CN110629258A - A kind of preparation method of porous copper absorbent core - Google Patents
A kind of preparation method of porous copper absorbent core Download PDFInfo
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- CN110629258A CN110629258A CN201910981893.5A CN201910981893A CN110629258A CN 110629258 A CN110629258 A CN 110629258A CN 201910981893 A CN201910981893 A CN 201910981893A CN 110629258 A CN110629258 A CN 110629258A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 38
- 239000010949 copper Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000002250 absorbent Substances 0.000 title claims description 30
- 230000002745 absorbent Effects 0.000 title claims description 28
- 239000003792 electrolyte Substances 0.000 claims abstract description 43
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000004070 electrodeposition Methods 0.000 claims abstract description 29
- 239000000758 substrate Substances 0.000 claims abstract description 29
- 238000000151 deposition Methods 0.000 claims abstract description 25
- 230000008021 deposition Effects 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 21
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 150000001875 compounds Chemical class 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 11
- 239000004094 surface-active agent Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229960003280 cupric chloride Drugs 0.000 claims 2
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 239000011148 porous material Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052801 chlorine Inorganic materials 0.000 abstract description 2
- 125000001309 chloro group Chemical group Cl* 0.000 abstract description 2
- 229910052731 fluorine Inorganic materials 0.000 abstract description 2
- 125000001153 fluoro group Chemical group F* 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 125000004430 oxygen atom Chemical group O* 0.000 abstract description 2
- 230000010287 polarization Effects 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000002659 electrodeposit Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 238000012356 Product development Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
Description
技术领域technical field
本发明涉及散热产品开发领域，具体涉及一种超薄均热板吸液芯结构及其生产工艺。The invention relates to the field of heat dissipation product development, in particular to a liquid absorbing core structure of an ultra-thin vapor chamber and a production process thereof.
背景技术Background technique
5G时代，电子设备呈现整合化、集成化和高频高速等发展趋势，内部电子芯片技术的发展，尺寸愈加缩小，功率愈加集中。半导体尺寸的缩小，热通量逐渐增加。电子产品的散热挑战愈趋严重。热管和均热板作为一种通过相变原理进行散热的器件，正在迅速应用于电子产品中，如高端智能手机，LED等产品。In the 5G era, electronic equipment has developed trends such as integration, integration, and high frequency and high speed. The development of internal electronic chip technology has reduced the size and concentrated power. As the size of the semiconductor shrinks, the heat flux gradually increases. The thermal challenges of electronic products are becoming more and more serious. As a device that dissipates heat through the principle of phase change, heat pipes and vapor chambers are rapidly being used in electronic products, such as high-end smartphones, LEDs and other products.
均热板正在加速应用于5G智能手机中。目前，均热板在制造过程中，吸液芯结构通常采用铜网或铜粉，通过烧结的方式将两者结合到一起。在成本和制造工艺角度考虑均不是最优解。随着研究人员的技术进展，逐渐开发一些原位制备吸液芯的方法，制备的多孔吸液芯结构强度非常弱，必须经过后续的进一步电流沉积强化或者烧结等方法才能将这一结构转化成具有实际应用价值的吸液芯。Vapor chambers are accelerating their adoption in 5G smartphones. At present, during the manufacturing process of the vapor chamber, the wick structure is usually made of copper mesh or copper powder, and the two are combined by sintering. It is not the optimal solution in terms of cost and manufacturing process. With the technical progress of researchers, some methods of in-situ preparation of absorbent cores have been gradually developed. The structure of the prepared porous absorbent cores is very weak, and it must be further strengthened by subsequent current deposition or sintering before this structure can be converted into Absorbent wick with practical application value.
发明内容SUMMARY OF THE INVENTION
本发明提供了一种多孔铜吸液芯的制备方法，能够解决上述现有技术问题中的一种或几种。The present invention provides a method for preparing a porous copper liquid absorbent core, which can solve one or more of the above problems in the prior art.
根据本发明的一个方面，提供了一种多孔铜吸液芯的制备方法，包括，According to one aspect of the present invention, there is provided a method for preparing a porous copper absorbent core, comprising:
A、配置电沉积电解液，电解液为氯化铜和盐酸的水溶液；A. Electrodeposition electrolyte is configured, and the electrolyte is an aqueous solution of copper chloride and hydrochloric acid;
B、对基底表面进行清洗；和，B. cleaning the surface of the substrate; and,
C、将处理后的基底在电解液中进行电沉积，得到多孔铜吸液芯。C. The treated substrate is electrodeposited in the electrolyte to obtain a porous copper absorbent core.
其有益效果是，氯原子的电负性极强，仅次于氟原子和氧原子。在电沉积过程中可以对基底进行活化，减弱极化作用，便可在减少氢气在孔壁结构中的产生，使得沉积得到的多孔壁得到强化。Its beneficial effect is that the electronegativity of the chlorine atom is extremely strong, second only to the fluorine atom and the oxygen atom. During the electrodeposition process, the substrate can be activated to weaken the polarization, which can reduce the generation of hydrogen in the pore wall structure, so that the deposited porous wall can be strengthened.
在一些实施方式中，步骤A中的电解液中，氯化铜的浓度为0.05-0.5mol/L，盐酸的浓度为1.0-2.0mol/L。浓度过低，沉积效果不明显，无法获得多孔结构。铜离子浓度过高，沉积比例过大，易形成致密薄膜；氢离子浓度过高，气泡生成速率过大，无法获得三维状态的孔隙结构。In some embodiments, in the electrolyte in step A, the concentration of copper chloride is 0.05-0.5 mol/L, and the concentration of hydrochloric acid is 1.0-2.0 mol/L. If the concentration is too low, the deposition effect is not obvious, and the porous structure cannot be obtained. If the copper ion concentration is too high, the deposition ratio is too large, and it is easy to form a dense film; if the hydrogen ion concentration is too high, the bubble generation rate is too large, and a three-dimensional pore structure cannot be obtained.
其有益效果是，本发明通过电化学沉积原理，提供了一种制备多孔铜吸液芯的配方，并在金属表面原位生长一层厚度可调，强度较高的多孔金属结构。这一方法可以灵活设计均热板的吸液芯结构，相对于现有技术中还需进一步电流沉积强化或者烧结等方法才能将这一结构转化成具有实际应用价值的吸液芯，本发明中的到的多孔铜吸液芯具有显著的降本增效的效果。The beneficial effect is that the invention provides a formula for preparing a porous copper liquid absorbent core through the principle of electrochemical deposition, and grows a layer of porous metal structure with adjustable thickness and high strength in situ on the metal surface. This method can flexibly design the liquid-absorbent core structure of the vapor chamber. Compared with the prior art, further methods such as current deposition strengthening or sintering are required to convert this structure into a liquid-absorbent core with practical application value. The obtained porous copper absorbent core has a significant effect of reducing cost and increasing efficiency.
在一些实施方式中，步骤A中的电解液中，电解液中盐酸和氯化铜的摩尔浓度比为2:1-40:1。In some embodiments, in the electrolyte in step A, the molar concentration ratio of hydrochloric acid and copper chloride in the electrolyte is 2:1-40:1.
在一些实施方式中，步骤B包括，采用表面活性剂和碱性化合物的混合溶液对基底表面进行清洗，再用去离子水清洗干净。其有益效果是，清洗基体表面，除去几天表面杂质。In some embodiments, step B includes cleaning the surface of the substrate with a mixed solution of a surfactant and an alkaline compound, and then cleaning with deionized water. Its beneficial effect is to clean the surface of the substrate and remove surface impurities for several days.
在一些实施方式中，步骤C中，的电沉积的电流密度为0.3-2A/cm2。其有益效果是，可根据需要控制电流密度，从而控制多孔铜吸液芯的形貌结构。电流密度过高，沉积速率及电解液流动行为不易控制，无法获得有规律的多孔结构；电流密度过低，沉积速率慢，无实用价值。In some embodiments, in step C, the current density of the electrodeposition is 0.3-2 A/cm 2 . The beneficial effect is that the current density can be controlled as required, so as to control the morphology and structure of the porous copper liquid-absorbing core. If the current density is too high, the deposition rate and the flow behavior of the electrolyte are not easy to control, and a regular porous structure cannot be obtained; if the current density is too low, the deposition rate is slow and has no practical value.
在一些实施方式中，步骤C中，的电沉积的电流密度为0.5-1.0A/cm2。In some embodiments, in step C, the current density of the electrodeposition is 0.5-1.0 A/cm 2 .
在一些实施方式中，步骤C中，沉积时间为20-300s。In some embodiments, in step C, the deposition time is 20-300s.
在一些实施方式中，步骤C中，沉积时间为30-100s。In some embodiments, in step C, the deposition time is 30-100s.
附图说明Description of drawings
图1为实施例1得到的多孔结构的铜吸液芯的孔隙率与沉积时间的关系曲线图。FIG. 1 is a graph showing the relationship between the porosity of the copper absorbent core with porous structure obtained in Example 1 and the deposition time.
具体实施方式Detailed ways
下面结合实施例对本发明作进一步详细的说明。The present invention will be described in further detail below in conjunction with the embodiments.
实施例1Example 1
本实施例提供了一种多孔铜吸液芯的制备方法，包括，This embodiment provides a method for preparing a porous copper absorbent core, comprising:
A、配置电沉积电解液，电解液为0.1mol/L氯化铜和1.0mol/L盐酸的水溶液；A, configure the electrodeposition electrolyte, the electrolyte is the aqueous solution of 0.1mol/L copper chloride and 1.0mol/L hydrochloric acid;
B、采用表面活性剂和碱性化合物的混合溶液对基底表面进行清洗，并用去离子水清洗干净；B. Use the mixed solution of surfactant and alkaline compound to clean the substrate surface, and clean it with deionized water;
C、将处理后的基底在电解液中进行电沉积，电沉积的电流密度为0.8A/cm2，沉积时间为20-180s得到多孔铜吸液芯。多孔结构的孔隙率与沉积时间的关系曲线如附图1所示。由图可知，沉积时间为20s时，产品孔隙率达到50％左右；沉积时间30s时，成品孔隙率可达60％以上；待沉积时间50s以后，孔隙率可达80％左右，基本上达到上限，形成了强度稳定的多孔结构。C. The treated substrate is electrodeposited in an electrolyte, the current density of electrodeposition is 0.8A/cm 2 , and the deposition time is 20-180s to obtain a porous copper liquid absorbing core. The relationship between the porosity of the porous structure and the deposition time is shown in Figure 1. It can be seen from the figure that when the deposition time is 20s, the porosity of the product reaches about 50%; when the deposition time is 30s, the porosity of the finished product can reach more than 60%; after the deposition time is 50s, the porosity can reach about 80%, basically reaching the upper limit. , forming a porous structure with stable strength.
实施例2Example 2
本实施例提供了一种多孔铜吸液芯的制备方法，包括，This embodiment provides a method for preparing a porous copper absorbent core, comprising:
A、配置电沉积电解液，电解液为0.5mol/L氯化铜和2.0mol/L盐酸的水溶液；A, configure the electrodeposition electrolyte, the electrolyte is the aqueous solution of 0.5mol/L copper chloride and 2.0mol/L hydrochloric acid;
B、采用表面活性剂和碱性化合物的混合溶液对基底表面进行清洗，并用去离子水清洗干净；B. Use the mixed solution of surfactant and alkaline compound to clean the substrate surface, and clean it with deionized water;
C、将处理后的基底在电解液中进行电沉积，电沉积的电流密度为2A/cm2，沉积时间为300s得到多孔铜吸液芯。C. The treated substrate is electrodeposited in an electrolyte, the current density of electrodeposition is 2A/cm 2 , and the deposition time is 300s to obtain a porous copper wick.
实施例3Example 3
本实施例提供了一种多孔铜吸液芯的制备方法，包括，This embodiment provides a method for preparing a porous copper absorbent core, comprising:
A、配置电沉积电解液，电解液为0.05mol/L氯化铜和1.0mol/L盐酸的水溶液；A, configure the electrodeposition electrolyte, the electrolyte is the aqueous solution of 0.05mol/L copper chloride and 1.0mol/L hydrochloric acid;
B、采用表面活性剂和碱性化合物的混合溶液对基底表面进行清洗，并用去离子水清洗干净；B. Use the mixed solution of surfactant and alkaline compound to clean the substrate surface, and clean it with deionized water;
C、将处理后的基底在电解液中进行电沉积，电沉积的电流密度为1A/cm2，沉积时间为100s得到多孔铜吸液芯。C. Electrodeposit the treated substrate in the electrolyte, the current density of the electrodeposition is 1A/cm 2 , and the deposition time is 100s to obtain a porous copper wick.
实施例4Example 4
本实施例提供了一种多孔铜吸液芯的制备方法，包括，This embodiment provides a method for preparing a porous copper absorbent core, comprising:
A、配置电沉积电解液，电解液为0.05mol/L氯化铜和1.0mol/L盐酸的水溶液；A, configure the electrodeposition electrolyte, the electrolyte is the aqueous solution of 0.05mol/L copper chloride and 1.0mol/L hydrochloric acid;
B、采用表面活性剂和碱性化合物的混合溶液对基底表面进行清洗，并用去离子水清洗干净；B. Use the mixed solution of surfactant and alkaline compound to clean the substrate surface, and clean it with deionized water;
C、将处理后的基底在电解液中进行电沉积，电沉积的电流密度为2A/cm2，沉积时间为200s得到多孔铜吸液芯。C. The treated substrate is electrodeposited in an electrolyte, the current density of electrodeposition is 2A/cm 2 , and the deposition time is 200s to obtain a porous copper wick.
实施例5Example 5
本实施例提供了一种多孔铜吸液芯的制备方法，包括，This embodiment provides a method for preparing a porous copper absorbent core, comprising:
A、配置电沉积电解液，电解液为0.1mol/L氯化铜和2mol/L盐酸的水溶液；A, configure the electrodeposition electrolyte, the electrolyte is the aqueous solution of 0.1mol/L copper chloride and 2mol/L hydrochloric acid;
B、采用表面活性剂和碱性化合物的混合溶液对基底表面进行清洗，并用去离子水清洗干净；B. Use the mixed solution of surfactant and alkaline compound to clean the substrate surface, and clean it with deionized water;
C、将处理后的基底在电解液中进行电沉积，电沉积的电流密度为2A/cm2，沉积时间为300s得到多孔铜吸液芯。C. The treated substrate is electrodeposited in an electrolyte, the current density of electrodeposition is 2A/cm 2 , and the deposition time is 300s to obtain a porous copper wick.
实施例6Example 6
本实施例提供了一种多孔铜吸液芯的制备方法，包括，This embodiment provides a method for preparing a porous copper absorbent core, comprising:
A、配置电沉积电解液，电解液为0.5mol/L氯化铜和2.0mol/L盐酸的水溶液；A, configure the electrodeposition electrolyte, the electrolyte is the aqueous solution of 0.5mol/L copper chloride and 2.0mol/L hydrochloric acid;
B、采用表面活性剂和碱性化合物的混合溶液对基底表面进行清洗，并用去离子水清洗干净；B. Use the mixed solution of surfactant and alkaline compound to clean the substrate surface, and clean it with deionized water;
C、将处理后的基底在电解液中进行电沉积，电沉积的电流密度为1A/cm2，沉积时间为100s得到多孔铜吸液芯。C. Electrodeposit the treated substrate in the electrolyte, the current density of the electrodeposition is 1A/cm 2 , and the deposition time is 100s to obtain a porous copper wick.
实施例7Example 7
本实施例提供了一种多孔铜吸液芯的制备方法，包括，This embodiment provides a method for preparing a porous copper absorbent core, comprising:
A、配置电沉积电解液，电解液为0.5mol/L氯化铜和2.0mol/L盐酸的水溶液；A, configure the electrodeposition electrolyte, the electrolyte is the aqueous solution of 0.5mol/L copper chloride and 2.0mol/L hydrochloric acid;
B、采用表面活性剂和碱性化合物的混合溶液对基底表面进行清洗，并用去离子水清洗干净；B. Use the mixed solution of surfactant and alkaline compound to clean the substrate surface, and clean it with deionized water;
C、将处理后的基底在电解液中进行电沉积，电沉积的电流密度为2A/cm2，沉积时间为200s得到多孔铜吸液芯。C. The treated substrate is electrodeposited in an electrolyte, the current density of electrodeposition is 2A/cm 2 , and the deposition time is 200s to obtain a porous copper wick.
实施例8Example 8
本实施例提供了一种多孔铜吸液芯的制备方法，包括，This embodiment provides a method for preparing a porous copper absorbent core, comprising:
A、配置电沉积电解液，电解液为0.5mol/L氯化铜和2mol/L盐酸的水溶液；A, configure electrodeposition electrolyte, the electrolyte is the aqueous solution of 0.5mol/L copper chloride and 2mol/L hydrochloric acid;
B、采用表面活性剂和碱性化合物的混合溶液对基底表面进行清洗，并用去离子水清洗干净；B. Use the mixed solution of surfactant and alkaline compound to clean the substrate surface, and clean it with deionized water;
C、将处理后的基底在电解液中进行电沉积，电沉积的电流密度为2A/cm2，沉积时间为300s得到多孔铜吸液芯。C. The treated substrate is electrodeposited in an electrolyte, the current density of electrodeposition is 2A/cm 2 , and the deposition time is 300s to obtain a porous copper wick.
实施例9Example 9
本实施例提供了一种多孔铜吸液芯的制备方法，包括，This embodiment provides a method for preparing a porous copper absorbent core, comprising:
A、配置电沉积电解液，电解液为0.5mol/L氯化铜和2mol/L盐酸的水溶液；A, configure electrodeposition electrolyte, the electrolyte is the aqueous solution of 0.5mol/L copper chloride and 2mol/L hydrochloric acid;
B、采用表面活性剂和碱性化合物的混合溶液对基底表面进行清洗，并用去离子水清洗干净；B. Use the mixed solution of surfactant and alkaline compound to clean the substrate surface, and clean it with deionized water;
C、将处理后的基底在电解液中进行电沉积，电沉积的电流密度为0.5A/cm2，沉积时间为300s得到多孔铜吸液芯。C. The treated substrate is electrodeposited in an electrolyte, the current density of electrodeposition is 0.5A/cm 2 , and the deposition time is 300s to obtain a porous copper wick.
以上所述的仅是本发明的一些实施方式。对于本领域的普通技术人员来说，在不脱离本发明创造构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。The foregoing are merely some of the embodiments of the present invention. For those of ordinary skill in the art, without departing from the inventive concept of the present invention, several modifications and improvements can be made, which all belong to the protection scope of the present invention.
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