CN113088837A - Medical high-elasticity tinned alloy wire and preparation method thereof - Google Patents
Medical high-elasticity tinned alloy wire and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/02—Pretreatment of the fibres or filaments
- C22C47/04—Pretreatment of the fibres or filaments by coating, e.g. with a protective or activated covering
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/08—Making alloys containing metallic or non-metallic fibres or filaments by contacting the fibres or filaments with molten metal, e.g. by infiltrating the fibres or filaments placed in a mould
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
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Abstract
The invention discloses a medical high-elasticity tinned alloy wire and a preparation method thereof, belonging to the field of tinned alloy wires and comprising the following specific steps: firstly, melting a copper base material and alloy particles, adding reinforcing particles, performing electromagnetic stirring under the pressure of 1-3Mpa, then casting into a copper alloy rod, then performing wire drawing, annealing treatment, acid washing, drying and tin plating to obtain the tin-plated alloy wire. According to the invention, electromagnetic stirring is adopted during melting, so that crystals in the copper alloy can be obviously refined, and simultaneously, along with pressurization, crystal grains are converted into a rose-shaped structure, a nearly spherical structure is increased, and finally, the crystal grains are completely converted into granular crystals, so that the structure is more uniformly refined in the subsequent wire drawing process, and the strength of the copper alloy rod is increased.
Description
Technical Field
The invention relates to a tinned alloy wire, in particular to a medical high-elasticity tinned alloy wire and a preparation method thereof.
Background
The tin-plated alloy wire has excellent electrical conductivity, thermal conductivity, ductility and corrosion resistance, and is widely applied to medical electrical components. At present, in the hot working and welding processes of the copper alloy wire in the market, stress cracks are easy to generate, and the elasticity is poor, so that the use performance of the copper alloy wire in the medical field is influenced.
Disclosure of Invention
The invention aims to solve at least one technical problem in the prior art and provides a medical high-elasticity tinned alloy wire and a preparation method thereof.
The technical solution of the invention is as follows:
a method for preparing high-elasticity tinned alloy wire for medical treatment includes such steps as smelting copper mother material and alloy particles, adding reinforcing particles, electromagnetic stirring under 1-3MPa, casting to obtain copper alloy rod, drawing, annealing, acid washing, drying and tinning.
As a preferable embodiment of the present invention, the alloy particles include Pt, and the preparation method thereof is: at H2PtCl6Adding KI into the DMF solution, stirring, adding PVP and methylamine aqueous solution after the solution is clear and bright yellow, heating to 150-160 ℃, reacting for 10-13h, cooling to obtain a brownish black colloidal solution, separating, and drying to obtain the down-ball-shaped nano-scale Pt particles.
In a preferred embodiment of the present invention, the reinforcing particles are vermicular carbon fibers.
As a preferred embodiment of the present invention, the reinforcing particles are prepared by the following method: mixing long carbon fiber and short carbon fiber uniformly to obtain carbon fiber group, soaking the carbon fiber group in ethanol, then carrying out chemical silvering, and quickly soaking the silvered carbon fiber into thiol with molecular concentration of 0.5 × 10-3-2×10-3Self-assembling for 12-48h in mol/L ethanol solution under the closed condition of 10-40 ℃, rinsing for 10-20 times by using deionized water and absolute ethyl alcohol respectively after taking out, and drying to obtain the enhanced particles.
In a preferred embodiment of the present invention, the thiol is an alkyl thiol, an aryl thiol or an aromatic heterocyclic thiol.
In a preferred embodiment of the present invention, the aspect ratio of the long fibers is 7 to 15:1, and the aspect ratio of the short fibers is 3 to 5: 1.
In a preferred embodiment of the present invention, a vermicular agent is further added during the melting.
As a preferable embodiment of the present invention, the melting temperature is 900-1300 ℃.
In a preferred embodiment of the present invention, the mass ratio of the copper base material, the alloy particles, and the reinforcing particles is 30 to 80:1 to 20:0.1 to 10.
The invention also discloses a medical high-elasticity tinned alloy wire prepared by the preparation method.
The invention has at least one of the following beneficial effects:
(1) according to the preparation method of the medical high-elasticity tinned alloy wire, electromagnetic stirring is adopted during melting, crystals in a copper alloy can be obviously refined, crystal grains are converted into rose-shaped structures along with pressurization, the nearly spherical structures are increased, and the crystal grains are finally converted into granular crystals completely.
(2) According to the preparation method of the medical high-elasticity tinned alloy wire, the napped spherical alloy particles are added, and spherical particles are uniformly distributed in the particles, so that the looseness of a copper alloy structure can be inhibited, and the fracture phenomenon of subsequent copper alloy rod drawing can be reduced.
(5) According to the preparation method of the medical high-elasticity tinned alloy wire, the vermicular carbon fiber is obtained by vermicularizing the carbon fiber during melting, and the vermicularized structure on the slender main body can be pulled in the subsequent wire drawing process, so that the copper alloy structure is difficult to slip, and the strength is improved.
(6) According to the preparation method of the medical high-elasticity tinned alloy wire, the carbon fibers are treated, the fiber group structure consisting of the carbon fibers with different lengths is adopted, the carbon fibers can freely enter a copper alloy gap in the wire drawing process, the tissue slippage is generated, in addition, the fiber surface is modified, and the sulfydryl-containing alkyl mercaptan compound is chemically adsorbed on the surface of the silver-coated carbon fibers through forming an S-Ag bond and forming a self-assembled film, so that the binding force of the carbon fibers and a copper alloy base material is improved, the strength is improved, and the possibility of defects in the subsequent process is reduced.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
DMF: n, N-dimethylformamide.
PVP: polyvinylpyrrolidone.
Example 1
A preparation method of a high-elasticity tinned alloy wire for medical treatment comprises the steps of firstly melting a copper base material and alloy particles, adding reinforcing particles, wherein the mass ratio of the copper base material to the alloy particles to the reinforcing particles is 36:11:0.3, carrying out electromagnetic stirring under the pressure of 1.2Mpa, then casting into a copper alloy rod, then carrying out wire drawing, annealing treatment, acid washing, drying and tinning to obtain the tinned alloy wire.
The alloy particles comprise Pt, and the preparation method comprises the following steps: in 0.5mL of H-containing solution with a concentration of 0.04mol/L2PtCl6Adding 0.032gKI into the DMF solution, stirring, adding 0.2g of PVP and 0.1mL of 40-40 wt% methylamine aqueous solution after the solution is clear and bright yellow, heating to 160 ℃, reacting for 13h, cooling to obtain a brownish black colloidal solution, separating, and drying to obtain the down-ball nano-scale Pt particles.
The reinforcing particles are vermicular carbon fibers; the preparation method of the reinforced particle comprises the following steps: uniformly mixing long carbon fibers and short carbon fibers in a mass ratio of 1:3 to obtain a carbon fiber group, soaking the carbon fiber group in ethanol, then carrying out chemical silvering, and quickly soaking the silvered carbon fibers into a solution with the mercaptan molecule concentration of 0.5 multiplied by 10-3And (3) carrying out self-assembly for 12h in an ethanol solution of mol/L under a closed condition at 12 ℃, taking out, respectively rinsing for 10 times by using deionized water and absolute ethyl alcohol, and drying to obtain the enhanced particles.
The thiol is 6-mercaptohexanol.
The aspect ratio of the long fibers is 7:1, and the aspect ratio of the short fibers is 3: 1.
Example 2
A preparation method of a high-elasticity tinned alloy wire for medical treatment comprises the steps of firstly melting a copper base material and alloy particles, adding reinforcing particles, wherein the mass ratio of the copper base material to the alloy particles to the reinforcing particles is 56:7:2, carrying out electromagnetic stirring under the pressure of 2Mpa, then casting into a copper alloy rod, then carrying out wire drawing, annealing treatment, acid washing, drying and tinning to obtain the tinned alloy wire.
The alloy particles comprise Pt, and the preparation method comprises the following steps: in 0.5mL of H with a concentration of 0.04mol/L2PtCl6Adding 0.032gKI into the DMF solution, stirring, adding 0.2g of PVP and 0.1mL of 40-40 wt% methylamine aqueous solution after the solution is clear and bright yellow, heating to 150 ℃, reacting for 11h, cooling to obtain a brownish black colloidal solution, separating, and drying to obtain the down-ball nano-scale Pt particles.
The reinforcing particles are vermicular carbon fibers; the preparation method of the reinforced particle comprises the following steps: uniformly mixing long carbon fibers and short carbon fibers in a mass ratio of 1:3 to obtain a carbon fiber group, soaking the carbon fiber group in ethanol, then carrying out chemical silvering, and quickly soaking the silvered carbon fibers into a solution with the mercaptan molecule concentration of 0.9 multiplied by 10-3And (3) carrying out self-assembly for 14h in an ethanol solution of mol/L under a closed condition at the temperature of 20 ℃, taking out, respectively rinsing with deionized water and absolute ethyl alcohol for 16 times, and drying to obtain the enhanced particles.
The mercaptan is 2-mercaptobenzothiazole.
The aspect ratio of the long fibers is 8:1, and the aspect ratio of the short fibers is 4: 1.
Example 3
A preparation method of a high-elasticity tinned alloy wire for medical treatment comprises the steps of firstly melting a copper base material and alloy particles, adding reinforcing particles, wherein the mass ratio of the copper base material to the alloy particles to the reinforcing particles is 78:14:0.9, carrying out electromagnetic stirring under the pressure of 3Mpa, then casting into a copper alloy rod, then carrying out wire drawing, annealing treatment, acid washing, drying and tinning to obtain the tinned alloy wire.
The alloy particles comprise Pt, and the preparation method comprises the following steps: in 0.5mL of H with a concentration of 0.04mol/L2PtCl6Adding 0.032gKI into DMF solution, stirring, adding 0.2g PVP and 0.1mL40 wt% methylamine water solution after the solution is clear and bright yellow, heating to 150-Reacting for 10-13h, cooling to obtain brownish black colloidal solution, separating, and drying to obtain napped spherical nano-grade Pt particles.
The reinforcing particles are vermicular carbon fibers; the preparation method of the reinforced particle comprises the following steps: uniformly mixing long carbon fibers and short carbon fibers in a mass ratio of 1:3 to obtain a carbon fiber group, soaking the carbon fiber group in ethanol, then carrying out chemical silvering, and quickly soaking the silvered carbon fibers into thiol with the molecular concentration of 1.2 multiplied by 10-3And (3) carrying out self-assembly for 23h in a mol/L ethanol solution under a closed condition of 30 ℃, taking out, respectively rinsing for 17 times by using deionized water and absolute ethyl alcohol, and drying to obtain the enhanced particles.
The thiol is 6-mercaptohexanol.
The aspect ratio of the long fibers is 9:1, and the aspect ratio of the short fibers is 5: 1.
Example 4
A preparation method of a high-elasticity tinned alloy wire for medical treatment comprises the steps of firstly melting a copper base material and alloy particles, adding reinforcing particles, wherein the mass ratio of the copper base material to the alloy particles to the reinforcing particles is 80:18:7, carrying out electromagnetic stirring under the pressure of 3Mpa, then casting into a copper alloy rod, then carrying out wire drawing, annealing treatment, acid washing, drying and tinning to obtain the tinned alloy wire.
The alloy particles comprise Pt, and the preparation method comprises the following steps: in 0.5mL of H with a concentration of 0.04mol/L2PtCl6Adding 0.032gKI into the DMF solution, stirring, adding 0.2g of PVP and 0.1mL of 40-40 wt% methylamine aqueous solution after the solution is clear and bright yellow, heating to 150-160 ℃, reacting for 10-13h, cooling to obtain a brownish black colloidal solution, separating, and drying to obtain the down-spherical nano-Pt particles.
The reinforcing particles are vermicular carbon fibers; the preparation method of the reinforced particle comprises the following steps: uniformly mixing long carbon fibers and short carbon fibers in a mass ratio of 1:3 to obtain a carbon fiber group, soaking the carbon fiber group in ethanol, then carrying out chemical silvering, and quickly soaking the silvered carbon fibers into thiol with the molecular concentration of 2 multiplied by 10-3Self-assembling for 48h in mol/L ethanol solution under the closed condition of 40 ℃, taking out, and then respectively using deionized water and anhydrousRinsing with ethanol for 20 times, and drying to obtain reinforced particles.
The mercaptan is 2-mercaptobenzothiazole.
The aspect ratio of the long fibers is 15:1, and the aspect ratio of the short fibers is 4: 1.
Example 5
This example is a modification of example 4, and specifically, a vermicular agent is added during the melting process, and the chemical composition (wt/%) is 35RE, 10Mg, 45Si, 9Al, 11 Ca; the melting temperature was 950 ℃.
Comparative example 1 (electromagnetic stirring without pressure)
A preparation method of a high-elasticity tinned alloy wire for medical treatment comprises the steps of firstly melting a copper base material and alloy particles, adding reinforcing particles, wherein the mass ratio of the copper base material to the alloy particles to the reinforcing particles is 56:7:2, then casting into a copper alloy rod, then carrying out wire drawing, annealing treatment, acid washing, drying and tinning, and thus obtaining the tinned alloy wire.
The alloy particles comprise Pt, and the preparation method comprises the following steps: in 0.5mL of H with a concentration of 0.04mol/L2PtCl6Adding 0.032gKI into the DMF solution, stirring, adding 0.2g of PVP and 0.1mL of 40-40 wt% methylamine aqueous solution after the solution is clear and bright yellow, heating to 150 ℃, reacting for 11h, cooling to obtain a brownish black colloidal solution, separating, and drying to obtain the down-ball nano-scale Pt particles.
The reinforcing particles are vermicular carbon fibers; the preparation method of the reinforced particle comprises the following steps: uniformly mixing long carbon fibers and short carbon fibers in a mass ratio of 1:3 to obtain a carbon fiber group, soaking the carbon fiber group in ethanol, then carrying out chemical silvering, and quickly soaking the silvered carbon fibers into a solution with the mercaptan molecule concentration of 0.9 multiplied by 10-3And (3) carrying out self-assembly for 14h in an ethanol solution of mol/L under a closed condition at the temperature of 20 ℃, taking out, respectively rinsing with deionized water and absolute ethyl alcohol for 16 times, and drying to obtain the enhanced particles.
The mercaptan is 2-mercaptobenzothiazole.
The aspect ratio of the long fibers is 8:1, and the aspect ratio of the short fibers is 4: 1.
Comparative example 2 (non-additive spherical particle)
A preparation method of a high-elasticity tinned alloy wire for medical treatment comprises the steps of firstly melting a copper base material and alloy particles, adding reinforcing particles, wherein the mass ratio of the copper base material to the alloy particles to the reinforcing particles is 56:7:2, carrying out electromagnetic stirring under the pressure of 2Mpa, then casting into a copper alloy rod, then carrying out wire drawing, annealing treatment, acid washing, drying and tinning to obtain the tinned alloy wire.
The reinforcing particles are vermicular carbon fibers; the preparation method of the reinforced particle comprises the following steps: uniformly mixing long carbon fibers and short carbon fibers in a mass ratio of 1:3 to obtain a carbon fiber group, soaking the carbon fiber group in ethanol, then carrying out chemical silvering, and quickly soaking the silvered carbon fibers into a solution with the mercaptan molecule concentration of 0.9 multiplied by 10-3And (3) carrying out self-assembly for 14h in an ethanol solution of mol/L under a closed condition at the temperature of 20 ℃, taking out, respectively rinsing with deionized water and absolute ethyl alcohol for 16 times, and drying to obtain the enhanced particles.
The mercaptan is alkyl mercaptan, aryl mercaptan or aromatic heterocyclic mercaptan.
The aspect ratio of the long fibers is 8:1, and the aspect ratio of the short fibers is 4: 1.
Comparative example 3 (carbon fiber No treatment)
A preparation method of a high-elasticity tinned alloy wire for medical treatment comprises the steps of firstly melting a copper base material and alloy particles, adding reinforcing particles, wherein the mass ratio of the copper base material to the alloy particles to the reinforcing particles is 56:7:2, carrying out electromagnetic stirring under the pressure of 2Mpa, then casting into a copper alloy rod, then carrying out wire drawing, annealing treatment, acid washing, drying and tinning to obtain the tinned alloy wire.
The alloy particles comprise Pt, and the preparation method comprises the following steps: in 0.5mL of H with a concentration of 0.04mol/L2PtCl6Adding 0.032gKI into the DMF solution, stirring, adding 0.2g of PVP and 0.1mL of 40-40 wt% methylamine aqueous solution after the solution is clear and bright yellow, heating to 150 ℃, reacting for 11h, cooling to obtain a brownish black colloidal solution, separating, and drying to obtain the down-ball nano-scale Pt particles.
The reinforcing particles are carbon fibers; the aspect ratio of the long fibers is 8:1, and the aspect ratio of the short fibers is 4: 1.
The above examples and comparative examples were subjected to the following performance tests, and the test results are shown in Table 1.
The tensile strength is referred to GB/T228.1-2010, and the elastic modulus is referred to GB/T22315-2008.
TABLE 1 Performance test values of examples and comparative examples
| Test specimen | Tensile strength (Mpa) | Modulus of elasticity (Gpa) |
| Example 1 | 498 | 124 |
| Example 2 | 501 | 125 |
| Example 3 | 496 | 122 |
| Example 4 | 499 | 123 |
| Example 5 | 511 | 129 |
| Comparative example 1 | 451 | 102 |
| Comparative example 2 | 449 | 106 |
| Comparative example 3 | 441 | 97 |
From the above table, it can be seen that the main reason for the performance of the examples is as follows, as shown by the analysis of comparative example 1, the electromagnetic stirring is adopted during melting in the examples, so that the crystals in the copper alloy can be obviously refined, and simultaneously the grains are transformed into rosette structures, the nearly spherical structures are increased, and finally all transformed into granular crystals, as the external dimension of the metal is changed during the wire drawing process, the corresponding deformation is generated inside the metal along with the deformation of the metal, in the direction of the maximum main deformation, the grains are elongated, attenuated or flattened, and meanwhile, the second phase (reinforcing particles) among the grains are elongated or crushed into a point chain arrangement, so that the granular crystals are more uniformly refined through the subsequent wire drawing treatment, and the strength of the copper alloy rod is increased. Analysis of comparative example 2 shows that by adding alloy Pt particles in a ball-shaped texture, which are uniformly distributed in the grains, the porosity of the copper alloy structure can be suppressed, and the fracture phenomenon of subsequent copper alloy rod drawing can be reduced. It can be seen from the comparative analysis of example 3 that, in the example, the carbon fibers are treated, the fiber group structure composed of carbon fibers with different lengths is adopted, the carbon fibers can enter the copper alloy gaps more freely during the wire drawing process, the tissue slippage can be generated, in addition, the surface of the carbon fibers is modified, the mercapto alkyl thiol compound is chemically adsorbed on the surface of the silver-coated carbon fibers by forming an S-Ag bond, and a self-assembled film is formed, so that the binding force between the carbon fibers and the copper alloy substrate is improved, therefore, the strength is improved, in addition, the performance of example 5 is optimal, mainly, the vermicular carbon fibers can be obtained by vermicularizing the carbon fibers during melting, and the vermicular carbon fibers can be pulled more slender in the subsequent wire drawing process, and the vermicular structure on the slender main body can make the copper alloy structure difficult to generate the slippage phenomenon, that is, it is difficult to break in each direction, and therefore, the strength and the elastic property are improved.
The above additional technical features can be freely combined and used in superposition by those skilled in the art without conflict.
In the description of the embodiments of the present invention, it should be understood that "-" and "-" indicate the same range of two numerical values, and the range includes the endpoints. For example: "A-B" means a range of greater than or equal to A and less than or equal to B. "A to B" means a range of not less than A and not more than B.
In the description of the embodiments of the present invention, the term "and/or" herein is only one kind of association relationship describing an associated object, and means that there may be three kinds of relationships, for example, a and/or B, and may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter related objects are in an "or" relationship.
The above description is only a preferred embodiment of the present invention, and the technical solutions that achieve the objects of the present invention by basically the same means are all within the protection scope of the present invention.
Claims (10)
1. A preparation method of a medical high-elasticity tinned alloy wire is characterized by comprising the following steps:
firstly, melting a copper base material and alloy particles, adding reinforcing particles, performing electromagnetic stirring under the pressure of 1-3Mpa, then casting into a copper alloy rod, then performing wire drawing, annealing treatment, acid washing, drying and tin plating to obtain the tin-plated alloy wire.
2. The method for preparing the medical high-elasticity tinned alloy wire according to claim 1The method is characterized in that: the alloy particles comprise Pt, and the preparation method comprises the following steps: at H2PtCl6Adding KI into the DMF solution, stirring, adding PVP and methylamine aqueous solution after the solution is clear and bright yellow, heating to 150-160 ℃, reacting for 10-13h, cooling to obtain a brownish black colloidal solution, separating, and drying to obtain the down-ball-shaped nano-scale Pt particles.
3. The method for producing a medical high-elasticity tin-plated alloy wire according to claim 1, wherein the method comprises the steps of: the reinforcing particles are vermiform carbon fibers.
4. The method for producing a medical high-elasticity tin-plated alloy wire according to claim 3, wherein the method comprises the steps of: the preparation method of the reinforced particle comprises the following steps: mixing long carbon fiber and short carbon fiber uniformly to obtain carbon fiber group, soaking the carbon fiber group in ethanol, then carrying out chemical silvering, and quickly soaking the silvered carbon fiber into thiol with molecular concentration of 0.5 × 10-3-2×10-3Self-assembling for 12-48h in mol/L ethanol solution under the closed condition of 10-40 ℃, rinsing for 10-20 times by using deionized water and absolute ethyl alcohol respectively after taking out, and drying to obtain the enhanced particles.
5. The method for producing a medical high-elasticity tin-plated alloy wire according to claim 4, wherein the method comprises the steps of: the mercaptan is alkyl mercaptan, aryl mercaptan or aromatic heterocyclic mercaptan.
6. The method for producing a medical high-elasticity tin-plated alloy wire according to claim 4, wherein the method comprises the steps of: the length-diameter ratio of the long fiber is 7-15:1, and the length-diameter ratio of the short fiber is 3-5: 1.
7. The method for producing a medical high-elasticity tin-plated alloy wire according to claim 1, wherein the method comprises the steps of: a vermiculizer is also added during the melting.
8. The method for producing a medical high-elasticity tin-plated alloy wire according to claim 1, wherein the method comprises the steps of: the melting temperature is 900-1300 ℃.
9. The method for producing a medical high-elasticity tin-plated alloy wire according to claim 1, wherein the method comprises the steps of: the mass ratio of the copper base material to the alloy particles to the reinforcing particles is 30-80:1-20: 0.1-10.
10. A medical high-elasticity tinned alloy wire is characterized in that: prepared by the preparation method as described in any one of claims 1 to 9.
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