WO2021259030A1 - Production method for liquid crystal polymer flexible copper-clad laminate - Google Patents

Production method for liquid crystal polymer flexible copper-clad laminate Download PDF

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Publication number
WO2021259030A1
WO2021259030A1 PCT/CN2021/098040 CN2021098040W WO2021259030A1 WO 2021259030 A1 WO2021259030 A1 WO 2021259030A1 CN 2021098040 W CN2021098040 W CN 2021098040W WO 2021259030 A1 WO2021259030 A1 WO 2021259030A1
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WIPO (PCT)
Prior art keywords
liquid crystal
crystal polymer
copper
clad laminate
turbulent
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PCT/CN2021/098040
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French (fr)
Chinese (zh)
Inventor
房兰霞
郭建君
虞成城
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深圳市信维通信股份有限公司
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Publication of WO2021259030A1 publication Critical patent/WO2021259030A1/en

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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
    • H05K3/022—Processes for manufacturing precursors of printed circuits, i.e. copper-clad substrates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/14—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by electrical means
    • B05D3/141—Plasma treatment
    • B05D3/145—After-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
    • B05D7/04—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber to surfaces of films or sheets

Definitions

  • the invention relates to the field of communication technology, and in particular to a method for preparing a liquid crystal polymer turbulent copper clad laminate.
  • 5G refers to 5th-Generation, the fifth-generation mobile communication network. Its outstanding feature is that the theoretical peak transmission speed can reach tens of Gb per second, which is hundreds of times faster than the transmission speed of the 4G network.
  • the carrier of 5G signal transmission is the antenna, which is like a road, providing a channel for information exchange. In order to achieve high-efficiency transmission speed, high requirements must be put forward for the signal transmission and reception capabilities of the carrier antenna.
  • the current mainstream 4G LTE technology belongs to the category of UHF and UHF, that is, the frequency is in the range of 0.3 to 30 GHz. 5G has the highest frequency, which is divided into two types: below 6GHz and above 24GHz. The ongoing 5G technology trials are mainly carried out at 28 GHz.
  • LCP film is a new type of thermoplastic organic material that can achieve high-frequency and high-speed transmission under the premise of ensuring high reliability.
  • LCP film has excellent performance characteristics: 1. Almost a constant dielectric constant in the entire radio frequency range up to 110 GHz, with good stability; 2. The loss tangent Df value is very small, only 0.002 at 10 GHz, even at 110 GHz It only increases to 0.0045, which is very suitable for millimeter wave applications; 3. Low moisture absorption (moisture absorption rate is about 0.01% ⁇ 0.02%, only 1/10 of the general PI substrate), which makes it have a good substrate and high reliability, which can be used as Ideal high-frequency FCCL material.
  • the technical problem to be solved by the present invention is to provide a method for preparing a liquid crystal polymer turbulent copper clad laminate, which can realize the processing and production of fine lines (line pitch 30 ⁇ m).
  • a method for preparing a liquid crystal polymer turbulent copper clad laminate coating an LCP solution on a substrate layer used to make a liquid crystal polymer film, and then sequentially performing curing treatment and annealing treatment to obtain a liquid crystal polymer film; Plasma activation treatment is performed on the polymer film; copper is deposited on the surface of the liquid crystal polymer film after plasma activation treatment to obtain a liquid crystal polymer film with a nano-level conductive copper layer; continuous copper plating is performed on the nano-level conductive copper layer , The liquid crystal polymer turbulent copper clad laminate is obtained.
  • the beneficial effects of the present invention are: first coat the LCP solution on the substrate layer to obtain a liquid crystal polymer film, the thickness of the liquid crystal polymer film can be controlled at about 6 ⁇ m; plasma activation treatment can increase the peeling strength of the copper layer and improve Product reliability; the roughness of the nano-level conductive copper layer is low, which can meet the needs of high-frequency and high-speed transmission; the thickness of the copper layer of the final liquid crystal polymer turbulent copper clad laminate can be controlled at about 3 ⁇ m (total thickness is about 9 ⁇ m), It can meet the development needs of miniaturization and thin filming of the device, and can realize the processing and production of fine lines (line pitch 30 ⁇ m) through the semi-additive process.
  • Figure 1 is an SEM image of a circuit prepared by an etching process of an existing electrolytic copper copper clad laminate
  • FIG. 3 is a circuit slice diagram of the liquid crystal polymer turbulent copper clad laminate prepared in the third embodiment of the present invention, which is prepared through an etching process.
  • the most critical idea of the present invention is: first forming a liquid crystal polymer film, and then copper plating, the thickness of the copper layer of the liquid crystal polymer turbulent copper clad laminate can be controlled to about 3 ⁇ m, and the processing of fine lines (line pitch 30 ⁇ m) can be realized Make.
  • a method for preparing a liquid crystal polymer turbulent copper clad laminate coating an LCP solution on a substrate layer used to make a liquid crystal polymer film, and then sequentially performing curing treatment and annealing treatment to obtain a liquid crystal polymer film; Plasma activation treatment is performed on the polymer film; copper is deposited on the surface of the liquid crystal polymer film after plasma activation treatment to obtain a liquid crystal polymer film with a nano-level conductive copper layer; continuous copper plating is performed on the nano-level conductive copper layer , The liquid crystal polymer turbulent copper clad laminate is obtained.
  • the beneficial effects of the present invention are: first coat the LCP solution on the substrate layer to obtain a liquid crystal polymer film, the thickness of the liquid crystal polymer film can be controlled at about 6 ⁇ m; plasma activation treatment can improve the copper layer High peel strength, improve product reliability; nano-scale conductive copper layer has low roughness, which can meet the needs of high-frequency and high-speed transmission; the thickness of the copper layer of the final liquid crystal polymer turbulent copper clad laminate can be controlled at about 3 ⁇ m (total thickness It is about 9 ⁇ m), which can meet the development needs of device miniaturization and thin film. After semi-additive process, it can realize the processing and production of fine lines (line pitch 30 ⁇ m).
  • the temperature of the annealing treatment is 150 to 250° C., and the time is 1 to 5 h.
  • the gas flow rate of the plasma activation treatment is 3-7SLM
  • the activation temperature is 80-120°C
  • the activation power is 7-13kW.
  • the current density of the continuous copper plating is 1 to 5 ASD, and the time is 4 to 15 minutes.
  • the material of the base material layer is PTFE, and the thickness of the base material layer is 30-70 ⁇ m.
  • the thickness of the liquid crystal polymer film is greater than or equal to 6 ⁇ m.
  • the thickness of the liquid crystal polymer film can be controlled as required, and the minimum thickness is about 6 ⁇ m.
  • the thickness of the nano-scale conductive copper layer is 20-100 nm.
  • the thickness of the copper layer of the liquid crystal polymer turbulent copper clad laminate is greater than or equal to 3 ⁇ m.
  • a semiconductor process is used to deposit copper on the surface of the liquid crystal polymer film after plasma activation treatment.
  • the first embodiment of the present invention is a method for preparing a liquid crystal polymer turbulent copper clad laminate, which includes the following steps:
  • the material of the substrate layer is PTFE
  • the thickness of the substrate layer is 30-70 ⁇ m
  • the substrate layer may be a continuous roll material.
  • the curing treatment is to remove the solvent in the LCP solution and heat curing can be carried out.
  • the temperature of the annealing treatment is 150 to 250° C., and the time is 1 to 5 h.
  • the thickness of the finally obtained liquid crystal polymer film is greater than or equal to 6 ⁇ m. When a liquid crystal polymer film of about 6 ⁇ m needs to be obtained, the coating thickness of the LCP solution is about 8 ⁇ m.
  • the gas flow rate of the plasma activation treatment is 3 ⁇ 7SLM, the activation temperature is 80 ⁇ 120°C, and the activation power is 7 ⁇ 13kW.
  • the plasma activation treatment can increase the surface activity of the liquid crystal polymer film and improve the nano-level conductivity. The peel strength between the copper layer and the liquid crystal polymer film.
  • Copper is deposited on the surface of the liquid crystal polymer film after plasma activation treatment to obtain a liquid crystal polymer film with a nano-level conductive copper layer.
  • a semiconductor process is used to deposit copper on the surface of the liquid crystal polymer film after plasma activation treatment, and the thickness of the nano-scale conductive copper layer is 20-100 nm.
  • the current density of the continuous copper plating is 1 to 5 ASD, and the time is 4 to 15 minutes.
  • the thickness of the copper layer of the liquid crystal polymer turbulent copper clad laminate is greater than or equal to 3 ⁇ m.
  • the second embodiment of the present invention is a method for preparing a liquid crystal polymer turbulent copper clad laminate.
  • the difference from the first embodiment is:
  • step 1 the thickness of the substrate layer is 50 ⁇ m; the temperature of the annealing treatment is 200° C. and the time is 3 hours. The thickness of the finally obtained liquid crystal polymer film was 6 ⁇ m.
  • step 2 the gas flow rate of the plasma activation treatment is 5 SLM, the activation temperature is 100° C., and the activation power is 10 kW.
  • the thickness of the nano-scale conductive copper layer is 60 nm.
  • step 4 the current density of continuous copper plating is 3 ASD, the time is 4.5 min, and the thickness of the copper layer of the finally obtained liquid crystal polymer turbulent copper clad laminate is 3 ⁇ m.
  • the third embodiment of the present invention is a method for preparing a liquid crystal polymer turbulent copper clad laminate.
  • the difference from the first embodiment is:
  • step 1 the thickness of the substrate layer is 40 ⁇ m; the temperature of the annealing treatment is 150° C. and the time is 5 hours. The thickness of the finally obtained liquid crystal polymer film was 6 ⁇ m.
  • step 2 the gas flow rate of the plasma activation treatment is 3SLM, the activation temperature is 120°C, and the activation power is 7kW.
  • the thickness of the nano-scale conductive copper layer is 20 nm.
  • step 4 the current density of continuous copper plating is 2 ASD and the time is 7 min.
  • the thickness of the copper layer of the finally obtained liquid crystal polymer turbulent copper clad laminate is about 3 ⁇ m.
  • the fourth embodiment of the present invention is a preparation method of a liquid crystal polymer turbulent copper clad laminate.
  • the difference from the first embodiment is:
  • step 1 the thickness of the substrate layer is 70 ⁇ m; the temperature of the annealing treatment is 250° C. and the time is 1 h. The thickness of the finally obtained liquid crystal polymer film was 6 ⁇ m.
  • step 2 the gas flow rate of the plasma activation treatment is 7SLM, the activation temperature is 80°C, and the activation power is 13kW.
  • the thickness of the nano-scale conductive copper layer is 100 nm.
  • step 4 the current density of continuous copper plating is 5 ASD and the time is 3 min.
  • the thickness of the copper layer of the finally obtained liquid crystal polymer turbulent copper clad laminate is about 3 ⁇ m.
  • liquid crystal polymer films prepared in Examples 2 to 4 were subjected to peel strength, dimensional stability, solder mask test, elastic modulus, expansion coefficient, dielectric constant, loss factor, water absorption, flame retardancy and roughness. Degree test. The test results are shown in Table 1:
  • the peeling strength of the turbulent copper clad laminate prepared by laminating the liquid crystal polymer film and the copper foil is about 0.51N/mm, while the peeling strength of the turbulent copper clad laminate prepared by the present invention is 0.6N/mm. Above mm, the reliability of the product can be greatly improved.
  • the liquid crystal polymer turbulent copper clad laminate prepared by the present invention has better dimensional stability, excellent solder resist performance, higher elastic modulus, low expansion coefficient, excellent dielectric properties and resistance. Combustion performance.
  • the rolled copper (RA) on the market (such as Mitsui, the model is 3EC-M2S-HTE, the rolled copper foil with a thickness of 12um) has an Ra of about 0.087 ⁇ m, Rz of about 0.75 ⁇ m, and electrolytic copper ( ED) Ra is about 0.282 ⁇ m, and Rz is about 1.872 ⁇ m.
  • the surface roughness of the copper layer prepared by the present invention is much lower than that of rolled copper and electrolytic copper on the market, and can meet the requirements of high-frequency and high-speed transmission.
  • Figure 1 is the SEM image of the circuit prepared by the etching process of the electrolytic copper copper clad laminate
  • Figure 2 is the SEM image of the circuit prepared by the etching process of the liquid crystal polymer turbulent copper clad laminate prepared in Example 2 of the present invention, as can be seen from the figure It is found that the surface of the etched circuit of electrolytic copper is rough, while the surface of the etched circuit of the present invention is smooth, and the combination between the copper layer and the liquid crystal polymer film is better.
  • the test results of the third embodiment and the fourth embodiment are similar, and will not be repeated here.
  • Figure 3 is a circuit slice diagram of the liquid crystal polymer turbulent copper clad laminate prepared by the etching process in the third embodiment of the present invention. It can be seen from the figure that the line width is 60.99 ⁇ m (approximately 61 ⁇ m), and the line spacing is 25.93 ⁇ m (approximately 26 ⁇ m), it can be seen that the preparation method of the liquid crystal polymer turbulent copper clad laminate may achieve fine line processing with a line pitch of about 30 ⁇ m.
  • the method for preparing liquid crystal polymer turbulent copper clad laminates provided by the present invention has good reliability, small overall thickness, and can realize the processing and production of fine lines (line pitch 30 ⁇ m).

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Abstract

Disclosed in the present invention is a production method for a liquid crystal polymer flexible copper-clad laminate: coating, with an LCP solution, a base material layer which is used for producing a liquid crystal polymer film, and then sequentially carrying out curing treatment and annealing treatment to obtain the liquid crystal polymer film; carrying out plasma activation treatment on the liquid crystal polymer film; carrying out electroless copper plating on the surface of the liquid crystal polymer film subjected to the plasma activation treatment to obtain a liquid crystal polymer film having a nanoscale conductive copper layer; and continuously plating copper on the nanoscale conductive copper layer to obtain the liquid crystal polymer flexible copper-clad laminate. The product produced in the present invention is good in reliability and small in overall thickness, and can realize processing and manufacturing of a fine line (the line spacing is 30 microns).

Description

液晶聚合物扰性覆铜板的制备方法Method for preparing liquid crystal polymer disturbing copper clad laminate 技术领域Technical field
本发明涉及通信技术领域，尤其涉及一种液晶聚合物扰性覆铜板的制备方法。The invention relates to the field of communication technology, and in particular to a method for preparing a liquid crystal polymer turbulent copper clad laminate.
背景技术Background technique
5G代指5th-Generation，第5代移动通信网络，其突出特点为理论峰值传输速度可达每秒数十Gb，比4G网络的传输速度快数百倍。5G信号传输的载体是天线，天线就如同公路一样，提供的是信息交互的通道。想要达到高效的传输速度，对于载体天线的信号收发能力势必要提出高的要求。目前主流的4G LTE技术属于特高频和超高频的范畴，即频率在0.3～30GHz范围。5G的频率最高，分为6GHz以下和24GHz以上两种。现在正在进行的5G技术试验主要在28GHz进行。5G refers to 5th-Generation, the fifth-generation mobile communication network. Its outstanding feature is that the theoretical peak transmission speed can reach tens of Gb per second, which is hundreds of times faster than the transmission speed of the 4G network. The carrier of 5G signal transmission is the antenna, which is like a road, providing a channel for information exchange. In order to achieve high-efficiency transmission speed, high requirements must be put forward for the signal transmission and reception capabilities of the carrier antenna. The current mainstream 4G LTE technology belongs to the category of UHF and UHF, that is, the frequency is in the range of 0.3 to 30 GHz. 5G has the highest frequency, which is divided into two types: below 6GHz and above 24GHz. The ongoing 5G technology trials are mainly carried out at 28 GHz.
由于电磁波具有频率越高，波长越短，越容易在传播介质中衰减的特点，频率越高，要求天线材料的损耗越小。随着天线技术的升级，天线材料变得越来越多样。最早的天线由铜和合金等金属制成，后来随着FPC工艺的出现，4G时代的天线制造材料开始采用PI膜（聚酰亚胺）FCCL。但PI在10GHz以上损耗明显，无法满足5G终端的需求，凭借介质损耗与导体损耗更小，具备灵活性、密封性等特性，LCP（Liquid Crystal Polymer，液晶聚合物）高性能柔性覆铜板逐渐得到应用。Since electromagnetic waves have the characteristics of higher frequency and shorter wavelength, the easier it is to attenuate in the propagation medium. The higher the frequency, the smaller the loss of the antenna material is required. With the upgrading of antenna technology, antenna materials have become more and more diverse. The earliest antennas were made of metals such as copper and alloys. Later, with the advent of the FPC process, the antenna manufacturing materials in the 4G era began to use PI film (polyimide) FCCL. However, PI has obvious loss above 10GHz, which cannot meet the needs of 5G terminals. With smaller dielectric loss and conductor loss, flexibility, sealing and other characteristics, LCP (Liquid Crystal Polymer, liquid crystal polymer) high-performance flexible copper clad laminates are gradually being used.
LCP薄膜是一种新型热塑性有机材料，可在保证较高可靠性的前提下实现高频高速传输。LCP薄膜具有优异的性能特征：1、在高达110GHz的全部射频范围几乎均能保持恒定的介电常数，稳定性好；2、损耗正切Df值非常小，10GHz时仅为0.002，即使在110GHz时也仅增加到0.0045，非常适合毫米波应用；3、低吸湿性（吸湿率约为0.01%~0.02%，只有一般PI基材的1/10）使其具有良好的基板高可靠性，可作为理想的高频FCCL材料。LCP film is a new type of thermoplastic organic material that can achieve high-frequency and high-speed transmission under the premise of ensuring high reliability. LCP film has excellent performance characteristics: 1. Almost a constant dielectric constant in the entire radio frequency range up to 110 GHz, with good stability; 2. The loss tangent Df value is very small, only 0.002 at 10 GHz, even at 110 GHz It only increases to 0.0045, which is very suitable for millimeter wave applications; 3. Low moisture absorption (moisture absorption rate is about 0.01%~0.02%, only 1/10 of the general PI substrate), which makes it have a good substrate and high reliability, which can be used as Ideal high-frequency FCCL material.
随着IT技术的发展，在装置的小型化及薄膜化加速的同时，LCP薄膜化市场需求正在增加，然而目前市面上常见的LCP薄膜厚度在25μm以上。且目前FPC产品朝着精细线路发展，需要细线距（50μm以下），现市面上的具有12μm厚铜层的LCP-FCCL无法满足精细线路的制作需求。With the development of IT technology, while the miniaturization and thinning of devices are accelerating, the market demand for LCP thin film is increasing. However, the thickness of the common LCP film on the market is above 25 μm. In addition, FPC products are currently developing towards fine circuits, requiring fine line spacing (below 50μm). The current LCP-FCCL with a 12μm thick copper layer on the market cannot meet the requirements for fine circuit production.
技术问题technical problem
本发明所要解决的技术问题是：提供一种液晶聚合物扰性覆铜板的制备方法，可实现精细线路（线距30μm）的加工制作。The technical problem to be solved by the present invention is to provide a method for preparing a liquid crystal polymer turbulent copper clad laminate, which can realize the processing and production of fine lines (line pitch 30 μm).
技术解决方案Technical solutions
为了解决上述技术问题，本发明采用的技术方案为：In order to solve the above technical problems, the technical solutions adopted by the present invention are:
一种液晶聚合物扰性覆铜板的制备方法，在用于制作液晶聚合物薄膜的基材层上涂布LCP溶液，然后依次进行固化处理和退火处理，得到液晶聚合物薄膜；将所述液晶聚合物薄膜进行等离子活化处理；在等离子活化处理后的液晶聚合物薄膜的表面进行沉铜，得到具有纳米级导电铜层的液晶聚合物薄膜；在所述纳米级导电铜层上进行连续镀铜，得到所述液晶聚合物扰性覆铜板。A method for preparing a liquid crystal polymer turbulent copper clad laminate, coating an LCP solution on a substrate layer used to make a liquid crystal polymer film, and then sequentially performing curing treatment and annealing treatment to obtain a liquid crystal polymer film; Plasma activation treatment is performed on the polymer film; copper is deposited on the surface of the liquid crystal polymer film after plasma activation treatment to obtain a liquid crystal polymer film with a nano-level conductive copper layer; continuous copper plating is performed on the nano-level conductive copper layer , The liquid crystal polymer turbulent copper clad laminate is obtained.
有益效果Beneficial effect
本发明的有益效果在于：先在基材层上涂布LCP溶液，得到液晶聚合物薄膜，液晶聚合物薄膜的厚度可以控制在6μm左右；进行等离子活化处理，可以提高铜层的剥离强度，提高产品的可靠性；纳米级导电铜层的粗糙度低，可满足高频、高速传输需求；最终的液晶聚合物扰性覆铜板的铜层厚度可控制在3μm左右（总厚度为9μm左右），可满足装置的小型化及薄膜化的发展需要，经半加成工艺，可实现精细线路（线距30μm）的加工制作。The beneficial effects of the present invention are: first coat the LCP solution on the substrate layer to obtain a liquid crystal polymer film, the thickness of the liquid crystal polymer film can be controlled at about 6 μm; plasma activation treatment can increase the peeling strength of the copper layer and improve Product reliability; the roughness of the nano-level conductive copper layer is low, which can meet the needs of high-frequency and high-speed transmission; the thickness of the copper layer of the final liquid crystal polymer turbulent copper clad laminate can be controlled at about 3μm (total thickness is about 9μm), It can meet the development needs of miniaturization and thin filming of the device, and can realize the processing and production of fine lines (line pitch 30μm) through the semi-additive process.
附图说明Description of the drawings
图1为现有的电解铜覆铜板通过蚀刻工艺制备得到的线路SEM图；Figure 1 is an SEM image of a circuit prepared by an etching process of an existing electrolytic copper copper clad laminate;
图2为本发明实施例二制备得到的液晶聚合物扰性覆铜板通过蚀刻工艺制备得到的线路SEM图；2 is a circuit SEM image of the liquid crystal polymer turbulent copper clad laminate prepared by the etching process in the second embodiment of the present invention;
图3为本发明实施例三制备得到的液晶聚合物扰性覆铜板通过蚀刻工艺制备得到的线路切片图。FIG. 3 is a circuit slice diagram of the liquid crystal polymer turbulent copper clad laminate prepared in the third embodiment of the present invention, which is prepared through an etching process.
本发明的实施方式Embodiments of the present invention
为详细说明本发明的技术内容、所实现目的及效果，以下结合实施方式并配合附图予以说明。In order to describe in detail the technical content, the achieved objectives and effects of the present invention, the following description will be given in conjunction with the embodiments and the accompanying drawings.
本发明最关键的构思在于：先成型液晶聚合物薄膜，然后进行镀铜，可将液晶聚合物扰性覆铜板的铜层厚度可控制在3μm左右，可实现精细线路（线距30μm）的加工制作。The most critical idea of the present invention is: first forming a liquid crystal polymer film, and then copper plating, the thickness of the copper layer of the liquid crystal polymer turbulent copper clad laminate can be controlled to about 3μm, and the processing of fine lines (line pitch 30μm) can be realized Make.
一种液晶聚合物扰性覆铜板的制备方法，在用于制作液晶聚合物薄膜的基材层上涂布LCP溶液，然后依次进行固化处理和退火处理，得到液晶聚合物薄膜；将所述液晶聚合物薄膜进行等离子活化处理；在等离子活化处理后的液晶聚合物薄膜的表面进行沉铜，得到具有纳米级导电铜层的液晶聚合物薄膜；在所述纳米级导电铜层上进行连续镀铜，得到所述液晶聚合物扰性覆铜板。A method for preparing a liquid crystal polymer turbulent copper clad laminate, coating an LCP solution on a substrate layer used to make a liquid crystal polymer film, and then sequentially performing curing treatment and annealing treatment to obtain a liquid crystal polymer film; Plasma activation treatment is performed on the polymer film; copper is deposited on the surface of the liquid crystal polymer film after plasma activation treatment to obtain a liquid crystal polymer film with a nano-level conductive copper layer; continuous copper plating is performed on the nano-level conductive copper layer , The liquid crystal polymer turbulent copper clad laminate is obtained.
从上述描述可知，本发明的有益效果在于：先在基材层上涂布LCP溶液，得到液晶聚合物薄膜，液晶聚合物薄膜的厚度可以控制在6μm左右；进行等离子活化处理，可以提高铜层的剥离强度，提高产品的可靠性；纳米级导电铜层的粗糙度低，可满足高频、高速传输需求；最终的液晶聚合物扰性覆铜板的铜层厚度可控制在3μm左右（总厚度为9μm左右），可满足装置的小型化及薄膜化的发展需要，经半加成工艺，可实现精细线路（线距30μm）的加工制作。From the above description, the beneficial effects of the present invention are: first coat the LCP solution on the substrate layer to obtain a liquid crystal polymer film, the thickness of the liquid crystal polymer film can be controlled at about 6μm; plasma activation treatment can improve the copper layer High peel strength, improve product reliability; nano-scale conductive copper layer has low roughness, which can meet the needs of high-frequency and high-speed transmission; the thickness of the copper layer of the final liquid crystal polymer turbulent copper clad laminate can be controlled at about 3μm (total thickness It is about 9μm), which can meet the development needs of device miniaturization and thin film. After semi-additive process, it can realize the processing and production of fine lines (line pitch 30μm).
进一步的，所述退火处理的温度为150~250℃，时间为1~5h。Further, the temperature of the annealing treatment is 150 to 250° C., and the time is 1 to 5 h.
由上述描述可知，退火处理的温度和时间可根据需要进行调整。It can be seen from the above description that the temperature and time of the annealing treatment can be adjusted as needed.
进一步的，所述等离子活化处理的气体流量为3~7SLM，活化温度为80~120℃，活化功率为7~13kW。Further, the gas flow rate of the plasma activation treatment is 3-7SLM, the activation temperature is 80-120°C, and the activation power is 7-13kW.
由上述描述可知，等离子活化处理的条件可以根据需要进行调整。It can be seen from the above description that the conditions of the plasma activation treatment can be adjusted as needed.
进一步的，所述连续镀铜的电流密度为1~5ASD，时间为4~15min。Further, the current density of the continuous copper plating is 1 to 5 ASD, and the time is 4 to 15 minutes.
进一步的，所述基材层的材质为PTFE，所述基材层的厚度为30~70μm。Further, the material of the base material layer is PTFE, and the thickness of the base material layer is 30-70 μm.
进一步的，所述液晶聚合物薄膜的厚度大于或等于6μm。Further, the thickness of the liquid crystal polymer film is greater than or equal to 6 μm.
由上述描述可知，液晶聚合物薄膜的厚度可以根据需要进行控制，最小厚度6μm左右。It can be seen from the above description that the thickness of the liquid crystal polymer film can be controlled as required, and the minimum thickness is about 6 μm.
进一步的，所述纳米级导电铜层的厚度为20~100nm。Further, the thickness of the nano-scale conductive copper layer is 20-100 nm.
进一步的，所述液晶聚合物扰性覆铜板的铜层厚度大于或等于3μm。Further, the thickness of the copper layer of the liquid crystal polymer turbulent copper clad laminate is greater than or equal to 3 μm.
进一步的，采用半导体工艺在等离子活化处理后的液晶聚合物薄膜的表面进行沉铜。Further, a semiconductor process is used to deposit copper on the surface of the liquid crystal polymer film after plasma activation treatment.
实施例一Example one
本发明的实施例一为液晶聚合物扰性覆铜板的制备方法，包括如下步骤：The first embodiment of the present invention is a method for preparing a liquid crystal polymer turbulent copper clad laminate, which includes the following steps:
1、在用于制作液晶聚合物薄膜的基材层上涂布LCP溶液，然后依次进行固化处理和退火处理，得到液晶聚合物薄膜。1. Coat the LCP solution on the substrate layer used to make the liquid crystal polymer film, and then sequentially perform curing treatment and annealing treatment to obtain the liquid crystal polymer film.
本实施例中，所述基材层的材质为PTFE，所述基材层的厚度为30~70μm，基材层可以是连续卷状材料。固化处理即除去LCP溶液中的溶剂，可以进行加热固化。所述退火处理的温度为150~250℃，时间为1~5h。最终得到液晶聚合物薄膜的厚度大于或等于6μm，当需要得到6μm左右的液晶聚合物薄膜时，LCP溶液的涂布厚度在8μm左右。In this embodiment, the material of the substrate layer is PTFE, the thickness of the substrate layer is 30-70 μm, and the substrate layer may be a continuous roll material. The curing treatment is to remove the solvent in the LCP solution and heat curing can be carried out. The temperature of the annealing treatment is 150 to 250° C., and the time is 1 to 5 h. The thickness of the finally obtained liquid crystal polymer film is greater than or equal to 6 μm. When a liquid crystal polymer film of about 6 μm needs to be obtained, the coating thickness of the LCP solution is about 8 μm.
2、将所述液晶聚合物薄膜进行等离子活化处理。2. Subjecting the liquid crystal polymer film to plasma activation treatment.
本实施例中，所述等离子活化处理的气体流量为3~7SLM，活化温度为80~120℃，活化功率为7~13kW，等离子活化处理可以提高液晶聚合物薄膜的表面活性，提高纳米级导电铜层与液晶聚合物薄膜之间的剥离强度。In this embodiment, the gas flow rate of the plasma activation treatment is 3~7SLM, the activation temperature is 80~120°C, and the activation power is 7~13kW. The plasma activation treatment can increase the surface activity of the liquid crystal polymer film and improve the nano-level conductivity. The peel strength between the copper layer and the liquid crystal polymer film.
3、在等离子活化处理后的液晶聚合物薄膜的表面进行沉铜，得到具有纳米级导电铜层的液晶聚合物薄膜。3. Copper is deposited on the surface of the liquid crystal polymer film after plasma activation treatment to obtain a liquid crystal polymer film with a nano-level conductive copper layer.
本实施例中，采用半导体工艺在等离子活化处理后的液晶聚合物薄膜的表面进行沉铜，所述纳米级导电铜层的厚度为20~100nm。In this embodiment, a semiconductor process is used to deposit copper on the surface of the liquid crystal polymer film after plasma activation treatment, and the thickness of the nano-scale conductive copper layer is 20-100 nm.
4、在所述纳米级导电铜层上进行连续镀铜，得到所述液晶聚合物扰性覆铜板。4. Perform continuous copper plating on the nano-level conductive copper layer to obtain the liquid crystal polymer turbulent copper clad laminate.
本实施例中，所述连续镀铜的电流密度为1~5ASD，时间为4~15min。所述液晶聚合物扰性覆铜板的铜层厚度大于或等于3μm。In this embodiment, the current density of the continuous copper plating is 1 to 5 ASD, and the time is 4 to 15 minutes. The thickness of the copper layer of the liquid crystal polymer turbulent copper clad laminate is greater than or equal to 3 μm.
实施例二Example two
本发明的实施例二为液晶聚合物扰性覆铜板的制备方法，与实施例一的不同之处在于：The second embodiment of the present invention is a method for preparing a liquid crystal polymer turbulent copper clad laminate. The difference from the first embodiment is:
步骤1中，基材层的厚度为50μm；退火处理的温度为200℃，时间为3h。最终得到的液晶聚合物薄膜的厚度为6μm。In step 1, the thickness of the substrate layer is 50 μm; the temperature of the annealing treatment is 200° C. and the time is 3 hours. The thickness of the finally obtained liquid crystal polymer film was 6 μm.
步骤2中，所述等离子活化处理的气体流量为5SLM，活化温度为100℃，活化功率为10kW。In step 2, the gas flow rate of the plasma activation treatment is 5 SLM, the activation temperature is 100° C., and the activation power is 10 kW.
步骤3中，纳米级导电铜层的厚度为60nm。In step 3, the thickness of the nano-scale conductive copper layer is 60 nm.
步骤4中，连续镀铜的电流密度为3ASD，时间为4.5min，最终得到的液晶聚合物扰性覆铜板的铜层厚度为3μm。In step 4, the current density of continuous copper plating is 3 ASD, the time is 4.5 min, and the thickness of the copper layer of the finally obtained liquid crystal polymer turbulent copper clad laminate is 3 μm.
实施例三Example three
本发明的实施例三为液晶聚合物扰性覆铜板的制备方法，与实施例一的不同之处在于：The third embodiment of the present invention is a method for preparing a liquid crystal polymer turbulent copper clad laminate. The difference from the first embodiment is:
步骤1中，基材层的厚度为40μm；退火处理的温度为150℃，时间为5h。最终得到的液晶聚合物薄膜的厚度为6μm。In step 1, the thickness of the substrate layer is 40 μm; the temperature of the annealing treatment is 150° C. and the time is 5 hours. The thickness of the finally obtained liquid crystal polymer film was 6 μm.
步骤2中，所述等离子活化处理的气体流量为3SLM，活化温度为120℃，活化功率为7kW。In step 2, the gas flow rate of the plasma activation treatment is 3SLM, the activation temperature is 120°C, and the activation power is 7kW.
步骤3中，纳米级导电铜层的厚度为20nm。In step 3, the thickness of the nano-scale conductive copper layer is 20 nm.
步骤4中，连续镀铜的电流密度为2ASD，时间为7min，最终得到的液晶聚合物扰性覆铜板的铜层厚度约为3μm。In step 4, the current density of continuous copper plating is 2 ASD and the time is 7 min. The thickness of the copper layer of the finally obtained liquid crystal polymer turbulent copper clad laminate is about 3 μm.
实施例四Embodiment four
本发明的实施例四为液晶聚合物扰性覆铜板的制备方法，与实施例一的不同之处在于：The fourth embodiment of the present invention is a preparation method of a liquid crystal polymer turbulent copper clad laminate. The difference from the first embodiment is:
步骤1中，基材层的厚度为70μm；退火处理的温度为250℃，时间为1h。最终得到的液晶聚合物薄膜的厚度为6μm。In step 1, the thickness of the substrate layer is 70 μm; the temperature of the annealing treatment is 250° C. and the time is 1 h. The thickness of the finally obtained liquid crystal polymer film was 6 μm.
步骤2中，所述等离子活化处理的气体流量为7SLM，活化温度为80℃，活化功率为13kW。In step 2, the gas flow rate of the plasma activation treatment is 7SLM, the activation temperature is 80°C, and the activation power is 13kW.
步骤3中，纳米级导电铜层的厚度为100nm。In step 3, the thickness of the nano-scale conductive copper layer is 100 nm.
步骤4中，连续镀铜的电流密度为5ASD，时间为3min，最终得到的液晶聚合物扰性覆铜板的铜层厚度约为3μm。In step 4, the current density of continuous copper plating is 5 ASD and the time is 3 min. The thickness of the copper layer of the finally obtained liquid crystal polymer turbulent copper clad laminate is about 3 μm.
性能测试Performance Testing
对实施例二至实施例四制备得到的液晶聚合物薄膜分别进行剥离强度、尺寸稳定性、阻焊测试、弹性模量、膨胀系数、介电常数、损耗因子、吸水率、阻燃性能和粗糙度测试。测试结果如表1所示：The liquid crystal polymer films prepared in Examples 2 to 4 were subjected to peel strength, dimensional stability, solder mask test, elastic modulus, expansion coefficient, dielectric constant, loss factor, water absorption, flame retardancy and roughness. Degree test. The test results are shown in Table 1:
表1 性能测试结果对比表Table 1 Comparison table of performance test results
Figure dest_path_image001
Figure dest_path_image001
通过将液晶聚合物薄膜与铜箔进行压合后制备得到的扰性覆铜板的剥离强度在0.51N/mm左右，而本发明制备得到的液晶聚合物扰性覆铜板的剥离强度在0.6N/mm以上，可大大提高产品的可靠性。且从表1可知，本发明制备得到的液晶聚合物扰性覆铜板具有较好的尺寸稳定性、优良的阻焊性能、较高的弹性模量、低膨胀系数、优异的介电性能和阻燃性能。The peeling strength of the turbulent copper clad laminate prepared by laminating the liquid crystal polymer film and the copper foil is about 0.51N/mm, while the peeling strength of the turbulent copper clad laminate prepared by the present invention is 0.6N/mm. Above mm, the reliability of the product can be greatly improved. And from Table 1, it can be seen that the liquid crystal polymer turbulent copper clad laminate prepared by the present invention has better dimensional stability, excellent solder resist performance, higher elastic modulus, low expansion coefficient, excellent dielectric properties and resistance. Combustion performance.
对于粗糙度测试，市面上的压延铜（RA）（如Mitsui公司，型号为3EC-M2S-HTE、厚度为12um的压延铜箔）的Ra在0.087μm左右，Rz在0.75μm左右，电解铜（ED）的Ra在0.282μm左右，Rz在1.872μm左右。而本发明制备得到的铜层表面的粗糙度远低于市面上的压延铜和电解铜，可满足高频、高速传输需求。For the roughness test, the rolled copper (RA) on the market (such as Mitsui, the model is 3EC-M2S-HTE, the rolled copper foil with a thickness of 12um) has an Ra of about 0.087μm, Rz of about 0.75μm, and electrolytic copper ( ED) Ra is about 0.282μm, and Rz is about 1.872μm. The surface roughness of the copper layer prepared by the present invention is much lower than that of rolled copper and electrolytic copper on the market, and can meet the requirements of high-frequency and high-speed transmission.
图1为电解铜覆铜板通过蚀刻工艺制备得到的线路SEM图，图2为本发明实施例二制备得到的液晶聚合物扰性覆铜板通过蚀刻工艺制备得到的线路SEM图，从图中可以看出，电解铜的蚀刻线路表面粗糙，而本发明的蚀刻线路表面光滑，铜层与液晶聚合物薄膜之间的结合更好。实施例三和实施例四的测试结果类似，在此就不一一进行赘述。Figure 1 is the SEM image of the circuit prepared by the etching process of the electrolytic copper copper clad laminate, and Figure 2 is the SEM image of the circuit prepared by the etching process of the liquid crystal polymer turbulent copper clad laminate prepared in Example 2 of the present invention, as can be seen from the figure It is found that the surface of the etched circuit of electrolytic copper is rough, while the surface of the etched circuit of the present invention is smooth, and the combination between the copper layer and the liquid crystal polymer film is better. The test results of the third embodiment and the fourth embodiment are similar, and will not be repeated here.
图3为本发明实施例三制备得到的液晶聚合物扰性覆铜板通过蚀刻工艺制备得到的线路切片图，从图中可以看出线宽60.99μm（近似于61μm），线距25.93μm（近似于26μm），由此可见，本液晶聚合物扰性覆铜板的制备方法可能过实现线距30μm左右的精细线路加工制作。Figure 3 is a circuit slice diagram of the liquid crystal polymer turbulent copper clad laminate prepared by the etching process in the third embodiment of the present invention. It can be seen from the figure that the line width is 60.99 μm (approximately 61 μm), and the line spacing is 25.93 μm (approximately 26μm), it can be seen that the preparation method of the liquid crystal polymer turbulent copper clad laminate may achieve fine line processing with a line pitch of about 30μm.
综上所述，本发明提供的一种液晶聚合物扰性覆铜板的制备方法，制备得到的产品可靠性好，整体厚度小，可实现精细线路（线距30μm）的加工制作。In summary, the method for preparing liquid crystal polymer turbulent copper clad laminates provided by the present invention has good reliability, small overall thickness, and can realize the processing and production of fine lines (line pitch 30 μm).
以上所述仅为本发明的实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书及附图内容所作的等同变换，或直接或间接运用在相关的技术领域，均同理包括在本发明的专利保护范围内。The above are only the embodiments of the present invention and do not limit the patent scope of the present invention. All equivalent transformations made using the content of the description and drawings of the present invention, or directly or indirectly applied in related technical fields, are included in the same reasoning. Within the scope of patent protection of the present invention.

Claims (9)

  1. 一种液晶聚合物扰性覆铜板的制备方法，其特征在于，在用于制作液晶聚合物薄膜的基材层上涂布LCP溶液，然后依次进行固化处理和退火处理，得到液晶聚合物薄膜；将所述液晶聚合物薄膜进行等离子活化处理；在等离子活化处理后的液晶聚合物薄膜的表面进行沉铜，得到具有纳米级导电铜层的液晶聚合物薄膜；在所述纳米级导电铜层上进行连续镀铜，得到所述液晶聚合物扰性覆铜板。A method for preparing a liquid crystal polymer turbulent copper clad laminate, which is characterized in that an LCP solution is coated on a substrate layer used to make a liquid crystal polymer film, and then curing treatment and annealing treatment are sequentially performed to obtain a liquid crystal polymer film; Plasma activation treatment is performed on the liquid crystal polymer film; copper is deposited on the surface of the liquid crystal polymer film after plasma activation treatment to obtain a liquid crystal polymer film with a nano-level conductive copper layer; on the nano-level conductive copper layer Continuous copper plating is performed to obtain the liquid crystal polymer turbulent copper clad laminate.
  2. 根据权利要求1所述的液晶聚合物扰性覆铜板的制备方法，其特征在于，所述退火处理的温度为150~250℃，时间为1~5h。The method for preparing a liquid crystal polymer turbulent copper clad laminate according to claim 1, wherein the temperature of the annealing treatment is 150 to 250° C., and the time is 1 to 5 h.
  3. 根据权利要求1所述的液晶聚合物扰性覆铜板的制备方法，其特征在于，所述等离子活化处理的气体流量为3~7SLM，活化温度为80~120℃，活化功率为7~13kW。The method for preparing a liquid crystal polymer turbulent copper clad laminate according to claim 1, wherein the gas flow rate of the plasma activation treatment is 3-7SLM, the activation temperature is 80-120°C, and the activation power is 7-13kW.
  4. 根据权利要求1所述的液晶聚合物扰性覆铜板的制备方法，其特征在于，所述连续镀铜的电流密度为1~5ASD，时间为4~15min。The method for preparing a liquid crystal polymer turbulent copper clad laminate according to claim 1, wherein the current density of the continuous copper plating is 1 to 5 ASD, and the time is 4 to 15 minutes.
  5. 根据权利要求1所述的液晶聚合物扰性覆铜板的制备方法，其特征在于，所述基材层的材质为PTFE，所述基材层的厚度为30~70μm。The method for preparing a liquid crystal polymer turbulent copper clad laminate according to claim 1, wherein the material of the substrate layer is PTFE, and the thickness of the substrate layer is 30-70 μm.
  6. 根据权利要求1所述的液晶聚合物扰性覆铜板的制备方法，其特征在于，所述液晶聚合物薄膜的厚度大于或等于6μm。The method for preparing a liquid crystal polymer turbulent copper clad laminate according to claim 1, wherein the thickness of the liquid crystal polymer film is greater than or equal to 6 μm.
  7. 根据权利要求1所述的液晶聚合物扰性覆铜板的制备方法，其特征在于，所述纳米级导电铜层的厚度为20~100nm。The method for preparing a liquid crystal polymer turbulent copper clad laminate according to claim 1, wherein the thickness of the nano-scale conductive copper layer is 20-100 nm.
  8. 根据权利要求1所述的液晶聚合物扰性覆铜板的制备方法，其特征在于，所述液晶聚合物扰性覆铜板的铜层厚度大于或等于3μm。The method for preparing a liquid crystal polymer turbulent copper clad laminate according to claim 1, wherein the thickness of the copper layer of the liquid crystal polymer turbulent copper clad laminate is greater than or equal to 3 μm.
  9. 根据权利要求1所述的液晶聚合物扰性覆铜板的制备方法，其特征在于，采用半导体工艺在等离子活化处理后的液晶聚合物薄膜的表面进行沉铜。The method for preparing a liquid crystal polymer turbulent copper clad laminate according to claim 1, wherein a semiconductor process is used to deposit copper on the surface of the liquid crystal polymer film after plasma activation treatment.
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