CN109926678B - Method for metallurgically connecting high-temperature alloy by liquid film - Google Patents
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Abstract
The invention discloses a method for metallurgically connecting high-temperature alloys by a liquid film, which comprises the following steps: placing an intermediate connection foil between the surfaces to be connected of the high-temperature alloy, placing the whole body in a vacuum diffusion furnace, wherein the intermediate connection foil is a composite intermediate connection foil composed of a Ni sheet or a Ni sheet and a Ti sheet, heating the vacuum diffusion furnace to a corresponding eutectic temperature after reducing the pressure in the vacuum diffusion furnace, applying and maintaining the connection pressure to the high-temperature alloy to be connected by utilizing the constant pressure movement of a pressure head, cooling and removing the connection pressure applied to the high-temperature alloy after continuously heating to a target connection temperature, preserving the temperature for a period of time, and naturally cooling the vacuum diffusion furnace to the room temperature. The method can realize reliable connection between high-temperature alloys at relatively low temperature, has short pressure application time and small pressure value, and is suitable for connecting complex components and producing in large batch.
Description
Technical Field
The invention belongs to the field of alloy connection, and particularly relates to a method for connecting high-temperature alloy through liquid film metallurgy.
Background
Many high temperature alloys, including TZM alloys, have high melting points, high elastic moduli, strong corrosion resistance, low coefficients of thermal expansion, good thermal conductivity, and excellent high temperature strength, and are therefore widely used in aerospace, engines, nuclear reactors, and other military applications. However, part of the high-temperature alloy has poor toughness, which can cause safety hazard to long-term service of parts of the high-temperature alloy. To solve this problem, a simple method is to connect a high temperature alloy with good toughness.
The melting point of the metal Nb is as high as 2467 ℃, and the Nb-based solid solution added with the alloy element has the toughness and the oxidation resistance of the alloy. And the Nb-based alloy has good plasticity and can be processed into parts with various complex shapes. In addition, Nb has lower brittle transition temperature and good corrosion resistance and welding performance, and the outstanding performances enable Nb and Nb alloy to be used for preparing key components such as rocket engines, missile shells, aircraft control rudders and wing plates. The elements added to Nb include Zr, V, etc., wherein the solubility of the Zr element and the Nb element is 100% at 500 ℃ or more, and the addition of Zr can prevent oxygen from diffusing to the grain boundary of niobium and improve the high temperature strength of the niobium alloy. Therefore, Zr is considered as one of the most suitable elements to be added to Nb, and Nb — Zr alloys formed based thereon are widely used in the aerospace field.
At present, direct diffusion welding, and diffusion welding and brazing by using a proper intermediate layer are mainly used for connecting dissimilar high-temperature alloys. Diffusion between each other is difficult to occur at lower diffusion welding temperatures, making it difficult to form effective joints; even if the temperature is increased, the diffusion coefficient is slightly increased, and cracks are generated due to the difference in thermal expansion coefficient between dissimilar metals, resulting in a low joint strength. In the brazing process, because certain high-temperature use requirements are met, the high-temperature brazing filler metal is indispensable, but a new intermetallic compound is easily introduced, so that the performance of the joint is not good. When a soft middle layer (such as a Ni middle layer) with good plasticity is adopted for diffusion welding, on one hand, Ni has good compatibility with a plurality of metal elements, the intersolubility is higher, and the element diffusion is easier to carry out; on the other hand, Ni has good plasticity, and can reduce residual stress in the joint by self-deformation to inhibit crack propagation. However, diffusion welding requires a large pressure to cause the material to yield and deform, and for complex components, it is complicated to design a proper fixture, apply a large pressure, and treat the surface of the component to achieve a high surface roughness requirement. Therefore, it is necessary to provide a simple and easy method for joining high temperature alloys.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a method for metallurgically connecting high-temperature alloys by using liquid films, which is simple, convenient and feasible and has strong applicability.
The technical purpose of the invention is realized by the following steps:
step 1: placing an intermediate connection foil between the surfaces to be connected of the high-temperature alloy, and integrally placing the intermediate connection foil in a vacuum diffusion furnace, wherein the intermediate connection foil is a Ni sheet or a composite intermediate connection foil with the atomic ratio of Ni to Ti of (35-80) to (20-65), and the integral thickness of the intermediate connection foil is less than 200 mu m;
step 2: reducing the pressure in the vacuum diffusion furnace to 1 x 10-3When the temperature is lower than MPa, the vacuum diffusion furnace is heated to the corresponding eutectic temperature at the speed of 10-20 ℃/min, and the constant pressure movement of a pressure head is utilized to apply the connection pressure of 5-10MPa to the high-temperature alloy to be connected and maintain the connection pressure;
and step 3: when the temperature is heated to the target connection temperature of 980-;
and 4, step 4: and after the heat preservation is finished, cooling to below 600 ℃ at the speed of 5 ℃/min, removing the connection pressure applied to the high-temperature alloy, and naturally cooling the vacuum diffusion furnace to room temperature.
In the above technical solution, the high temperature alloy joint surface may be a joint surface between a TZM alloy and a Nb-Zr alloy, or a joint surface between Nb-Zr alloys.
In the above technical scheme, the Nb-Zr alloy includes Nb-1Zr, Nb-5Zr, Nb-15Zr and other niobium-zirconium alloys.
In the technical scheme, the intermediate connection foil can be a foil with the Ni content of 99% (mass percentage) and the thickness of 30-120 μm, and the composite intermediate connection foil consists of a Ti sheet and a Ni sheet.
In the above technical solution, the composite intermediate connection foil may be in a form of stacking one Ti sheet and one Ni sheet, or in a form of stacking one Ni sheet and one Ti sheet and one Ni sheet.
In the above technical solution, when the composite intermediate connection foil is composed of Ti sheets and Ni sheets, the ratio of the sum of Ti atoms of all Ti sheets to the sum of Ni atoms of all Ni sheets is 76:24, or the ratio of the sum of Ti atoms of all Ti sheets to the sum of Ni atoms of all Ni sheets is 39: 61.
In the technical scheme, the method further comprises a pretreatment process, wherein the pretreatment process comprises the steps of polishing the high-temperature alloy to-be-connected surface with sand paper to be smooth, polishing the intermediate connection foil with sand paper to remove surface oxide skin, and then putting the high-temperature alloy and the intermediate connection foil into a washing solution to be washed.
In the technical scheme, the abrasive paper is 1000# diamond abrasive paper.
In the technical scheme, the cleaning solution is acetone, and ultrasonic cleaning is adopted for 5-10 min.
Compared with the prior art, the liquid metal is formed by utilizing the eutectic reaction between the intermediate layer element and the base material part element (such as the eutectic reaction between Ni, Nb and Zr), and the reliable connection between the high-temperature alloys can be realized at relatively low temperature.
Compared with direct diffusion welding and intermediate layer diffusion welding, the method has the advantages that the requirement on the surface roughness of the material to be welded is low, the pressure application time is short, the pressure value is small, and the method is suitable for connecting complex components and producing the complex components in large batch. Compared with the brazing connection of high-temperature alloy, the liquid film with the surface roughness scale equivalent to that of the high-temperature alloy is formed by applying micro pressure when the liquid phase is fully formed, and the high-strength reliable metallurgical connection is formed by solidification, so that intermetallic compounds with adverse effects on the performance in the brazing joint are greatly reduced or even eliminated, and the room-temperature and high-temperature connection performance of the joint is greatly improved.
Drawings
FIG. 1 is a graph showing the heating and pressurizing curves used in the method for joining a superalloy by liquid film metallurgy in example 1 of the present invention;
FIG. 2 is a scanning electron microscope comparison of typical tissue joining TZM alloy and Nb-Zr alloy joints of example 1 using Ni intermediate foil contact reaction brazing;
a picture is a scanning electron microscope contrast picture of a typical structure of a contact reaction soldered joint using Ni interlayer foil;
b is a scanning electron microscope comparison image of a typical tissue of the joint in example 1;
FIG. 3 is a graph of room temperature shear strength as a function of joining temperature for a joint joining a TZM alloy and a Nb-Zr alloy with example 1 using Ni intermediate foil contact reaction brazing.
The specific implementation mode is as follows:
in order to make the advantages, technical solutions and objects of the present invention more apparent, the present invention is further described below with reference to examples. The following examples are given to further illustrate the present invention, but not to limit the scope of the present invention.
Example 1
TZM alloy (TZM alloy composition: 0.5% Ti, 0.08% Zr, 0.02% C, balance Mo, purchased from Tianjin aeronautical and electrical Co., Ltd.) was processed into 10 mm. times.15 mm. times.3 mm pieces, Nb-15Zr alloy (purchased from Li Hua Ti alloy Co., Ltd., Bao Ji) was processed into 5 mm. times.5 mm pieces, and Ni foil with a Ni content of 99% (mass content) of 120 μm thickness was cut into 6 mm. times.6 mm pieces. Sequentially polishing TZM alloy and Nb-15Zr alloy by using diamond sand paper of No. 120, No. 240, No. 600, No. 800 and No. 1000 to smooth to-be-bonded surfaces, polishing oxide skins on the surfaces of the Ni foil by using diamond sand paper of No. 1000, putting the Ni foil and the Ni foil into acetone to perform ultrasonic cleaning for 5min, putting the cleaned Ni foil between the cleaned TZM alloy and Nb-15Zr alloy to-be-bonded surfaces, putting the cleaned Ni foil into a vacuum diffusion furnace after assembly, and reducing the pressure in the vacuum diffusion furnace to 1 x 10-3When the temperature is lower than the MPa, starting to heat the vacuum diffusion furnace to 800 ℃ at the speed of 20 ℃/min, then preserving heat for 10min, then continuing to heat at the heating rate of 10 ℃/min, and when the temperature is increased to 1010 ℃ which is the Ni-Zr eutectic point, applying 10MPa of connection pressure to the high-temperature alloy to be connected by utilizing the constant-pressure movement of a pressure head and maintaining the connection pressure; and when the temperature is heated to the target connection temperature of 1200 ℃, preserving the heat for 30min, cooling to 400 ℃ at the speed of 5 ℃/min after preserving the heat at the target connection temperature, removing the connection pressure applied to the high-temperature alloy, and naturally cooling the vacuum diffusion furnace to the room temperature. FIG. 1 is a graph showing the heating and pressing curves used in the present example for joining superalloys using liquid film metallurgy.
The control was performed using contact reaction brazing, as follows: the TZM alloy is processed into small blocks of 10mm multiplied by 15mm multiplied by 3mm, and the Nb-Zr alloy is processed into 5mm.times.5 mmx.5 5mm pieces, 120 μm thick Ni foil were cut into 6 mmx.6 6mm pieces. The TZM alloy and the Nb-Zr alloy are sequentially polished to be flat by using No. 120-1000 diamond abrasive paper, the surface oxide skin of the Ni foil is polished by using No. 1000 diamond abrasive paper, the Ni foil and the Ni foil are placed into acetone to be ultrasonically cleaned for 5min, and the vacuum diffusion furnace is placed after the Ni foil and the acetone are assembled. The vacuum degree of the vacuum chamber is pumped to 1 x 10-3Heating to 800 deg.C at a temperature-rising rate of 20 deg.C/min under MPa, maintaining the temperature at 800 deg.C for 10min, heating to 1200 deg.C at a temperature-rising rate of 10 deg.C/min, and maintaining the temperature at 1200 deg.C for 30 min. And after the heat preservation is finished, cooling to 600 ℃ at the speed of 5 ℃/min, stopping heating, and naturally cooling the vacuum diffusion furnace to room temperature.
As can be seen from a comparison graph of a typical structure scanning electron microscope of the joint in FIG. 2, in a graph a, two Ni-Nb-Zr ternary compounds exist in a brazing seam with different depths, and the influence area of the Ni-Nb-Zr ternary compounds can reach 1 mm; in the b picture, only a small amount of Ni-Nb-Zr ternary compounds exist, and a large amount of original grain boundaries are reserved in the Nb-15Zr base material, which shows that a large amount of intermetallic compounds are eliminated by adopting a liquid film metallurgical connection method, the interface bonding is good, and no obvious holes and cracks exist. FIG. 3 shows that after room temperature shear strength test (brazing joint strength test method; Standard No. GB/T11363) 1989, a testing instrument is a microcomputer-controlled electronic universal tester, model No. INSTRON 1186, when the connection temperature is changed between 1150 ℃ and 1225 ℃, the joint shear strength is improved by about 30% by adopting a liquid film metallurgy connection method, the highest strength is obtained at 1200 ℃, and the maximum value is 528 MPa.
Example 2
Respectively processing Nb-5Zr alloy into small blocks of 10mm multiplied by 15mm multiplied by 3mm and 5mm multiplied by 5mm, and sequentially grinding and flattening by using diamond sand paper of No. 120, No. 240, No. 600, No. 800 and No. 1000; cutting 50 μm Ti foil and 20 μm Ni foil into 6mm × 6mm pieces, polishing off oxide skin with 1000# diamond sand paper, ultrasonic cleaning in acetone for 10min, assembling according to the sequence of Nb-5Zr-50 μmTi-20 μmNi-50 μmTi-Nb-5Zr (total atomic ratio of Ti and Ni is 76: 24), and placing in a vacuum diffusion furnace. Reducing the pressure in the vacuum diffusion furnace to 1 x 10-3Starting to expand the vacuum at a rate of 10 ℃/min below MPaHeating the bulk furnace to 800 ℃, then preserving heat for 10min, then continuously heating at the heating rate of 10 ℃/min, and applying a connection pressure of 10MPa to the high-temperature alloy to be connected by utilizing the constant-pressure movement of a pressure head when the temperature is increased to 942 ℃ to maintain the connection pressure; and (3) when the temperature is heated to the target connection temperature of 980 ℃, preserving the heat for 5min, cooling to 400 ℃ at the speed of 5 ℃/min after preserving the heat at the target connection temperature, removing the connection pressure applied to the high-temperature alloy, and naturally cooling the vacuum diffusion furnace to the room temperature.
The Nb-5Zr alloy connecting piece obtained by the metallurgical connection of the liquid film with Ti-Ni as the intermediate layer has good interface combination and no obvious holes and cracks, and the shear strength of the obtained joint reaches 325MPa through room temperature shear strength test, compared with the intermetallic compound in the joint obtained by contact reaction brazing, the shear strength at room temperature is greatly reduced by 20 percent.
Example 3
Respectively processing the TZM alloy and the Nb-1Zr alloy into small blocks of 10mm multiplied by 15mm multiplied by 3mm and 5mm multiplied by 5mm, and sequentially grinding and flattening by using diamond sand paper of No. 120, No. 240, No. 600, No. 800 and No. 1000; cutting a Ti foil sheet with the thickness of 60 mu m and a Ni foil sheet with the thickness of 60 mu m into small pieces with the thickness of 6mm multiplied by 6mm, polishing away oxide scales on the surfaces by using No. 1000 diamond abrasive paper, putting the small pieces into acetone for ultrasonic cleaning for 10min, assembling according to the sequence of TZM-60 mu mTi-60 mu mNi-Nb-1 Zr (the total atomic ratio of Ti and Ni is 39: 61), and putting the small pieces into a vacuum diffusion furnace. Reducing the pressure in the vacuum diffusion furnace to 1 x 10-3When the temperature is lower than the MPa, the vacuum diffusion furnace is heated to 800 ℃ at the speed of 10 ℃/min, then the temperature is kept for 10min, then the temperature is continuously raised at the temperature raising speed of 10 ℃/min, when the temperature is raised to 1118 ℃ of the Ti-Ni eutectic point, the constant pressure movement of a pressure head is utilized to apply the connection pressure of 10MPa to the high-temperature alloy to be connected, and the connection pressure is maintained; and (3) after heating to a target connection temperature of 1225 ℃, preserving heat for 45min, cooling to 600 ℃ at a speed of 5 ℃/min after preserving heat at the target connection temperature, removing the connection pressure applied to the high-temperature alloy, and naturally cooling the vacuum diffusion furnace to room temperature.
The connector of TZM/Nb-1Zr alloy obtained by the metallurgical connection of the liquid thin film with Ti-Ni as the intermediate layer has good interface combination and no obvious holes and cracks, and the shear strength of the obtained connector reaches 340MPa through room temperature shear strength test, and is improved by 22 percent compared with the shear strength of the connector obtained by contact reaction brazing at room temperature.
Claims (7)
1. The method for metallurgically connecting the high-temperature alloys by the liquid film is characterized by comprising the following steps:
step 1: placing an intermediate connection foil between the surfaces to be connected of the high-temperature alloy, and integrally placing the intermediate connection foil in a vacuum diffusion furnace, wherein the intermediate connection foil is a Ni sheet or the atomic ratio of Ni to Ti is (35-80): (20-65) a composite intermediate connection foil, the overall thickness of the intermediate connection foil being less than 200 μm;
step 2: reducing the pressure in the vacuum diffusion furnace to 1 x 10-3When the temperature is lower than MPa, the vacuum diffusion furnace is heated to the corresponding eutectic temperature at the speed of 10-20 ℃/min, and the constant pressure movement of a pressure head is utilized to apply the connection pressure of 5-10MPa to the high-temperature alloy to be connected and maintain the connection pressure;
and step 3: when the temperature is heated to the target connection temperature of 980-;
and 4, step 4: after the heat preservation is finished, cooling to below 600 ℃ at the speed of 5 ℃/min, removing the connection pressure applied to the high-temperature alloy, and naturally cooling the vacuum diffusion furnace to room temperature;
the high-temperature alloy to-be-connected surface is a connected surface between the TZM alloy and the Nb-Zr alloy.
2. The method of claim 1, wherein the intermediate connection foil is a foil having a Ni content of 99% (mass%) and a thickness of 30-120 μm, and the composite intermediate connection foil is composed of Ti pieces and Ni pieces.
3. The method of claim 1, wherein the composite intermediate connection foil is in the form of a Ti sheet on a Ni sheet, or in the form of a Ni sheet on a Ti sheet on a Ni sheet.
4. The method for liquid film metallurgical bonding of superalloys of claim 1, wherein the composite intermediate bonding foil has an atomic ratio of Ti to Ni of 76:24 or 39: 61.
5. The method for joining superalloys in liquid film metallurgy according to claim 1, further comprising a pretreatment process comprising sanding the surface of the superalloy to be joined, removing surface scale from the intermediate joining foil, and washing the superalloy and the intermediate joining foil in a washing solution.
6. The method for joining superalloys in liquid film metallurgy according to claim 5, wherein the sandpaper is 1000# diamond sandpaper.
7. The method for liquid film metallurgical bonding of high-temperature alloys according to claim 5, wherein the cleaning solution is acetone, and the cleaning is performed by ultrasonic cleaning for 5-10 min.
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