally obtained.
2. The invention takes nano tungsten powder or nano molybdenum powder as the first brazing filler metal connected between the first metal layer and the second metal layer, and the nano powder has the characteristic of high activity, so that solid phase metallurgy can be realized at a lower temperature, the metallurgical temperature between the first metal layer and the second metal layer is effectively reduced, the efficiency of subsequent vacuum hot-press welding is improved, and simultaneously, because the components of the nano powder are the same as those of the first metal layer or the second metal layer, elements with low melting points and elements which can possibly produce eutectic melting reduction are not introduced, the high-temperature cleanliness and the high-temperature working stability of the composite anode are effectively ensured, and the service life of the composite anode is prolonged.
3. According to the invention, the active graphene or the active ultrafine graphite powder is used as a second brazing filler metal connected between the second metal layer and the nonmetal layer, under the high-temperature and high-pressure conditions of subsequent vacuum hot-press welding, the active graphene or the active ultrafine graphite powder reacts with molybdenum or molybdenum alloy in the second metal layer, C element diffuses into the second metal layer matrix crystal through a gap diffusion mechanism, and simultaneously C element diffuses into microscopic defect parts such as crystal boundaries and pores of the second metal layer matrix through a rapid channel diffusion mechanism, so that a diffusion channel is rapidly opened to play a role in inducing diffusion, the nonmetal layer can rapidly form diffusion connection with the second metal layer, the effective connection between the nonmetal layer and the second metal layer is realized, no new element is added, no impurity is introduced, and the welding strength of a welding surface is effectively ensured.
4. In the high-temperature vacuum hot-pressing welding process, the welding temperature of the first metal layer and the second metal layer and the welding temperature of the second metal layer and the nonmetal layer are taken into consideration, the welding is carried out at the high temperature of more than 1700 ℃, the specific pressure, the temperature rise and fall rate and the heat preservation time are adopted, the welding temperature is far higher than the service temperature (1300 ℃) of the composite anode, and the high-temperature service performance of the composite anode is effectively ensured; the pressure and the heat preservation time adopted by the high-temperature vacuum hot-pressing welding solve the problems of insufficient driving force, no diffusion or insufficient diffusion caused by interface pores and the like in the welding process, so that the welding strength is influenced and the like.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
Fig. 1 is a schematic view of vacuum thermocompression bonding of a composite anode pre-welded part in example 1 of the present invention.
FIG. 2 is a phase diagram of a Mo-C binary alloy in the composite anode in example 1 of the present invention.
Fig. 3 is a partial sectional view of a composite anode prepared in example 1 of the present invention.
Fig. 4 is a schematic view of vacuum thermocompression bonding of the composite anode pre-welded part in example 2 of the present invention.
Description of the reference numerals
1 — a first metal layer; 2-a second metal layer; 3-a non-metallic layer;
4-a first brazing filler metal; 5-second brazing filler metal; and 6, welding the tool.
Detailed Description
Example 1
The preparation method of this example includes the following steps:
firstly, according to a target product, a tungsten circular plate with the diameter of 110mm and the thickness of 10mm is taken to be machined to obtain a first metal layer 1, the superposed surface of the first metal layer and a second metal layer is polished to the roughness Ra of 1.6, a molybdenum circular plate with the diameter of 110mm and the thickness of 10mm is taken to be machined to obtain a second metal layer 2, the upper surface and the lower surface of the second metal layer are polished to the roughness Ra of 1.6, a three-high graphite disk with the diameter of 110mm and the thickness of 40mm is taken to be machined to obtain a non-metal layer 3, the surface of the non-metal layer is polished to the roughness Ra of 3.2, and then the non-metal layer and the non-metal layer are sequentially superposed from top to bottom;
step two, the first brazing filler metal 4 is adjusted to be pasty and smeared on the upper surface of the second metal layer 2, and the smearing thickness is controlled to be 0.1 mm; the first brazing filler metal 4 adopts nano molybdenum powder with the granularity of 200 nm;
thirdly, spraying a second brazing filler metal 5 on the lower surface of the second metal layer 2, and controlling the coating thickness to be 0.05mm to obtain a composite anode prewelded part; the second brazing filler metal 5 adopts superfine graphite powder with the granularity of 1 mu m;
step four, placing the composite anode prewelded part obtained in the step three in a welding tool 6 for vacuum hot-press welding, as shown in fig. 1, wherein an arrow in fig. 1 indicates the direction of pressure F, forming a transition layer between the second metal layer and the nonmetal layer after welding, and processing to obtain the composite anode; the vacuum degree of the vacuum hot-press welding is 10-1Pa, the pressure is 30MPa, the temperature is 1700 ℃, the heat preservation time is 3h, the heating rate of the vacuum hot-press welding is 5 ℃/min, and the cooling rate after heat preservation is 15 ℃/min.
Fig. 2 is a phase diagram of a Mo-C binary alloy in the composite anode in example 1 of the present invention, and it can be seen from fig. 2 that C and Mo have good reaction and solid solution intervals, and in the Mo-C binary alloy having a carbon content of 10 wt%, MoC, β' solid solution are used as main products, and the composition of the products provides a good theoretical basis for the combination of molybdenum and graphite.
Fig. 3 is a partial cross-sectional view of the composite anode prepared in this embodiment, and it can be seen from fig. 3 that the composite anode prepared in this embodiment has a good appearance, the bonding layer of the tungsten layer and the molybdenum layer is flat and clear, the transition layer exists between the bonding layer of the molybdenum layer and the graphite layer, the transition between the molybdenum layer and the graphite layer is good, and the interface is flat and clear.
Through detection, the composite anode prepared by the embodiment has no abnormal volatilization after degassing at high temperature of 1600 ℃, no obvious change in the structure of a parent metal, no abnormal growth, no impurity pollution, no obvious pores on an interface, 1.3g.cm of dynamic balance before weight removal and good dynamic balance performance.
Example 2
The preparation method of this example includes the following steps:
firstly, according to a target product, a tungsten-rhenium alloy circular plate with the diameter of 110mm and the thickness of 10mm is taken to be machined to obtain an annular first metal layer 1, the superposed surface of the annular first metal layer 1 and a second metal layer is polished to the roughness Ra of 0.8, a TZM circular plate with the diameter of 110mm and the thickness of 40mm is taken to be machined to obtain a second metal layer 2, the upper surface and the lower surface of the second metal layer are polished to the roughness Ra of 0.8, a three-high graphite circular plate with the diameter of 110mm and the thickness of 40mm is taken to be machined to obtain a non-metal layer 3, the surface of the non-metal layer is polished to the roughness Ra of 1.6, and then the non-metal layer and the non-metal layer are sequentially superposed from top to bottom;
step two, the first brazing filler metal 4 is adjusted to be pasty and smeared on the upper surface of the second metal layer 2, and the smearing thickness is controlled to be 0.05 mm; the first brazing filler metal 4 adopts nano tungsten powder with the granularity of 100 nm;
step three, adjusting the second brazing filler metal 5 to be pasty and coating the second brazing filler metal on the lower surface of the second metal layer 2, and controlling the coating thickness to be 0.1mm to obtain a composite anode pre-welded part; the second brazing filler metal 5 is made of graphene with the granularity of 0.2 mu m;
step four, placing the composite anode prewelded part obtained in the step three in a welding tool 6 for vacuum hot-press welding, as shown in fig. 4, wherein an arrow in fig. 4 indicates the direction of pressure F, forming a transition layer between the second metal layer and the nonmetal layer after welding, and processing to obtain the composite anode; the vacuum degree of the vacuum hot-press welding is 10-2Pa, the pressure is 20MPa, the temperature is 1900 ℃, the heat preservation time is 1.5h, the heating rate of the vacuum hot-press welding is 6 ℃/min, and the cooling rate after heat preservation is 10 ℃/min.
Through detection, the composite anode prepared by the embodiment has no abnormal volatilization after degassing at high temperature of 1600 ℃, no obvious change in the structure of the parent metal, no abnormal growth, no impurity pollution, no obvious pores on the interface, 1.4g.cm of dynamic balance before weight removal and good dynamic balance performance.
Example 3
The preparation method of this example includes the following steps:
according to a target product, a tungsten-rhenium alloy circular plate with the diameter of 150mm and the thickness of 10mm is taken to be machined to obtain an annular first metal layer 1, the superposed surface of the annular first metal layer 1 and a second metal layer is polished to the roughness Ra of 0.8, a TZM circular plate with the diameter of 150mm and the thickness of 30mm is taken to be machined to obtain a second metal layer 2, the upper surface and the lower surface of the second metal layer are polished to the roughness Ra of 0.8, a three-high graphite circular plate with the diameter of 150mm and the thickness of 60mm is taken to be machined to obtain a non-metal layer 3, the surface of the non-metal layer is polished to the roughness Ra of 1.6, and then the non-metal layer and the non-metal layer are sequentially superposed from top to bottom;
step two, adjusting the first brazing filler metal 4 to be emulsion-coated on the upper surface of the second metal layer 2, and controlling the coating thickness to be 0.05 mm; the first brazing filler metal 4 adopts nano tungsten powder with the granularity of 100 nm;
step three, adjusting the second brazing filler metal 5 to be pasty and coating the second brazing filler metal on the lower surface of the second metal layer 2, and controlling the coating thickness to be 0.1mm to obtain a composite anode pre-welded part; the second brazing filler metal 5 adopts superfine graphite powder with the granularity of 0.5 mu m;
step four, placing the composite anode prewelded part obtained in the step three in a welding tool 6 for vacuum hot-press welding, as shown in fig. 4, wherein an arrow in fig. 4 indicates the direction of pressure F, forming a transition layer between the second metal layer and the nonmetal layer after welding, and processing to obtain the composite anode; the vacuum degree of the vacuum hot-press welding is 10-2Pa, the pressure is 10MPa, the temperature is 2000 ℃, the heat preservation time is 1h, the heating rate of the vacuum hot-press welding is 10 ℃/min, and the cooling rate after heat preservation is 10 ℃/min.
Through detection, the composite anode prepared by the embodiment has no abnormal volatilization after degassing at high temperature of 1600 ℃, no obvious change in the structure of the parent metal, no abnormal growth, no impurity pollution, no obvious pores on the interface, 2.7g.cm of dynamic balance before weight removal and good dynamic balance performance.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (3)
1. A preparation method of a multilayer high-temperature-resistant composite anode is characterized by comprising the following steps:
step one, respectively preparing a first metal layer (1), a second metal layer (2) and a nonmetal layer (3) according to a target product composite anode, and sequentially stacking from top to bottom; the first metal layer (1) is made of tungsten or tungsten alloy, the second metal layer (2) is made of molybdenum or molybdenum alloy, and the nonmetal layer (3) is made of graphite;
step two, adding a first brazing filler metal (4) between the stacking surfaces of the first metal layer (1) and the second metal layer (2) in the step one; the first brazing filler metal (4) is nano powder, the nano powder is nano tungsten powder or nano molybdenum powder, and the particle size of the nano powder is not more than 200 nm; the first brazing filler metal (4) is added in a mode of brushing or pasting, and the thickness of the first brazing filler metal (4) is not more than 0.1 mm;
step three, adding a second brazing filler metal (5) between the non-metal layer (3) in the step one and the stacking surface of the second metal (2) added with the first brazing filler metal (4) in the step two to obtain a composite anode pre-welded part; the second brazing filler metal (5) is graphene or superfine graphite powder, and the granularity of the second brazing filler metal (5) is not more than 1 mu m; the second brazing filler metal (5) is added in a spraying or paste coating mode, and the thickness of the second brazing filler metal (5) is not more than 0.1 mm;
and step four, carrying out high-temperature vacuum hot-press welding on the composite anode prewelded part obtained in the step three, forming a transition layer between the second metal layer (2) and the nonmetal layer (3) after welding, and then processing to obtain the multi-layer high-temperature-resistant composite anode which is degassed at the high temperature of 1600 ℃ and has no abnormal volatilization.
2. The preparation method of the multilayer high temperature resistant composite anode according to claim 1, wherein in the first step, the surface roughness of the stacking surface of the first metal layer (1) and the second metal layer (2), the surface roughness of the stacking surface of the second metal layer (2) and the first metal layer (1), the surface roughness Ra of the stacking surface of the second metal layer (2) and the non-metal layer (3) is less than or equal to 1.6, and the surface roughness Ra of the stacking surface of the non-metal layer (3) and the second metal layer (2) is less than or equal to 3.2.
3. The method for preparing the multilayer high-temperature-resistant composite anode according to claim 1, wherein the vacuum degree of the high-temperature vacuum hot-pressing welding in the fourth step is not more than 10-1Pa, the pressure is 10 MPa-30 MPa, the temperature is 1700-2000 ℃, the heat preservation time is 1-3 h, the heating rate of the high-temperature vacuum hot-pressing welding is 5 ℃/min-10 ℃/min, and the cooling rate after heat preservation is not more than 15 ℃/min.
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