A platinum alloy wire and its preparation method and application

Abstract

The present invention relates to a platinum alloy wire and a preparation method and application thereof, and relates to a new material. The preparation method comprises the following steps: ball milling and sintering metal powder to obtain an alloy ingot, and hot extruding to obtain the platinum alloy wire. The preparation method can solve defects such as inclusions in ingots and uneven composition, and can also improve material utilization.

Description

Technical Field

[0001] The invention relates to new materials, in particular to a platinum alloy wire and a preparation method and application thereof. Background Art

[0002] At present, the preparation process of platinum alloy wire can be mainly divided into smelting, rolling and drawing. First, the materials are mixed according to the nominal composition and then smelted and cast using induction smelting to obtain an ingot, which is then forged and rolled before being drawn to obtain the alloy wire.

[0003] In order to ensure uniform melting, the molten alloy liquid needs to be kept warm for a long time. Losses will occur during this process, causing the actual composition to deviate from the nominal composition. The alloy ingot obtained by casting will inevitably produce defects such as shrinkage cavities, shrinkage and uneven composition. In addition, the shrinkage cavities need to be cut off during the rolling process, and the material utilization rate is not high; during the drawing process, some defects such as shrinkage will gradually be exposed, affecting the surface quality of the alloy wire. Defects coated inside the alloy wire will cause the alloy wire to break during the drawing process; uneven composition will lead to uneven performance of the alloy wire and low yield rate. Summary of the invention

[0004] In view of the above problems, the present invention provides a method for preparing platinum alloy wire, which can solve the defects of ingot inclusions, uneven composition and the like, and can also improve material utilization.

[0005] In order to achieve the above object, the present invention provides a method for preparing platinum alloy wire, comprising the following steps: ball milling and sintering metal powder to obtain alloy ingots, and hot extruding to obtain platinum alloy wire.

[0006] In order to overcome the defects introduced by the casting process and the uneven composition in the existing preparation process of platinum alloy wire, which further lead to the problem of unstable surface quality and performance of the alloy wire, the inventors proposed to adopt powder metallurgy to micro-alloy the metal powder through ball milling, so as to solve the defects of inclusion and uneven composition of the alloy wire blank, and then sinter to form an alloy ingot, and then obtain an alloy wire material of a specific shape instead of a metal block or metal ingot by hot extrusion and extrusion molding. The above preparation method can not only solve the defects of inclusion and uneven composition of the ingot, but also improve the material utilization rate. The prepared platinum alloy wire has uniform composition and low inclusions.

[0007] In one embodiment, the metal powder includes platinum.

[0008] In one embodiment, the ball milling is high energy ball milling.

[0009] In one embodiment, the ball milling medium comprises n-heptane.

[0010] In one embodiment, the ball-to-material ratio of the high-energy ball mill is 4:1-10:1, and the rotation speed is 200-500 r / min.

[0011] In one embodiment, the high-energy ball milling includes a cycle of ball milling procedures, and the ball milling procedure includes ball milling for 40 to 50 minutes and resting for 10 to 20 minutes; the ball milling time in the high-energy ball milling is a total of 15 to 30 hours.

[0012] In one embodiment, the sintering method includes hot isostatic pressing.

[0013] A dense alloy can be formed by the hot isostatic pressing described above.

[0014] In one embodiment, the hot isostatic pressing conditions include: temperature of 1000-1200° C., pressure of 100-200 MPa, and heat preservation for 3-4 hours.

[0015] In one embodiment, the hot extrusion conditions include: a temperature of 950-1100° C., a heat preservation and pressure holding time of ≥3 hours, and an extrusion ratio of (8-12):1.

[0016] The invention also provides a platinum alloy wire obtained by the preparation method.

[0017] The present invention also provides application of the platinum alloy wire in preparing medical devices.

[0018] The present invention also provides a medical device prepared by using the platinum alloy wire.

[0019] The platinum alloy wire prepared by the present invention has the characteristics of uniform composition and uniform performance, and is suitable for preparing medical devices with high requirements for precision and performance, including but not limited to electrodes, sensors, wires and other devices in medical devices.

[0020] The invention also discloses an electrode, a sensor and / or a wire of a medical device, which are prepared by adopting the platinum alloy wire.

[0021] Compared with the prior art, the present invention has the following beneficial effects:

[0022] The present invention discloses a platinum alloy wire and a preparation method and application thereof. The preparation method can solve defects such as ingot inclusions and uneven composition, and can also improve material utilization. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 This is a surface morphology of the wire sample 1 (PtW alloy wire prepared by the method of this case) in the embodiment;

[0024] Figure 2This is a surface morphology of wire sample 2 (PtW alloy wire prepared by smelting process) in the embodiment;

[0025] Figure 3 This is a surface morphology of wire sample 3 (PtIr alloy wire prepared by the method of this case) in the embodiment;

[0026] Figure 4 This is a surface morphology of wire sample 4 (PtIr alloy wire prepared by smelting process) in the embodiment. DETAILED DESCRIPTION

[0027] In order to facilitate the understanding of the present invention, the present invention will be described more fully below with reference to the relevant drawings. The preferred embodiments of the present invention are given in the drawings. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the understanding of the disclosure of the present invention more thorough and comprehensive.

[0028] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used in the specification of the present invention herein are only for the purpose of describing specific embodiments and are not intended to limit the present invention.

[0029] source:

[0030] Unless otherwise specified, the reagents, materials, and equipment used in this example are all commercially available; the experimental methods are all conventional experimental methods in the art unless otherwise specified.

[0031] Example

[0032] 1. A method for preparing platinum alloy wire.

[0033] In a glove box filled with high-purity argon, high-purity (≥99.99%) metal powder with a diameter of 20 to 30 μm is weighed according to the designed mass ratio and placed in a ball mill. To prevent the metal powder from welding during the ball milling process, 1 to 3% wt. n-heptane is added. The high-energy ball milling process is: ball-to-material ratio 4:1 to 10:1, speed 200 to 500 r / min, to avoid excessive energy in the ball milling tank, the high-energy ball mill program is set as: run for 45 minutes, stop for 15 minutes, and circulate ball milling for 15 to 30 hours, and mechanical alloying powder material is obtained after taking it out.

[0034] The alloy powder material after ball milling was placed in a bag with a diameter of 10 cm and evacuated to 3×10 -4 After Pa, seal the package. Put the sealed package into the hot isostatic pressing equipment and sinter it by hot isostatic pressing. The hot isostatic pressing process is: 1000-1200℃, 100-200MPa, and keep warm for 3-4 hours. Take out the alloy ingot after cooling.

[0035] The alloy ingot and the extrusion die are placed in a box furnace and heated to 950-1100°C, and kept at this temperature and pressure for more than 3 hours. The heated alloy ingot and the extrusion die are then placed in an extruder with an extrusion ratio of 10:1 to obtain an alloy wire with a diameter of 1 cm.

[0036] 2. Preparation of PtW alloy wire.

[0037] 1. Prepare PtW alloy wire using the method in step 1 of this embodiment.

[0038] A high-quality platinum-based alloy wire, in terms of mass percentage, includes 92% Pt and 8% W in the alloy, the raw materials are high-purity Pt powder and W powder, and the particle size is 20-30 μm. The preparation method thereof includes the following steps:

[0039] In a glove box filled with high-purity argon, high-purity (≥99.99%) platinum powder and tungsten powder were weighed according to the mass ratio and put into the ball mill. To prevent the metal powder from welding during the ball milling process, 3wt% n-heptane was added. The high-energy ball milling process is: ball-to-material ratio 10:1, speed 500r / min, to avoid excessive energy in the ball mill, the high-energy ball mill program is set as: 45 minutes of operation, 15 minutes of downtime, 30 hours of cyclic ball milling (downtime is not included), and platinum-tungsten alloy powder is obtained.

[0040] The platinum-tungsten alloy powder obtained above was placed in a bag with a diameter of 10 cm and evacuated to 3×10 -4 The sealed package is placed in a hot isostatic pressing device, and the hot isostatic pressing process is: 1100℃, 160MPa, keep warm for 4 hours, and take out the alloy ingot after cooling.

[0041] The alloy ingot and the extrusion die are placed in a box furnace and heated to 1000°C, and kept at this temperature and pressure for more than 3 hours. The heated alloy ingot and the extrusion die are then placed in an extruder with an extrusion ratio of 10:1 to obtain an alloy wire with a diameter of 1 cm.

[0042] The platinum-tungsten alloy wire with a diameter of 1 cm was drawn to 0.3 mm using a multi-mode wire drawing machine.

[0043] The prepared platinum-tungsten alloy block (ingot sample 1) and wire (wire sample 1) were subjected to composition detection and surface quality detection:

[0044] Table 1 shows the composition test data of ingot sample 1. The results show that the actual composition of the main elements in the upper, middle and lower parts of the ingot is very close to the nominal composition.

[0045] Figure 1 This is the surface morphology of wire sample 1. The results show that the surface of wire sample 1 is smooth without obvious defects.

[0046] Table 1 Composition test of ingot sample 1

[0047] element Top content Middle content Bottom content Pt 91.96％ 91.98 91.97 W 7.99 7.97 8.01

[0048] 2. Prepare PtW alloy wire by smelting process.

[0049] In comparison, platinum-tungsten alloy with a nominal composition of 92% Pt and 8% W was induction melted, cast, and rolled to obtain a 5×5 mm alloy wire, which was then drawn using a multi-mode wire drawing machine to obtain an alloy wire with a diameter of 0.3 mm.

[0050] The prepared platinum-tungsten alloy block (ingot sample 2) and wire (wire sample 2) were subjected to composition detection and surface quality detection:

[0051] Table 2 shows the composition test of ingot sample 2. The results show that the actual composition of the main elements in the upper, middle and lower parts of the ingot is relatively large compared with the nominal composition, and the differences between the parts are also relatively large.

[0052] Figure 2 This is the surface morphology of wire sample 2. The results show that the surface of wire sample 2 prepared by the traditional process has obvious defects and small pits.

[0053] Table 2 Composition detection of ingot sample 2

[0054] element Top content Middle content Bottom content Pt 91.98％ 91.81 91.98 W 7.92 8.11 7.94

[0055] 3. Preparation of PtIr alloy wire.

[0056] 1. Prepare PtIr alloy wire using the method in step 1 of this embodiment.

[0057] A high-quality platinum-based alloy wire, in which the alloy includes 90% Pt and 10% Ir by mass percentage, and the raw materials are high-purity Pt powder and Ir powder, and the particle size is 20-30 μm. The preparation method thereof comprises the following steps:

[0058] In a glove box filled with high-purity argon, high-purity (≥99.99%) platinum powder and iridium powder were weighed according to the mass ratio and put into the ball mill. To prevent the metal powder from welding during the ball milling process, 1wt% n-heptane was added. The high-energy ball milling process is: ball-to-material ratio 4:1, speed 200r / min, to avoid excessive energy in the ball mill, the high-energy ball mill program is set as: run for 45 minutes, stop for 15 minutes, 15 hours of cycle ball milling, and take out the platinum-iridium alloy powder.

[0059] The platinum-iridium alloy powder obtained above was placed in a bag with a diameter of 10 cm and evacuated to 3×10 -4After the package is sealed, the sealed package is placed in the hot isostatic pressing equipment. The hot isostatic pressing process is: 1050℃, 140MPa, and keep warm for 3 to 4 hours. After cooling, take out the alloy ingot.

[0060] The alloy ingot and the extrusion die are placed in a box furnace and heated to 1000°C for more than 3 hours. The heated alloy ingot and the extrusion die are then placed in an extruder with an extrusion ratio of 10:1 to obtain an alloy wire with a diameter of 1 cm.

[0061] The platinum-iridium alloy wire with a diameter of 1 cm was drawn to 0.3 mm using a multi-mode wire drawing machine.

[0062] The prepared platinum-iridium alloy block (ingot sample 3) and wire (wire sample 3) were subjected to composition detection and surface quality detection:

[0063] Table 3 shows the composition test of ingot sample 3. The results show that the actual composition of the main elements in the upper, middle and lower parts of the ingot is very close to the nominal composition.

[0064] Figure 3 This is the surface morphology of wire sample 3. The results show that the surface of wire sample 3 is smooth without obvious defects.

[0065] Table 3 Composition detection of ingot sample 3

[0066] element Top content Middle content Bottom content Pt 90.02％ 90.00 90.07 Ir 9.89 9.92 9.85

[0067] 2. Prepare PtIr alloy wire by smelting process.

[0068] For comparison, a platinum-iridium alloy with a nominal composition of 90% Pt and 10% Ir was induction melted, cast, and rolled to obtain a 5×5 mm alloy wire, which was then drawn using a multi-mode wire drawing machine to obtain an alloy wire with a diameter of 0.3 mm.

[0069] The prepared platinum-iridium alloy block (ingot sample 4) and wire (wire sample 4) were subjected to composition detection and surface quality detection:

[0070] Table 4 is the composition test of ingot sample 4. The results show that the actual composition of the main elements in the upper, middle and lower parts of the ingot is relatively large compared with the nominal composition, and the differences between the parts are also large.

[0071] Figure 4 This is the surface morphology of wire sample 4. The results show that the surface of wire sample 4 prepared by the traditional process has obvious defects, and pits of different sizes appear.

[0072] Table 4 Composition test of ingot sample 4

[0073] element Top content Middle content Bottom content Pt 90.22％ 89.76 90.12 Ir 9.65 10.14 9.79

[0074] The technical features of the above-described embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0075] The above-mentioned embodiments only express several implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. A method for preparing a platinum alloy wire, characterized in that: The following steps are involved: Metal powder is ball-milled and sintered to obtain alloy ingots, which are then hot-extruded to obtain platinum alloy wires.

2. The preparation method according to claim 1, characterized in that: The ball milling is high energy ball milling.

3. The preparation method according to claim 2, characterized in that: The ball-to-material ratio of the high-energy ball mill is 4:1-10:1, and the rotation speed is 200-500 r / min.

4. The preparation method according to claim 2, characterized in that: The high-energy ball milling includes a cycle of ball milling procedures, and the ball milling procedure includes ball milling for 40 to 50 minutes and resting for 10 to 20 minutes; the ball milling time in the high-energy ball milling is a total of 15 to 30 hours.

5. The preparation method according to claim 1, characterized in that: The sintering method includes hot isostatic pressing.

6. The preparation method according to claim 5, characterized in that: The conditions of the hot isostatic pressing include: a temperature of 1000-1200° C., a pressure of 100-200 MPa, and heat preservation for 3-4 hours.

7. The preparation method according to claim 1, characterized in that: The conditions for hot extrusion include: a temperature of 950-1100° C., a heat preservation and pressure holding time of ≥3 hours, and an extrusion ratio of (8-12):

1.

8. The platinum alloy wire obtained by the preparation method according to any one of claims 1 to 7.

9. Use of the platinum alloy wire according to claim 8 in the preparation of medical devices.

10. A medical device, characterized in that: It is prepared by using the platinum alloy wire described in claim 8.

Images