CN112391587A - Preparation method and application of amorphous alloy material toughened in cryogenic cycle combined pre-deformation mode - Google Patents

Preparation method and application of amorphous alloy material toughened in cryogenic cycle combined pre-deformation mode Download PDF

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CN112391587A
CN112391587A CN202011070613.4A CN202011070613A CN112391587A CN 112391587 A CN112391587 A CN 112391587A CN 202011070613 A CN202011070613 A CN 202011070613A CN 112391587 A CN112391587 A CN 112391587A
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amorphous alloy
deformation
alloy
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CN112391587B (en
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乔珺威
朱前勇
杨慧君
石晓辉
张敏
王雪姣
晋玺
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Taiyuan University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C45/00—Amorphous alloys
    • C22C45/10—Amorphous alloys with molybdenum, tungsten, niobium, tantalum, titanium, or zirconium or Hf as the major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/11—Making amorphous alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D3/00—Yielding couplings, i.e. with means permitting movement between the connected parts during the drive
    • F16D3/02—Yielding couplings, i.e. with means permitting movement between the connected parts during the drive adapted to specific functions
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D3/00—Yielding couplings, i.e. with means permitting movement between the connected parts during the drive
    • F16D3/02—Yielding couplings, i.e. with means permitting movement between the connected parts during the drive adapted to specific functions
    • F16D3/12—Yielding couplings, i.e. with means permitting movement between the connected parts during the drive adapted to specific functions specially adapted for accumulation of energy to absorb shocks or vibration

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Abstract

本发明公开了一种深冷循环组合预变形方式增韧非晶合金材料的制备方法及应用，属于非晶合金应用技术领域。深冷循环组合预变形方式处理增韧非晶合金的柔性联轴器膜片，利用真空电弧炉熔炼，水冷铜模快速吸铸成板状非晶合金，深冷循环处理,进行5%的轧制预变形之后粗、精加工成所需膜片。本发明提供的深冷循环组合预变形方式处理增韧的非晶合金膜片具有高的弹性极限（2%）、高硬度、高强度、耐磨、使用寿命长等优点。该柔性联轴器膜片采用Zr基非晶制造，拓宽了柔性联轴器在高端、精密、特殊需求场合的应用，具有很高的商业使用价值。

Figure 202011070613

The invention discloses a preparation method and application of a cryogenic cycle combined pre-deformation toughening amorphous alloy material, and belongs to the technical field of amorphous alloy application. The flexible coupling diaphragm of the toughened amorphous alloy is treated by a combination of cryogenic circulation and pre-deformation. It is smelted in a vacuum arc furnace, and the water-cooled copper mold is quickly sucked and cast into a plate-shaped amorphous alloy. After cryogenic circulation treatment, 5% rolling is performed. After making pre-deformation, rough and finish the required diaphragm. The amorphous alloy diaphragm treated and toughened by the cryogenic cycle combined pre-deformation method provided by the invention has the advantages of high elastic limit (2%), high hardness, high strength, wear resistance, long service life and the like. The flexible coupling diaphragm is made of Zr-based amorphous material, which broadens the application of the flexible coupling in high-end, precision, and special-demand occasions, and has high commercial use value.

Figure 202011070613

Description

Preparation method and application of amorphous alloy material toughened in cryogenic cycle combined pre-deformation mode
Technical Field
The invention relates to a preparation method and application of a cryogenic cycle combined pre-deformation mode toughened amorphous alloy material, and belongs to the technical field of preparation and application of amorphous alloys.
Background
The amorphous alloy has many excellent performances, such as large elastic limit (elastic limit 2%), high breaking strength, high hardness, good corrosion resistance, friction resistance and the like, due to the unique structural characteristics of long-range disorder, short-range order, no grain boundary and the like, and is a structural material with wide application prospect. These unique properties provide excellent elastic behavior, which is rare in crystalline metals. However, the plastic deformation of room temperature amorphous alloys is limited to shear bands of the order of 10 nm, and the amorphous alloys exhibit brittle fracture due to the rapid propagation of a single shear band. Room temperature brittleness seriously hinders the practical application of amorphous alloys as structural materials. In recent years, researchers find that the room temperature brittleness of the amorphous alloy can be effectively improved by performing Deep cryogenic cycle treatment (DCT for short) on the amorphous alloy. Cryogenic cyclic treatment is a method of cyclic "hot" treatment between room temperature and low temperature. Compared with toughening treatment methods such as surface shot blasting, notch forming, radiation treatment and the like, the cryogenic circulating treatment has the advantages of low cost, simplicity in operation, no size limitation, no damage to samples, no crystallization and the like. Cryogenic cyclic treatment is considered an effective "hot" treatment method to improve the toughness of amorphous alloys. Meanwhile, the mode of increasing the toughness of the amorphous alloy by the pre-deformation mode has been widely researched. Amorphous alloys with large elastic limit and high strength have been used in the fields of golf clubs (drivers, push rods), watches, mobile phone electromagnetic device housings, optical lenses, and the like. In the mechanical transmission equipment devices in various industries at present, the flexible coupling well solves the problem of damage to equipment caused by impact generated by frequent acceleration and deceleration of the equipment on different occasions. The most important accessory on the flexible coupling is the diaphragm, and when the flexible coupling is transmitted to the diaphragm in the acceleration and deceleration process of the equipment, the diaphragm can well absorb impact to play a role in buffering; but also angular and axial deviations can be compensated for by the membrane. Zero gyration clearance, the same gyration characteristic is had in the same direction of flow transmission. This drives the need for membranes having high elasticity, high stiffness, wear resistance, fatigue resistance, etc. In the prior art, the flexible coupling diaphragm is mostly made of stainless steel, and although the stainless steel diaphragm is higher in strength and more wear-resistant compared with an early carbon steel diaphragm, the flexible coupling diaphragm cannot meet the requirements of customers in occasions with high precision, high rotating speed and special requirements. The amorphous alloy flexible coupling diaphragm toughened by the cryogenic circulating treatment well makes up the defects of the stainless steel diaphragm in the aspect.
Disclosure of Invention
The invention aims to provide a preparation method of an amorphous alloy material toughened by a cryogenic cycle combined predeformation mode and application of the amorphous alloy material in preparing a flexible coupling diaphragm, wherein the amorphous alloy diaphragm toughened by the cryogenic cycle combined predeformation mode has the advantages of high elastic limit (2%), high hardness, high strength, wear resistance, long service life and the like; the application of the flexible coupling in high-precision and special-demand occasions is widened.
The invention uses deep cooling circulation combined predeformation mode to process toughened flexible coupling diaphragm, and the high elastic diaphragm of the flexible coupling adopts Zr55Al10Ni5Cu29Y1Manufacturing an amorphous alloy; for the problems of high element purity, high smelting vacuum degree, amorphous forming capability and the like of amorphous alloy preparation, the Y element is added into a Zr-Al-Ni-Cu amorphous alloy system to improve the amorphous forming capability and reduce the cost of amorphous alloy smelting preparation; the toughness of the amorphous alloy subjected to the deep cooling circulation combined with the pre-deformation treatment is improved.
The invention provides a method for preparing a cryogenic circulation combined pre-deformation mode toughened amorphous alloy material, which comprises the following steps:
step one, pretreatment: respectively cleaning the amorphous alloy raw materials of Zr, Al, Ni, Cu and Y metals by a file, then respectively putting the raw materials into ultrasonic cleaning equipment filled with absolute ethyl alcohol for ultrasonic cleaning for 10-20 minutes to remove oil stains and impurities on the surfaces of the raw materials, and then drying the required raw materials by a drying oven;
step two, batching: according to the atomic percentage of Zr, Al, Ni, Cu and Y elements of 55: 10: 5: 29: 1, calculating the mass required by each pure metal raw material;
step three, smelting and suction casting:
(1) putting the pure metal raw materials weighed in the step two into the same copper mold crucible from bottom to top in sequence according to the sequence of the melting points of the elements from low to high, and ensuring that the high-melting-point raw materials can be completely melted; placing the titanium sponge block for testing the oxygen content into another copper mold crucible, and then closing a furnace door of the crucible;
(2) pumping the cavity to below 5 Pa by using a first-stage mechanical pump, closing a closing valve, opening a second-stage mechanical pump and a molecular pump to make the interior of the furnace chamber reach a high vacuum state, and when the vacuum degree of the furnace chamber reaches 1 × 10-3When Pa, closing a valve at the molecular pump; then filling high-purity argon to ensure that the pressure of the furnace chamber is 0.5 atm;
(3) firstly, smelting a titanium sponge block to check the oxygen content in the furnace, and smelting alloy after the titanium sponge block is smelted and cooled and has no color change, wherein the smelting process adopts electric arc smelting, and an alloy ingot is repeatedly turned and smelted for 5 times to ensure uniform components;
(4) placing alloy ingots with uniform components at the edge of a crucible, cutting the alloy ingots into alloy mother ingots with the mass of 30-40 g suitable for suction casting by using electric arcs, moving the alloy mother ingots into a suction casting copper mold crucible by using a mechanical arm, smelting the alloy ingots by using the electric arcs, quickly opening a suction casting valve switch after the alloy ingots are completely molten, quickly suction casting the alloy into a water-cooling copper mold by using pressure difference, and quickly cooling the alloy by the water-cooling copper mold to obtain plate-shaped amorphous alloys with the length, the width and the thickness of 85 multiplied by 30 multiplied by 2 mm;
step four, primary processing:
sequentially grinding and polishing the plate-shaped amorphous alloy obtained in the step three by using sand paper of different types of 240 #, 400 #, 600 #, 800 #, 1000 #, 1500 # and 2000 #, and removing oil stains and impurities by using ultrasonic waves; simultaneously, mechanically polishing the side surface of the plate-shaped test sample by using diamond polishing paste, and then cleaning the test sample by using ultrasonic waves;
step five, cryogenic circulating treatment:
in order to improve the mechanical property of the amorphous alloy and enable the amorphous alloy to be in a higher energy state, the amorphous alloy is subjected to cryogenic circular treatment. Carrying out cryogenic circulating treatment on the amorphous alloy in the fourth step: firstly, placing an amorphous alloy sample into a liquid nitrogen container for 5 minutes, then quickly placing the amorphous alloy sample into a boiled water container for 1 minute, heating to 50-80 ℃, and then standing in a room-temperature environment for 4 minutes; performing cyclic subzero treatment for 20-60 times respectively by using the above step as subzero cyclic treatment; and obtaining the amorphous alloy material.
In the second step of the preparation method, the clean pure metal raw material processed in the first step is weighed by using an electronic balance with the precision of 0.001g, and the weighing mass error range is ensured to be within the range of +/-0.003 g.
In the preparation method, the purity of the argon in the third step is 99.999%.
In the third step of the preparation method, the current is controlled to be 180-200 mA during arc melting.
The invention provides application of the amorphous alloy material prepared by the preparation method in a flexible coupling diaphragm.
The application specifically comprises the following steps:
(1) rolling and pre-deforming:
in order to further improve the amorphous toughness, the plate-shaped sample obtained after the deep cooling circulating treatment is rolled by adopting an ATMR series electric miniature reversible two-high mill, and the rolling process is finished in multiple passes; the rolling process adopts a longitudinal rolling two-dimensional rolling mode, after each rolling pass is finished, the sample is horizontally rotated by 180 degrees, and the two directions are alternately rolled until the required 5 percent of pre-deformation amount is obtained;
(2) finish machining:
polishing the alloy surface after the pre-deformation treatment to a thickness of 0.3-0.5 mm of a diaphragm, polishing, and removing oil stains by using ultrasonic cleaning equipment; then, according to a design dimension drawing of the flexible coupling diaphragm, precisely perforating the diaphragm by using the rotating heads with different diameters so as to install a fixing bolt; using a rotary head to open holes according to the principle of opening holes from small to large successively; then, accurately cutting according to the design size drawing and the structure and precision requirements by using a low-speed precision cutting machine; then, utilizing a polishing machine to polish the side surface and the front surface and the back surface of the membrane into mirror surfaces by water grinding; cleaning oil stains and impurities on the finished membrane by using ultrasonic cleaning equipment; and manufacturing the flexible coupling diaphragm.
Furthermore, in the rolling pre-deformation process, the reduction of each roller is not allowed to exceed 0.01mm, the rolling frequency is not less than 15 rolling processes, and the reduction of each pass is 0.01 mm.
Further, the diameters of the used rotor heads are 2, 3, 4, 5 and 6mm respectively.
The invention has the beneficial effects that:
the flexible coupling diaphragm for treating toughened amorphous alloy by using the deep cooling circulation combined pre-deformation mode has the advantages of high elastic limit (elastic limit is 2%), high hardness, high strength, wear resistance, long service life and the like. Compared with a flexible coupling diaphragm made of stainless steel, the flexible coupling diaphragm has wider application range, widens the application field of the flexible coupling in occasions with high-end precision and special requirements, and has very high commercial use value.
Drawings
FIG. 1 is stress-strain curves of compressive mechanical properties of amorphous alloys before and after treatment with combined pre-deformation of cryogenic cycles (0, 20, 40, 60 cycles) in example 1, and it is found by comparison that the toughness of amorphous alloys is improved with the increase of the number of cryogenic cycles.
FIG. 2 is a comparison XRD chart before and after the treatment of the deep cooling cycle (0, 20, 40, 60 cycles) combined with the pre-deformation mode in example 1, and it can be seen that the sample is still in an amorphous structure after the cast state deep cooling treatment.
Fig. 3 is DSC curves before and after the treatment in the combined pre-deformation mode of the cryogenic cycles (0, 20, 40, 60 cycles) in example 1, and it was found by curve calculation that the enthalpy value of release before and after the treatment in the combined pre-deformation mode of the cryogenic cycles was increased, that is, the content of free volume in the material before and after the treatment in the combined pre-deformation mode of the cryogenic cycles was increased.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following examples.
Example 1:
this example is a deep cooling circulation combined pre-deformation mode for treating toughened Zr55Al10Ni5Cu29Y1A preparation method and application of amorphous alloy material.
The embodiment is that the Zr-Al-Ni-Cu-Y amorphous alloy material toughened by the deep cooling circulation combined pre-deformation mode treatment consists of five elements of Zr, Al, Ni, Cu and Y, wherein the atomic percent of the Zr-Al-Ni-Cu-Y amorphous alloy material is Zr55Al10Ni5Cu29Y1Wherein Ti, Zr, V, Cu and Be are subjected to smelting and suction casting to form plate-shaped amorphous alloy after removing oxides from blocky Zr, Al, Ni, Cu and Y with the purity of more than or equal to 99.999 percent by a file, cleaning by alcohol and drying by an oven, and then performing cryogenic circulating treatment and pre-deformation rolling.
Zr proposed in this example55Al10Ni5Cu29Y1The preparation process of the diaphragm of the amorphous alloy flexible coupling toughened by the deep cooling circulation combined pre-deformation mode treatment comprises the following steps:
step one, pretreatment: respectively cleaning oxide skins of Zr, Al, Ni, Cu and Y metals serving as amorphous alloy raw materials by using a file, then respectively putting the raw materials into ultrasonic cleaning equipment filled with absolute ethyl alcohol for ultrasonic cleaning for 10-20 minutes to remove oil stains and impurities on the surfaces of the raw materials, and then drying the required raw materials by using a drying oven.
Step two, batching: according to the atomic percentage of Zr, Al, Ni, Cu and Y elements of 55: 10: 5: 29: 1 calculating the mass required for each raw material pure metal. And weighing the clean pure metal raw material processed in the step one by adopting an electronic balance with the precision of 0.001g, wherein the weighing mass error range is ensured to be less than +/-0.003 g.
Step three, smelting and suction casting:
(1) putting the pure metal raw materials weighed in the step two into the same copper mold crucible from bottom to top in sequence according to the sequence of the melting points of the elements from low to high, and ensuring that the high-melting-point raw materials can be completely melted; placing the titanium sponge block for testing the oxygen content into another copper mold crucible, and then closing the furnace door;
(2) pumping the cavity to below 5 Pa by using a first-stage mechanical pump, closing a closing valve, opening a second-stage mechanical pump and a molecular pump to make the interior of the furnace chamber reach a high vacuum state, and when the vacuum degree of the furnace chamber reaches 1 × 10-3When Pa, closing a valve at the molecular pump; then filling high-purity argon to ensure that the pressure of the furnace chamber is 0.5 atm;
(3) firstly, smelting a titanium sponge block to check the oxygen content in the furnace, and smelting alloy after the titanium sponge block is smelted and cooled and has no color change, wherein the smelting process adopts electric arc smelting (the current is controlled to be 180 mA), and an alloy ingot is repeatedly turned and smelted for 5 times to ensure uniform components;
(4) placing an alloy ingot with uniform components at the edge of a crucible, cutting the alloy ingot into alloy mother ingots with the mass of 30g and suitable for suction casting by using an electric arc, moving the alloy mother ingots into a suction casting copper mold crucible by using a mechanical arm, smelting the alloy ingots by using the electric arc (the control current is 180 mA), quickly opening a suction casting valve switch after the alloy ingots are completely molten, quickly suction casting the alloy into a water-cooling copper mold by using pressure difference, and quickly cooling the alloy by using the water-cooling copper mold to obtain the plate-shaped amorphous alloy with the length, width and thickness of 85 multiplied by 30 multiplied by 2 mm.
Step four, primary processing:
sequentially grinding and polishing the plate-shaped amorphous alloy obtained in the step three by using sand paper of different types of 240 #, 400 #, 600 #, 800 #, 1000 #, 1500 # and 2000 #, and removing oil stains and impurities by using ultrasonic waves; simultaneously, mechanically polishing the side surface of the plate-shaped test sample by using diamond polishing paste, and then cleaning the test sample by using ultrasonic waves;
step five, cryogenic circulating treatment:
in order to improve the mechanical property of the amorphous alloy and enable the amorphous alloy to be in a higher energy state, the amorphous alloy is subjected to cryogenic circular treatment. And D, carrying out deep cooling circulation treatment on the amorphous alloy in the fourth step. Firstly, an amorphous alloy sample is put into a liquid nitrogen container for 5 minutes, then is quickly put into a boiled water container for 1 minute to be heated to 50 ℃, and then is kept still in a room temperature environment for 4 minutes. The treatment is a cryogenic cycle treatment, and 20, 40 and 60 cycles of cryogenic treatment are respectively carried out.
Step six, rolling and pre-deforming:
in order to further improve the amorphous toughness, after the deep cooling cycle treatment, an ATMR series electric miniature reversible two-roll mill is adopted for rolling, and the rolling process is completed in multiple steps: the reduction of each roller is not allowed to exceed 0.01mm, the reduction frequency of the roller is not less than 15 times of rolling processes, and the reduction of each pass is 0.01 mm. And a longitudinal rolling two-dimensional rolling mode is adopted in the rolling process, after each rolling pass is finished, the sample is horizontally rotated by 180 degrees, and the two directions are alternately rolled until the required 5% pre-deformation amount is obtained.
Step seven, fine machining:
and (3) polishing the alloy surface treated by the deep cooling circulation combined predeformation mode to the thickness of 0.3 mm of the diaphragm, polishing, and removing oil stains by using ultrasonic cleaning equipment. And then, according to a flexible coupling diaphragm design size drawing, utilizing the rotary heads with different diameters to precisely open holes in the diaphragm so as to install the fixing bolts. And (4) using a rotary head to perform hole opening according to the principle of opening holes from small to large successively. The diameter specifications of the rotating head are respectively 2, 3, 4, 5 and 6 mm. And then, accurately cutting according to the structure and the precision requirement by using a low-speed precision cutting machine according to the design dimension drawing. And then, polishing the side surface and the front surface and the back surface of the membrane into a mirror surface by using a polishing machine. And (4) cleaning oil stains and impurities of the finished membrane by using ultrasonic cleaning equipment.
And (3) carrying out a performance detection process on the obtained product and according to the following steps:
(1) from finished samplesSelecting a cuboid compression sample of 2 × 2 × 4mm, performing quasi-static compression test by using an Instron5696 electronic mechanical testing machine, wherein the compression rate is 1 × 10-4s-1Therefore, the change of the mechanical property of the material after the combined pre-deformation treatment of the cryogenic cycle (0, 20, 40 and 60 times) of the amorphous material is analyzed and compared, as shown in figure 1.
(2) A 3 × 3mm rectangular piece is taken from the finished sample and tested by an XRD device at a scanning rate of 10 °/min and a test angle ranging from 10 ° to 90 °, so as to analyze and compare the change of the crystal structure of the material after the amorphous material deep cooling cycle (0, 20, 40 and 60 times) combined pre-deformation treatment, as shown in FIG. 2.
(3) And taking 20mg of sample from the finished sample to carry out DSC test, and selecting 20K/min as the heating rate so as to analyze and compare the change of the thermodynamic property of the material after the amorphous material is subjected to combined pre-deformation treatment in cryogenic cycles (0, 20, 40 and 60 times), as shown in figure 3.
And (3) performance test results:
in fig. 1, stress-strain curves of compressive mechanical properties of the amorphous alloy before and after the treatment in the deep cooling cycle (0, 20, 40, and 60 times) combined pre-deformation mode are compared, and it is found that the toughness of the amorphous alloy is improved with the increase of the number of times of the deep cooling cycle treatment.
In fig. 2, XRD comparison patterns before and after the deep cooling cycle (0, 20, 40, and 60 times) combined pre-deformation treatment show that the sample is still amorphous compared to the sample after the as-cast state cryogenic treatment.
In the DSC curves before and after the deep cooling cycle (0, 20, 40, 60 times) combined pre-deformation mode treatment in fig. 3, it is found through curve calculation that the enthalpy value of release increases before and after the deep cooling cycle combined pre-deformation mode treatment, that is, the free volume content in the material increases before and after the deep cooling cycle combined pre-deformation mode treatment.
Example 2:
this example is a deep cooling circulation combined pre-deformation mode for treating toughened Zr55Al10Ni5Cu29Y1A preparation method and application of amorphous alloy material.
This exampleThe Zr-Al-Ni-Cu-Y amorphous alloy material is toughened by a cryogenic circulating combined pre-deformation mode and consists of five elements of Zr, Al, Ni, Cu and Y, wherein the atomic percent of the Zr-Al-Ni-Cu-Y amorphous alloy material is Zr55Al10Ni5Cu29Y1Wherein Ti, Zr, V, Cu and Be are subjected to smelting and suction casting to form plate-shaped amorphous alloy after removing oxides from blocky Zr, Al, Ni, Cu and Y with the purity of more than or equal to 99.999 percent by a file, cleaning by alcohol and drying by an oven, and then performing cryogenic circulating treatment and pre-deformation rolling.
Zr proposed in this example55Al10Ni5Cu29Y1The preparation process of the diaphragm of the amorphous alloy flexible coupling toughened by the deep cooling circulation combined pre-deformation mode treatment comprises the following steps:
step one, pretreatment: respectively cleaning oxide skins of Zr, Al, Ni, Cu and Y metals serving as amorphous alloy raw materials by using a file, then respectively putting the raw materials into ultrasonic cleaning equipment filled with absolute ethyl alcohol for ultrasonic cleaning for 10-20 minutes to remove oil stains and impurities on the surfaces of the raw materials, and then drying the required raw materials by using a drying oven.
Step two, batching: according to the atomic percentage of Zr, Al, Ni, Cu and Y elements of 55: 10: 5: 29: 1 calculating the mass required for each raw material pure metal. And weighing the clean pure metal raw material processed in the step one by adopting an electronic balance with the precision of 0.001g, wherein the weighing mass error range is ensured to be less than +/-0.003 g.
Step three, smelting and suction casting:
(1) putting the pure metal raw materials weighed in the step two into the same copper mold crucible from bottom to top in sequence according to the sequence of the melting points of the elements from low to high, and ensuring that the high-melting-point raw materials can be completely melted; placing the titanium sponge block for testing the oxygen content into another copper mold crucible, and then closing the furnace door;
(2) pumping the cavity to below 5 Pa by using a first-stage mechanical pump, closing a closing valve, opening a second-stage mechanical pump and a molecular pump to make the interior of the furnace chamber reach a high vacuum state, and when the vacuum degree of the furnace chamber reaches 1 × 10-3When Pa, closing a valve at the molecular pump;then filling high-purity argon to ensure that the pressure of the furnace chamber is 0.5 atm;
(3) firstly, smelting a titanium sponge block to check the oxygen content in the furnace, and smelting alloy after the titanium sponge block is smelted and cooled and has no color change, wherein the smelting process adopts electric arc smelting (the current is controlled to be 190 mA), and an alloy ingot is repeatedly turned and smelted for 5 times to ensure uniform components;
(4) placing an alloy ingot with uniform components at the edge of a crucible, cutting the alloy ingot into alloy mother ingots with the mass of about 35g suitable for suction casting by using an electric arc, moving the alloy mother ingots into a suction casting copper mold crucible by using a mechanical arm, smelting the alloy ingots by using the electric arc (the control current is 190 mA), quickly opening a suction casting valve switch after the alloy ingots are completely molten, quickly suction casting the alloy into a water-cooling copper mold by using pressure difference, and quickly cooling the alloy by the water-cooling copper mold to obtain the plate-shaped amorphous alloy with the length, the width and the thickness of 85 multiplied by 30 multiplied by 2 mm.
Step four, primary processing:
sequentially grinding and polishing the plate-shaped amorphous alloy obtained in the step three by using sand paper of different types of 240 #, 400 #, 600 #, 800 #, 1000 #, 1500 # and 2000 #, and removing oil stains and impurities by using ultrasonic waves; simultaneously, mechanically polishing the side surface of the plate-shaped test sample by using diamond polishing paste, and then cleaning the test sample by using ultrasonic waves;
step five, cryogenic circulating treatment:
in order to improve the mechanical property of the amorphous alloy and enable the amorphous alloy to be in a higher energy state, the amorphous alloy is subjected to cryogenic circular treatment. And D, carrying out deep cooling circulation treatment on the amorphous alloy in the fourth step. Firstly, an amorphous alloy sample is put into a liquid nitrogen container for 5 minutes, then is quickly put into a boiled water container for 1 minute to be heated to 65 ℃, and then is kept still in a room temperature environment for 4 minutes. The treatment is a cryogenic cycle treatment, and 40 cycles of cryogenic treatment are carried out.
Step six, rolling and pre-deforming:
in order to further improve the amorphous toughness, after the deep cooling cycle treatment, an ATMR series electric miniature reversible two-roll mill is adopted for rolling, and the rolling process is completed in multiple steps: the reduction of each roller is not allowed to exceed 0.01mm, the reduction frequency of the roller is not less than 15 times of rolling processes, and the reduction of each pass is 0.01 mm. And a longitudinal rolling two-dimensional rolling mode is adopted in the rolling process, after each rolling pass is finished, the sample is horizontally rotated by 180 degrees, and the two directions are alternately rolled until the required 5% pre-deformation amount is obtained.
Step seven, fine machining:
and (3) polishing the alloy surface treated by the deep cooling circulation combined predeformation mode to the thickness of 0.4 mm of the diaphragm, polishing, and removing oil stains by using ultrasonic cleaning equipment. And then, according to a flexible coupling diaphragm design size drawing, utilizing the rotary heads with different diameters to precisely open holes in the diaphragm so as to install the fixing bolts. And (4) using a rotary head to perform hole opening according to the principle of opening holes from small to large successively. The diameter specifications of the rotating head are respectively 2, 3, 4, 5 and 6 mm. And then, accurately cutting according to the structure and the precision requirement by using a low-speed precision cutting machine according to the design dimension drawing. And then, polishing the side surface and the front surface and the back surface of the membrane into a mirror surface by using a polishing machine. And (4) cleaning oil stains and impurities of the finished membrane by using ultrasonic cleaning equipment.
Example 3:
this example is a deep cooling circulation combined pre-deformation mode for treating toughened Zr55Al10Ni5Cu29Y1A preparation method and application of amorphous alloy material.
The embodiment is that the Zr-Al-Ni-Cu-Y amorphous alloy material toughened by the deep cooling circulation combined pre-deformation mode treatment consists of five elements of Zr, Al, Ni, Cu and Y, wherein the atomic percent of the Zr-Al-Ni-Cu-Y amorphous alloy material is Zr55Al10Ni5Cu29Y1Wherein Ti, Zr, V, Cu and Be are subjected to smelting and suction casting to form plate-shaped amorphous alloy after removing oxides from blocky Zr, Al, Ni, Cu and Y with the purity of more than or equal to 99.999 percent by a file, cleaning by alcohol and drying by an oven, and then performing cryogenic circulating treatment and pre-deformation rolling.
Zr proposed in this example55Al10Ni5Cu29Y1Method for processing toughened amorphous alloy flexible coupling by cryogenic circulation combined predeformation modeThe preparation process of the membrane is as follows:
step one, pretreatment: respectively cleaning oxide skins of Zr, Al, Ni, Cu and Y metals serving as amorphous alloy raw materials by using a file, then respectively putting the raw materials into ultrasonic cleaning equipment filled with absolute ethyl alcohol for ultrasonic cleaning for 10-20 minutes to remove oil stains and impurities on the surfaces of the raw materials, and then drying the required raw materials by using a drying oven.
Step two, batching: according to the atomic percentage of Zr, Al, Ni, Cu and Y elements of 55: 10: 5: 29: 1 calculating the mass required for each raw material pure metal. And weighing the clean pure metal raw material processed in the step one by adopting an electronic balance with the precision of 0.001g, wherein the weighing mass error range is ensured to be less than +/-0.003 g.
Step three, smelting and suction casting:
(1) putting the pure metal raw materials weighed in the step two into the same copper mold crucible from bottom to top in sequence according to the sequence of the melting points of the elements from low to high, and ensuring that the high-melting-point raw materials can be completely melted; placing the titanium sponge block for testing the oxygen content into another copper mold crucible, and then closing the furnace door;
(2) pumping the cavity to below 5 Pa by using a first-stage mechanical pump, closing a closing valve, opening a second-stage mechanical pump and a molecular pump to make the interior of the furnace chamber reach a high vacuum state, and when the vacuum degree of the furnace chamber reaches 1 × 10-3When Pa, closing a valve at the molecular pump; then filling high-purity argon to ensure that the pressure of the furnace chamber is 0.5 atm;
(3) firstly, smelting a titanium sponge block to check the oxygen content in the furnace, and smelting alloy after the titanium sponge block is smelted and cooled and has no color change, wherein the smelting process adopts electric arc smelting (the current is controlled to be 200 mA), and an alloy ingot is repeatedly turned and smelted for 5 times to ensure uniform components;
(4) placing an alloy ingot with uniform components at the edge of a crucible, cutting the alloy ingot into alloy mother ingots with the mass of about 40g suitable for suction casting by using an electric arc, moving the alloy mother ingots into a suction casting copper mold crucible by using a mechanical arm, smelting the alloy ingots by using the electric arc (the control current is 200 mA), quickly opening a suction casting valve switch after the alloy ingots are completely molten, quickly suction casting the alloy into a water-cooling copper mold by using pressure difference, and quickly cooling the alloy by the water-cooling copper mold to obtain the plate-shaped amorphous alloy with the length, width and thickness of 85 multiplied by 30 multiplied by 2 mm.
Step four, primary processing:
sequentially grinding and polishing the plate-shaped amorphous alloy obtained in the step three by using sand paper of different types of 240 #, 400 #, 600 #, 800 #, 1000 #, 1500 # and 2000 #, and removing oil stains and impurities by using ultrasonic waves; simultaneously, mechanically polishing the side surface of the plate-shaped test sample by using diamond polishing paste, and then cleaning the test sample by using ultrasonic waves;
step five, cryogenic circulating treatment:
in order to improve the mechanical property of the amorphous alloy and enable the amorphous alloy to be in a higher energy state, the amorphous alloy is subjected to cryogenic circular treatment. And D, carrying out deep cooling circulation treatment on the amorphous alloy in the fourth step. Firstly, an amorphous alloy sample is put into a liquid nitrogen container for 5 minutes, then is quickly put into a boiled water container for 1 minute to be heated to 80 ℃, and then is kept stand in a room temperature environment for 4 minutes. The treatment is a cryogenic cycle treatment, and 60 cycles of cryogenic treatment are carried out.
Step six, rolling and pre-deforming:
in order to further improve the amorphous toughness, after the deep cooling cycle treatment, an ATMR series electric miniature reversible two-roll mill is adopted for rolling, and the rolling process is completed in multiple steps: the reduction of each roller is not allowed to exceed 1 scale value (1 scale value is 0.01 mm) of the dividing plate, the reduction frequency of the roller is not less than 15 times of rolling processes, and the reduction of each pass is 0.01 mm. And a longitudinal rolling two-dimensional rolling mode is adopted in the rolling process, after each rolling pass is finished, the sample is horizontally rotated by 180 degrees, and the two directions are alternately rolled until the required 5% pre-deformation amount is obtained.
Step seven, fine machining:
and (3) polishing the alloy surface treated by the deep cooling circulation combined predeformation mode to the thickness of 0.5mm of the diaphragm, polishing, and removing oil stains by using ultrasonic cleaning equipment. And then, according to a flexible coupling diaphragm design size drawing, utilizing the rotary heads with different diameters to precisely open holes in the diaphragm so as to install the fixing bolts. And (4) using a rotary head to perform hole opening according to the principle of opening holes from small to large successively. The diameter specifications of the rotating head are respectively 2, 3, 4, 5 and 6 mm. And then, accurately cutting according to the structure and the precision requirement by using a low-speed precision cutting machine according to the design dimension drawing. And then, polishing the side surface and the front surface and the back surface of the membrane into a mirror surface by using a polishing machine. And (4) cleaning oil stains and impurities of the finished membrane by using ultrasonic cleaning equipment.

Claims (8)

1.一种深冷循环组合预变形方式增韧非晶合金材料的制备方法，其特征在于包括以下步骤：1. a preparation method of a cryogenic cycle combined pre-deformation toughening amorphous alloy material is characterized in that comprising the following steps: 步骤一、预处理：将非晶合金原料Zr、Al、Ni、Cu、Y金属分别用锉刀进行氧化皮清理，之后将原料分别放入盛有无水乙醇的超声清洗设备中进行超声清洗10-20分钟，以清除原料表面的油污、杂质，之后将所需原料利用烘干箱烘干；Step 1. Pretreatment: The amorphous alloy raw materials Zr, Al, Ni, Cu, and Y metals are respectively cleaned with a file for oxide skin, and then the raw materials are respectively put into ultrasonic cleaning equipment filled with absolute ethanol for ultrasonic cleaning for 10- 20 minutes to remove oil stains and impurities on the surface of the raw materials, and then use the drying box to dry the required raw materials; 步骤二、配料：按照Zr、Al、Ni、Cu、Y元素的原子百分比55：10：5：29：1计算出每种纯金属原料所需的质量；Step 2. Ingredients: Calculate the required mass of each pure metal raw material according to the atomic percentage of Zr, Al, Ni, Cu, and Y elements 55:10:5:29:1; 步骤三、熔炼、吸铸：Step 3: Smelting and suction casting: （1）将步骤二称量好的纯金属原料按照各元素熔点由低到高的顺序依次在坩埚中从下往上放入同一铜模坩埚中，保证高熔点原料能完全熔化；将用于检验氧气含量的海绵钛块放入另一铜模坩埚中，之后关闭坩埚炉门；(1) Put the pure metal raw materials weighed in step 2 into the same copper mold crucible from bottom to top in the order of melting point of each element from low to high in order to ensure that the high melting point raw materials can be completely melted; Put the sponge titanium block for testing the oxygen content into another copper mold crucible, and then close the crucible furnace door; （2）使用一级机械泵将腔体抽至5 Pa以下关闭隔断阀，打开二级机械泵和分子泵，使炉腔内部达到高真空状态，当炉腔真空度达到1×10-3Pa时，关闭分子泵处的阀门；之后充入高纯氩气使得炉腔压强为0.5atm；(2) Use the primary mechanical pump to pump the cavity to below 5 Pa, close the block valve, open the secondary mechanical pump and molecular pump, and make the interior of the furnace chamber reach a high vacuum state. When the vacuum degree of the furnace chamber reaches 1×10 -3 Pa When , close the valve at the molecular pump; then fill with high-purity argon to make the furnace chamber pressure 0.5atm; （3）首先熔炼海绵钛块检验炉内氧气含量，待海绵钛块熔炼冷却之后无颜色变化后开始熔炼合金，熔炼过程采用电弧熔炼，为保证成分均匀合金锭反复翻转熔炼5次；(3) First, smelt the sponge titanium block to check the oxygen content in the furnace. After the sponge titanium block is smelted and cooled, there is no color change, and then the alloy is smelted. The smelting process adopts arc smelting. In order to ensure the uniform composition of the alloy ingot, the alloy ingot is repeatedly turned and smelted 5 times; （4）将成分均匀的合金锭置于坩埚边缘，利用电弧分割成质量30~40g的适合吸铸的合金母锭，之后将合金母锭利用机械臂移动到吸铸铜模坩埚中，利用电弧熔炼合金锭，待合金锭完全熔化后，迅速打开吸铸阀门开关利用压力差将合金快速吸铸到水冷铜模中，经水冷铜模快速冷却得到长宽厚为85×30×2mm的板状非晶合金；(4) Place the alloy ingot with uniform composition on the edge of the crucible, and divide it into alloy master ingots with a mass of 30~40g suitable for suction casting by electric arc. Smelting the alloy ingot, after the alloy ingot is completely melted, quickly open the suction and casting valve switch and use the pressure difference to quickly suction and cast the alloy into the water-cooled copper mold. crystal alloy; 步骤四、初加工：Step 4. Preliminary processing: 将步骤三得到的板状非晶合金依次采用240 #、400 #、600 #、800 #、1000 #、1500 #与2000 #不同型号的砂纸逐次打磨后并抛光，再用超声波去除油污、杂质；同时使用金刚石抛光膏对板状试样侧面进行机械抛光，之后利用超声波清洗试样；The plate-shaped amorphous alloy obtained in step 3 is successively ground and polished with different types of sandpapers of 240 #, 400 #, 600 #, 800 #, 1000 #, 1500 # and 2000 #, and then ultrasonic waves are used to remove oil stains and impurities; At the same time, use diamond polishing paste to mechanically polish the side of the plate sample, and then use ultrasonic to clean the sample; 步骤五、深冷循环处理：Step 5. Cryogenic cycle treatment: 将步骤四中的非晶合金进行深冷循环处理：首先,将非晶合金样品放入液氮容器中5分钟，然后迅速通过放入开水容器中1分钟进行加热到50~80℃，之后再静置室温环境中4分钟；以此为一个深冷循环处理，分别进行20~60次循环深冷处理；制得非晶合金材料铜模吸铸出来的板状样品。The amorphous alloy in step 4 is subjected to cryogenic cycle treatment: first, the amorphous alloy sample is placed in a liquid nitrogen container for 5 minutes, and then quickly heated to 50~80 ° C by placing it in a boiling water container for 1 minute, and then Stand at room temperature for 4 minutes; take this as a cryogenic cycle treatment, and perform 20 to 60 cycles of cryogenic treatment respectively; obtain a plate-shaped sample of amorphous alloy material copper mold suction casting. 2.根据权利要求1所述的深冷循环组合预变形方式增韧非晶合金材料的制备方法，其特征在于：所述步骤二中，称量采用精度为0.001g的电子天平将步骤一处理干净的纯金属原料进行称量，称量质量误差范围保证在±0.003g范围内。2. The preparation method of the cryogenic cycle combined pre-deformation toughening amorphous alloy material according to claim 1, characterized in that: in the step 2, the weighing adopts an electronic balance with an accuracy of 0.001g to process the step 1 Clean pure metal raw materials are weighed, and the weighing quality error range is guaranteed to be within the range of ±0.003g. 3.根据权利要求1所述的深冷循环组合预变形方式增韧非晶合金材料的制备方法，其特征在于：所述步骤三中，氩气的纯度为99.999%。3 . The preparation method of the cryogenic cycle combined pre-deformation toughening amorphous alloy material according to claim 1 , wherein in the third step, the purity of argon is 99.999%. 4 . 4.根据权利要求1所述的深冷循环组合预变形方式增韧非晶合金材料的制备方法，其特征在于：所述步骤三中，电弧熔炼时，控制电流大小为180~200mA。4 . The preparation method of the cryogenic cycle combined pre-deformation toughening amorphous alloy material according to claim 1 , wherein in the step 3, during arc melting, the control current is 180-200 mA. 5 . 5.一种权利要求1~4任一项所述的方法制得的非晶合金材料在柔性联轴器膜片中的应用。5. Application of the amorphous alloy material prepared by the method according to any one of claims 1 to 4 in a flexible coupling diaphragm. 6.根据权利要求5所述的应用，其特征在于包括以下步骤：6. application according to claim 5 is characterized in that comprising the following steps: （1）轧制预变形：(1) Rolling pre-deformation: 采用ATMR系列电动微型可逆式二辊轧机，对深冷循环处理之后的非晶合金材料板状样品进行轧制，轧制过程分多道次完成；轧制过程采用纵轧二维轧制方式，在每个轧制道次完成后，将试样水平旋转180°，两个方向交替轧制，直到获得所需的5%的预变形量；The ATMR series electric miniature reversible two-high rolling mill is used to roll the amorphous alloy material plate sample after cryogenic cycle treatment. The rolling process is completed in multiple passes; the rolling process adopts the longitudinal rolling two-dimensional rolling method. After the completion of each rolling pass, rotate the sample horizontally by 180° and alternately roll in both directions until the desired 5% pre-deformation is obtained; （2）精加工：(2) Finishing: 将预变形处理后的合金表面打磨到膜片0.3~0.5mm厚度、抛光，并利用超声波清洗设备清除油污；然后根据柔性联轴器膜片设计尺寸图纸，利用不同直径的转头对膜片进行精准开孔，以便安装固定螺栓；使用转头依据从小到大逐次开孔的原则进行开孔；之后利用低速精密切割机按照设计尺寸图纸按照结构和精度要求进行精准切割；随后利用抛光机，对膜片侧面及正反两面进行水磨抛光成镜面；利用超声清洗设备对成品膜片进行油污、杂质清洗；制得柔性联轴器膜片。Grind the pre-deformed alloy surface to a thickness of 0.3~0.5mm of the diaphragm, polish, and use ultrasonic cleaning equipment to remove oil; Precisely drill holes for the installation of fixing bolts; use the rotor to drill holes according to the principle of opening holes from small to large; then use a low-speed precision cutting machine to perform precise cutting according to the structure and accuracy requirements according to the design size drawings; then use a polishing machine to cut the holes. The side and front and back sides of the diaphragm are water-grinded and polished to a mirror surface; the finished diaphragm is cleaned of oil stains and impurities by ultrasonic cleaning equipment; the flexible coupling diaphragm is obtained. 7.根据权利要求6所述的应用，其特征在于：所述轧制预变形过程中，每次轧辊压下量不允许超过0.01mm，轧辊压下频率不少于15次轧制过程，每个道次压下量为0.01mm。7. The application according to claim 6, characterized in that: in the pre-deformation process of rolling, the reduction amount of each roll is not allowed to exceed 0.01mm, and the frequency of roll reduction is not less than 15 times during the rolling process. The reduction amount of each pass is 0.01mm. 8.根据权利要求6所述的应用，其特征在于：所用转头的直径分别为2、3、4、5、6mm。8. The application according to claim 6, wherein the diameters of the rotors used are 2, 3, 4, 5, and 6 mm, respectively.
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CN117490409A (en) * 2023-12-29 2024-02-02 河南梦瑶科技有限公司 Smelting device of high-phosphorus copper alloy
CN117490409B (en) * 2023-12-29 2024-03-22 河南梦瑶科技有限公司 Smelting device of high-phosphorus copper alloy

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