CN115889765A - Preparation process of high-pressure-billet-strength low-apparent-density copper powder - Google Patents
Preparation process of high-pressure-billet-strength low-apparent-density copper powder Download PDFInfo
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Abstract
The invention relates to the field of copper powder, in particular to a preparation process of copper powder with high-pressure blank strength and low apparent density, which is used for solving the problems that the existing copper powder preparation process seriously pollutes the environment and has high energy consumption, and the prepared copper powder has high apparent density and low green blank strength; the copper powder is formed by spraying in the preparation process, the pollution to the environment is greatly reduced, the energy consumption is low, the copper powder formed by spraying can form powder with an irregular shape, the shape of the sintered copper powder is more complex, the loose packing density of the copper powder is reduced, graphene grows on the surface of the copper powder during sintering, the tensile strength, hardness, friction and abrasion resistance and other performances of the material are greatly improved, the generated copper powder graphene composite material is more irregular due to the fact that the isolating agent is corroded, the copper powder is not sintered together and is fully wrapped by the graphene, the loose packing density of the copper powder can be further reduced, and the green strength is improved.
Description
Technical Field
The invention relates to the field of copper powder, in particular to a preparation process of copper powder with high-pressure blank strength and low apparent density.
Background
With the development of science and technology, the speed of a high-speed railway is continuously improved, the use conditions of a brake device of the high-speed railway are more and more rigorous, people require the brake device to stop a high-speed railway in a short time, the huge kinetic energy of the high-speed railway is converted into the friction heat energy of a brake pad, the surface of a friction pair can be rapidly increased, the friction coefficient of a friction material is influenced, and the safety and the reliability of the high-speed railway are reduced. Therefore, in order to meet the comprehensive technical indexes of high-speed railways, high-performance brake materials need to be continuously researched and developed.
The braking material needs to meet the performance requirements of the following aspects at the same time: it should have high and stable friction factor, good thermal crack resistance and wear resistance, high strength and proper density.
Copper powder is one of basic raw materials of high-iron brake materials, the production method of the copper powder is mainly an electrolytic method, the production history of the electrolytic method is long, the process is mature, the copper powder produced by the electrolytic method has a dendritic microscopic shape, and has the characteristics of developed specific surface, high purity, good forming performance and the like, but the copper powder produced by the electrolytic method has the defects of serious environmental pollution and high energy consumption. The method can replace the first-push atomization powder preparation method of an electrolytic method in the aspect of copper powder production, but practice proves that the copper powder produced by a single atomization method has the defects of large apparent density, poor formability and the like, the green strength is very low and generally does not exceed 5MPa, the copper powder can only be added in a small proportion in partial metallurgical products, and the electrolytic copper powder cannot be replaced in practical application.
How to improve the defects that the existing copper powder preparation process has serious environmental pollution and high energy consumption, and the prepared copper powder has large apparent density and very low green strength, therefore, a preparation process of the copper powder with high-pressure blank strength and low apparent density is urgently needed to solve the problems.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a preparation process of copper powder with high-pressure billet strength and low apparent density, which comprises the following steps: the method comprises the steps of adding electrolytic copper into a smelting furnace for smelting treatment to obtain copper liquid, cooling the copper liquid, introducing nitrogen into the copper liquid, fishing out floating slag on the liquid level of the copper liquid to obtain purified copper liquid, performing spray treatment on the purified copper liquid to obtain copper powder, placing the copper powder into a vacuum drying box for vacuum drying to obtain dried copper powder, adding the dried copper powder and magnesium oxide nano powder into a mixing machine for stirring and mixing to obtain mixed powder, placing the mixed powder into a quartz tube, placing the quartz tube into a CVD (chemical vapor deposition) furnace, performing high-temperature heat treatment in an argon and hydrogen atmosphere, introducing methane for vapor-phase chemical deposition, and cooling to room temperature to obtain the copper powder with high-pressure blank strength and low loose packing density.
The purpose of the invention can be realized by the following technical scheme:
a preparation process of copper powder with high-pressure billet strength and low apparent density comprises the following steps:
step one, smelting: adding electrolytic copper into a smelting furnace for smelting treatment to obtain copper liquid;
step two, dehydrogenation: cooling the copper liquid, introducing nitrogen into the copper liquid, and fishing out floating slag on the liquid level of the copper liquid to obtain purified copper liquid;
step three, atomization: spraying the purified copper liquid to obtain copper powder;
step four, vacuum drying: putting the copper powder in a vacuum drying oven for vacuum drying to obtain dried copper powder;
step five, powder mixing: adding the dried copper powder and the magnesium oxide nano powder into a mixer, and stirring and mixing to obtain mixed powder;
step six, vapor deposition: and placing the mixed powder into a quartz tube, placing the quartz tube into a CVD furnace, carrying out high-temperature heat treatment in the atmosphere of argon and hydrogen, introducing methane for carrying out gas-phase chemical deposition, cooling to room temperature to obtain high-pressure blank strength low-apparent-density copper powder, then placing the high-pressure blank strength low-apparent-density copper powder into dilute hydrochloric acid for soaking, then carrying out vacuum filtration, washing and drying a filter cake to obtain the high-pressure blank strength low-apparent-density copper powder.
As a further scheme of the invention: the smelting temperature of the electrolytic copper in the first step is 1380-1620 ℃.
As a further scheme of the invention: the cooling temperature of the copper liquid in the step two is 1150-1200 ℃, and the ratio of the copper liquid to the nitrogen is 1kg:0.8-1.6L, and the hydrogen content in the purified copper liquid is less than 2mL/kg.
As a further scheme of the invention: the pressure of the purified copper liquid spray treatment in the third step is 30-40MPa.
As a further scheme of the invention: and the vacuum drying temperature of the copper powder in the fourth step is 100-130 ℃.
As a further scheme of the invention: the mass ratio of the dried copper powder to the magnesium oxide nano powder in the fifth step is 1:3-5.
As a further scheme of the invention: in the sixth step, the argon flow is 300-350sccm, the hydrogen flow is 50-60sccm, the methane flow is 50-250sccm, and the mass fraction of the dilute hydrochloric acid is 6-10%.
The invention has the beneficial effects that:
the invention relates to a preparation process of high-pressure billet strength low-apparent density copper powder, which comprises the steps of adding electrolytic copper into a smelting furnace for smelting treatment to obtain copper liquid, cooling the copper liquid, introducing nitrogen into the copper liquid, fishing out floating slag on the liquid level of the copper liquid to obtain purified copper liquid, spraying the purified copper liquid to obtain copper powder, placing the copper powder into a vacuum drying box for vacuum drying to obtain dried copper powder, adding the dried copper powder and magnesium oxide nano powder into a mixing machine for stirring and mixing to obtain mixed powder, placing the mixed powder into a quartz tube, placing the quartz tube into a CVD furnace, carrying out high-temperature heat treatment under the atmosphere of argon and hydrogen, introducing methane for gas-phase chemical deposition, and cooling to room temperature to obtain the high-pressure billet strength low-apparent density copper powder; the preparation process utilizes spraying to form copper powder, and copper powder is prepared without adopting an electrolytic method, so that the pollution to the environment is greatly reduced, the energy consumption is low, the copper powder formed by spraying can form powder with irregular shape, the sintered copper powder has more complicated shape, the apparent density of the copper powder is reduced, graphene grows on the surface of the copper powder when the copper powder is sintered, the chemical property of the graphene is very stable, the graphene independently exists in a copper powder matrix and cannot form a solid solution with the copper powder, dislocation slippage can be hindered by the independent phases when the copper powder is subjected to external force, the properties of the material such as tensile strength, hardness and frictional wear resistance of the material can be greatly improved by the inhibition effect of dislocation, and the specific gravity of the reinforced particles is small, and the reinforced particles independently exist in the matrix, so that the copper powder graphene composite material can keep the original good thermal conductivity, the copper powder has high tensile strength, high friction and wear resistance and other performances, so that the copper powder has good mechanical properties, is suitable for preparing high-speed rail brake materials, prolongs the service life of the brake materials, and even improves the safety and reliability of high-speed rails.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a flow chart of a process for preparing copper powder with high green strength and low apparent density according to the present invention;
FIG. 2 is an SEM image of high green strength low apparent density copper powder in example 3 of the present invention;
FIG. 3 is an enlarged SEM photograph of high green strength low apparent density copper powder in example 3 of the present invention;
FIG. 4 is an SEM photograph of high green strength and low apparent density copper powder in example 1 of the present invention;
FIG. 5 is an enlarged SEM photograph of high green strength low apparent density copper powder in example 1 of the present invention;
FIG. 6 is an SEM image of copper powder of high green strength and low apparent density of comparative example 1 in accordance with the present invention;
FIG. 7 is an enlarged SEM of a high green strength low apparent density copper powder of comparative example 1 in accordance with the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
as shown in fig. 1, this embodiment is a process for preparing copper powder with high green strength and low apparent density, which comprises the following steps:
the method comprises the following steps: adding electrolytic copper into a smelting furnace, and carrying out smelting treatment at the temperature of 1380 ℃ to obtain copper liquid;
step two: cooling the copper liquid to 1150 ℃, then introducing nitrogen into the copper liquid until the hydrogen content in the copper liquid is less than 2mL/kg, and fishing out scum on the liquid level of the copper liquid to obtain purified copper liquid;
step three: spraying the purified copper liquid under the condition that the pressure is 30MPa to obtain copper powder;
step four: putting the copper powder in a vacuum drying oven, and carrying out vacuum drying for 20h at the temperature of 100 ℃ to obtain dried copper powder;
step five: adding the dried copper powder and the magnesium oxide nano powder into a mixer, and stirring and mixing for 0.5h at the temperature of 15 ℃ and the stirring speed of 3000 r/min to obtain mixed powder;
step six: placing the mixed powder into a quartz tube, placing the quartz tube into a CVD furnace, heating to 900 ℃ under the conditions that the argon flow is 300sccm and the hydrogen flow is 50sccm, controlling the heating rate to be 10 ℃/min, then preserving heat by 20 min, heating to 1050 ℃, controlling the heating rate to be 3 ℃/min, then preserving heat by 10 min, then introducing methane, preserving heat by 30 min, controlling the methane flow to be 50sccm, then stopping introducing the methane, keeping the argon flow and the hydrogen flow unchanged, cooling to room temperature under the conditions that the cooling rate is 10 ℃/min, then placing into dilute hydrochloric acid with the mass fraction of 6% for soaking for 10h, then carrying out vacuum filtration, washing a filter cake by distilled water for 3 times, then placing into a vacuum drying box, and carrying out vacuum drying for 20h under the condition that the temperature is 80 ℃ to obtain the copper powder with high-pressure blank strength and low apparent density.
Example 2:
as shown in fig. 1, this embodiment is a process for preparing copper powder with high green strength and low apparent density, which comprises the following steps:
the method comprises the following steps: adding electrolytic copper into a smelting furnace, and carrying out smelting treatment at the temperature of 1500 ℃ to obtain copper liquid;
step two: cooling the copper liquid to 1175 ℃, then introducing nitrogen into the copper liquid until the hydrogen content in the copper liquid is less than 2mL/kg, and fishing out scum on the liquid level of the copper liquid to obtain purified copper liquid;
step three: spraying the purified copper liquid under the condition that the pressure is 35MPa to obtain copper powder;
step four: putting the copper powder in a vacuum drying oven, and carrying out vacuum drying for 25h at the temperature of 115 ℃ to obtain dried copper powder;
step five: adding the dried copper powder and the magnesium oxide nano powder into a mixer, and stirring and mixing for 1.0h at the temperature of 18 ℃ and the stirring speed of 4000 r/min to obtain mixed powder;
step six: placing the mixed powder into a quartz tube, placing the quartz tube into a CVD furnace, heating to 912 ℃ under the conditions that the argon flow is 325sccm and the hydrogen flow is 55sccm, controlling the heating rate to be 12 ℃/min, then keeping the temperature for 25 min, heating to 1070 ℃, controlling the heating rate to be 4 ℃/min, then keeping the temperature for 12 min, then introducing methane, keeping the temperature for 40 min, controlling the methane flow to be 150sccm, then stopping introducing the methane, keeping the argon flow and the hydrogen flow unchanged, cooling to room temperature under the conditions that the cooling rate is 15 ℃/min, then placing into dilute hydrochloric acid with the mass fraction of 8% for soaking for 11h, then carrying out vacuum filtration, washing a filter cake for 4 times by using distilled water, then placing into a vacuum drying box, and carrying out vacuum drying for 25h under the condition that the temperature is 90 ℃ to obtain the copper powder with high-pressure blank strength and low apparent density.
Example 3:
as shown in fig. 1, this embodiment is a process for preparing copper powder with high green strength and low apparent density, which comprises the following steps:
the method comprises the following steps: adding electrolytic copper into a smelting furnace, and carrying out smelting treatment at the temperature of 1620 ℃ to obtain copper liquid;
step two: cooling the copper liquid to 1200 ℃, then introducing nitrogen into the copper liquid until the hydrogen content in the copper liquid is less than 2mL/kg, and fishing out floating slag on the liquid level of the copper liquid to obtain purified copper liquid;
step three: spraying the purified copper liquid under the condition that the pressure is 40MPa to obtain copper powder;
step four: putting the copper powder in a vacuum drying oven, and carrying out vacuum drying for 30h at the temperature of 130 ℃ to obtain dried copper powder;
step five: adding the dried copper powder and the magnesium oxide nano powder into a mixer, and stirring and mixing for 1.5 hours at the temperature of 20 ℃ and the stirring speed of 5000 r/min to obtain mixed powder;
step six: placing the mixed powder into a quartz tube, placing the quartz tube into a CVD furnace, heating to 925 ℃ under the conditions of 350sccm argon flow and 60sccm hydrogen flow, controlling the heating rate to be 15 ℃/min, then preserving heat for 30 min, heating to 1085 ℃, controlling the heating rate to be 5 ℃/min, then preserving heat for 15 min, then introducing methane, preserving heat for 50 min, controlling the methane flow to be 250sccm, then stopping introducing the methane, keeping the argon flow and the hydrogen flow unchanged, cooling to room temperature under the conditions of 20 ℃/min of the cooling rate, then placing into dilute hydrochloric acid with the mass fraction of 10% for soaking for 12h, then carrying out vacuum filtration, washing a filter cake for 5 times by using distilled water, then placing into a vacuum drying box, and carrying out vacuum drying for 30h under the condition of 100 ℃ to obtain the copper powder with high-pressure blank strength and low apparent density.
Comparative example 1:
the preparation process of the copper powder with high-pressure billet strength and low apparent density comprises the following steps:
the method comprises the following steps: adding electrolytic copper into a smelting furnace, and carrying out smelting treatment at the temperature of 1620 ℃ to obtain copper liquid;
step two: cooling the copper liquid to 1200 ℃, then introducing nitrogen into the copper liquid until the hydrogen content in the copper liquid is less than 2mL/kg, and fishing out floating slag on the liquid level of the copper liquid to obtain purified copper liquid;
step three: spraying the purified copper liquid under the condition that the pressure is 40MPa to obtain copper powder;
step four: putting the copper powder in a vacuum drying oven, and carrying out vacuum drying for 30h at the temperature of 130 ℃ to obtain dried copper powder;
step five: adding the dried copper powder and the magnesium oxide nano powder into a mixer, and stirring and mixing for 1.5 hours at the temperature of 20 ℃ and the stirring speed of 5000 r/min to obtain mixed powder;
step six: and placing the mixed powder into a quartz tube, placing the quartz tube into a CVD furnace, heating to 925 ℃ under the conditions of 350sccm argon flow and 60sccm hydrogen flow, controlling the heating rate to be 15 ℃/min, then preserving heat for 30 min, heating to 1085 ℃, controlling the heating rate to be 5 ℃/min, then preserving heat for 65 min, then maintaining the flow of argon and hydrogen unchanged, and cooling to room temperature under the condition of 20 ℃/min cooling rate to obtain the high-pressure blank low-loose-density copper powder.
Scanning the high-pressure-billet-strength low-apparent-density copper powder obtained in the example 1, the example 3 and the comparative example 1 by an electron microscope to obtain SEM pictures as shown in FIGS. 2 to 7;
as shown in fig. 2-3, fig. 2 and fig. 3 are SEM pictures of the high-pressure green-strength low-apparent-density copper powder of example 3, and fig. 3 is an enlarged schematic view of fig. 2, and it can be seen from the SEM pictures that the surface of the high-pressure green-strength low-apparent-density copper powder is smooth and flat and has texture due to the fact that the surface of the copper powder is covered with a layer of graphene;
as shown in fig. 4-5, fig. 4 and 5 are SEM pictures of the high-pressure green strength and low-apparent density copper powder of example 1, and fig. 5 is an enlarged schematic view of fig. 4, and it can be seen from the SEM pictures that the surface of the high-pressure green strength and low-apparent density copper powder begins to have unevenness and wrinkles due to the fact that the surface of the copper powder is covered by a layer of graphene, which is thinner than the graphene in example 3, and due to the difference between the thermal expansion coefficients of the graphene and the copper powder, the graphene has wrinkles or even cracks during cooling, so that the surface of the copper powder is slightly oxidized by air;
as shown in fig. 6-7, fig. 6 and 7 are SEM pictures of the high-pressure green strength low-apparent-density copper powder of comparative example 1, and fig. 5 is an enlarged schematic view of fig. 4, and it can be seen from the SEM pictures that the surface of the high-pressure green strength low-apparent-density copper powder is very rough, because the surface of the copper powder is heavily oxidized due to the absence of protection of graphene, and thus, it can be shown that graphene has a strong oxidation resistance, and can be used as a protective layer for a metal surface, mainly due to the chemical inertness and non-permeability of graphene.
The performances of examples 1 to 3 and comparative example 1 were examined and the results are shown in the following table:
| sample (I) | Example 1 | Example 2 | Example 3 | Comparative example 1 |
| Green strength, MPa | 15.5 | 16.2 | 17.1 | 6.4 |
| Bulk density, g/cm | 1.76 | 1.69 | 1.54 | 3.44 |
Referring to the data in the table, it can be seen that the copper powder after vapor deposition of graphene has a lower apparent density and a high green strength, as compared to examples 1-3 and comparative example 1.
In the description herein, references to the description of "one embodiment," "an example," "a specific example," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (7)
1. A preparation process of copper powder with high-pressure blank strength and low apparent density is characterized by comprising the following steps:
step one, smelting: adding electrolytic copper into a smelting furnace for smelting treatment to obtain copper liquid;
step two, dehydrogenation: cooling the copper liquid, introducing nitrogen into the copper liquid, and fishing out floating slag on the liquid level of the copper liquid to obtain purified copper liquid;
step three, atomization: spraying the purified copper liquid to obtain copper powder;
step four, vacuum drying: putting the copper powder in a vacuum drying oven for vacuum drying to obtain dried copper powder;
step five, powder mixing: adding the dried copper powder and the magnesium oxide nano powder into a mixer, and stirring and mixing to obtain mixed powder;
step six, vapor deposition: and placing the mixed powder into a quartz tube, placing the quartz tube into a CVD furnace, carrying out high-temperature heat treatment in the atmosphere of argon and hydrogen, introducing methane for carrying out gas-phase chemical deposition, cooling to room temperature to obtain high-pressure blank strength low-apparent-density copper powder, then placing the high-pressure blank strength low-apparent-density copper powder into dilute hydrochloric acid for soaking, then carrying out vacuum filtration, washing and drying a filter cake to obtain the high-pressure blank strength low-apparent-density copper powder.
2. The process for preparing copper powder with high green strength and low apparent density as claimed in claim 1, wherein the smelting temperature of the electrolytic copper in the first step is 1380-1620 ℃.
3. The process for preparing the copper powder with high-pressure billet strength and low apparent density as claimed in claim 1, wherein the cooling temperature of the copper liquid in the step two is 1150-1200 ℃, and the ratio of the consumption of the copper liquid to the consumption of nitrogen is 1kg:0.8-1.6L, and the hydrogen content in the purified copper liquid is less than 2mL/kg.
4. The process for preparing copper powder with high green strength and low apparent density as claimed in claim 1, wherein the pressure of the purified copper liquid spray treatment in step three is 30-40MPa.
5. The process for preparing copper powder with high green strength and low apparent density as claimed in claim 1, wherein the vacuum drying temperature of the copper powder in the fourth step is 100-130 ℃.
6. The process for preparing the copper powder with high green strength and low apparent density as claimed in claim 1, wherein the mass ratio of the dried copper powder to the magnesium oxide nano powder in the fifth step is 1:3-5.
7. The process for preparing the copper powder with high pressure billet strength and low apparent density as claimed in claim 1, wherein in the sixth step, the argon flow is 300-350sccm, the hydrogen flow is 50-60sccm, the methane flow is 50-250sccm, and the mass fraction of the dilute hydrochloric acid is 6-10%.
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| KR102324720B1 (en) * | 2020-08-26 | 2021-11-11 | 주식회사 유디 | Manufacturing method of Hydrogen functionalized Graphene-Metal composite casting materials |
| CN113897590A (en) * | 2020-06-22 | 2022-01-07 | 上海新池能源科技有限公司 | Method for growing graphene film on surface of copper powder |
| CN114974647A (en) * | 2021-02-18 | 2022-08-30 | 上海新池能源科技有限公司 | Ultrahigh-conductivity wire and cable and preparation method thereof |
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2022
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20180007700A (en) * | 2016-07-13 | 2018-01-23 | 조선대학교산학협력단 | Cu composite reinforced by 3D graphite or graphene network and preparing method thereof |
| CN110216282A (en) * | 2019-05-30 | 2019-09-10 | 上海新池能源科技有限公司 | The preparation method of acid bronze alloy contact |
| CN113897590A (en) * | 2020-06-22 | 2022-01-07 | 上海新池能源科技有限公司 | Method for growing graphene film on surface of copper powder |
| KR102324720B1 (en) * | 2020-08-26 | 2021-11-11 | 주식회사 유디 | Manufacturing method of Hydrogen functionalized Graphene-Metal composite casting materials |
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