CN111910112B - Tungsten-copper alloy material and preparation method and application thereof - Google Patents
Tungsten-copper alloy material and preparation method and application thereof Download PDFInfo
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- CN111910112B CN111910112B CN202010626454.5A CN202010626454A CN111910112B CN 111910112 B CN111910112 B CN 111910112B CN 202010626454 A CN202010626454 A CN 202010626454A CN 111910112 B CN111910112 B CN 111910112B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
Abstract
The invention discloses a tungsten-copper alloy material for an optical communication module for transmitting 400G signals in the field of 5G, which comprises the following components in parts by weight: 78.6-81.2 parts of tungsten; 18.6-21.10 parts of copper; 0.02-0.25 part of silver; 0.15-0.23 part of silicon. The invention also provides a preparation method of the tungsten-copper alloy material, which comprises the following steps: mixing tungsten, copper, silver, silicon and a wax-based binder, banburying to prepare particles, performing near net shape injection molding, performing extraction method for debonding, and sintering to obtain the tungsten-copper alloy material. The invention also provides an application of the tungsten-copper alloy material. According to the invention, the tungsten-copper alloy and the kovar alloy (4J29) are well welded by continuously adjusting the components of the tungsten-copper alloy, and the thermal conductivity and the thermal expansion coefficient meet the requirements of the optical communication module on materials.
Description
Technical Field
The invention belongs to the field of alloy materials, and particularly relates to a tungsten-copper alloy material as well as a preparation method and application thereof.
Background
In recent years, the communication industry has been rapidly developed, and the 5G network era has come, but no matter any 5G optical fiber communication, a 5G optical communication module is required. Before the 400G signal optical communication module is applied, for example, the 20G, 40G and 100G optical communication modules adopt kovar alloy or kovar alloy for assistance, and the W70Cu is used for realizing the kovar alloy, and when the 400G signal optical communication module is used, the W70Cu material cannot meet the transmission requirement.
At present, tungsten-copper alloy material products required by a 400GQSFP-DDER4-Lite signal optical communication module in the 5G field are manufactured by the traditional process, and the process route is as follows: 1. smelting metal to manufacture a plate; 2. blanking by a plate sawing machine; 3. CNC smoothing knives (which generate metal scrap); 4. punching a thread hole; 5. and (5) precision wire cutting. The existing process has low efficiency, is labor-wasting and high in cost, is not suitable for large-scale batch production, and cannot meet the requirement of the market on 5G products. Patent CN109402478A discloses a tungsten-copper alloy and an injection molding process thereof, which can better solve the technical problems existing in the conventional processes by preparing the tungsten-copper alloy through a near net shape injection molding process.
Although the technical problem existing in the traditional process can be solved by the metal powder injection molding process, the existing tungsten-copper alloy material for transmitting 400G signal optical communication modules in the 5G field still has at least the following problems: 1. problems with MIM raw material fusion; 2. failure to weld well to the valve alloy (4J 29); 3. the heat conductivity and the expansion coefficient of the tungsten-copper alloy are difficult to meet the requirements of transmitting 400G signal optical communication modules in the 5G field.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings in the background technology, and provides a tungsten-copper alloy material which is good in tungsten-copper fusion and easy to be mutually welded with a valve alloy (4J29), and a preparation method and application thereof. In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a tungsten-copper alloy material for an optical communication module emitting 400G signals in the 5G field comprises the following components in parts by weight:
in the tungsten-copper alloy material, the total weight of the silver and the silicon is preferably 1 to 1.5% of the weight of the copper. In the invention, silver and silicon are used as regulating elements, and the silver and the silicon jointly act to regulate and control the performance of the tungsten-copper alloy, and the two elements are not necessary. The research shows that the total amount of the tungsten alloy and the copper alloy has great influence on whether the performance of the tungsten alloy and the copper alloy can meet the performance requirement of an optical communication module, and the optimization shows that when the total mass of the tungsten alloy and the copper alloy is 1-1.5% of the mass of copper, the comprehensive performance of the tungsten alloy and the copper alloy is better, and the weldability of the tungsten alloy and the kovar alloy is good. When the amount of silver and silicon is too large, the solderability of the tungsten-copper alloy and the kovar alloy is deteriorated.
In the above tungsten-copper alloy material, preferably, the true density of the tungsten-copper alloy material is more than 15.2g/cm3Hardness of more than 260HV and thermal conductivity of 140--1·K-1The coefficient of thermal expansion is 8.6-8.8 (10)-6/° c). The optical communication module capable of transmitting 400G signals in the 5G field mainly comprises a shell made of tungsten-copper alloy and kovar alloy, and other electronic devices such as a circuit board, glass, a cover plate, a chip and the like are arranged in the shell, so that the tungsten-copper alloy and the kovar alloy are required to have mutually adaptive thermal expansion coefficients in severe environment. The thermal expansion coefficient can meet the requirements, the thermal conductivity can play a good heat dissipation effect on the chip, and the chip can be protected from normal work.
In the above tungsten-copper alloy material, preferably, the shear force of the welding surface when the tungsten-copper alloy material and the kovar alloy are welded to each other is greater than 25 KG. According to the invention, the tungsten-copper alloy can meet the mutual welding requirement by using a laser welding process (power is 25W, focal length is 100cm) and kovar alloy (4J29), and the shearing force of a welding surface is more than 25KG, so that the tungsten-copper alloy meets the process requirement of packaging and manufacturing an optical communication module under the condition.
As a general technical concept, the present invention also provides a preparation method of the above tungsten-copper alloy material, comprising the steps of: mixing tungsten, copper, silver, silicon and a wax-based binder, banburying to prepare particles, performing near net shape injection molding, performing extraction method for debonding, and sintering to obtain the tungsten-copper alloy material.
In the above preparation method, preferably, the wax-based binder comprises 55-60 parts by weight of polystyrene, 23-27 parts by weight of methylcellulose and 20-25 parts by weight of mineral oil, and the polystyrene, the methylcellulose and the mineral oil are heated to 90-110 ℃ and mixed and stirred for 1-3h to obtain the wax-based binder.
In the above preparation method, preferably, when the tungsten, copper, silver, and silicon are mixed with the wax-based binder, the tungsten powder, the copper powder, the silver, and the silicon are first ball-milled to obtain submicron-based powder particles, and then the submicron-based powder particles and the wax-based binder are mixed in a volume ratio of (10-15): (85-90) mixing uniformly.
In the preparation method, preferably, the banburying temperature is 90-110 ℃ and the time is 4-6 h; the temperature of the material is controlled to be 80-110 ℃, the mold temperature is controlled to be 50-70 ℃ and the injection pressure is 120 +/-10 MPa during the near net shape injection molding.
In the preparation method, preferably, the degreasing process is stopped when the flow rate of the solution is controlled to be not more than 3cm/s and the weight loss rate is 3.6-4.2% during degreasing by the extraction method; the sintering is carried out under the hydrogen atmosphere and at the peak temperature of 1300-1500 ℃ for 2-3 h. Under the protection of hydrogen atmosphere, the metal copper is fully fused with the metal tungsten through the liquid-phase and solid-phase sintering processes under the fluxing action of the trace elements of silver and silicon to obtain the required high-density tungsten-copper alloy product.
As a general technical concept, the invention also provides an application of the tungsten-copper alloy material prepared by the preparation method, the tungsten-copper alloy material is used for preparing an optical communication module which emits 400G signals in the 5G field, the optical communication module comprises a tungsten-copper alloy material and a kovar alloy which are mutually welded, the tungsten-copper alloy material and the kovar alloy are used as an optical communication module shell, and a circuit board and a chip are arranged in the optical communication module shell.
In the invention, the addition of silver and silicon is related to the characteristics of tungsten and copper metal, such as the hardness of tungsten and the heat conduction and dissipation of copper, and the addition of silver and silicon can solve the problem of large difference of melting points of tungsten and copper. The elements of silver and silicon are added into the tungsten-copper alloy, the tungsten-copper blank subjected to injection molding is sintered at the liquid phase state of 1300-1500 ℃, tungsten is used as base phase alloy powder, copper is used as liquid phase alloy powder, the addition of silver and silicon plays a role of a fluxing agent, so that tungsten and copper are sintered at the lowest eutectic point, the crystal structure and the tungsten crystal structure of copper are recombined and fused to form a high-density part, the high-efficiency fusion between tungsten and copper can be realized, and the high-density tungsten-copper alloy is obtained.
In the invention, the tungsten-copper alloy material has high requirements on the dosage of tungsten, copper, silver and silicon, and research shows that the proportion of tungsten, copper, silver and silicon can influence the welding performance of the subsequent tungsten-copper alloy material and kovar alloy, and can influence the density, hardness, thermal conductivity and thermal expansion coefficient of the subsequent product. By adopting the MIM process, the real density of more than 15.2g/cm can be obtained by optimizing the proportion of tungsten and copper, regulating and optimizing silver and silicon, and adjusting the dosage of tungsten, copper, silver and silicon to realize the mutual synergistic effect of the components3Hardness of more than 260HV and thermal conductivity of 140--1·K-1The coefficient of thermal expansion is 8.6-8.8 (10)-6/° c), and the weldability with kovar alloy is good, so that the requirement of an optical communication module emitting 400G signals in the 5G field on the material is met.
Compared with the prior art, the invention has the advantages that:
1. according to the invention, by adding silver and silicon elements into the tungsten-copper alloy, high-efficiency fusion between high-content tungsten and copper can be realized, easy sintering invariance under a hydrogen atmosphere is facilitated, the skeleton appearance is maintained, the densification speed, the density of a final product and the appearance of the final product are improved, and the product quality is higher.
2. According to the invention, the tungsten-copper alloy and the kovar alloy (4J29) are well welded by continuously adjusting the components of the tungsten-copper alloy, and the thermal conductivity and the thermal expansion coefficient meet the requirements of the optical communication module on materials.
3. The tungsten-copper alloy is easy to realize modular production, has high production efficiency, and reduces the generation of processing waste.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
a tungsten-copper alloy material comprises the following components in parts by weight (percentage):
the preparation method of the tungsten-copper alloy material comprises the following steps:
(1) heating 56 parts by weight of polystyrene, 23 parts by weight of methylcellulose and 22 parts by weight of mineral oil in a closed container to 110 ℃, mixing and stirring for 2 hours to obtain a wax-based binder; carrying out ball milling on tungsten powder, copper powder, silver and silicon according to the dosage ratio (the rotating speed is 800rpm, and the time is 4 hours) to obtain submicron-base powder particles; and then mixing the submicron-base powder particles with the wax-base binder according to the volume ratio of 12: 88 mixing evenly;
(2) banburying the mixture of the submicron-based powder particles and the wax-based binder at 98 ℃ for 6 hours to obtain a granular tungsten-copper material;
(3) designing a near net shape injection mold according to the shape of the product and the material shrinkage ratio, controlling the material temperature to be 90 ℃, the mold temperature to be 65 ℃ and the injection pressure to be 110MPa during injection, and obtaining an injection blank through a near net shape injection molding process;
(4) performing solution debonding on the injection blank by adopting an extraction method, controlling the flow rate of the solution to be not more than 3cm/s, paying attention to the control of the filling amount of a debonding groove, reducing the deformation of the blank, and stopping a degreasing process when the weight loss rate is 3.8%;
(5) and (3) preserving the heat for 2 hours at the peak temperature of 1340 ℃ in a hydrogen atmosphere to obtain the tungsten-copper alloy material.
The actual density, hardness, thermal conductivity and thermal expansion coefficient of the tungsten-copper alloy material in the embodiment are measured, the density is directly measured (normal temperature) by using a density analyzer, the hardness is measured (normal temperature) by using a vickers hardness tester, the thermal conductivity measuring instrument comprises an electronic balance, a thermal conductivity meter and a differential scanning calorimeter, and the test environment is as follows: the temperature was 22 ℃ and the humidity was 52% RH. Coefficient of thermal expansion using thermomechanical analyzer (TMA) model: q400EM, test temperature 23.1 deg.C, humidity 52% RH. The shearing force adopts a push-pull force tester.
The actual density of the tungsten-copper alloy material obtained in the embodiment is measured to be 15.26g/cm3A hardness of 268HV and a thermal conductivity of 152 W.M-1·K-1Coefficient of thermal expansion of 8.65 (10)-6/℃)。
The optical communication module for transmitting 400G signals in the 5G field is prepared by using the tungsten-copper alloy material in the embodiment, the optical communication module comprises the tungsten-copper alloy material and a kovar alloy shell which are mutually welded, and a circuit board and a chip are arranged in the optical communication module shell. In this embodiment, the tungsten-copper alloy and the kovar alloy (4J29) are welded by a laser welding process (power 25W, focal length 100cm), and the shearing force of the welding surface when the tungsten-copper alloy and the kovar alloy are welded to each other is 26.5 KG.
Example 2:
the tungsten-copper alloy material comprises the following components in parts by weight:
the preparation method of the tungsten-copper alloy material in this example is the same as that in example 1.
The performance test method of the tungsten-copper alloy in the present embodiment is the same as that of embodiment 1.
The actual density of the tungsten-copper alloy material obtained in the embodiment is 15.32g/cm3A hardness of 272HV and a thermal conductivity of 158 W.M-1·K-1Coefficient of thermal expansion of 8.68 (10)-6/℃)。
In the embodiment, the tungsten-copper alloy material is used for preparing the module capable of emitting 400G signals in the 5G optical communication field, in the embodiment, the tungsten-copper alloy and the kovar alloy (4J29) use a laser welding process (power 25W, focal length 100cm), and the shearing force of the welding surface is 26KG when the tungsten-copper alloy and the kovar alloy are welded with each other.
Example 3:
the tungsten-copper alloy material comprises the following components in parts by weight:
the preparation method of the tungsten-copper alloy material in this example is the same as that in example 1.
The performance test method of the tungsten-copper alloy in the present embodiment is the same as that of embodiment 1.
The actual density of the tungsten-copper alloy material obtained in the embodiment is 15.33g/cm3Hardness of 285HV and thermal conductivity of 167 W.M-1·K-1Coefficient of thermal expansion of 8.75 (10)-6/℃)。
In the embodiment, the tungsten-copper alloy material is used for preparing the module capable of emitting 400G signals in the 5G optical communication field, in the embodiment, the tungsten-copper alloy and the kovar alloy (4J29) use a laser welding process (power 25W, focal length 100cm), and the shearing force of the welding surface is 32KG when the tungsten-copper alloy and the kovar alloy are welded with each other.
Example 4:
the tungsten-copper alloy material comprises the following components in parts by weight:
the preparation method of the tungsten-copper alloy material in this example is the same as that in example 1.
The performance test method of the tungsten-copper alloy in the present embodiment is the same as that of embodiment 1.
The actual density of the tungsten-copper alloy material obtained in the embodiment is 15.3g/cm through measurement3A hardness of 278HV and a thermal conductivity of 160 W.M-1·K-1Coefficient of thermal expansion of 8.75 (10)-6/℃)。
In the embodiment, the tungsten-copper alloy material is used for preparing the module capable of emitting 400G signals in the 5G optical communication field, in the embodiment, the tungsten-copper alloy and the kovar alloy (4J29) use a laser welding process (power 25W, focal length 100cm), and the shearing force of the welding surface is 30KG when the tungsten-copper alloy and the kovar alloy are welded with each other.
Example 5:
the tungsten-copper alloy material comprises the following components in parts by weight:
the preparation method of the tungsten-copper alloy material in this example is the same as that in example 1.
The performance test method of the tungsten-copper alloy in the present embodiment is the same as that of embodiment 1.
The actual density of the tungsten-copper alloy material obtained in the embodiment is 15.3g/cm through measurement3A hardness of 275HV and a thermal conductivity of159W·M-1·K-1Coefficient of thermal expansion of 8.6 (10)-6/℃)。
In the embodiment, the tungsten-copper alloy material is used for preparing the module capable of emitting 400G signals in the 5G optical communication field, in the embodiment, the tungsten-copper alloy and the kovar alloy (4J29) use a laser welding process (power 25W, focal length 100cm), and the shearing force of the welding surface is 28.5KG when the tungsten-copper alloy and the kovar alloy are welded with each other.
Comparative example 1:
the tungsten-copper alloy material comprises the following components in parts by weight:
80 parts of tungsten;
20 parts of copper.
The tungsten-copper alloy material in this comparative example was prepared in the same manner as in example 1.
The method for testing the performance of the tungsten-copper alloy in the comparative example is the same as that of example 1.
The actual density of the tungsten-copper alloy material obtained in the comparative example is measured to be 15.2g/cm3A hardness of 258HV and a thermal conductivity of 55 W.M-1·K-1Coefficient of thermal expansion of 34.3 (10)-6/℃)。
In the comparative example, when the tungsten-copper alloy and the kovar alloy (4J29) are subjected to a laser welding process (with the power of 25W and the focal length of 100cm), the tungsten-copper alloy and the kovar alloy are not easy to weld, the welding force is extremely small, and the detection is difficult.
Comparative example 2:
the tungsten-copper alloy material comprises the following components in parts by weight:
79.9 parts of tungsten;
19.9 parts of copper;
0.2 part of silver.
The tungsten-copper alloy material in this comparative example was prepared in the same manner as in example 1.
The method for testing the performance of the tungsten-copper alloy in the comparative example is the same as that of example 1.
The actual density of the tungsten-copper alloy material obtained in the comparative example is 14.98g/cm3Hardness of242HV, and 57 W.M in thermal conductivity-1·K-1Coefficient of thermal expansion of 4.6 (10)-6/℃)。
In the comparative example, the tungsten-copper alloy and the kovar alloy (4J29) use a laser welding process (power 25w, focal length 100cm), and the shearing force of the welding surface is 12KG when the tungsten-copper alloy and the kovar alloy are welded with each other.
Comparative example 3:
the tungsten-copper alloy material comprises the following components in parts by weight:
79.9 parts of tungsten;
19.9 parts of copper;
0.2 part of silicon.
The tungsten-copper alloy material in this comparative example was prepared in the same manner as in example 1.
The method for testing the performance of the tungsten-copper alloy in the comparative example is the same as that of example 1.
The actual density of the tungsten-copper alloy material obtained in the comparative example is 14.88g/cm3Hardness of 240HV and thermal conductivity of 60 W.M-1·K-1A coefficient of thermal expansion of 5.0 (10)-6/℃)。
In the comparative example, the tungsten-copper alloy and the kovar alloy (4J29) use a laser welding process (power 25w, focal length 100cm), and the shearing force of the welding surface is 7KG when the tungsten-copper alloy and the kovar alloy are welded with each other.
Comparative example 4:
the tungsten-copper alloy material comprises the following components in parts by weight:
the tungsten-copper alloy material in this comparative example was prepared in the same manner as in example 1.
The method for testing the performance of the tungsten-copper alloy in the comparative example is the same as that of example 1.
The actual density of the tungsten-copper alloy material obtained in the comparative example is 14.85g/cm3A hardness of 236HV and a thermal conductivity of 43 W.M-1·K-1Coefficient of thermal expansion of 3.9 (10)-6/℃)。
In the comparative example, the tungsten-copper alloy and the kovar alloy (4J29) use a laser welding process (power 25W, focal length 100cm), and the shearing force of the welding surface is 10KG when the tungsten-copper alloy and the kovar alloy are welded with each other.
Comparative example 5:
the tungsten-copper alloy material comprises the following components in parts by weight:
the tungsten-copper alloy material in this comparative example was prepared in the same manner as in example 1.
The method for testing the performance of the tungsten-copper alloy in the comparative example is the same as that of example 1.
The actual density of the tungsten-copper alloy material obtained in the comparative example is measured to be 15.05g/cm3A hardness of 259HV and a thermal conductivity of 62 W.M-1·K-1Coefficient of thermal expansion of 5.1 (10)-6/℃)。
In the comparative example, the tungsten-copper alloy and the kovar alloy (4J29) use a laser welding process (power 25W, focal length 100cm), and the shearing force of the welding surface is 5KG when the tungsten-copper alloy and the kovar alloy are welded with each other.
Claims (7)
1. A tungsten-copper alloy material for an optical communication module emitting 400G signals in the 5G field is characterized by comprising the following components in parts by weight:
80.2 parts of tungsten;
19.57 parts of copper;
0.08 part of silver;
0.15 part of silicon;
the tungsten-copper alloy material has the true density of 15.33g/cm high-speed fruit train, the hardness of 285HV and the thermal conductivity of 167 W.M-1·K-1Coefficient of thermal expansion of 8.75X 10-6/℃；
The shearing force of the welding surface when the tungsten-copper alloy material and the kovar alloy are welded with each other is 32 KG.
2. The preparation method of the tungsten-copper alloy material according to claim 1, characterized by comprising the following steps: mixing tungsten, copper, silver, silicon and a wax-based binder, banburying to prepare particles, performing near net shape injection molding, performing extraction method for debonding, and sintering to obtain the tungsten-copper alloy material.
3. The preparation method according to claim 2, wherein the wax-based binder comprises 55-60 parts by weight of polystyrene, 23-27 parts by weight of methylcellulose and 20-25 parts by weight of mineral oil, and the polystyrene, the methylcellulose and the mineral oil are heated to 90-110 ℃ and mixed and stirred for 1-3h to obtain the wax-based binder.
4. The preparation method according to claim 2, wherein when the tungsten, the copper, the silver and the silicon are mixed with the wax-based binder, the tungsten powder, the copper powder, the silver and the silicon are firstly ball-milled to obtain submicron-based powder particles, and then the submicron-based powder particles and the wax-based binder are mixed in a volume ratio of (10-15): (85-90) mixing uniformly.
5. The preparation method according to any one of claims 2 to 4, characterized in that the banburying temperature is 90-110 ℃ and the time is 4-6 h; the temperature of the material is controlled to be 80-110 ℃, the mold temperature is controlled to be 50-70 ℃ and the injection pressure is 120 +/-10 MPa during the near net shape injection molding.
6. The preparation method according to any one of claims 2 to 4, characterized in that the degreasing process is terminated when the solution flow rate is controlled to be not more than 3cm/s and the weight loss rate is 3.6-4.2% during degreasing by the extraction method; the sintering is carried out under the hydrogen atmosphere and at the peak temperature of 1300-1500 ℃ for 2-3 h.
7. The application of the tungsten-copper alloy material according to claim 1 or the tungsten-copper alloy material prepared by the preparation method according to any one of claims 2 to 6 is characterized in that the tungsten-copper alloy material is used for preparing an optical communication module which emits 400G signals in the 5G field, the optical communication module comprises the tungsten-copper alloy material and kovar alloy which are welded with each other, the tungsten-copper alloy material and the kovar alloy are used as an optical communication module shell, and a circuit board and a chip are arranged inside the optical communication module shell.
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