CN101774009B - Device and method for forming an amorphous alloy thin-walled slender tube - Google Patents

Abstract

The invention provides a device and a method for shaping an amorphous alloy thin-wall slim pipe, and relates to a device and a method for shaping an amorphous alloy pipe. The invention aims at solving the problems that the thin-wall positions of the prior prepared amorphous alloy pipe can not fill and an inductive crucible easily reacts with the amorphous alloy. The device is a shaping device with a mold cavity, which is formed by the assembly of an arc-melting furnace, a copper crucible, a temperature measuring device, a suction casting valve, a mechanical pump, a tungsten electrode, a metal mold, a suction casting controller and a melting current controller. The method comprises the following steps: an alloy ingot is input; the vacuum degree is 5.0*10<-3>-6.0*10<-3>Pa; the melting current is 250-400A; and when the bottom temperature of the alloy ingot is more than the liquid-phase temperature, the suction casting controller opens the suction casting valve, the mechanical pump draws the air out of the inner cavity of the arc-melting furnace, the alloy liquid flows into the mold cavity, the alloy liquid in contact with the side wall forms a very thin metal scull on the side wall of the mold cavity, and the unsolidified alloy liquid in the center is drawn out of the mold. The invention is used for shaping of the slim alloy pipe.

Description

Device and method for forming an amorphous alloy thin-walled slender tube

technical field

The invention relates to a device and method for forming an elongated amorphous alloy tube.

Background technique

Amorphous alloys have excellent physical and chemical properties such as high elastic limit, high strength, high hardness, high wear resistance, and high corrosion resistance because they do not have a microstructure with long-range atomic order. At present, amorphous alloy tubes have been used as sensor components of mass flow meters. Amorphous alloy is a kind of rapid solidification material. The methods for preparing amorphous alloy pipe mainly include copper mold casting method, core pulling method and induction suction casting method. The copper mold casting method mainly injects amorphous alloy liquid into In the mold, so as to rapidly solidify and form an amorphous alloy pipe, the material of the amorphous alloy pipe mold is generally pure copper. The alloy tube method, the patent belongs to the copper mold casting method, although the patent has the characteristics of simple process, but because the mold and the core are copper, there is a problem that the core and the amorphous alloy tube are difficult to separate when taking the core . The core pulling method is to first fill the amorphous alloy liquid into a mold with a core and cool it to room temperature, then heat the core, and the inner wall of the amorphous alloy tube in contact with the core is also heated. At the temperature of the cold liquid phase region, since the amorphous alloy has superplasticity in the supercooled liquid phase region, the core can be pulled out with a small external force, and at the same time, this method can ensure that the amorphous alloy pipe has a smooth inner wall. However, the copper mold casting method and the core pulling method are only suitable for the preparation of thick-walled amorphous alloy pipes. When preparing thin-walled amorphous alloy pipes (with a wall thickness less than 1mm), the problem that the mold cannot be filled at the thin-walled part will occur when the above two methods are used. The induction suction casting method is to suck the liquid amorphous alloy liquid from the bottom into the cold tubular mold, and the amorphous alloy liquid in contact with the mold wall will quickly solidify to form a tubular solidified shell, while the amorphous alloy liquid at the center of the mold cannot immediately Solidification, when the flow rate of the alloy liquid produced by suction casting reaches a certain value, the amorphous alloy liquid in the center of the mold is sucked away because it has not been solidified, leaving an amorphous alloy tube. The induction suction casting method does not have the problem of thin-wall filling. Thus, thin-walled elongated tubes can be produced. However, when an alloy containing an active metal is prepared by the induction suction casting method, the induction crucible is likely to react with the amorphous alloy, and the structure of the preparation device of the induction suction casting method is relatively complicated.

Contents of the invention

The purpose of the present invention is to solve the problem that existing methods for preparing amorphous alloy pipes mainly include copper mold casting, core pulling and induction suction casting, and copper mold casting and core pulling prepare thin-walled amorphous alloy pipes (wall thickness is less than 1mm). ), the thin-walled part cannot be filled; when the induction suction casting method is used to prepare alloys containing active metals, the induction crucible is likely to react with the amorphous alloy. A thin-walled elongated tube forming device for amorphous alloy is provided. and methods.

The invention includes arc melting furnace, copper crucible, graphite tube, connecting pipe, support pad, quartz glass, temperature measuring device, infrared sensor, suction casting valve, mechanical pump, tungsten rod, metal mold, suction casting controller and melting current control One end of the connecting pipe is set on the side wall of the arc melting furnace, the other end of the connecting pipe is connected with the mechanical pump, the suction casting valve is installed on the connecting pipe, the quartz glass is installed in the center hole at the bottom of the arc melting furnace, and the temperature measuring device is located in the arc melting furnace. Below the central hole at the bottom of the melting furnace, the infrared sensor is located below the temperature measuring device. There is a pit on the upper surface of the copper crucible. The center of the copper crucible is provided with a stepped graphite tube hole communicating with the pit. The graphite tube is installed in the In the stepped graphite tube hole, the tungsten end of the tungsten rod is located in the pit. The metal mold is composed of two symmetrically arranged semi-cylinders. There is a mold cavity on the central axis of the metal mold. The inner diameter of the mold cavity is Φ2.5 ～Φ3.5mm, the length of the metal mold is 200～300mm, the metal mold is installed in the arc melting furnace through the support pad, the lower end surface of the copper crucible is connected with the metal mold and the upper end surface of the arc melting furnace, and the tube hole of the graphite tube is connected with the The mold cavity is facing, the infrared sensor and the suction casting valve are respectively connected to the suction casting controller through wires, and the suction casting controller is connected to the melting current controller through wires.

The method of the present invention is realized through the following steps: Step 1: first put the alloy ingot into the bottom of the pit in the copper crucible; Step 2: the degree of vacuum in the arc melting furnace is 5.0×10 ^-3 ~ 6.0×10 ^-3 Pa ; Step 3: The melting current controller controls the melting current to be 250-400A, and the melting time is 2-3S; Step 4: When the temperature at the bottom of the alloy ingot reaches above the liquidus temperature, the alloy ingot melts into an alloy liquid. The casting controller opens the suction casting valve, the mechanical pump pumps out the gas in the inner cavity of the arc melting furnace, and a negative pressure is formed between the upper and lower inner cavity of the arc melting furnace, and the alloy liquid is sucked into the mold of the metal mold under the action of negative pressure. In the cavity, when the alloy liquid enters the mold cavity, the alloy liquid in contact with the side wall of the cavity cools rapidly and solidifies on the side wall of the cavity to form a thin-walled metal solidified shell. The thickness of the metal solidified shell is less than 1mm and is located in the center of the cavity. The unsolidified alloy liquid is sucked out of the mold under the action of pressure difference, and the solidified thin-walled alloy shell on the side wall of the mold cavity is an amorphous alloy thin-walled slender tube.

The advantages of the present invention are: 1. The method of the present invention utilizes a metal mold, and by controlling the melting current and opening of the suction casting valve, an amorphous alloy thin-walled elongated tube can be obtained. wall pipe. Since the invention adopts the arc melting method to melt the alloy ingot, the crucible will not react with the amorphous alloy ingot. 2. The structure of the device of the present invention is simple, and the method and device of the present invention are used to prepare Ti-based, Zr-based and other amorphous alloy tubes containing active metals.

Description of drawings

Fig. 1 is a main cross-sectional view of the structure of Embodiment 1; Fig. 2 is a state diagram when the unsolidified alloy liquid located in the center of cavity 4-1 is sucked out of the mold under the action of pressure difference in step 4 of Embodiment 4; Fig. 3 is a state diagram of the thin-walled alloy solidified shell formed by solidification on the side wall of the mold cavity 4-1 in step 4 of the specific embodiment 4; Fig. 4 is a schematic structural view of the multilayer composite amorphous alloy tube prepared by the present invention; Fig. 5 is a sample appearance diagram of the amorphous alloy thin tube obtained when the composition of alloy ingot 17 is Zr ₄₁ Ti ₁₄ Ni ₁₀ Cu ₁₂ Be ₂₃ ; Fig. 6 is the composition of alloy ingot 17 is Ti ₄₀ Zr ₂₅ Ni ₃ Cu ₁₂ When Be ₂₀ , the appearance diagram of the sample of the obtained amorphous alloy thin tube; Fig. 7 is the sample of the obtained amorphous alloy thin tube when the composition of alloy ingot 17 is Fe ₄₁ Co ₇ Cr ₁₅ Mo ₁₄ C ₁₅ B ₆ Y ₂ Appearance view; Figure 8 is a scanning electron microscope image of the cross-section of the amorphous alloy tube made when the composition of alloy ingot 17 is Zr ₄₁ Ti ₁₄ Ni ₁₀ Cu ₁₂ Be ₂₃ ; Figure 9 is the composition of alloy ingot 17 is Zr ₄₁ Ti ₁₄ When Ni ₁₀ Cu ₁₂ Be ₂₃ , Ti ₄₀ Zr ₂₅ Ni ₃ Cu ₁₂ Be ₂₀ or Fe ₄₁ Co ₇ Cr ₁₅ Mo ₁₄ C ₁₅ B ₆ Y ₂ , the X-ray diffraction pattern of the thin tube sample of amorphous alloy obtained.

Detailed ways

Specific Embodiment 1: This embodiment is described in conjunction with FIGS. 1 to 3. This embodiment includes an arc melting furnace 1, a copper crucible 2, a graphite tube 3, a connecting pipe 5, a support pad 6, quartz glass 7, a temperature measuring device 8, an infrared Sensor 9, suction casting valve 10, mechanical pump 11, tungsten rod 15, metal mold 4, suction casting controller 12 and melting current controller 13, one end of connecting pipe 5 is arranged on the side wall of arc melting furnace 1, connecting pipe 5 The other end of the pump is connected to the mechanical pump 11, the suction casting valve 10 is installed on the connecting pipe 5, the quartz glass 7 is installed in the bottom center hole of the arc melting furnace 1, and the temperature measuring device 8 is located below the bottom center hole of the arc melting furnace 1, The infrared sensor 9 is located below the temperature measuring device 8, the upper end surface of the copper crucible 2 is provided with a pit 2-1, and the center of the copper crucible 2 is provided with a stepped graphite tube hole 2-2 communicating with the pit 2-1, The graphite tube 3 is installed in the stepped graphite tube hole 2-2, the tungsten pole of the tungsten rod 15 is located in the pit 2-1, the metal mold 4 is composed of two symmetrically arranged half cylinders, and the central axis of the metal mold 4 There is a mold cavity 4-1, the inner diameter of the mold cavity 4-1 is Φ2.5～Φ3.5mm, the length of the metal mold 4 is 200～300mm, the metal mold 4 is installed in the arc melting furnace 1 through the support pad 6, The lower end surface of the copper crucible 2 is connected to the metal mold 4 and the upper end surface of the arc melting furnace 1, and the tube hole of the graphite tube 3 is directly opposite to the mold cavity 4-1, and the infrared sensor 9 and the suction casting valve 10 are connected to the suction casting valve through wires respectively. The controller 12 is connected, and the suction casting controller 12 is connected with the melting current controller 13 through wires. The tungsten rod 15 is connected to the power supply 14 through wires, the copper crucible 2 is connected to the power supply 14 through wires, and the suction casting controller 12 and the melting current controller 13 are respectively connected to the power supply 14 through wires. The melting current controller 13 is used to adjust the melting current of the electric arc furnace. The temperature measuring device 8 and the infrared sensor 9 are used to detect the temperature of the alloy ingot 17 at the bottom of the pit 2 - 1 on the copper crucible 2 . By changing the inner diameter of the mold cavity 4-1, the opening time of the suction casting valve and the melting current, amorphous alloy thin-walled tubes with different outer diameters and wall thicknesses can be obtained.

Specific Embodiment 2: This embodiment is described with reference to FIGS. 1 to 3 . In this embodiment, the inner diameter of the mold cavity 4 - 1 of the metal mold 4 is Φ3 mm, and the length of the metal mold 4 is 250 mm. The present invention is suitable for preparing thin-walled amorphous alloy tubes. When the inner diameter of the mold cavity 4-1 and the length of the metal mold 4 are the above values, the thin-walled and elongated amorphous alloy tube has the best effect. Other components and connections are the same as those in the first embodiment.

Specific embodiment three: This embodiment is described in conjunction with Fig. 1. The difference between this embodiment and specific embodiment one is that: the device is also added with a sealing gasket 16, and the upper end surface of the metal mold 4 is provided with an annular groove 4-2, sealing Pad 16 fits in annular groove 4-2. This design increases the sealing performance between the lower end surface of the copper crucible 2 and the upper end surface of the metal mold 4 . Other components and connections are the same as those in the first embodiment.

Specific embodiment four: illustrate this embodiment in conjunction with Fig. 1, this embodiment is realized by the following steps: Step 1: first alloy ingot 17 is put into the pit 2-1 bottom in the copper crucible 2, utilizes electric arc to alloy ingot 17 Melting; Step 2: The vacuum degree in the arc melting furnace 1 is 5.0×10 ^-3 ~ 6.0×10 ^-3 Pa; Step 3: The melting current controller 13 controls the melting current to 250-400A, and the melting time is 2-3S; Step 4: When the temperature at the bottom of the alloy ingot 17 reaches above the liquidus temperature, the alloy ingot 17 is melted into alloy liquid. At this time, the suction casting controller 12 opens the suction casting valve 10, and the mechanical pump 11 turns the inner cavity of the arc melting furnace 1 The gas in the arc melting furnace 1 is drawn out, and a negative pressure is formed between the upper and lower inner chambers of the arc melting furnace 1. The alloy liquid is sucked into the mold cavity 4-1 of the metal mold 4 under the action of negative pressure. When the alloy liquid enters the mold cavity 4-1 Finally, the alloy liquid in contact with the side wall of the mold cavity 4-1 cools rapidly and solidifies on the side wall of the mold cavity 4-1 to form a very thin metal solidified shell. 1 The unsolidified alloy liquid in the center is sucked out of the mold under the action of pressure difference, as shown in Figure 2, the solidified thin-walled alloy shell on the side wall of the mold cavity 4-1 is the amorphous alloy thin-walled elongated tube 18, As shown in Figure 3. It takes a certain amount of time for the unsolidified alloy liquid located in the center of the mold cavity 4-1 to solidify. Due to the large pressure difference between the upper and lower cavities and the good fluidity of the alloy liquid, the flow rate of the alloy liquid in the mold is very high. Therefore, the alloy liquid in the center of the mold The liquid is easily sucked out of the mold before it solidifies, as shown in Figure 2. The composition of alloy ingot 17 is Zr ₄₁ Ti ₁₄ Ni ₁₀ Cu ₁₂ Be ₂₃ (at.%), Ti ₄₀ Zr ₂₅ Ni ₃ Cu ₁₂ Be ₂₀ (at.%) or Fe ₄₁ Co ₇ Cr ₁₅ Mo ₁₄ C ₁₅ B ₆ Y ₂ (at.%). By changing the inner diameter of the mold cavity 4-1 of the metal mold 4, controlling the process parameters such as the melting current and the opening time of the suction casting valve 10, amorphous thin-walled elongated tubes with different outer diameters and wall thicknesses below 1 mm can be obtained.

Embodiment 5: This embodiment is described with reference to FIGS. 1 to 3 . The material of the metal mold 4 in Step 4 of this embodiment is pure copper. Pure copper has excellent electrical and thermal conductivity, ductility and corrosion resistance. Other steps are the same as in Embodiment 4.

Embodiment 6: This embodiment is described in conjunction with FIG. 4. The difference between this embodiment and Embodiment 4 is that the present invention also includes Step 5: repacking the amorphous alloy thin-walled elongated tube 18 prepared in Step 4. In the mold cavity 4-1 of the metal mold 4, repeat steps 2, 3, and 4 to obtain a two-layer composite amorphous alloy thin-walled elongated tube 19 .

Embodiment 7: This embodiment is described in conjunction with FIG. 4. The difference between this embodiment and Embodiment 6 is that the present invention also includes Step 6: the two-layer composite amorphous alloy thin-walled elongated tube 19 prepared in Step 5 Put it into the mold cavity 4-1 of the metal mold 4 again, and repeat steps 2, 3, and 4 to obtain a three-layer composite amorphous alloy thin-walled elongated tube 20 . In the present invention, by changing the inner diameter of the mold cavity 4-1 of the metal mold 4 and controlling the process parameters such as the melting current and the opening time of the suction casting valve 10, a multilayer composite amorphous alloy tube can be obtained.

Application example of the present invention:

(1), the composition of the alloy ingot 17 is selected as Zr ₄₁ Ti ₁₄ Ni ₁₀ Cu ₁₂ Be ₂₃ (at.%), the mass of the alloy ingot 17 is 10 grams, the melting current is 300A, the melting time is 2.5S, and the vacuum degree of the electric arc furnace is 5.5×10 ^-3 Pa, the sample appearance of the obtained amorphous alloy thin tube is shown in Fig. 5 . Fig. 7 is a scanning electron microscope picture of a Zr ₄₁ Ti ₁₄ Ni ₁₀ Cu ₁₂ Be ₂₃ amorphous alloy tube sample section, the tube outer diameter is 3 mm, and the tube wall is 0.5 mm. It can be clearly seen from Fig. 8 that through the device and method of the present invention The prepared thin-walled non-transistor has a uniform tube diameter, a rounded inner diameter, and a smooth inner wall of the tube.

(2), the composition of the alloy ingot 17 is selected as Ti ₄₀ Zr ₂₅ Ni ₃ Cu ₁₂ Be ₂₀ (at.%), the mass of the alloy ingot 17 is 10 grams, the melting current is 270A, the melting time is 2.5S, and the vacuum degree of the electric arc furnace is 6.0×10 ^-3 Pa, the sample appearance of the obtained amorphous alloy thin tube is shown in Fig. 6 .

(3) The composition of the alloy ingot 17 is selected as Fe ₄₁ Co ₇ Cr ₁₅ Mo ₁₄ C ₁₅ B ₆ Y ₂ (at.%), the mass of the alloy ingot 17 is 10 grams, the melting current is 350A, the melting time is 2.5S, and the arc The vacuum degree of the furnace was 5.0×10 ^-3 Pa, and the appearance of the sample of the obtained amorphous alloy thin tube is shown in FIG. 7 .

From the above three examples, it can be clearly seen that the dimensional accuracy and surface quality of the prepared amorphous alloy tubes are guaranteed by using the device and method of the present invention. From the X-ray diffraction pattern in Figure 9, it can be clearly seen that Zr ₄₁ Ti ₁₄ Ni ₁₀ Cu ₁₂ Be ₂₃ (a in Figure 9), Ti ₄₀ Zr ₂₅ Ni ₃ Cu ₁₂ Be ₂₀ (b in Figure 9) or Fe ₄₁ Co ₇ Cr ₁₅ Mo ₁₄ C ₁₅ B ₆ Y ₂ (c in Figure 9) alloy tube samples are all amorphous.

Claims (7)

1. amorphous alloy thin-wall slim pipe building mortion, described device comprises arc-melting furnace (1), copper crucible (2), graphite-pipe (3), take over (5), supporting pad (6), quartz glass (7), temperature measuring equipment (8), infrared sensor (9), inhale casting valve (10), mechanical pump (11) and tungsten electrode rod (15), an end of taking over (5) is arranged on the sidewall of arc-melting furnace (1), the other end of taking over (5) is connected with mechanical pump (11), inhaling casting valve (10) is contained in the adapter (5), quartz glass (7) is contained in the bottom centre hole of arc-melting furnace (1), temperature measuring equipment (8) is positioned at the below in the bottom centre hole of arc-melting furnace (1), infrared sensor (9) is positioned at the below of temperature measuring equipment (8), the upper surface of copper crucible (2) is provided with pit (2-1), the center of copper crucible (2) is provided with the stairstepping graphite pore (2-2) that communicates with pit (2-1), graphite-pipe (3) is contained in the stairstepping graphite pore (2-2), the tungsten electrode end of tungsten electrode rod (15) is arranged in pit (2-1), it is characterized in that: described device also comprises metal die (4), inhale casting controller (12) and fusion current controller (13), metal die (4) is made of two symmetrically arranged semicylinders, the central axis place of metal die (4) is provided with die cavity (4-1), the internal diameter of die cavity (4-1) is Φ 2.5～Φ 3.5mm, the length of metal die (4) is 200～300mm, metal die (4) is contained in the arc-melting furnace (1) by supporting pad (6), the lower surface of copper crucible (2) is connected with the upper surface of metal die (4) with arc-melting furnace (1), and the pore of graphite-pipe (3) and die cavity (4-1) over against, infrared sensor (9) is connected by lead and suction casting controller (12) respectively with suction casting valve (10), and suction is cast controller (12) and is connected with fusion current controller (13) by lead.

2. according to the described a kind of amorphous alloy thin-wall slim pipe building mortion of claim 1, it is characterized in that: die cavity (4-1) internal diameter of described metal die (4) is Φ 3mm, and the length of metal die (4) is 250mm.

3. according to claim 1 or 2 described a kind of amorphous alloy thin-wall slim pipe building mortions, it is characterized in that: described device also comprises sealing gasket (16), and the upper surface of metal die (4) is provided with cannelure (4-2), and sealing gasket (16) is contained in the cannelure (4-2).

4. one kind is utilized the described device of claim 1 to realize a kind of amorphous alloy thin-wall slim pipe manufacturing process, and it is characterized in that: described method realizes by following steps: step 1: pit (2-1) bottom of at first alloy pig (17) being put into copper crucible (2); Step 2: the vacuum in the arc-melting furnace (1) is 5.0 * 10 ^-3～6.0 * 10 ^-3Pa; Step 3: fusion current controller (13) control fusion current is 250～400A, and fusing time is 2～3S; Step 4: when the temperature of alloy pig (17) bottom reaches liquidus temperature when above, alloy pig (17) is fused into alloy liquid, at this moment, suction casting controller (12) will be inhaled casting valve (10) and open, mechanical pump (11) is extracted the gas in arc-melting furnace (1) inner chamber out, on the inner chamber of arc-melting furnace (1), form negative pressure down, alloy liquid is inhaled under suction function in the die cavity (4-1) of metal die (4), after alloy liquid enters die cavity (4-1), the alloy liquid that contacts with die cavity (4-1) sidewall cools off rapidly and is set in the very thin metal scull of formation on die cavity (4-1) sidewall, the thickness of metal scull (t) is below the 1mm, be positioned at the not solidified alloy liquid in die cavity (4-1) center and be sucked out mould under the effect of pressure reduction, the thin wall alloy scull that solidifies on die cavity (4-1) sidewall is amorphous alloy thin-wall slim pipe (18).

5. according to the described a kind of amorphous alloy thin-wall slim pipe manufacturing process of claim 4, it is characterized in that: the material of metal die in the described step 4 (4) is a fine copper.

6. according to the described a kind of amorphous alloy thin-wall slim pipe manufacturing process of claim 4, it is characterized in that: described method also comprises step 5: the amorphous alloy thin-wall slim pipe (18) that step 4 preparation is finished is packed in the die cavity (4-1) of metal die (4) once more, repeating step two, three, four promptly obtains two layers of composite amorphous alloy thin-wall slim pipe (19).

7. according to the described a kind of amorphous alloy thin-wall slim pipe manufacturing process of claim 6, it is characterized in that: described method also comprises step 6: two layers of composite amorphous alloy thin-wall slim pipe (19) that step 5 preparation is finished are packed in the die cavity (4-1) of metal die (4) once more, repeating step two, three, four promptly obtains three layers of composite amorphous alloy thin-wall slim pipe (20).

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