CN114199806A - A method for detecting organic matter distribution on the surface of micro-nano rough copper foil by AFM-IR - Google Patents
A method for detecting organic matter distribution on the surface of micro-nano rough copper foil by AFM-IR Download PDFInfo
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- CN114199806A CN114199806A CN202111513883.2A CN202111513883A CN114199806A CN 114199806 A CN114199806 A CN 114199806A CN 202111513883 A CN202111513883 A CN 202111513883A CN 114199806 A CN114199806 A CN 114199806A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000011889 copper foil Substances 0.000 title claims abstract description 44
- 238000009826 distribution Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims description 17
- 239000005416 organic matter Substances 0.000 title abstract description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 27
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 11
- 238000001514 detection method Methods 0.000 claims abstract description 8
- 238000001228 spectrum Methods 0.000 claims abstract description 5
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 238000004566 IR spectroscopy Methods 0.000 abstract description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 abstract description 5
- 229910000077 silane Inorganic materials 0.000 abstract description 5
- 238000000862 absorption spectrum Methods 0.000 abstract description 2
- 238000004630 atomic force microscopy Methods 0.000 abstract description 2
- 239000007822 coupling agent Substances 0.000 abstract description 2
- 239000011888 foil Substances 0.000 description 9
- 239000000523 sample Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- -1 polydithio-dipropyl Polymers 0.000 description 3
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 2
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- RMKZLFMHXZAGTM-UHFFFAOYSA-N [dimethoxy(propyl)silyl]oxymethyl prop-2-enoate Chemical compound CCC[Si](OC)(OC)OCOC(=O)C=C RMKZLFMHXZAGTM-UHFFFAOYSA-N 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 108010010803 Gelatin Proteins 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
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- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
用AFM‑IR检测微纳米粗糙的铜箔表面有机物分布的方法，应用基于原子力显微成像‑红外光谱技术对PCB用铜箔表面任意一点进行红外光谱全谱扫描，获取铜箔表面吸附的硅烷偶联剂的红外特征吸收谱图，选择谱图中的硅烷偶联剂强度最大的特征峰作为AFM‑IR的红外检测波长，然后用这一检测波长对5μm×5μm区域进行扫描以获取该区域内的硅烷偶联剂的信号强度分布数据，使用数据处理软件进行数据处理，生成铜箔表面硅烷偶联剂的三维立体分布图像，表征硅烷偶联剂的空间分布状态。
AFM-IR is used to detect the distribution of organic matter on the surface of micro-nano rough copper foil. Atomic force microscopy imaging-infrared spectroscopy is used to scan the full spectrum of infrared spectrum at any point on the surface of copper foil for PCB to obtain the silane molecules adsorbed on the surface of copper foil. Infrared characteristic absorption spectrum of the coupling agent, select the characteristic peak with the highest intensity of the silane coupling agent in the spectrum as the infrared detection wavelength of AFM‑IR, and then use this detection wavelength to scan the 5μm×5μm area to obtain the area within this area. The signal intensity distribution data of the silane coupling agent was processed using data processing software to generate a three-dimensional distribution image of the silane coupling agent on the copper foil surface to characterize the spatial distribution state of the silane coupling agent.
Description
Technical Field
The invention relates to a method for detecting the distribution of trace organic matters on the surface of a metal foil by applying atomic force microscopic imaging-infrared spectroscopy (AFM-IR), in particular to a method for detecting the distribution of a coupling agent on the uneven surface of a copper foil for a high-frequency high-speed Printed Circuit Board (PCB).
Background
For the characterization of trace organic matters on the surface of metal foil (aluminum foil, copper foil, silver foil, gold foil and the like), a method for performing in-situ infrared ATR on the surface is used in the past, the average infrared spectrum signal distribution in one area is characterized, the spatial resolution is 5 mu m, and the nano-scale resolution distribution of the trace organic matters cannot be accurately measured. Patent document 1: CN 108603303 reports that the amount of silane attached to the surface of copper foil is measured by a fluorescent X-ray analyzer. The limit of the concentration of the sample to be measured of the total reflection X-ray fluorescence spectrum can reach 10-3-10-6μ g/g, but the range measured by this method is 500 μm, and the spatial resolution is low. The surface of the copper foil for the PCB has micro-nano roughness (the surface roughness Rz is 0.1-1.5 mu m), and the prior analysis method can not represent the ultrahigh-resolution spatial distribution on the concave-convex surface.
The ultra-low profile copper foil is one of the basic materials of a high-frequency and high-speed Printed Circuit Board (PCB) for 5G communication, and the enhancement of the bonding performance between the copper foil and a resin matrix in the PCB becomes an important influence factor in industrial application. In the existing copper foil production process, various additives are added during electrolytic production of copper foil, and commonly used additives comprise sodium polydithio-dipropyl Sulfonate (SP), hydroxyethyl cellulose (HEC), polyethylene glycol (PEG), polyoxyethylene nonyl phenyl ether, fatty amine ethoxylate sulfonate, rare earth salt, gelatin, thiourea and the like. At present, the surface of the copper foil is mainly treated by using a silane coupling agent to enhance the bonding performance of the copper foil, and additives added in the electrolytic process can be adsorbed on the surface of the copper foil to influence the enhancement effect of the silane coupling agent on the bonding performance of the surface of the copper foil. Infrared spectroscopy is a common characterization method for detecting organic structures. The intensity of the infrared spectral peak of an organic can be used to describe the relative content of the organic. However, the diffraction limit of the conventional optical device is limited, the spatial resolution of the infrared spectrometer is only about 5 μm, the type and content of total organic matters existing in the region can be expressed, and the three-dimensional distribution on the concave-convex surface cannot be measured. Patent document 2: CN 110366686 a, does not report the thickness distribution of the coating layer of organic matter on the surface with micro-nano roughness.
Disclosure of Invention
The purpose of the invention is as follows: AFM-IR is used for detecting the distribution of trace organic matters on the surface of metal foil (aluminum foil, copper foil, silver foil, gold foil and the like), and the distribution characteristics of the trace organic matters are analyzed on a nanoscale scale.
The method for detecting the distribution of the organic matters on the surface of the micro-nano rough copper foil by AFM-IR comprises the following steps: performing infrared spectrum full-spectrum scanning on multiple points on the surface of copper foil for PCB by AFM-IR technology to obtain infrared characteristic absorption spectrogram of silane coupling agent adsorbed on the surface of copper foil, and selecting 1720cm characteristic peak with maximum silane coupling agent intensity in the spectrogram-1As the infrared detection wavelength of AFM-IR, an arbitrary 5 μm.times.5 μm area was scanned with this wavelength to acquire the distribution data of the silane coupling agent in the area, while the surface morphology of the area was simultaneously measured by applying an atomic force microscope in the technique for AFM-IR. Using Surface Works software of the instrument to process data, and measuring the appearance of the Surface of the copper foil and the characteristic infrared spectrum peak 1720cm of the silane coupling agent-1The spatial distribution data are combined, and the Surface Works software can automatically generate 1720cm of silane coupling agent-1Three-dimensional stereo distribution image of intensity. 1720cm of silane coupling agent-1The relative intensity of the characteristic peak represents the relative thickness of the silane coupling agent at the point, the relative thickness of the silane coupling agent on the surface of the copper foil is determined by the method, and the spatial distribution state of the silane coupling agent on the micro-nano rough surface is represented.
All AFM-IR experiments in the present invention were performed on a Vistasscope Vista-IR microscope.
Principle based on atomic force microscopy-infrared spectroscopy (AFM-IR):
AFM-IR combines atomic force microscopy with infrared spectroscopy, utilizes light-induced force techniques, obtains local polarization of a sample through tip-enhanced illumination, and uses an atomic force microscope probe with ultra-high sensitivity to measure local polarization force between a tip and the sample, which reflects near-field optical interaction between the tip and the sample. The traditional optical detection method is replaced by the method. The application of the light induction force technology greatly improves the resolution of the infrared spectrum, and the spatial resolution of the infrared spectrum is about 10nm, so that the infrared spectrum can detect the distribution condition of different organic matters on the same position of the surface of a sample. And judging the type of the organic matter according to the relation between the wavelength of the infrared absorption peak and the corresponding group. And detecting the relative intensity of the absorption peak to obtain the relative content of the organic matters, thereby obtaining the distribution condition of the organic matters.
The high-frequency high-speed PCB board for 5G communication can use the copper foil with ultralow profile degree, and in order to meet the specific requirements of use, the surface of the copper foil needs to be subjected to superfine roughening treatment, and the surface of the copper foil has uneven appearance by the treatment mode. The surface of the copper foil is treated by using the silane coupling agent, and the distribution of the silane coupling agent at different shapes of the surface of the copper foil influences the bonding performance of the copper foil.
The method has the advantages that:
the AFM-IR technology is used for detecting the surface appearance of the copper foil and the distribution state of the silane coupling agent by utilizing the characteristics of high sensitivity and high spatial resolution, and a basis is provided for improving the bonding performance between the copper foil and a matrix.
The method can be widely applied to the distribution detection of trace organic matters on the surfaces of aluminum foils, silver foils, gold foils and other metal foils.
Drawings
FIG. 1: AFM-IR (atomic force microscopy-IR) detection of infrared spectrogram of surface of copper foil treated by silane coupling agent
FIG. 2: at 1720cm-1Three-dimensional distribution of characteristic peak infrared intensity characterized copper foil surface silane coupling agent
The specific implementation method comprises the following steps:
examples
Selecting a copper foil with the surface roughness Rz of 1.5-1.8 mu m, coating a silane coupling agent of acryloyloxy propyl trimethoxy silane according to a common spraying method, cutting the copper foil into squares with the side length of 2 cm, washing the surfaces of the squares with water, and drying to obtain the cleaned copper foil. AFM-IR experiments were all performed on a vistasscope Vista-IR (Molecular Vista, USA). To any point on the surface of the copper foilAnd (3) scanning the whole infrared spectrum to obtain a complete infrared absorption spectrum of the silane coupling agent acryloxypropyltrimethoxysilane. Then, different infrared absorption peak wavelengths are selected to scan a 5 μm × 5 μm area to obtain distribution data. And (4) carrying out data processing by using Surface Works software carried by the instrument. The surface topography and infrared intensity distribution of the copper foil are shown in FIG. 2, wherein different colors in the infrared distribution three-dimensional graph represent carbonyl stretching vibration absorption peaks (1720 cm: 1720 cm) in infrared spectrum of the silane coupling agent on the surface of the copper foil-1) The higher the strength and the relative strength, the darker the color, indicating that the silane coupling agent was deposited thicker at the position on the surface of the copper foil.
Claims (1)
1. A method for detecting the distribution of micro-nano rough copper foil surface organic matters by AFM-IR, it is characterized in that the atomic force microscope principle is applied to detect infrared spectrum, the full spectrum scanning of the infrared spectrum is carried out on any point on the surface of the copper foil used by the high-frequency high-speed printed circuit board, the infrared characteristic absorption spectrogram of the silane coupling agent adsorbed on the surface of the copper foil is obtained, the characteristic peak with the maximum strength of the silane coupling agent in the spectrogram is selected as the infrared detection wavelength of AFM-IR, and then scanning a 5-micron multiplied by 5-micron area by using the detection wavelength to acquire signal intensity distribution data of the silane coupling agent in the area, performing data processing by using data processing software, automatically generating a three-dimensional distribution image of the silane coupling agent on the surface of the copper foil by using the data processing software, determining the relative thickness of the silane coupling agent on different positions of the surface of the copper foil, and representing the spatial distribution of the silane coupling agent.
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| CN202111513883.2A CN114199806B (en) | 2021-12-10 | 2021-12-10 | Method for detecting organic matter distribution on micro-nano roughened copper foil surface by AFM-IR |
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| CN202111513883.2A CN114199806B (en) | 2021-12-10 | 2021-12-10 | Method for detecting organic matter distribution on micro-nano roughened copper foil surface by AFM-IR |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118150510A (en) * | 2024-05-11 | 2024-06-07 | 中国地质大学（北京） | A method for determining the adsorption capacity of organic matter |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118150510A (en) * | 2024-05-11 | 2024-06-07 | 中国地质大学（北京） | A method for determining the adsorption capacity of organic matter |
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