阅读说明：本技术 一种高柔韧性石墨材质或石墨烯材质散热部件制备方法 (Preparation method of high-flexibility graphite or graphene heat dissipation component ) 是由 庞美兴 于 2021-09-08 设计创作，主要内容包括：本发明公开了一种高柔韧性石墨材质或石墨烯材质散热部件制备方法,包括以下步骤：1)对石墨或石墨烯原材进行等离子清洗；2)取包括以下重量百分比的活化剂的制备材料：硫酸10-20％,OP-10表面活性剂0.05-1％,十二烷基硫酸钠0.05-1％,余量为水；3)使用活化剂继续清洗石墨或石墨烯原材；4)去离子水清洗石墨或石墨烯原材；5)在石墨或石墨烯原材的表面进行电镀加工,形成铜膜层；6)石墨或石墨烯原材使用去离子水继续清洗；7)通过浸泡的方式在石墨或石墨烯原材上形成保护膜；8)干燥电镀了铜膜层的石墨或石墨烯原材。本发明相较于现有技术,活化剂处理后的石墨或石墨烯表面,在电镀时铜膜层结合质量好且均匀,增强制备的散热部件的柔韧性。(The invention discloses a preparation method of a high-flexibility graphite or graphene heat dissipation component, which comprises the following steps: 1) carrying out plasma cleaning on a graphite or graphene raw material; 2) taking a preparation material comprising the following activating agents in percentage by weight: 10-20% of sulfuric acid, 0.05-1% of OP-10 surfactant, 0.05-1% of sodium dodecyl sulfate and the balance of water; 3) continuously cleaning the graphite or graphene raw material by using an activating agent; 4) washing a graphite or graphene raw material by deionized water; 5) electroplating the surface of the graphite or graphene raw material to form a copper film layer; 6) continuously cleaning the graphite or graphene raw material by using deionized water; 7) forming a protective film on the graphite or graphene raw material in a soaking mode; 8) and drying the graphite or graphene raw material electroplated with the copper film layer. Compared with the prior art, the graphite or graphene surface treated by the activating agent has good and uniform copper film layer combination quality during electroplating, and the flexibility of the prepared heat dissipation component is enhanced.)

1. A preparation method of a high-flexibility graphite material or graphene material heat dissipation component is characterized by comprising the following steps:

1) carrying out plasma cleaning on a graphite or graphene raw material;

2) taking a preparation material comprising the following activating agents in percentage by weight: 10-20% of sulfuric acid, 0.05-1% of OP-10 surfactant, 0.05-1% of sodium dodecyl sulfate and the balance of water;

3) mixing the components of the activating agent to prepare the activating agent, and continuously cleaning the graphite or graphene raw material by using the activating agent;

4) continuously cleaning the graphite or graphene raw material by using deionized water;

5) electroplating the surface of the graphite or graphene raw material to form a copper film layer;

6) continuously cleaning the graphite or graphene raw material with the copper film layer plated on the surface by using deionized water;

7) forming a protective film on the graphite or graphene raw material in a soaking mode;

8) and drying the graphite or graphene raw material electroplated with the copper film layer.

2. The method for preparing a high-flexibility graphite or graphene heat dissipation component as claimed in claim 1, wherein in step 1), the graphite or graphene raw material is placed in a plasma cleaning machine for cleaning.

3. The method for preparing a high-flexibility graphite or graphene heat dissipation component as claimed in claim 1, wherein in the step 2), the activating agent comprises the following components in percentage by weight: 12 to 16 percent of sulfuric acid, 0.05 to 0.5 percent of OP-10 surfactant, 0.05 to 0.5 percent of sodium dodecyl sulfate and the balance of water.

4. The method for preparing a high-flexibility graphite or graphene heat dissipation component as claimed in claim 3, wherein in the step 2), the activating agent comprises the following components in percentage by weight: 15% of sulfuric acid, 0.1% of OP-10 surfactant, 0.1% of sodium dodecyl sulfate and the balance of water.

5. The method for preparing a high-flexibility graphite or graphene heat dissipation component as claimed in claim 1, wherein in the step 5), two electroplating processes are performed on the graphite or graphene raw material by using an electroplating solution, wherein the electroplating solution comprises the following components in percentage by weight: 5% of copper ions; 14% of sulfuric acid; 0.8% of brightener; 0.06 percent of auxiliary agent; 0.06 percent of leveling agent; the balance being water.

6. The method for manufacturing a highly flexible heat dissipating component made of graphite or graphene according to claim 5, wherein in the step 5), the first time of electroplating the graphite or graphene raw material with the electroplating solution is performed, the temperature is 40 ℃ and the time is 20 minutes; and when the electroplating liquid medicine is used for electroplating the graphite or graphene raw material for the second time, the temperature is 40 ℃, and the time is 15 minutes.

7. The method for preparing a high-flexibility graphite or graphene heat dissipation component according to claim 1, wherein in the step 6), the graphite or graphene raw material is firstly soaked in 5g/L methylbenzotriazole solution for 20-30 seconds to form a first protective film, and then is placed in 0.5g/L cetyl pyridinium bromide solution for 20-30 seconds to form a second protective film.

Technical Field

The invention belongs to the field of preparation of graphite or graphene parts, and particularly relates to a preparation method of a high-flexibility graphite or graphene heat dissipation part.

Background

Graphite is a mixture of carbon atoms in sp²The hybrid tracks form a hexagonal honeycomb lattice two-dimensional carbon nanomaterial. The graphite has very good heat conduction performance, the heat conduction coefficient of pure defect-free single-layer graphite is as high as 5300W/mK, and is the carbon material with the highest heat conduction coefficient up to now, and is higher than that of single-wall carbon nano tubes (3500W/mK) and multi-wall carbon nano tubes (3000W/m)K) In that respect When it is used as carrier, its thermal conductivity can be up to 600W/mK. In addition, the ballistic thermal conductivity of graphite may shift the lower limit of the ballistic thermal conductivity of carbon nanotubes per unit circumference and length down.

Various electronic elements in electronic products need to dissipate heat, when the traditional graphite or graphene is applied to heat dissipation of the electronic elements, a metal layer is mainly fixed on the surface of the graphite or graphene, specifically, the metal layer is fixed on the graphite or graphene in a bonding or electroplating mode, and the electroplating mode is better than the bonding mode in heat conduction efficiency.

In order to ensure the electroplating quality of the metal layer on the surface of the graphite or graphene material, a plurality of cleaning processes are generally performed on the surface of the graphite or graphene material before electroplating. In the cleaning process, after the surface of graphite or graphene is treated by using the OP-10 surfactant, the smoothness of the surface of the graphite or graphene is general, so that the bonding effect of a metal layer electroplated on the surface of the graphite or graphene is poor, the thickness of the metal layer is uneven, the flexibility of the prepared heat dissipation part is influenced, and creases are easily generated on the surface of the heat dissipation part.

Disclosure of Invention

The invention aims to: the preparation method of the high-flexibility graphite or graphene heat dissipation component comprises the steps of firstly carrying out plasma cleaning on the surface of graphite or graphene, and then treating the surface of the graphite or graphene by using an activating agent compounded by sulfuric acid, an OP-10 surfactant and sodium dodecyl sulfate, so that the surface smoothness of the material is good, the good and uniform combination quality of a copper film plated on the surface of the graphite or graphene is ensured, the flexibility of the prepared heat dissipation component is enhanced, and creases are not easily generated on the surface of the heat dissipation component.

In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of a high-flexibility graphite material or graphene material heat dissipation component comprises the following steps:

1) carrying out plasma cleaning on a graphite or graphene raw material;

2) taking a preparation material comprising the following activating agents in percentage by weight: 10-20% of sulfuric acid, 0.05-1% of OP-10 surfactant, 0.05-1% of sodium dodecyl sulfate and the balance of water;

3) mixing the components of the activating agent to prepare the activating agent, and continuously cleaning the graphite or graphene raw material by using the activating agent;

4) continuously cleaning the graphite or graphene raw material by using deionized water;

5) electroplating the surface of the graphite or graphene raw material to form a copper film layer;

6) continuously cleaning the graphite or graphene raw material with the copper film layer plated on the surface by using deionized water;

7) forming a protective film on the graphite or graphene raw material in a soaking mode;

8) and drying the graphite or graphene raw material electroplated with the copper film layer.

As a further description of the above technical solution:

in step 1), the graphite or graphene raw material is placed in a plasma cleaning machine for cleaning.

As a further description of the above technical solution:

in the step 2), the activating agent comprises the following components in percentage by weight: 12 to 16 percent of sulfuric acid, 0.05 to 0.5 percent of OP-10 surfactant, 0.05 to 0.5 percent of sodium dodecyl sulfate and the balance of water.

As a further description of the above technical solution:

in the step 2), the activating agent comprises the following components in percentage by weight: 15% of sulfuric acid, 0.1% of OP-10 surfactant, 0.1% of sodium dodecyl sulfate and the balance of water.

As a further description of the above technical solution:

in the step 5), the graphite or graphene raw material is subjected to twice electroplating processing through electroplating liquid medicine, wherein the electroplating liquid medicine comprises the following components in percentage by weight: 5% of copper ions; 14% of sulfuric acid; 0.8% of brightener; 0.06 percent of auxiliary agent; 0.06 percent of leveling agent; the balance being water.

As a further description of the above technical solution:

electroplating the graphite or graphene raw material by using electroplating liquid for the first time at 40 ℃ for 20 minutes; and when the electroplating liquid medicine is used for electroplating the graphite or graphene raw material for the second time, the temperature is 40 ℃, and the time is 15 minutes.

As a further description of the above technical solution:

in the step 6), the graphite or graphene raw material is firstly soaked in 5g/L of methylbenzotriazole solution for 20-30 seconds to form a first layer of protective film, and then is put into 0.5g/L of cetyl pyridinium bromide solution for 20-30 seconds to form a second layer of protective film.

In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:

1. in the invention, the graphite or graphene raw material is firstly placed in a plasma cleaning machine for plasma cleaning, and then the surface of the graphite or graphene is treated by using an activating agent compounded by sulfuric acid, OP-10 surfactant and sodium dodecyl sulfate. The sulfuric acid can wash off oil stains of the graphite or graphene raw material, the OP-10 surfactant improves the surface smoothness of the graphite or graphene raw material, the sodium dodecyl sulfate improves the dispersibility of the graphite or graphene, and further improves the surface smoothness of the graphite or graphene raw material, so that the electroplated copper film layer is good and uniform in combination quality, the flexibility of the prepared heat dissipation component is enhanced, creases are not easily generated on the surface of the heat dissipation component, and the heat dissipation and acid and alkali resistance of the heat dissipation component are improved.

2. According to the invention, after the copper film layer is formed on the graphite or graphene raw material by electroplating, the graphite or graphene raw material plated with the copper film layer is firstly soaked in 5g/L methyl benzotriazole solution for 20-30 seconds to form a first protective film on the copper film layer, and then is placed in 0.5g/L cetyl pyridinium bromide solution for 20-30 seconds to form a second protective film on the copper film layer, so that the copper film layer is effectively prevented from discoloring.

Detailed Description

Exemplary embodiments of the present disclosure will be described in more detail below. While exemplary embodiments of the present disclosure have been shown, it should be understood that the present disclosure may be embodied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.

The first embodiment is as follows:

the embodiment of the invention provides a preparation method of a high-flexibility graphite material or graphene material heat dissipation component, which comprises the following steps:

1) placing the graphite or graphene raw material in a plasma cleaning machine for plasma cleaning, wherein the air pressure of the plasma cleaning machine is 2MPa, the power is 550-600W, and the time is 30 minutes;

2) taking a preparation material comprising the following activating agents in percentage by weight: 15% of sulfuric acid, 0.1% of OP-10 surfactant, 0.1% of sodium dodecyl sulfate and the balance of water;

3) mixing the components of the activating agent to prepare the activating agent, and continuously cleaning the graphite or graphene raw material by using the activating agent;

4) continuously cleaning the graphite or graphene raw material by using deionized water;

5) performing electroplating processing twice on the surface of the graphite or graphene raw material to form a copper film layer;

6) continuously cleaning the graphite or graphene raw material with the copper film layer plated on the surface by using deionized water;

7) firstly, soaking a graphite or graphene raw material plated with a copper film layer in a 5g/L methyl benzotriazole solution for 20-30 seconds to form a first protective film on the copper film layer, then placing the first protective film in a 0.5g/L cetyl pyridinium bromide solution for 20-30 seconds to form a second protective film on the copper film layer, and effectively preventing the copper film layer from discoloring;

8) and drying the graphite or graphene raw material electroplated with the copper film layer.

Step 5) comprises two electroplating procedures: firstly, carrying out primary electroplating on a graphite or graphene raw material by using electroplating liquid; and secondly, carrying out secondary electroplating on the graphite or graphene raw material by using electroplating liquid. The electroplating liquid medicine comprises the following components in percentage by weight: 5% of copper ions; 14% of sulfuric acid; 0.8% of brightener; 0.06 percent of auxiliary agent; 0.06 percent of leveling agent; the balance being water. The electroplating process can be synchronously performed with acid cleaning, so that the heat dissipation part has good smoothness.

The process parameters of example one are shown in the following table:

example two

The embodiment of the invention provides a preparation method of a high-flexibility graphite material or graphene material heat dissipation component, which comprises the following steps:

1) placing the graphite or graphene raw material in a plasma cleaning machine for plasma cleaning, wherein the air pressure of the plasma cleaning machine is 2MPa, the power is 550-600W, and the time is 30 minutes;

2) taking a preparation material comprising the following activating agents in percentage by weight: 16% of sulfuric acid, 0.2% of OP-10 surfactant, 0.2% of sodium dodecyl sulfate and the balance of water;

3) mixing the components of the activating agent to prepare the activating agent, and continuously cleaning the graphite or graphene raw material by using the activating agent;

4) continuously cleaning the graphite or graphene raw material by using deionized water;

5) performing electroplating processing twice on the surface of the graphite or graphene raw material to form a copper film layer;

6) continuously cleaning the graphite or graphene raw material with the copper film layer plated on the surface by using deionized water;

7) firstly, soaking a graphite or graphene raw material plated with a copper film layer in a 5g/L methyl benzotriazole solution for 20-30 seconds to form a first protective film on the copper film layer, then placing the first protective film in a 0.5g/L cetyl pyridinium bromide solution for 20-30 seconds to form a second protective film on the copper film layer, and effectively preventing the copper film layer from discoloring;

8) and drying the graphite or graphene raw material electroplated with the copper film layer.

In summary, the method for manufacturing a high-flexibility graphite or graphene heat dissipation component provided in the embodiments has the following advantages compared to the prior art: when the copper film layer is electroplated, firstly, the graphite or graphene raw material is placed in a plasma cleaning machine for plasma cleaning, and then the surface of the graphite or graphene is treated by using an activating agent compounded by sulfuric acid, OP-10 surfactant and sodium dodecyl sulfate. The sulfuric acid can wash off oil stains of the graphite or graphene raw material, the OP-10 surfactant improves the surface smoothness of the graphite or graphene raw material, the sodium dodecyl sulfate improves the dispersibility of the graphite or graphene, and further improves the surface smoothness of the graphite or graphene raw material, so that the electroplated copper film layer is good and uniform in combination quality, the flexibility of the prepared heat dissipation component is enhanced, creases are not easily generated on the surface of the heat dissipation component, and the heat dissipation and acid and alkali resistance of the heat dissipation component are improved. After a copper film layer is formed on a graphite or graphene raw material through electroplating, the graphite or graphene raw material plated with the copper film layer is firstly soaked in a 5g/L methyl benzotriazole solution for 20-30 seconds to form a first protective film on the copper film layer, and then the first protective film is placed in a 0.5g/L cetyl pyridinium bromide solution for 20-30 seconds to form a second protective film on the copper film layer, so that the copper film layer is effectively prevented from discoloring.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.