Preparation method of tungsten-copper composite material

Abstract

The invention discloses a preparation method of a tungsten-copper composite material, which comprises the following steps: step 1, uniformly mixing tungsten and copper according to a weight ratio of 5: 2, then adding the mixture into an interface agent which is 3-5 times of the total amount of the tungsten, carrying out ultrasonic oscillation treatment, and after the ultrasonic treatment is finished, washing, carrying out suction filtration and drying; and 2, uniformly mixing and stirring the dried product in the step 1 and the modified liquid according to a weight ratio of 7: 3, and after stirring is finished, washing, carrying out suction filtration and drying. According to the tungsten-copper composite material, tungsten and copper are matched, ultrasonic oscillation treatment is carried out in an interface agent, stirring is carried out in cooperation with modified liquid, the tungsten-copper composite material is obtained through synergistic improvement of the tungsten and the copper, pre-hot pressing treatment and sintering improvement treatment, the strength performance, the heat conduction performance and the abrasion resistance of a product are improved in a balanced and coordinated mode, and the use efficiency of the product is improved.

Description

Technical Field

[0001] The invention relates to the technical field of tungsten-copper, and in particular to a preparation method of a tungsten-copper composite material. Background Art

[0002] The tungsten-copper composite material is a two-phase structure pseudo alloy mainly composed of tungsten and copper elements, with a copper content of 7% to 50%, and is a metal-based composite material. Since tungsten and copper are mutually insoluble, the tungsten-copper composite material has the low expansion, wear resistance, and corrosion resistance of tungsten and the high electrical and thermal conductivity of copper. However, due to the poor interface compatibility of the existing tungsten-copper composite materials, it is difficult to balance and coordinate the improvement of the strength performance, thermal conductivity and wear resistance of the product, which limits the use efficiency of the product. Based on this, the present invention further improves it. Summary of the invention

[0003] In view of the defects of the prior art, the purpose of the present invention is to provide a method for preparing a tungsten-copper composite material to solve the problems raised in the above background technology.

[0004] The present invention solves the technical problem by adopting the following technical solution: The present invention provides a method for preparing a tungsten-copper composite material, comprising the following steps: Step 1: Mix tungsten and copper in a weight ratio of 5:2, then add them into an interface agent that is 3-5 times the total amount of tungsten for ultrasonic oscillation treatment. After the ultrasonic treatment is completed, wash with water, filter and dry; Step 2: Mix the dried product of step 1 and the modified liquid in a weight ratio of 7:3, and stir until the stirring is complete, wash with water, filter, and dry; Step 3: The product of step 2 is preheated and pressed for 10-15 minutes, and after the treatment is completed, a hot-pressed composite is obtained; Step 4: The hot pressed composite agent is subjected to sintering improvement treatment. After the treatment is completed, a tungsten-copper composite material can be obtained.

[0005] Preferably, the oscillation power of the ultrasonic oscillation treatment is 350-400W, and the oscillation time is 20-30min; the stirring speed of the mixing and stirring treatment is 300-400r / min, and the stirring is for 2h.

[0006] Preferably, the pre-heat pressing treatment has a pressure of 10-20 MPa, a heat pressing temperature of 100° C., and a heat pressing time of 1-2 h.

[0007] Preferably, the preparation method of the interface agent is: S1: treating bentonite with proton irradiation, and obtaining irradiated bentonite after the irradiation is completed; S2: The irradiated bentonite is first mixed with a sufficient amount of sodium lignin sulfonate solution to obtain a bentonite solution; S3: 4-7 parts of bentonite solution, 1-3 parts of silane coupling agent KH550, 2-5 parts of lanthanum nitrate solution, 1-3 parts of yttrium oxide and 2-6 parts of sodium alginate are fully mixed to obtain an interface agent.

[0008] Preferably, the proton irradiation treatment has an irradiation power of 350-400 W and an irradiation time of 20-30 min.

[0009] Preferably, the mass fraction of the sodium lignin sulfonate solution is 5-8%; the mass fraction of the lanthanum nitrate solution is 2-5%.

[0010] Preferably, the preparation method of the modified liquid is: S11: heat treating the graphene at 150-170°C for 10-15min, then heating to 210-220°C at a rate of 1-3°C / min, keeping the temperature for 2-5min, and finally air cooling to room temperature; S12: 4-7 parts of S11 graphene, 2-5 parts of silane coupling agent KH560, 1-3 parts of sodium dodecylbenzene sulfonate solution, 4-7 parts of dopamine hydrochloride solution, and 1-2 parts of nano-silicon dioxide are fully mixed to obtain a modified solution.

[0011] Preferably, the mass fraction of the dopamine hydrochloride solution is 2-5%; the mass fraction of the sodium dodecylbenzene sulfonate solution is 4-7%.

[0012] Preferably, the sintering improvement treatment is first heated to 210-220°C at a rate of 1-3°C / min, kept warm for 10-15min, then heated to 1000-1050°C at a rate of 3-5°C / min, sintered for 1-2h, and after sintering, air-cooled to room temperature.

[0013] Compared with the prior art, the present invention has the following beneficial effects: The tungsten-copper composite material of the present invention adopts tungsten and copper, is subjected to ultrasonic oscillation treatment in an interface agent, and is stirred with a modified liquid. The tungsten-copper composite material is obtained by the coordinated improvement of the two, and is further subjected to preheating and pressing treatment and sintering improvement treatment. The strength performance, thermal conductivity and wear resistance of the product are balanced and coordinated improved, thereby improving the use efficiency of the product. DETAILED DESCRIPTION

[0014] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0015] A method for preparing a tungsten-copper composite material of this embodiment includes the following steps: Step 1: Mix tungsten and copper in a weight ratio of 5:2, then add them into an interface agent that is 3-5 times the total amount of tungsten for ultrasonic oscillation treatment. After the ultrasonic treatment is completed, wash with water, filter and dry; Step 2: Mix the dried product of step 1 and the modified liquid in a weight ratio of 7:3, and stir until the stirring is complete, wash with water, filter, and dry; Step 3: The product of step 2 is preheated and pressed for 10-15 minutes, and after the treatment is completed, a hot-pressed composite is obtained; Step 4: The hot pressed composite agent is subjected to sintering improvement treatment. After the treatment is completed, a tungsten-copper composite material can be obtained.

[0016] The oscillation power of the ultrasonic oscillation treatment in this embodiment is 350-400W, and the oscillation time is 20-30min; the stirring speed of the mixing and stirring treatment is 300-400r / min, and the stirring is for 2h.

[0017] The pre-heat pressing treatment pressure in this embodiment is 10-20 MPa, the hot pressing temperature is 100° C., and the hot pressing time is 1-2 h.

[0018] The preparation method of the interface agent of this embodiment is: S1: treating bentonite with proton irradiation, and obtaining irradiated bentonite after the irradiation is completed; S2: The irradiated bentonite is first mixed with a sufficient amount of sodium lignin sulfonate solution to obtain a bentonite solution; S3: 4-7 parts of bentonite solution, 1-3 parts of silane coupling agent KH550, 2-5 parts of lanthanum nitrate solution, 1-3 parts of yttrium oxide and 2-6 parts of sodium alginate are fully mixed to obtain an interface agent.

[0019] The irradiation power of the proton irradiation treatment in this embodiment is 350-400W, and the irradiation time is 20-30min.

[0020] The mass fraction of the sodium lignin sulfonate solution in this embodiment is 5-8%; the mass fraction of the lanthanum nitrate solution is 2-5%.

[0021] The preparation method of the modified liquid of this embodiment is: S11: heat treating the graphene at 150-170°C for 10-15min, then heating to 210-220°C at a rate of 1-3°C / min, keeping the temperature for 2-5min, and finally air cooling to room temperature; S12: 4-7 parts of S11 graphene, 2-5 parts of silane coupling agent KH560, 1-3 parts of sodium dodecylbenzene sulfonate solution, 4-7 parts of dopamine hydrochloride solution, and 1-2 parts of nano-silicon dioxide are fully mixed to obtain a modified solution.

[0022] The mass fraction of the dopamine hydrochloride solution in this embodiment is 2-5%; the mass fraction of the sodium dodecylbenzene sulfonate solution is 4-7%.

[0023] The sintering improvement treatment of this embodiment is to first increase the temperature to 210-220°C at a rate of 1-3°C / min, keep the temperature for 10-15min, then increase the temperature to 1000-1050°C at a rate of 3-5°C / min, sinter for 1-2h, and then air cool to room temperature after sintering.

[0024] Example 1. A method for preparing a tungsten-copper composite material of this embodiment includes the following steps: Step 1: Mix tungsten and copper in a weight ratio of 5:2, then add them into an interface agent that is 3-5 times the total amount of tungsten for ultrasonic oscillation treatment. After the ultrasonic treatment is completed, wash with water, filter and dry; Step 2: Mix the dried product of step 1 and the modified liquid in a weight ratio of 7:3, and stir until the stirring is complete, wash with water, filter, and dry; Step 3: The product of step 2 is preheated and pressed for 10 minutes, and after the treatment is completed, a hot-pressed composite is obtained; Step 4: The hot pressed composite agent is subjected to sintering improvement treatment. After the treatment is completed, a tungsten-copper composite material can be obtained.

[0025] The oscillation power of the ultrasonic oscillation treatment in this embodiment is 350W, and the oscillation time is 20min; the stirring speed of the mixing and stirring treatment is 300r / min, and the stirring is 2h.

[0026] The pre-heat pressing treatment pressure in this embodiment is 10 MPa, the hot pressing temperature is 100° C., and the hot pressing time is 1 hour.

[0027] The preparation method of the interface agent of this embodiment is: S1: treating bentonite with proton irradiation, and obtaining irradiated bentonite after the irradiation is completed; S2: The irradiated bentonite is first mixed with a sufficient amount of sodium lignin sulfonate solution to obtain a bentonite solution; S3: 4 parts of bentonite solution, 1 part of silane coupling agent KH550, 2 parts of lanthanum nitrate solution, 1 part of yttrium oxide and 2 parts of sodium alginate are fully mixed to obtain an interface agent.

[0028] The irradiation power of the proton irradiation treatment in this embodiment is 350W, and the irradiation time is 20 minutes.

[0029] The mass fraction of the sodium lignin sulfonate solution in this embodiment is 5%; the mass fraction of the lanthanum nitrate solution is 2%.

[0030] The preparation method of the modified liquid of this embodiment is: S11: heat treating the graphene at 150°C for 1 min, then heating to 210°C at a rate of 1°C / min, keeping the temperature for 2 min, and finally air cooling to room temperature; S12: 4 parts of S11 graphene, 2 parts of silane coupling agent KH560, 1 part of sodium dodecylbenzene sulfonate solution, 4 parts of dopamine hydrochloride solution, and 1 part of nano-silicon dioxide are fully mixed to obtain a modified solution.

[0031] The mass fraction of the dopamine hydrochloride solution in this embodiment is 2%; the mass fraction of the sodium dodecylbenzenesulfonate solution is 4%.

[0032] The sintering improvement treatment of this embodiment is to first increase the temperature to 210°C at a rate of 1°C / min, keep the temperature for 10 minutes, then increase the temperature to 1000°C at a rate of 3°C / min, sinter for 1 hour, and then air cool to room temperature after the sintering is completed.

[0033] Example 2. A method for preparing a tungsten-copper composite material of this embodiment includes the following steps: Step 1: Mix tungsten and copper in a weight ratio of 5:2, then add them into an interface agent that is 5 times the total amount of tungsten for ultrasonic oscillation treatment. After the ultrasonic treatment is completed, wash with water, filter and dry; Step 2: Mix the dried product of step 1 and the modified liquid in a weight ratio of 7:3, and stir until the stirring is complete, wash with water, filter, and dry; Step 3: The product of step 2 is preheated and pressed for 15 minutes, and after the treatment is completed, a hot-pressed composite is obtained; Step 4: The hot pressed composite agent is subjected to sintering improvement treatment. After the treatment is completed, a tungsten-copper composite material can be obtained.

[0034] The oscillation power of the ultrasonic oscillation treatment in this embodiment is 400 W, and the oscillation time is 30 min; the stirring speed of the mixing and stirring treatment is 400 r / min, and the stirring is 2 h.

[0035] The pre-heat pressing treatment pressure in this embodiment is 20 MPa, the hot pressing temperature is 100° C., and the hot pressing time is 2 h.

[0036] The preparation method of the interface agent of this embodiment is: S1: treating bentonite with proton irradiation, and obtaining irradiated bentonite after the irradiation is completed; S2: The irradiated bentonite is first mixed with a sufficient amount of sodium lignin sulfonate solution to obtain a bentonite solution; S3: 7 parts of bentonite solution, 3 parts of silane coupling agent KH550, 5 parts of lanthanum nitrate solution, 3 parts of yttrium oxide and 6 parts of sodium alginate are fully mixed to obtain an interface agent.

[0037] The irradiation power of the proton irradiation treatment in this embodiment is 400W, and the irradiation time is 30 minutes.

[0038] The mass fraction of the sodium lignin sulfonate solution in this embodiment is 8%; the mass fraction of the lanthanum nitrate solution is 5%.

[0039] The preparation method of the modified liquid of this embodiment is: S11: heat treating the graphene at 170°C for 15 min, then heating to 220°C at a rate of 3°C / min, keeping the temperature for 5 min, and finally air cooling to room temperature; S12: 7 parts of S11 graphene, 5 parts of silane coupling agent KH560, 3 parts of sodium dodecylbenzene sulfonate solution, 7 parts of dopamine hydrochloride solution and 2 parts of nano-silicon dioxide are fully mixed to obtain a modified solution.

[0040] The mass fraction of the dopamine hydrochloride solution in this embodiment is 5%; the mass fraction of the sodium dodecylbenzene sulfonate solution is 7%.

[0041] The sintering improvement treatment of this embodiment is to first increase the temperature to 220°C at a rate of 3°C / min, keep the temperature for 15 minutes, then increase the temperature to 1050°C at a rate of 5°C / min, sinter for 2 hours, and then air cool to room temperature after the sintering is completed.

[0042] Example 3. A method for preparing a tungsten-copper composite material of this embodiment includes the following steps: Step 1: Mix tungsten and copper in a weight ratio of 5:2, then add them into an interface agent that is 4 times the total amount of tungsten for ultrasonic oscillation treatment. After the ultrasonic treatment is completed, wash with water, filter and dry; Step 2: Mix the dried product of step 1 and the modified liquid in a weight ratio of 7:3, and stir until the stirring is complete, wash with water, filter, and dry; Step 3: The product of step 2 is preheated and pressed for 12.5 minutes, and after the treatment is completed, a hot-pressed composite is obtained; Step 4: The hot pressed composite agent is subjected to sintering improvement treatment. After the treatment is completed, a tungsten-copper composite material can be obtained.

[0043] The oscillation power of the ultrasonic oscillation treatment in this embodiment is 370W, and the oscillation time is 5min; the stirring speed of the mixing and stirring treatment is 350r / min, and the stirring is 2h.

[0044] The pre-heat pressing treatment pressure in this embodiment is 15 MPa, the hot pressing temperature is 100° C., and the hot pressing time is 1.5 h.

[0045] The preparation method of the interface agent of this embodiment is: S1: treating bentonite with proton irradiation, and obtaining irradiated bentonite after the irradiation is completed; S2: The irradiated bentonite is first mixed with a sufficient amount of sodium lignin sulfonate solution to obtain a bentonite solution; S3: 5.5 parts of bentonite solution, 2 parts of silane coupling agent KH550, 3.5 parts of lanthanum nitrate solution, 2 parts of yttrium oxide and 4 parts of sodium alginate are fully mixed to obtain an interface agent.

[0046] The irradiation power of the proton irradiation treatment in this embodiment is 375W, and the irradiation time is 25 minutes.

[0047] The mass fraction of the sodium lignin sulfonate solution in this embodiment is 6.5%; the mass fraction of the lanthanum nitrate solution is 3.5%.

[0048] The preparation method of the modified liquid of this embodiment is: S11: heat treating the graphene at 160°C for 12.5 min, then heating to 215°C at a rate of 2°C / min, keeping the temperature for 3.5 min, and finally air cooling to room temperature; S12: 5.5 parts of S11 graphene, 3.5 parts of silane coupling agent KH560, 2 parts of sodium dodecylbenzene sulfonate solution, 5.5 parts of dopamine hydrochloride solution, and 1.5 parts of nano-silicon dioxide were fully mixed to obtain a modified solution.

[0049] The mass fraction of the dopamine hydrochloride solution in this embodiment is 3.5%; the mass fraction of the sodium dodecylbenzene sulfonate solution is 5.5%.

[0050] The sintering improvement treatment of this embodiment is to first increase the temperature to 215°C at a rate of 2°C / min, keep the temperature for 12.5 minutes, then increase the temperature to 1025°C at a rate of 4°C / min, sinter for 1.5 hours, and then air cool to room temperature after the sintering is completed.

[0051] Comparative Example 1. The difference from Example 3 is that no interface agent is added.

[0052] Comparative Example 2. The difference from Example 3 is that no bentonite liquid is added to the interface agent.

[0053] Comparative Example 3. The difference from Example 3 is that no lanthanum nitrate solution and yttrium oxide are added to the interface agent.

[0054] Comparative Example 4. The difference from Example 3 is that no modifying liquid is added.

[0055] Comparative Example 5. The difference from Example 3 is that no S11 graphene is added to the modified liquid.

[0056] Comparative Example 6. The difference from Example 3 is that no dopamine hydrochloride solution or nano silicon dioxide is added to the modified liquid.

[0057] The product performance tests of Examples 1-3 and Comparative Examples 1-6 are as follows:

[0058] It can be seen from Comparative Examples 1-6 and Examples 1-3 that the strength, thermal conductivity and wear resistance of the product of the present invention can be improved in a coordinated manner. At the same time, the product does not add an interface agent or a modifying liquid, and the performance of the product deteriorates significantly. The coordinated combination of the two has the most significant performance effect of the product. When bentonite liquid is not added to the interface agent, lanthanum nitrate solution and yttrium oxide are not added to the interface agent, S11 graphene is not added to the modifying liquid, and dopamine hydrochloride solution and nano-silicon dioxide are not added to the modifying liquid, the performance of the product tends to deteriorate. Only when the interface agent and modifying liquid of the present invention are used, the performance effect of the product is most significant.

[0059] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be considered exemplary and non-restrictive in all respects, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention.

[0060] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. A method for preparing a tungsten-copper composite material, characterized in that: The following steps are involved: Step 1: Mix tungsten and copper in a weight ratio of 5:2, then add them into an interface agent that is 3-5 times the total amount of tungsten for ultrasonic oscillation treatment. After the ultrasonic treatment is completed, wash with water, filter and dry; Step 2: Mix the dried product of step 1 and the modified liquid in a weight ratio of 7:3, and stir until the stirring is complete, wash with water, filter, and dry; Step 3: The product of step 2 is preheated and pressed for 10-15 minutes, and after the treatment is completed, a hot-pressed composite is obtained; Step 4: The hot pressed composite agent is subjected to sintering improvement treatment. After the treatment is completed, a tungsten-copper composite material can be obtained.

2. The method for preparing a tungsten-copper composite material according to claim 1, characterized in that: The oscillation power of the ultrasonic oscillation treatment is 350-400W, and the oscillation time is 20-30min; the stirring speed of the mixing and stirring treatment is 300-400r / min, and the stirring is for 2h.

3. The method for preparing a tungsten-copper composite material according to claim 1, characterized in that: The preheating and pressing treatment has a pressure of 10-20 MPa, a hot pressing temperature of 100° C., and a hot pressing time of 1-2 h.

4. The method for preparing a tungsten-copper composite material according to claim 1, characterized in that: The preparation method of the interface agent is: S1: treating bentonite with proton irradiation, and obtaining irradiated bentonite after the irradiation is completed; S2: The irradiated bentonite is first mixed with a sufficient amount of sodium lignin sulfonate solution to obtain a bentonite solution; S3: 4-7 parts of bentonite solution, 1-3 parts of silane coupling agent KH550, 2-5 parts of lanthanum nitrate solution, 1-3 parts of yttrium oxide and 2-6 parts of sodium alginate are fully mixed to obtain an interface agent.

5. The method for preparing a tungsten-copper composite material according to claim 4, characterized in that: The proton irradiation treatment has an irradiation power of 350-400W and an irradiation time of 20-30min.

6. The method for preparing a tungsten-copper composite material according to claim 4, characterized in that: The mass fraction of the sodium lignin sulfonate solution is 5-8%; the mass fraction of the lanthanum nitrate solution is 2-5%.

7. The method for preparing a tungsten-copper composite material according to claim 1, characterized in that: The preparation method of the modified liquid is: S11: heat treating the graphene at 150-170°C for 10-15min, then heating to 210-220°C at a rate of 1-3°C / min, keeping the temperature for 2-5min, and finally air cooling to room temperature; S12: 4-7 parts of S11 graphene, 2-5 parts of silane coupling agent KH560, 1-3 parts of sodium dodecylbenzene sulfonate solution, 4-7 parts of dopamine hydrochloride solution, and 1-2 parts of nano-silicon dioxide are fully mixed to obtain a modified solution.

8. The method for preparing a tungsten-copper composite material according to claim 7, characterized in that: The mass fraction of the dopamine hydrochloride solution is 2-5%; the mass fraction of the sodium dodecylbenzene sulfonate solution is 4-7%.

9. The method for preparing a tungsten-copper composite material according to claim 1, characterized in that: The sintering improvement treatment is firstly to heat up to 210-220°C at a rate of 1-3°C / min, keep warm for 10-15min, then to heat up to 1000-1050°C at a rate of 3-5°C / min, sinter for 1-2h, and after sintering, air cool to room temperature.

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