CN117881071A - Composite superconducting cavity with aluminum coated on niobium substrate and preparation method and application thereof - Google Patents

Composite superconducting cavity with aluminum coated on niobium substrate and preparation method and application thereof Download PDF

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Publication number
CN117881071A
CN117881071A CN202410003821.4A CN202410003821A CN117881071A CN 117881071 A CN117881071 A CN 117881071A CN 202410003821 A CN202410003821 A CN 202410003821A CN 117881071 A CN117881071 A CN 117881071A
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aluminum
cavity
niobium
composite superconducting
pure
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徐孟鑫
何源
王志军
张升学
刘鲁北
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Institute of Modern Physics of CAS
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Institute of Modern Physics of CAS
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E40/00Technologies for an efficient electrical power generation, transmission or distribution
    • Y02E40/60Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment

Abstract

The invention discloses a composite superconducting cavity with aluminum covered on a niobium substrate, and a preparation method and application thereof. The invention provides an aluminum-niobium composite superconducting cavity, which comprises the following components: a pure niobium substrate cavity, an aluminum cladding layer, and a mesophase layer between the pure niobium substrate cavity and the aluminum cladding layer. The aluminum-niobium composite superconducting cavity has the advantages of high mechanical stability and thermal stability, light weight, low manufacturing cost, simple manufacturing process and the like.

Description

Composite superconducting cavity with aluminum coated on niobium substrate and preparation method and application thereof
Technical Field
The invention belongs to the technical field of particle accelerators and radio frequency superconductors, and particularly relates to a composite superconducting cavity with aluminum coated on a niobium substrate, and a preparation method and application thereof.
Background
The radio frequency superconducting resonant cavity (superconducting cavity for short) is a core acceleration unit of the superconducting particle accelerator, and is used for providing energy for charged particles. At present, a pure niobium superconducting cavity is widely used for various large devices, but has the following defects in operation: 1. the cavity wall of the pure niobium superconducting cavity is thinner and is usually not more than 3-4mm, the vibration of a low-temperature station and the fluctuation of liquid helium can cause the fluctuation of the superconducting cavity wall, so that the mechanical stability of the cavity is affected, and frequency detuning is easy to cause; 2. the heat conduction capability of the cavity wall of the pure niobium superconducting cavity is poor, the local heating of the superconducting cavity cannot be transmitted to liquid helium in time, and the phenomenon of thermal instability is easily caused; if the wall thickness is increased to improve the mechanical stability, the heat conductivity of the superconducting cavity is further reduced, so that the problem of serious heat instability is caused, and meanwhile, the cost of the niobium cavity is greatly increased due to the fact that the niobium is high in price; in addition, the helium tank using the liquid cooling method is relatively expensive to manufacture.
In order to overcome the defects, a superconducting cavity (copper-niobium composite cavity for short) manufactured based on a copper-niobium composite material becomes one of hot spots for research in recent years, and is mainly characterized in that the high heat conductivity of copper is utilized, and the operation mechanical stability and the heat stability of the superconducting cavity are improved on the basis of ensuring good heat conduction of the superconducting cavity by increasing the wall thickness (6 mm) of the cavity, such as CN113373483A. However, the copper-niobium composite cavity has the advantages and brings new problems: firstly, copper is high in specific gravity, so that the copper-niobium composite cavity is large in weight, a certain difficulty is caused to subsequent processing and assembly of the cavity, and the mechanical size and frequency control difficulty of the cavity in the copper layer thickening process are large because the weight of the copper layer is far greater than that of the niobium layer; second, copper is expensive; thirdly, as copper and niobium are not mutually dissolved, the binding force between the electroplated oxygen-free copper layer and the outer surface of the pure niobium cavity can not meet the practical requirement, and a layer of eutectic copper layer with good binding force is deposited on the outer surface of the pure niobium cavity, and then the oxygen-free copper layer is electroplated on the outer surface of the copper layer, the manufacturing difficulty of the copper-niobium composite cavity is very high, and the manufacturing period is overlong.
For this purpose, the present invention has been made.
Disclosure of Invention
The invention aims to provide a composite superconducting cavity with aluminum covered on a niobium substrate, which has higher mechanical stability and thermal stability and overcomes the problems of heavy weight, high price and complex manufacturing process of a copper-niobium composite cavity.
In order to achieve the above purpose, the present invention provides the following technical solutions:
in a first aspect, the present invention provides an aluminum niobium composite superconducting cavity comprising the following components: the device comprises a pure niobium substrate cavity, an aluminum coating layer positioned on the surface layer and a middle phase layer between the pure niobium substrate cavity and the aluminum coating layer.
The thickness of the intermediate phase layer is 25-35 mu m.
The thickness of the aluminum coating layer is 5-10mm.
The pure niobium substrate cavity is made of a niobium material with RRR > 300.
The pure niobium substrate cavity is prepared by adopting a conventional superconducting cavity preparation process in the field.
In a second aspect, the present invention further provides a method for preparing the aluminum-niobium composite superconducting cavity, which includes the following steps:
s1, roughening the surface of a pure niobium substrate cavity;
s2, assembling the roughened pure niobium substrate cavity with a hot-cast aluminum die and a cooling pipeline to form an assembly body with a cavity;
and S3, filling aluminum materials into the cavity of the assembly body, and performing hot casting to obtain the aluminum-niobium composite superconducting cavity.
In the step S1, the mesh number of the sand paper used in the roughening treatment is 80-180 meshes. The roughening treatment aims to increase the contact area between aluminum water and the surface of the pure niobium substrate cavity.
In step S1, cleaning and drying the pure niobium substrate cavity after roughening treatment.
The cleaning is ultrasonic cleaning to remove surface impurities.
The cleaning liquid used for cleaning is prepared from high-purity water with the resistivity of 18.2MΩ & cm and Micro90 cleaning agent according to the volume ratio of 100:1 concentration.
And heating the cleaning liquid, and then carrying out ultrasonic cleaning on the pure niobium substrate cavity.
In step S2, the materials of the hot-cast aluminum mold and the cooling pipe are stainless steel, such as 304 stainless steel.
In step S2, the assembly is performed according to the following steps: and fixing the cooling pipeline clamp on the pure niobium substrate cavity, and then installing the hot-cast aluminum die on the surface of the pure niobium substrate cavity, wherein an aluminum-coated cavity structure with the thickness of 5-10mm is formed between the hot-cast aluminum die and the pure niobium substrate cavity.
In the step S3, the aluminum material is aluminum powder with the purity of 99.99 percent or aluminum particles with the particle size of less than 10mm.
In step S3, the hot casting is performed in a high vacuum annealing furnace; the conditions of the hot casting are as follows: the temperature is 700-800 ℃, preferably 780 ℃, and the time is 3-5h, preferably 3h.
The preparation method further comprises the following steps: and (3) cooling the aluminum-niobium composite superconducting cavity obtained in the step (S3) to 80 ℃, opening the furnace, taking out, removing the hot-cast aluminum die, welding a cavity flange and a liquid helium pipeline interface flange, and carrying out finish machining on the cavity mounting support.
In a third aspect, the present invention further provides a superconducting particle accelerator comprising the above aluminum-niobium composite superconducting cavity.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention provides the high-purity aluminum as the cladding material of the pure niobium substrate cavity for the first time, and the high heat conductivity of the high-purity aluminum can be utilized to improve the operation mechanical stability and the heat stability of the superconducting cavity on the basis of ensuring the good heat conduction of the superconducting cavity by increasing the wall thickness of the cavity; meanwhile, the specific gravity of aluminum is smaller, so that the weight of the composite superconducting cavity can be greatly reduced on the premise of the same wall thickness, and the subsequent surface treatment, testing, assembly and transportation and the like are convenient; in addition, the price of aluminum is low, and the cost of the preparation raw materials of the composite superconducting cavity can be reduced.
2. According to the invention, the composite superconducting cavity is prepared by adopting a high-temperature hot casting process, and an aluminum coating layer is formed, so that an intermediate phase is formed between the outer coating aluminum material and the bottom cavity niobium material, and the bonding strength between the aluminum coating layer and the bottom cavity is obviously improved; meanwhile, compared with a composite process of depositing a copper layer and then electroplating an oxygen-free copper layer adopted by the copper-niobium composite cavity, the invention greatly simplifies the composite process and obtains the composite cavity with high bonding strength by one-step method; in addition, the hot casting temperature of the invention is lower than the recrystallization temperature of the niobium material, and the crystal grain growth of the pure niobium substrate cavity is not caused in the hot casting process, so that the conditions that the high-frequency surface roughness of the cavity is large and the running performance of the cavity is influenced due to the fact that the large crystal grain is polished again by acid liquor are avoided.
3. The hot-casting aluminum of the invention has simple process and short period, one heating period is different according to the size of the furnace and the size of the cavity, 1 to 5 composite superconducting cavities can be hot-cast, and the time period is not longer than one week; in addition, the hot casting die can be made of stainless steel materials, the material cost is low, the cast aluminum die can be reused for mass production, and the production cost is greatly reduced.
In conclusion, the aluminum-niobium composite superconducting cavity provided by the invention can stably operate with high acceleration gradient, and meanwhile, the construction cost and the operation cost of the accelerator are reduced.
Drawings
FIG. 1 is an assembly drawing of a process die and a pure niobium substrate cavity for aluminum cladding outside a 1.3GHz single cell aluminum niobium composite superconducting cavity provided in example 1.
Fig. 2 is a graph comparing the results of thermal conductivity testing of aluminum niobium composite samples.
FIG. 3 is a graph comparing tensile strength test results of high purity aluminum, high purity niobium, and aluminum niobium composite samples; in the figure: a) Representing the relationship between the tensile distance and the stress; b) Representing stress and strain testing of the casting process.
FIG. 4 is a scanning image of the electron microscope scanning interface morphology and EDS bonding interface line of the aluminum-niobium composite sample; in the figure: the left image is the form of the scanning interface of the electron microscope; the right panel shows the EDS combined interface line scan results.
Detailed Description
The invention will be further illustrated with reference to the following specific examples, but the invention is not limited to the following examples.
The experimental methods used in the following examples are conventional methods unless otherwise specified.
Reagents, materials, instruments and the like used in the examples described below are commercially available unless otherwise specified.
Examples, preparation of aluminum niobium composite superconducting Cavity
The embodiment provides a preparation method of a 1.3GHz single cell ellipsoidal aluminum niobium composite superconducting cavity, which comprises the following specific steps as shown in fig. 1:
s1, preparing a niobium-based superconducting cavity:
preparing a pure niobium substrate cavity from the niobium material according to a superconducting niobium cavity processing flow; wherein the thickness of the niobium material is 1-2mm, and RRR is greater than 300;
s2, treating the outer surface of a pure niobium substrate cavity:
roughening the outer surface of the pure niobium substrate cavity by using 80-mesh sand paper to increase the contact area between aluminum and the niobium surface; heating the cleaning liquid to 50 ℃ to clean the pure niobium substrate cavity for 1h, and then airing in a thousand-level clean shed; wherein the cleaning liquid is prepared from high-purity water with the resistivity of 18.2mΩ & cm and Micro90 cleaning agent according to the volume ratio of 100:1 concentration composition;
s3, preparing cast aluminum conditions:
the hot-cast aluminum die is manufactured by stamping and welding 304 stainless steel; the cooling pipe is formed by bending a stainless steel pipe; the aluminum material is high-purity aluminum powder with the purity of 99.99 or high-purity aluminum particles with the diameter of less than 10 mm;
s4, assembling the assembly and filling materials:
firstly, assembling and fixing a cooling pipeline and a pure niobium substrate cavity, and then installing a hot-cast aluminum die to obtain an assembly body with the cavity thickness of 5-10 mm; the aluminum material enters the assembly body through the aluminum inlet;
s5, placing the assembly obtained in the step S4 into a vacuum annealing furnace for heating, wherein the heating maximum temperature is 780 ℃, keeping the temperature for 3 hours, closing the heating, naturally cooling to 80 ℃ along with the furnace, opening the furnace, taking out the assembly, and removing the die;
s6, welding the cavity niobium-titanium flange by an electron beam welding machine, welding the liquid helium pipeline interface flange, and carrying out finish machining on the cavity mounting support to meet the cavity mounting requirement.
And (3) effect test:
the following aluminum niobium composite samples were prepared as follows:
and (3) putting the pure niobium material and the aluminum material into a die, heating in a vacuum annealing furnace at the highest temperature of 780 ℃, preserving heat for 3 hours, closing the heating, naturally cooling to 80 ℃ along with the furnace, opening the furnace, taking out, and removing the die to obtain the aluminum-niobium composite sample with the aluminum coating layer thickness of 6 mm.
1. Thermal conductivity
As can be seen from fig. 2, the thermal conductivity of the aluminum-niobium composite sample with the aluminum purity of 99.5% is the lowest, the thermal conductivity of the aluminum-niobium composite sample with the aluminum purity of 99.7% is improved to a certain extent, and the thermal conductivity of the aluminum-niobium composite sample with the aluminum purity of 4N (99.99%) is the highest, namely the higher the aluminum purity is, the better the thermal conductivity of the aluminum-niobium composite sample is; although the thermal conductivity of the sample after casting is reduced, the sample can still be kept at a very high level, and the thermal conductivity still reaches 582.6W/(m.K) at the temperature of 4K, and the thermal conductivity of pure niobium at the same temperature is only 80W/(m.K). Therefore, the aluminum-niobium composite superconducting cavity formed on the outer surface of the high-purity aluminum-coated pure-niobium guide cavity has higher thermal conductivity, is favorable for the guiding out of radio-frequency heating of the superconducting cavity, can further cool the superconducting cavity in a solid conduction cooling mode, and can ensure good operation mechanical stability and thermal stability of the superconducting cavity by forming a thicker cavity wall.
2. Tensile strength of
And testing by adopting a GBT 6396-2008 composite steel plate mechanical and technological performance test method. The test results show that:
as can be seen from fig. 3 a), the tensile limit of the high-purity niobium sample is 9.2KN, and the tensile limit of the aluminum-niobium composite sample is 9.06KN, which indicates that the aluminum-niobium composite sample has the tensile limit at the same level as the high-purity niobium sample. As can be seen from fig. 3 b), the tensile strength of the high-purity niobium sample is 153.43MPa, the tensile strength of the 99.99% pure aluminum sample is 31.85MPa, and the tensile strength of the aluminum-niobium composite sample is 100.72MPa, which is far greater than that of pure aluminum; therefore, the intermediate phase layer formed in the hot casting process can remarkably improve the bonding capability between the external aluminum material and the bottom cavity niobium material.
3. Cost of preparation
99.99% high purity aluminum has a price of about 35 yuan/kg, and high purity oxygen free copper (OFHC) has a price of about 90 yuan/kg, and the specific gravity of aluminum is 2.7g/cm 3 The specific gravity of the high-purity oxygen-free copper is 8.9g/cm 3 Therefore, the dosage of the aluminum material covered outside the superconducting cavity is only about 30 percent of that of the copper material under the premise of the same thickness and space, and the aluminum material is adopted as the outer cover for the same superconducting cavityThe material cost of the material is only 11.7 percent of the price of the copper material. Therefore, the preparation cost of the composite superconducting cavity can be greatly reduced by adopting pure aluminum as an cladding material of the superconducting cavity. In addition, the hot-cast aluminum process is simple, the period is short, the die can be recycled, and the manufacturing cost is further reduced.
4. Bonding layer
As shown in the left hand graph of fig. 4, the aluminum niobium composite sample includes an Al overcoat, a mesophase, and a pure Nb substrate. The mesophase layer exhibits a relatively uniform and complete appearance, with the side adjacent to the Nb substrate appearing smoother and the side adjacent to the Al overcoat exhibiting a saw tooth like texture. Notably, the mesophase layer has visible voids and inclusions with an average thickness of 25 to 35 μm. Therefore, in the hot casting process under the vacuum environment, firm chemical bonds are formed between the Al outer coating and the pure Nb substrate through element diffusion, and high-strength metallurgical bonding is further realized.
In view of the strict cleanliness requirements of the inner surface of the cavity and in view of the influence of element diffusion on superconducting performance, EDS line scanning is performed along the vertical direction of the composite layer, and as a result, as shown in the right diagram of fig. 4, a layer of mesophase composite layer appears between metals in the intermediate bonding region. The Al and Nb contents gradually decrease to zero on both sides of the composite layer. Therefore, the diffusion distance of elements in the liquid-solid combination process is limited, and the inner surface of the Nb material is not influenced, so that the superconducting performance of the niobium substrate cavity is maintained.
While the invention has been described in detail in the foregoing general description and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.

Claims (10)

1. An aluminum-niobium composite superconducting cavity comprises the following components: a pure niobium substrate cavity, an aluminum cladding layer, and a mesophase layer between the pure niobium substrate cavity and the aluminum cladding layer.
2. The aluminum-niobium composite superconducting cavity according to claim 1, wherein: the thickness of the intermediate phase layer is 25-35 mu m.
3. An aluminum-niobium composite superconducting cavity according to claim 1 or 2, wherein: the thickness of the aluminum coating layer is 5-10mm.
4. A method of preparing the aluminum niobium composite superconducting cavity as claimed in any one of claims 1 to 3, comprising the steps of:
s1, roughening the surface of a pure niobium substrate cavity;
s2, assembling the roughened pure niobium substrate cavity with a hot-cast aluminum die and a cooling pipeline to form an assembly body with a cavity;
and S3, filling aluminum materials into the cavity of the assembly body, and performing hot casting to obtain the aluminum-niobium composite superconducting cavity.
5. The method for preparing the aluminum-niobium composite superconducting cavity according to claim 4, wherein the method comprises the following steps: in the step S1, the mesh number of the sand paper used in the roughening treatment is 80-180 meshes;
and cleaning and drying the pure niobium substrate cavity after roughening treatment.
6. The method for preparing the aluminum-niobium composite superconducting cavity according to claim 4 or 5, wherein the method comprises the following steps: in step S2, the materials of the hot-cast aluminum mold and the cooling pipeline are stainless steel.
7. The method for preparing the aluminum-niobium composite superconducting cavity according to any one of claims 4 to 6, wherein: in step S2, the assembly is performed according to the following steps:
and fixing the cooling pipeline clamp on the pure niobium substrate cavity, and then installing the hot-cast aluminum die on the surface of the pure niobium substrate cavity, wherein an aluminum-coated cavity structure with the thickness of 5-10mm is formed between the hot-cast aluminum die and the pure niobium substrate cavity.
8. The method for preparing an aluminum-niobium composite superconducting cavity according to any one of claims 4 to 7, wherein: in the step S3, the aluminum material is aluminum powder with the purity of 99.99 percent or aluminum particles with the particle size of less than 10mm.
9. The method for preparing an aluminum-niobium composite superconducting cavity according to any one of claims 4 to 8, wherein: in step S3, the hot casting is performed in a high vacuum annealing furnace;
the conditions of the hot casting are as follows: the temperature is 700-800 ℃ and the time is 3-5h.
10. A superconducting particle accelerator comprising the aluminum-niobium composite superconducting cavity of any one of claims 1-3.
CN202410003821.4A 2024-01-02 2024-01-02 Composite superconducting cavity with aluminum coated on niobium substrate and preparation method and application thereof Pending CN117881071A (en)

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