CN115341111A - Ni-Sn series intermetallic compound and preparation method and application thereof - Google Patents
Ni-Sn series intermetallic compound and preparation method and application thereof Download PDFInfo
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- CN115341111A CN115341111A CN202211004376.0A CN202211004376A CN115341111A CN 115341111 A CN115341111 A CN 115341111A CN 202211004376 A CN202211004376 A CN 202211004376A CN 115341111 A CN115341111 A CN 115341111A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention discloses a Ni-Sn series intermetallic compound and a preparation method and application thereof. The preparation method of the Ni-Sn series intermetallic compound comprises the following steps: and pressing and molding the ball-milled mixed powder of the Ni powder and the Sn powder, and then carrying out vacuum melting to obtain the Ni-Sn intermetallic compound. By pressing the Ni powder and the Sn powder, the relative positions of Ni and Sn can be fixed, and then the Ni and Sn can fully react when the Ni and Sn are subjected to vacuum melting, so that the phenomenon that a barrier layer of an intermetallic compound of Ni-Sn is generated in the reaction process to influence the continuous reaction of Ni and Sn is avoided. Therefore, the Ni — Sn intermetallic compound in the form of powder can be crushed by means of ball milling again or the like of the Ni — Sn intermetallic compound obtained in high purity by melting. The method combines a powder metallurgy method and a mechanical alloying method, overcomes the defects and limitations of a single method, has complete reaction and single component, and is easy for large-scale production.
Description
Technical Field
The invention relates to the technical field of high-temperature alloys, in particular to a Ni-Sn intermetallic compound and a preparation method and application thereof.
Background
The intermetallic compound phase is an important composition phase of the engineering alloy and has higher yield strength, considerable creep resistance and reasonable corrosion resistance. The tin-nickel alloy plating layer is pink and slightly black plating layer which is difficult to change color, has particularly good corrosion resistance, and is suitable for being applied to products such as bicycles, automobiles, electronics and the like. The alloy composition change can obtain bright bluish white, pink slightly black to bright black, and can make the color uniform, not only can be used as decorative coating to replace traditional copper-nickel-chromium system, but also can be used as functional coating. Ni-Sn systems (e.g. Ni) 3 Sn 4 ) The remelting temperature of the first intermetallic target phase is 1067.5K (794.5 ℃ C.). In combination with this, the excellent corrosion resistance of Ni makes this system more versatile for high temperature applications in various industrial fields.
The conventional Ni — Sn intermetallic compound is generally used as a coating material in the form of alloy powder, and the intermetallic compound powder is generally produced mainly by an atomization method. The atomization method is characterized in that Ni and Sn metal powder are used as raw materials and are heated and melted, then high-pressure inert gas is used for crushing alloy liquid into fine liquid drops, then the fine liquid drops are cooled into solid powder, and then the cooled solid powder is subjected to ball milling and sieving to finally obtain intermetallic compound powder. The main disadvantages are: the particle size of the powder formed by atomization is larger than 100 mu m, and the subsequent ball milling and refining difficulty is high after high-temperature alloying, so that oxidation is easily caused in the atomization process to form oxide impurities.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The present invention is directed to provide an Ni — Sn intermetallic compound, and a method for producing the same and use thereof, which can improve the above-mentioned problems.
The invention is realized in the following way:
in a first aspect, the present invention provides a method for producing an Ni — Sn-based intermetallic compound, comprising: and pressing and molding the ball-milled mixed powder of the Ni powder and the Sn powder, and then carrying out vacuum melting to obtain the Ni-Sn intermetallic compound.
Alternatively, the compression molding is to tablet the ball-milled mixed powder.
Optionally, the pressure of the tablet is 1-2 MPa;
optionally, the pressed flaky Ni-Sn mixture has a thickness of 2 to 5mm, preferably 2.5 to 3.5mm, and optionally, the flaky Ni-Sn mixture is a circular piece having a diameter of 8 to 15mm.
Optionally, the temperature of the vacuum melting is 1400 to 1600 ℃, preferably 1450 to 1550 ℃, more preferably 1500 ℃, and the time of the vacuum melting is 20 to 40min, preferably 25 to 35min, more preferably 30min.
Optionally, the preparation method further comprises preparing a ball-milled mixed powder: and putting the Ni powder and the Sn powder into a high-energy ball mill for ball milling and mixing.
Optionally, the rotation speed of the ball mill is 400-600 r/min, and the ball milling time is at least 20min, preferably 30-60 min.
Optionally, the particle sizes of the Ni powder and the Sn powder are both smaller than 300 meshes; and/or the purity of the Ni powder and the Sn powder is more than 99.9 percent, and the preferred purity is 99.99 percent;
alternatively, the molar ratio of the Ni powder to the Sn powder is 3 3 Sn 4 An intermetallic compound.
Optionally, the preparation method further comprises the steps of casting the molten Ni-Sn alloy obtained by vacuum melting into a mold, cooling to prepare a metal wire, cutting the metal wire, and cutting the cut Ni 3 Sn 4 And putting the metal section into a high-energy ball mill for ball milling.
Optionally, on ball-milled Ni 3 Sn 4 The powder is screened for particle size, preferably less than 3 μm.
Optionally, the diameter of the wire is 0.8 to 1mm, preferably 0.9mm;
and/or Ni obtained by cutting a metal wire 3 Sn 4 The length of the metal section is 2-4 mm, preferably 3mm;
and/or the ball mill has a material-ball ratio of 15-25, and the grinding balls are made of ZrO 2 The ball milling time is at least 48 hours;
and/or adding absolute ethyl alcohol into the ball mill, wherein the mass ratio of the absolute ethyl alcohol to the Ni powder is 6-10: 1.
optionally, adding Ni 3 Sn 4 Before ball milling of the metal segment, ni is added 3 Sn 4 The metal section is cleaned, preferably by ultrasonic cleaning of Ni 3 Sn 4 And cleaning the metal section.
In a second aspect, the present invention also provides a Ni — Sn-based intermetallic compound produced by the above production method, optionally, the Ni — Sn-based intermetallic compound is a powder having a particle size of less than 3 μm.
In a third aspect, the invention also provides an application of the Ni-Sn intermetallic compound in preparing plating layers of bicycles, automobiles, composite electronic solder reinforcements or electronic products.
The invention has the following beneficial effects: by pressing the Ni powder and the Sn powder, the relative positions of Ni and Sn can be fixed, and further, when the Ni and the Sn are subjected to vacuum melting, the Ni and the Sn can fully react to form an Ni-Sn intermetallic compound, so that the barrier layer of the Ni-Sn intermetallic compound is prevented from being generated in the reaction process, and the continuous reaction of the Ni and the Sn is prevented from being influenced. Therefore, by this method, a high-purity Ni — Sn intermetallic compound can be obtained by melting, and a high-purity Ni — Sn intermetallic compound in the form of powder can be obtained by crushing by means of ball milling again or the like. The method combines a powder metallurgy method and a mechanical alloying method, overcomes the defects and limitations of a single method, has complete reaction and single component, and is easy for large-scale production.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and those skilled in the art can also obtain other related drawings based on the drawings without inventive efforts.
FIG. 1 is a schematic flow chart of a method for producing an intermetallic Ni-Sn compound according to an embodiment of the present invention;
FIG. 2 shows Ni of example 1 3 Sn 4 XRD examination of the powder;
FIG. 3 shows Ni of example 1 3 Sn 4 SEM scanning electron micrographs of the powder.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following is a detailed description of the Ni-Sn intermetallic compound provided by the present invention, and the preparation method and application thereof.
Some embodiments of the present invention provide a method of preparing an Ni — Sn based intermetallic compound, including: and pressing and molding the ball-milled mixed powder of the Ni powder and the Sn powder, and then carrying out vacuum melting to obtain the Ni-Sn intermetallic compound.
The inventor discovers through a great deal of research and practice that Ni powder and Sn powder can be fully and uniformly mixed in a ball milling mode, then the Ni powder and the Sn powder are pressed, so that the relative positions of Ni and Sn can be fixed, further, when the Ni and the Sn are melted in vacuum, the pressed Ni and the pressed Sn in a fixed form can be in-situ melted, further, the Ni and the pressed Sn in a blank in the fixed form can be fully reacted to form a Ni-Sn intermetallic compound, the purity is high, the Ni powder or the Sn powder is remained as little as possible, and the complete reaction of the Ni powder and the Sn powder is basically realized. The above operation avoids the following disadvantages caused by directly melting the loosely mixed powder of the Ni powder and the Sn powder: a barrier layer of Ni-Sn intermetallic compound is generated in the reaction process, and the continuous reaction of Ni and Sn is influenced.
Therefore, by this method, a high-purity Ni — Sn intermetallic compound can be obtained by melting, and a high-purity Ni — Sn intermetallic compound in the form of powder can be obtained by crushing by means of ball milling again or the like. The method combines a powder metallurgy method and a mechanical alloying method, overcomes the defects and limitations of a single method, has complete reaction and single component, and is easy for large-scale production.
It should be noted that, in the above method, the main reactions that occur are:
3Ni+Sn→Ni 3 Sn (1)
3Ni+2Sn→Ni 3 Sn 2 (2)
3Ni+4Sn→Ni 3 Sn 4 (3)
Ni 3 Sn+Sn→Sn 3 Sn 2 (4)
Ni 3 Sn+3Sn→Ni 3 Sn 4 (5)
Ni 3 Sn 2 +2Sn→Ni 3 Sn 4 (6)
specifically, in some embodiments, in order to allow the reaction to proceed better, the compression molding is performed by tabletting the ball-milled mixed powder. Namely, the mixed powder after ball milling is put into a die and is tabletted in a tabletting machine. In order to make the shape of the pressed blank more stable and the positions of Ni and Sn can be sufficiently fixed, the pressure of the pressed sheet is 1 to 2MPa in some embodiments, and for example, 1.1MPa, 1.2MPa, 1.3MPa, 1.4MPa, 1.5MPa, 1.6MPa, 1.7MPa, 1.8MPa, 1.9MPa or 2MPa can be selected.
In some embodiments, the thickness of the pressed flake Ni — Sn mixture is 2 to 5mm, preferably 2.5 to 3.5mm, for example 3mm may be selected. The flake Ni-Sn mixture is a circular flake having a diameter of 8 to 15mm, for example, 8mm, 9mm, 10mm, 11mm, 12mm, 13mm, 14mm, or the like. In other embodiments, blanks of other shapes can be pressed according to requirements, and the size of the blank can be selected according to requirements.
Further, in some embodiments, in order to enable a sufficient melting reaction between the Ni powder and the Sn powder, the temperature of the vacuum melting is 1400 to 1600 ℃, preferably 1450 to 1550 ℃, more preferably 1500 ℃, and the time of the vacuum melting is 20 to 40min, preferably 25 to 35min, more preferably 30min.
In some embodiments, the method of making further comprises making a ball-milled mixed powder: and putting the Ni powder and the Sn powder into a high-energy ball mill for ball milling and mixing. Specifically, the rotating speed of the ball mill is 400-600 r/min, and the ball milling time is at least 20min, preferably 30-60 min. For example, the rotation speed can be 400r/min, 500r/min or 600r/min. It should be noted that the ball milling process is performed under an inert gas or vacuum environment to isolate air and avoid oxidation.
In summary, according to the growth kinetics of the Ni-Sn intermetallic compound, when the particle sizes of the Ni powder and the Sn powder are smaller than 300 meshes, a Ni-Sn intermetallic compound barrier layer is less likely to be formed between the Ni powder and the Sn powder due to the small particle size, and the Ni and the Sn can react sufficiently. In order to enable the Ni-Sn intermetallic compound generated by the reaction to have higher purity, the purity of Ni powder and Sn powder is more than 99.9 percent, and the preferred purity is 99.99 percent;
in some embodiments, the molar ratio of the Ni powder to the Sn powder is 3, the Ni-Sn based intermetallic compound is Ni 3 Sn 4 An intermetallic compound.
Further, in some embodiments, the preparation method further comprises casting the molten Ni-Sn alloy obtained by vacuum melting into a mold to be cooled to prepare the metal wire, cutting the metal wire, and cutting the cut Ni 3 Sn 4 And putting the metal section into a high-energy ball mill for ball milling. Then the ball-milled Ni is treated 3 Sn 4 The powder is screened for particle size, preferably less than 3 μm.
In particular, in some embodiments, the wire has a diameter of 0.8 to 1mm, preferably 0.9mm, and/or the wire is cut to obtain Ni 3 Sn 4 The length of the metal section is 2-4 mm, preferably 3mm; and/or the ball mill has a material-ball ratio of 15-25, and the grinding balls are made of ZrO 2 The ball milling time is at least 48 hours. The particle size of the metal powder is reduced along with the increase of the ball milling time, and the minimum particle size can reach a nanometer level.In order to isolate air and avoid oxidation in the ball milling process, anhydrous ethanol is added into the ball mill, and the addition amount of the anhydrous ethanol is 60ml.
Further, to ensure impurities are introduced during ball milling, in some embodiments, ni is added 3 Sn 4 Before ball milling of the metal segment, ni is added 3 Sn 4 The metal section is cleaned, preferably by ultrasonic cleaning of Ni 3 Sn 4 And cleaning the metal section. Ni to be obtained by cooling 3 Sn 4 And putting the metal section into a beaker filled with alcohol, and cleaning the metal section in an ultrasonic cleaning machine.
See FIG. 1, to obtain Ni 3 Sn 4 As an example, some embodiments of the present invention provide a method for preparing Ni — Sn intermetallic compound powder, which specifically includes:
1) Ni powder with purity of 99.99% and grain size of 300 meshes and Sn powder are mixed according to the proportion of Ni 3 Sn 4 The stoichiometric ratio of (a).
2) And (3) putting the obtained Ni-Sn powder into a high-energy ball mill for fully mixing, wherein the rotating speed of the ball mill is 500r/min, and the time is 30min, so that the aim of uniformly dispersing the Sn powder of the Ni powder is fulfilled.
3) Putting the mixed powder into a die, tabletting in a tabletting machine under the pressure of 1.5MPa to obtain the flaky Ni-Sn with the thickness of 3mm and the diameter of 10mm, wherein the tabletting is to fix the relative positions of Ni and Sn so as to avoid the subsequent generation of Ni 3 Sn 4 Barrier layer, blocking Ni 3 Sn 4 And (4) reacting.
4) And (3) putting the flaky Ni-Sn alloy into a non-consumable vacuum melting furnace with the temperature of 1500 ℃, keeping the temperature for 30 minutes, wherein the number of the flaky Ni-Sn alloy is 6.
5) The molten Ni-Sn alloy was suction-cast into a die having a hole diameter of 0.9mm, and naturally cooled as shown in FIG. 1, thereby obtaining a wire having a diameter of 0.9 mm.
6) Cooling the obtained Ni 3 Sn 4 The wire was cut with wire cutters containing nickel and chromium, each section having a length of 3mm.
7) Mixing the obtained Ni 3 Sn 4 Putting the metal section into a beaker filled with a proper amount of alcohol, cleaning the metal section in an ultrasonic cleaning machine, and removing Ni 3 Sn 4 Impurities on the surface of the metal segment;
8) The cleaned Ni 3 Sn 4 After the metal sections are weighed, zrO 1 is added according to a ball-to-feed ratio of 20 2 Grinding ball, placing into high-energy ball mill, adding appropriate amount of alcohol, and preventing Ni 3 Sn 4 Oxidized, and the ball milling time is 72 hours;
9) Taking out the ball-milled powder, putting the ball-milled powder into a 3-micron screen, and screening out Ni meeting the requirement 3 Sn 4 And (3) powder.
Some embodiments of the present invention also provide a Ni — Sn-based intermetallic compound prepared by the preparation method provided in any of the above embodiments, optionally, the Ni — Sn-based intermetallic compound is a powder having a particle size of less than 3 μm.
Some embodiments of the invention also provide application of the Ni-Sn intermetallic compound in preparing plating layers of bicycles, automobiles, composite electronic solder reinforcements or electronic products.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
This example specifically provides an intermetallic compound Ni of Ni-Sn series 3 Sn 4 The preparation method of the powder specifically comprises the following steps:
1) Ni powder and Sn powder with the purity of 99.99 percent and the grain diameter of 300 meshes are mixed according to the proportion of Ni 3 Sn 4 5.2823g of Ni powder, 14.2452g of Sn powder.
2) Putting the Ni-Sn powder obtained in the step 1) into a high-energy ball mill for fully mixing, wherein the rotating speed of the ball mill is 500r/min, and the time is 30min, so that the aim of uniformly dispersing the Sn powder of the Ni powder is fulfilled.
3) Putting the powder mixed in the step 2) into a die, and tabletting in a tabletting machine under the pressure of 1.5MPa to obtain the flaky Ni-Sn with the thickness of 3mm and the diameter of 10mm.
4) Putting the flaky Ni-Sn alloy blank obtained in the step 3) into a non-consumable vacuum melting furnace with the temperature of 1500 ℃, wherein the number of the flaky Ni-Sn alloy blanks is 6, and keeping the temperature for 30 minutes.
5) And (5) suction casting the molten Ni-Sn alloy obtained in the step 4) into a die with a hole diameter of 0.9mm, and naturally cooling to obtain the metal wire with the diameter of 0.9 mm.
6) Cooling the Ni obtained in the step 5) 3 Sn 4 The wire was cut with wire cutters containing nickel and chromium, each section having a length of 3mm.
7) Subjecting the Ni obtained in step 6) 3 Sn 4 Putting the metal section into a beaker filled with alcohol, cleaning the metal section in an ultrasonic cleaning machine, and removing Ni 3 Sn 4 Impurities on the surface of the metal segment.
8) Ni obtained after cleaning in the step 7) 3 Sn 4 After the metal section is weighed, zrO is added according to a ball-to-feed ratio of 20 2 Grinding ball, placing into high-energy ball mill, adding 60ml alcohol to prevent Ni 3 Sn 4 Oxidized and the ball milling time is 72h.
9) Taking out the powder subjected to ball milling in the step 8), putting the powder into a 3-micron screen, and screening out Ni meeting the requirements 3 Sn 4 And (3) powder.
Example 2
This example specifically provides an intermetallic compound Ni of Ni-Sn series 3 Sn 4 The preparation method of the powder specifically comprises the following steps:
1) Ni powder and Sn powder with the purity of 99.99 percent and the grain diameter of 300 meshes are mixed according to the proportion of Ni 3 Sn 4 5.2823g of Ni powder, 14.2452g of Sn powder.
2) Putting the Ni-Sn powder obtained in the step 1) into a high-energy ball mill for fully mixing, wherein the rotating speed of the ball mill is 500r/min, and the time is 60min, so that the aim of uniformly dispersing the Sn powder of the Ni powder is fulfilled.
3) Putting the powder mixed in the step 2) into a die, and tabletting in a tabletting machine under the pressure of 1.5MPa to obtain the flaky Ni-Sn with the thickness of 3mm and the diameter of 10mm.
4) Putting the flaky Ni-Sn alloy blank obtained in the step 3) into a non-consumable vacuum melting furnace with the temperature of 1500 ℃, wherein the number of the flaky Ni-Sn alloy blanks is 6, and keeping the temperature for 30 minutes.
5) And (3) carrying out suction casting on the Ni-Sn alloy melted in the step 4) into a die with a hole diameter of 0.9mm, and naturally cooling to obtain the metal wire with the diameter of 0.9 mm.
6) Cooling the Ni obtained in the step 5) 3 Sn 4 The wire was cut with wire cutters containing nickel and chromium, each section having a length of 3mm.
7) Subjecting the Ni obtained in step 6) 3 Sn 4 Putting the metal section into a beaker filled with alcohol, cleaning the metal section in an ultrasonic cleaning machine, and removing Ni 3 Sn 4 Impurities on the surface of the metal segment.
8) Ni obtained after cleaning in the step 7) 3 Sn 4 After the metal sections are weighed, zrO 1 is added according to a ball-to-feed ratio of 20 2 Grinding ball, placing into high energy ball mill, and adding 60ml alcohol to prevent Ni 3 Sn 4 Oxidized and the ball milling time is 84h.
9) Taking out the powder subjected to ball milling in the step 8), putting the powder into a 3-micron screen, and screening out Ni meeting the requirements 3 Sn 4 And (3) powder.
Example 3
This example specifically provides an intermetallic compound Ni of Ni-Sn series 3 Sn 4 The preparation method of the powder specifically comprises the following steps:
1) Ni powder and Sn powder with the purity of 99.99 percent and the grain diameter of 300 meshes are mixed according to the proportion of Ni 3 Sn 4 The stoichiometric ratio of (A) was measured, and Ni powder 8.0996g, sn powder 21.8426g were weighed.
2) Putting the Ni-Sn powder obtained in the step 1) into a high-energy ball mill for fully mixing, wherein the rotating speed of the ball mill is 500r/min, and the time is 60min, so that the aim of uniformly dispersing the Sn powder of the Ni powder is fulfilled.
3) Putting the powder mixed in the step 2) into a die, and tabletting in a tabletting machine under the pressure of 1.5MPa to obtain the flaky Ni-Sn with the thickness of 3mm and the diameter of 10mm.
4) Putting the flaky Ni-Sn alloy blank obtained in the step 3) into a non-consumable vacuum melting furnace with the temperature of 1500 ℃, wherein the number of the flaky Ni-Sn alloy blanks is 6, and keeping the temperature for 30 minutes.
5) And (3) carrying out suction casting on the Ni-Sn alloy melted in the step 4) into a die with a hole diameter of 0.9mm, and naturally cooling to obtain the metal wire with the diameter of 0.9 mm.
6) Cooling the step 5) to obtainTo Ni 3 Sn 4 The wire was cut with wire cutters containing nickel and chromium, each section having a length of 3mm.
7) Subjecting the Ni obtained in step 6) 3 Sn 4 Putting the metal section into a beaker filled with alcohol, cleaning the metal section in an ultrasonic cleaning machine, and removing Ni 3 Sn 4 Impurities on the surface of the metal segment.
8) Ni obtained after cleaning in the step 7) 3 Sn 4 After the metal sections are weighed, zrO 1 is added according to a ball-to-feed ratio of 20 2 Grinding ball, placing into high energy ball mill, and adding 60ml alcohol to prevent Ni 3 Sn 4 Oxidized and the ball milling time is 84h.
9) Taking out the powder subjected to ball milling in the step 8), putting the powder into a 3-micron screen, and screening out Ni meeting the requirements 3 Sn 4 And (3) powder.
Ni obtained according to examples 1 to 3 3 Sn 4 The powder masses are given in Table 1.
TABLE 1
For Ni obtained in example 1 3 Sn 4 The powder was subjected to XRD phase analysis, and the results are shown in FIG. 2. For Ni obtained in example 1 3 Sn 4 The powder was observed by scanning electron microscopy, and the results are shown in FIG. 3. As can be seen from FIGS. 2 and 3, ni 3 Sn 4 The powder has single phase and high purity.
As described above, high purity Ni powder and Sn powder having a particle size of 300 mesh were obtained in terms of Ni due to their small particle size 3 Sn 4 Growth kinetics, a Ni-Sn intermetallic compound barrier layer is not formed, and Ni and Sn can fully react. Tabletting the weighed Ni-Sn powder, fixing the relative positions of Ni and Sn, reacting at 1500 ℃ to prevent forming a Ni-Sn metal piece compound barrier layer and prevent further Ni and SnReaction to form Ni 3 Sn 4 Can make Ni and Sn fully react to form Ni 3 Sn 4 . Further, the above method produces Ni 3 Sn 4 In the process, no cosolvent is added, no acid washing is needed, and the method is environment-friendly; proper amount of alcohol is added in the ball milling process to play a role in isolating air, the ball milling time is long enough, and the obtained Ni 3 Sn 4 The powder has small and uniform particle size. And the air is isolated in the smelting and cooling processes, so that the prepared Ni 3 Sn 4 The purity is high.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for producing an Ni-Sn based intermetallic compound, characterized by comprising:
and pressing and molding the ball-milled mixed powder of the Ni powder and the Sn powder, and then carrying out vacuum melting to obtain the Ni-Sn intermetallic compound.
2. The production method according to claim 1, wherein the press molding is performed by tableting the ball-milled mixed powder;
preferably, the pressure of the tabletting is 1-2 MPa;
preferably, the thickness of the pressed flaky Ni-Sn mixture is 2 to 5mm, preferably 2.5 to 3.5mm, and preferably, the flaky Ni-Sn mixture is a circular flake with a diameter of 8 to 15mm.
3. The method of claim 1, wherein the temperature of the vacuum melting is 1400 to 1600 ℃, preferably 1450 to 1550 ℃, more preferably 1500 ℃, and the time of the vacuum melting is 20 to 40min, preferably 25 to 35min, more preferably 30min.
4. The production method according to any one of claims 1 to 3, further comprising preparing the ball-milled mixed powder: putting Ni powder and Sn powder into a high-energy ball mill for ball milling and mixing;
preferably, the rotation speed of the ball mill is 400-600 r/min, and the ball milling time is at least 20min, preferably 30-60 min.
5. The production method according to claim 4, wherein the particle sizes of the Ni powder and the Sn powder are each less than 300 mesh; and/or the purity of the Ni powder and the purity of the Sn powder are both more than 99.9 percent, and the preferred purity is 99.99 percent;
preferably, the molar ratio of the Ni powder to the Sn powder is 3:4, and the Ni-Sn intermetallic compound is Ni 3 Sn 4 An intermetallic compound.
6. The method according to claim 1, further comprising casting the Ni — Sn alloy in a molten state obtained by the vacuum melting into a mold, cooling the Ni — Sn alloy to prepare a wire, cutting the wire, and cutting the cut Ni 3 Sn 4 Putting the metal section into a high-energy ball mill for ball milling;
preferably, ni after ball milling 3 Sn 4 The powder is screened for particle size, preferably less than 3 μm.
7. The method of claim 6, wherein the wire has a diameter of 0.8 to 1mm, preferably 0.9mm;
and/or Ni obtained by cutting the metal wire 3 Sn 4 The length of the metal section is 2-4 mm, preferably 3mm;
and/or the ball mill has a material-ball ratio of 15-25, and the grinding balls are made of ZrO 2 The ball milling time is at least 48 hours;
and/or adding absolute ethyl alcohol into the ball mill, wherein the mass ratio of the absolute ethyl alcohol to the Ni powder is 6-10: 1.
8. the method of claim 6Is characterized in that the Ni is added 3 Sn 4 Before ball milling of the metal segments, the Ni is added 3 Sn 4 Cleaning the metal section, preferably by ultrasonic treatment of the Ni 3 Sn 4 And cleaning the metal section.
9. An Ni-Sn-based intermetallic compound produced by the production method according to any one of claims 1 to 8, preferably, the Ni-Sn-based intermetallic compound is a powder having a particle size of less than 3 μm.
10. Use of the Ni-Sn-based intermetallic compound according to claim 9 for producing a plating layer for bicycles, automobiles, composite electronic solder reinforcements, or electronic products.
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| CN106498197A (en) * | 2016-10-18 | 2017-03-15 | 广西大学 | A kind of preparation method of Sn Cu Al series lead-free solders |
| CN108374104A (en) * | 2018-03-09 | 2018-08-07 | 广西大学 | A kind of low melting point Sn-Bi-Al series lead-free solder alloy materials and preparation method thereof |
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| JP2009074106A (en) * | 2007-09-18 | 2009-04-09 | Tokyo Institute Of Technology | Method for forming and manufacturing object composed of intermetallic-compound alloy containing low-melting-point metal and high-melting-point metal |
| CN106498197A (en) * | 2016-10-18 | 2017-03-15 | 广西大学 | A kind of preparation method of Sn Cu Al series lead-free solders |
| CN108374104A (en) * | 2018-03-09 | 2018-08-07 | 广西大学 | A kind of low melting point Sn-Bi-Al series lead-free solder alloy materials and preparation method thereof |
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