CN110057401A - A kind of transparent ultrathin membrane refractive index and method for measuring thickness - Google Patents
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Abstract
本发明属于薄膜测量表征领域,并具体公开了一种透明超薄膜折射率及厚度测量方法,包括如下步骤:S1以2πdT/λ为变量对透明超薄膜椭偏比ρ1进行二阶泰勒展开获得幂级数形式:S2分离出幂级数形式中与透明超薄膜相关的参量T1和T2,并获得表达式;S3计算幂级数形式的实部与虚部平方的斜率R,根据斜率R计算的具体值;S4将计算的具体值带入步骤S2的表达式中求解出透明超薄膜的折射率nT,并根据折射率计算透明超薄膜的厚度。本发明可实现透明超薄膜的折射率和厚度的快速、直接、准确测量,具有适用范围广,测量准确,无复杂分析过程等优点。
The invention belongs to the field of thin film measurement and characterization, and specifically discloses a method for measuring the refractive index and thickness of a transparent ultra-thin film . Obtain the power series form: S2 separates out the parameters T 1 and T 2 related to the transparent ultrathin film in the power series form, and obtains Expression; S3 calculates the slope R of the square of the real part and the imaginary part in the form of a power series, calculated according to the slope R The specific value of ; S4 will calculate the The specific value is brought into the expression of step S2 to solve the refractive index n T of the transparent ultra-thin film, and the thickness of the transparent ultra-thin film is calculated according to the refractive index. The invention can realize fast, direct and accurate measurement of the refractive index and thickness of the transparent ultra-thin film, and has the advantages of wide application range, accurate measurement, and no complicated analysis process.
Description
技术领域technical field
本发明属于薄膜测量表征领域,更具体地,涉及一种透明超薄膜折射率及厚度测量方法,适用于多种基底上透明超薄膜折射率和厚度的快速精确测量。The invention belongs to the field of thin film measurement and characterization, and more particularly relates to a method for measuring the refractive index and thickness of transparent ultra-thin films, which is suitable for fast and accurate measurement of the refractive index and thickness of transparent ultra-thin films on various substrates.
背景技术Background technique
透明超薄膜指消光系数为零的超薄膜,包括有机薄膜,聚合物薄膜,金属氧化物等,在减反镀膜,生物传感器,太阳能电池等方面都有广泛的应用。透明超薄膜的厚度对其光学性质有很大影响,不同厚度的透明超薄膜其光学常数不同。而透明超薄膜的厚度、光学常数决定了其透射、反射等光学性质,也决定了它们部分物理特性,因此需要对透明超薄膜的厚度及其光学常数进行测量。Transparent ultra-thin films refer to ultra-thin films with zero extinction coefficient, including organic films, polymer films, metal oxides, etc., and are widely used in anti-reflection coatings, biosensors, solar cells, etc. The thickness of the transparent ultra-thin film has a great influence on its optical properties, and the optical constants of the transparent ultra-thin film with different thickness are different. The thickness and optical constants of transparent ultra-thin films determine their optical properties such as transmission and reflection, and also determine some of their physical properties. Therefore, it is necessary to measure the thickness and optical constants of transparent ultra-thin films.
目前,超薄膜的测量表征方法主要包括石英晶体微天平、表面等离激元、光度法、椭偏仪等。对于薄层硬质薄膜,石英晶体微天平可以使用Sauerbrey公式,根据传感器振动计算吸附层的质量得到膜层的厚度。但是对于相对基底较软的薄膜或浸没在液体中的薄膜,薄膜分子和其中的液体对质量增加都有影响,石英晶体微天平无法确定薄膜厚度。表面等离激元是由于费米能级附近导带上的自由电子在电磁场的驱动下在金属表面发生集体震荡产生,通过棱镜耦合等方式满足波矢匹配条件,利用菲涅尔公式和等离激元结合可以计算薄膜厚度,但该方法一般用于测量金属膜或要求薄膜基底需要为金属材料。光度法基于分光光度计测量薄膜的透射率和反射率来确定薄膜的厚度,分为包络线法、全光谱拟合法等,其中包络线法是最为常用的一种,但是一般要求薄膜较厚,对于超薄膜并不合适;全谱拟合法需要借助色散模型,选用不同的振子对拟合结果有较大影响。椭偏法测量具有无损非接触、灵敏度精度高等优点,其对厚度的灵敏度可以达到0.01nm,但是椭偏法是一种非直接测量方法,需要通过计算机拟合才能求得薄膜的厚度和光学常数(包括折射率和消光系数)。椭偏仪在测量超薄膜时,由于厚度和光学常数之间具有很强的耦合关系,很难得到唯一的拟合结果。针对这种困难,可以采用多样品法、在线测量,多种周围介质条件测量等方法解决。但是上述方法都存在各自的局限性,多样品分析的前提是假设薄膜的光学常数不随厚度变化,而实际上,对于超薄膜其光学常数随厚度变化会发生改变;在线测量也存在和多样品法一样的缺陷;多种周围介质条件引入了复杂的液体测量环境,薄膜需要不与介质发生反应,且不能是多孔材料。At present, the measurement and characterization methods of ultra-thin films mainly include quartz crystal microbalance, surface plasmon, photometry, ellipsometer and so on. For thin hard films, the quartz crystal microbalance can use the Sauerbrey formula to calculate the mass of the adsorption layer according to the vibration of the sensor to obtain the thickness of the film. However, for films that are relatively soft to the substrate or immersed in liquid, both the film molecules and the liquid in them have an effect on the mass increase, and the quartz crystal microbalance cannot determine the film thickness. Surface plasmon is generated due to the collective oscillation of free electrons in the conduction band near the Fermi level on the metal surface driven by an electromagnetic field. The wave vector matching conditions are satisfied by means of prism coupling. The excimer combination can calculate the film thickness, but this method is generally used to measure metal films or require that the film substrate needs to be a metal material. The photometric method is based on measuring the transmittance and reflectance of the film to determine the thickness of the film. It can be divided into envelope method and full spectrum fitting method. It is not suitable for ultra-thin films; the full spectrum fitting method needs to rely on the dispersion model, and the selection of different oscillators has a great influence on the fitting results. Ellipsometry measurement has the advantages of non-destructive and non-contact, high sensitivity and precision, and its sensitivity to thickness can reach 0.01nm, but ellipsometry is an indirect measurement method, which requires computer fitting to obtain the thickness and optical constant of the film (including refractive index and extinction coefficient). When an ellipsometer is used to measure ultrathin films, it is difficult to obtain a unique fitting result due to the strong coupling relationship between thickness and optical constants. In view of this difficulty, methods such as multi-sample method, online measurement, and measurement of various surrounding medium conditions can be used. However, the above methods all have their own limitations. The premise of multi-sample analysis is to assume that the optical constant of the thin film does not change with the thickness. In fact, the optical constant of the ultra-thin film will change with the thickness. There are also online measurement methods and multi-sample methods. The same drawbacks; multiple ambient media conditions introduce a complex liquid measurement environment, the membrane needs to be non-reactive with the media and cannot be a porous material.
乌克兰的Andriy Kostruba等(Method for determination of the parametersof transparent ultrathin films deposited on transparent substrates underconditions of low optical contrast,Applied optics,2015,54(20):6208-6216)针对透明基底上的透明薄膜提出了一种测量方法,该方法通过多入射角测量找到特定的入射角,在该角度下,椭偏参数幅值比(Ψ)不会随薄膜厚度的变化而变化,椭偏参数相位差(Δ)与薄膜厚度成线性关系。该方法的缺点在于使用范围局限,只能用于测量与基底折射率很接近的透明超薄膜且基底材料需要完全没有吸收。Ukraine's Andriy Kostruba et al. (Method for determination of the parameters of transparent ultrathin films deposited on transparent substrates underconditions of low optical contrast, Applied optics, 2015, 54(20): 6208-6216) proposed a method for transparent films on transparent substrates Measurement method, this method finds a specific incident angle by measuring multiple incident angles, at this angle, the ellipsometry parameter amplitude ratio (Ψ) does not change with the change of the film thickness, and the ellipsometry parameter phase difference (Δ) is related to the film thickness. The thickness is linear. The disadvantage of this method is that the scope of application is limited, and it can only be used to measure transparent ultra-thin films with a refractive index very close to that of the substrate, and the substrate material needs to have no absorption at all.
发明内容SUMMARY OF THE INVENTION
针对现有技术的以上缺陷或改进需求,本发明提供了一种透明超薄膜折射率及厚度测量方法,其通过对椭偏比进行二阶泰勒展开并通过变换和计算实现透明超薄膜的折射率和厚度的快速、直接、准确计算和测量,具有适用范围广,测量准确,无复杂分析过程等优点。In view of the above defects or improvement requirements of the prior art, the present invention provides a method for measuring the refractive index and thickness of a transparent ultra-thin film, which realizes the refractive index of the transparent ultra-thin film by performing second-order Taylor expansion on the ellipsometric ratio and transforming and calculating. It has the advantages of fast, direct and accurate calculation and measurement of thickness and thickness, and has the advantages of wide application range, accurate measurement and no complicated analysis process.
为实现上述目的,本发明提出了一种透明超薄膜折射率及厚度测量方法,其包括如下步骤:To achieve the above object, the present invention proposes a transparent ultra-thin film refractive index and a thickness measurement method, which comprises the following steps:
S1以2πdT/λ为变量对待测透明超薄膜椭偏比ρ1进行二阶泰勒展开获得幂级数形式,其中,dT为待测透明超薄膜的厚度,λ为入射光的波长:S1 takes 2πd T /λ as the variable to perform the second-order Taylor expansion of the ellipsometry ratio ρ 1 of the transparent ultra-thin film to be measured to obtain a power series form, where d T is the thickness of the transparent ultra-thin film to be measured, and λ is the wavelength of the incident light:
S2分离出幂级数形式中与透明超薄膜厚度相关的参量T1和T2,并获得以下表达式:S2 separates out the parameters T 1 and T 2 related to the thickness of transparent ultrathin films in power series form and obtains the following expressions:
其中,n0为周围介质的折射率,ns为基底折射率,nT为待测透明超薄膜的折射率,基底为透明或近似透明;Wherein, n 0 is the refractive index of the surrounding medium, n s is the refractive index of the substrate, n T is the refractive index of the transparent ultra-thin film to be measured, and the substrate is transparent or approximately transparent;
S3计算幂级数形式的实部与虚部平方的斜率R,根据斜率R计算的具体值;S3 calculates the slope R of the square of the real part and the imaginary part in the form of a power series, and calculates according to the slope R the specific value of ;
S4将步骤S3计算的具体值带入步骤S2的表达式中求解出透明超薄膜的折射率nT,并根据透明超薄膜的折射率nT计算获得透明超薄膜的厚度dT。S4 will be calculated in step S3 The specific value is brought into the expression of step S2 to solve the refractive index n T of the transparent ultra-thin film, and the thickness d T of the transparent ultra-thin film is obtained by calculating according to the refractive index n T of the transparent ultra-thin film.
作为进一步优选的,步骤S1中的幂级数形式具体为:As a further preference, the power series form in step S1 is specifically:
其中,ρ0为透明超薄膜所用基底的椭偏比,dT为待测透明超薄膜的厚度,λ为入射光的波长,ρ1'、ρ″a和ρ″b均为系数。Wherein, ρ 0 is the ellipsometry ratio of the substrate used for the transparent ultra-thin film, d T is the thickness of the transparent ultra-thin film to be measured, λ is the wavelength of the incident light, and ρ 1 ′, ρ″ a and ρ″ b are coefficients.
作为进一步优选的,步骤S2中的参量T1和T2具体为:As a further preference, the parameters T 1 and T 2 in step S2 are specifically:
作为进一步优选的,步骤S3中的斜率R具体采用如下公式计算:As a further preference, the slope R in step S3 is calculated by the following formula:
其中,Reρ0和Reρ1分别为基底椭偏比ρ0的实部和透明超薄膜椭偏比ρ1的实部,Imρ0和Imρ1分别为基底椭偏比ρ0的虚部和透明超薄膜椭偏比ρ1的虚部。where Reρ 0 and Reρ 1 are the real part of the substrate ellipsometry ratio ρ 0 and the real part of the transparent ultra-thin film ellipsometry ratio ρ 1 , respectively, and Imρ 0 and Imρ 1 are the imaginary part of the substrate ellipsometry ratio ρ 0 and the transparent ultra-thin film ellipsometry ratio ρ 1, respectively. The imaginary part of the film ellipsometry ratio ρ1.
作为进一步优选的,步骤S3中的具体值采用如下公式计算:As a further preference, in step S3 The specific value of is calculated using the following formula:
其中,n0为周围介质的折射率,ns为基底折射率,θ0为入射光的入射角,θ1为入射光在基底的折射角,R为斜率。Among them, n 0 is the refractive index of the surrounding medium, ns is the refractive index of the substrate, θ 0 is the incident angle of the incident light, θ 1 is the refraction angle of the incident light on the substrate, and R is the slope.
作为进一步优选的,步骤S4中nT和dT具体采用如下方式确定:As a further preference, in step S4, n T and d T are specifically determined in the following manner:
S41判断预先测定的透明超薄膜椭偏比ρ1和基底椭偏比ρ0是否相等,若是,则nT=ns,然后根据透明超薄膜的折射率nT计算ρ1',并利用公式计算透明超薄膜的厚度dT,其中,Imρ1为透明超薄膜椭偏比ρ1的虚部,λ为入射光的波长;若否,则转入步骤S42;S41 judges whether the pre-measured transparent ultra-thin film ellipsometric ratio ρ 1 and substrate ellipsometric ratio ρ 0 are equal, if so, n T = ns , then calculate ρ 1 ' according to the refractive index n T of the transparent ultra-thin film, and use the formula Calculate the thickness d T of the transparent ultra-thin film, wherein, Imρ 1 is the imaginary part of the ellipsometry ratio ρ 1 of the transparent ultra-thin film, and λ is the wavelength of the incident light; if not, then go to step S42;
S42通过下式计算出透明超薄膜的两个折射率:S42 calculates the two refractive indices of the transparent ultra-thin film by the following equations:
S43根据透明超薄膜的两个折射率利用公式分别计算出两个厚度,然后利用厚度需为正的物理条件判断出正确的折射率。S43 utilizes the formula according to the two refractive indices of the transparent ultra-thin film Calculate the two thicknesses separately, and then use the physical condition that the thickness needs to be positive to determine the correct refractive index.
作为进一步优选的,ρ1'采用如下公式计算:As a further preference, ρ 1 ' is calculated by the following formula:
其中,n0为周围介质的折射率,ns为基底折射率,θ0为入射光的入射角,θ1为入射光在基底的折射角,nT为步骤S4求解出的透明超薄膜的折射率。Among them, n 0 is the refractive index of the surrounding medium, n s is the refractive index of the substrate, θ 0 is the incident angle of the incident light, θ 1 is the refraction angle of the incident light at the substrate, and n T is the transparent ultra-thin film calculated in step S4. refractive index.
总体而言,通过本发明所构思的以上技术方案与现有技术相比,主要具备以下的技术优点:In general, compared with the prior art, the above technical solutions conceived by the present invention mainly have the following technical advantages:
本发明通过对椭偏比进行二阶泰勒展开获得幂级数形式,并通过一系列转换和计算可实现透明超薄膜(厚度在5nm-20nm范围内)的折射率和厚度的快速测量计算,与现有透明超薄膜测量表征方法相比,本发明方法避免了建模拟合过程中的厚度不唯一性,操作简便、无复杂分析过程,且对透明超薄膜及基底无特殊要求,可适用于在透明或近似透明基底上的任意透明超薄膜,适用范围广,测量准确。本发明直接通过少量的公式计算即可获得透明超薄膜的折射率,并基于透明超薄膜的折射率计算得到透明超薄膜的厚度,测量快速准确,在透明超薄膜测量表征领域有广泛的应用前景。The present invention obtains the power series form by performing second-order Taylor expansion on the ellipsometry ratio, and can realize the rapid measurement and calculation of the refractive index and thickness of the transparent ultra-thin film (thickness in the range of 5nm-20nm) through a series of conversions and calculations. Compared with the existing transparent ultra-thin film measurement and characterization methods, the method of the present invention avoids the thickness non-uniqueness in the modeling and fitting process, is easy to operate, has no complicated analysis process, and has no special requirements for the transparent ultra-thin film and the substrate, and can be applied to Any transparent ultra-thin film on a transparent or nearly transparent substrate has a wide range of applications and accurate measurement. The method can directly obtain the refractive index of the transparent ultra-thin film through a small amount of formula calculation, and calculate the thickness of the transparent ultra-thin film based on the refractive index of the transparent ultra-thin film, the measurement is fast and accurate, and has wide application prospects in the field of measurement and characterization of the transparent ultra-thin film .
附图说明Description of drawings
图1是本发明实施例提供的透明超薄膜的折射率及厚度计算方法的流程图;Fig. 1 is the flow chart of the refractive index and the thickness calculation method of the transparent ultra-thin film that the embodiment of the present invention provides;
图2是本发明实施例提供的玻璃基底在600~1000nm波段范围的光学常数光谱曲线;Fig. 2 is the optical constant spectral curve of the glass substrate provided in the embodiment of the present invention in the wavelength range of 600-1000 nm;
图3是本发明实施例提供的玻璃基底氧化铝薄膜样品光学模型示意图;3 is a schematic diagram of an optical model of a glass-substrate alumina film sample provided in an embodiment of the present invention;
图4是本发明实施例提供的利用光谱椭偏仪测量玻璃基底氧化铝薄膜椭偏参数示意图;4 is a schematic diagram of measuring ellipsometry parameters of glass-substrate alumina thin films using a spectral ellipsometer provided by an embodiment of the present invention;
图5是本发明实施例提供的在入射角60°、入射光波长在600-1000nm范围内时计算得到的玻璃基底上氧化铝超薄膜的折射率;5 is the refractive index of the alumina ultra-thin film on the glass substrate calculated when the incident angle is 60° and the incident light wavelength is in the range of 600-1000nm according to the embodiment of the present invention;
图6是本发明实施例提供的在入射角60°、入射光波长在600-1000nm范围内时计算得到的玻璃基底上氧化铝超薄膜的厚度。FIG. 6 is the thickness of the ultra-thin aluminum oxide film on the glass substrate calculated and obtained when the incident angle is 60° and the incident light wavelength is in the range of 600-1000 nm according to the embodiment of the present invention.
在所有附图中,相同的附图标记用来表示相同的元件或结构,其中:Throughout the drawings, the same reference numbers are used to refer to the same elements or structures, wherein:
1-光源、2-起偏臂、3-样品台、4-检偏臂、5-探测器、6-待测样品。1-light source, 2-polarizing arm, 3-sample stage, 4-analyzing arm, 5-detector, 6-sample to be tested.
具体实施方式Detailed ways
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合附图及实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。此外,下面所描述的本发明各个实施方式中所涉及到的技术特征只要彼此之间未构成冲突就可以相互组合。In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention, but not to limit the present invention. In addition, the technical features involved in the various embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.
如图1所示,本发明实施例提供的一种透明超薄膜的折射率及厚度测量方法,用于实现透明超薄膜折射率和厚度的快速准确测量,测量之前先获取各项测量参数,包括入射光波长λ范围Γ、入射光的入射角θ0、基底折射率ns、周围介质折射率n0、入射光进入基底的折射角θ1、透明超薄膜的椭偏比ρ1和基底的椭偏比ρ0。具体的,根据材料特性、所用仪器等实际情况,选择测量波长范围Γ和入射角θ0;通过实验测量、查阅文献或数据库等途径,获取所选取的波长范围Γ内相关材料(包括基底材料、周围介质材料等)的光学常数(基底折射率ns和周围介质折射率n0),根据计算方法的要求基底材料需要满足透明或近似透明条件(消光系数小于0.01);入射光进入基底的折射角θ1通过n0sin(θ0)=nssin(θ1)计算;通过椭偏仪或成像椭偏仪等测得透明超薄膜的椭偏参数幅值比Ψ1和相位差Δ1,基底的椭偏参数幅值比Ψ0和相位差Δ0,计算获得透明超薄膜椭偏比ρ1=tanΨ1×exp(iΔ1)和基底的椭偏比ρ0=tanΨ0×exp(iΔ0)。As shown in FIG. 1, a method for measuring the refractive index and thickness of a transparent ultra-thin film provided by an embodiment of the present invention is used to realize the fast and accurate measurement of the refractive index and thickness of the transparent ultra-thin film. Before the measurement, various measurement parameters are obtained, including The wavelength λ range Γ of the incident light, the incident angle θ 0 of the incident light, the refractive index of the substrate ns , the refractive index of the surrounding medium n 0 , the refraction angle θ 1 of the incident light entering the substrate, the ellipsometry ratio ρ 1 of the transparent ultra-thin film and the Ellipsometry ratio ρ 0 . Specifically, according to the actual conditions such as material characteristics and instruments used, the measurement wavelength range Γ and the incident angle θ 0 are selected; through experimental measurement, reference to literature or databases, etc., obtain the selected wavelength range Γ. Related materials (including substrate materials, The optical constants (substrate refractive index n s and surrounding medium refractive index n 0 ) of surrounding medium materials, etc., according to the requirements of the calculation method, the substrate material needs to meet the transparent or nearly transparent conditions (extinction coefficient is less than 0.01); the refraction of incident light entering the substrate The angle θ 1 is calculated by n 0 sin(θ 0 )= ns sin(θ 1 ); the ellipsometry parameter amplitude ratio Ψ 1 and phase difference Δ 1 of the transparent ultra-thin film are measured by ellipsometer or imaging ellipsometer, etc. , the ellipsometry parameter amplitude ratio Ψ 0 and the phase difference Δ 0 of the substrate, the transparent ultra-thin film ellipsometry ratio ρ 1 =tanΨ 1 ×exp(iΔ 1 ) and the substrate ellipsometry ratio ρ 0 =tanΨ 0 ×exp( iΔ 0 ).
对于任意透明超薄膜而言,本发明的测量方法包括以下步骤:For any transparent ultra-thin film, the measuring method of the present invention comprises the following steps:
S1以2πdT/λ为变量对透明超薄膜椭偏比ρ1进行二阶泰勒展开获得幂级数形式(二阶近似形式):S1 takes 2πd T /λ as the variable to perform the second-order Taylor expansion of the ellipsometry ratio ρ 1 of the transparent ultra-thin film to obtain the power series form (second-order approximate form):
首先,利用入射光的p光反射系数与入射光的s光反射系数之比表达透明超薄膜椭偏比ρ1,关系如下:First, the ratio of the p light reflection coefficient of the incident light to the s light reflection coefficient of the incident light is used to express the ellipsometry ratio ρ 1 of the transparent ultra-thin film, and the relationship is as follows:
其中,rp为入射光的p光的反射系数,其具体计算公式如下:Among them, r p is the reflection coefficient of the p light of the incident light, and its specific calculation formula is as follows:
其中,ns为基底折射率,n0为周围介质的折射率,λ为入射光波长,dT为待测透明超薄膜的厚度,θ1为入射光进入基底的折射角,nT为待测透明超薄膜的折射率;where n s is the refractive index of the substrate, n 0 is the refractive index of the surrounding medium, λ is the wavelength of the incident light, d T is the thickness of the transparent ultra-thin film to be measured, θ 1 is the refraction angle of the incident light entering the substrate, and n T is the Measuring the refractive index of transparent ultra-thin films;
rs为入射光的s光反射系数,其具体计算公式如下:rs is the s light reflection coefficient of the incident light, and its specific calculation formula is as follows:
然后,将式(1)-(3)所描述的公式围绕2πdT/λ展开成幂级数形式,并省去二阶以上高阶项得:Then, expand the formula described by equations (1)-(3) into a power series form around 2πd T /λ, and omit the higher-order terms above the second order:
其中,系数项分别为:Among them, the coefficient terms are:
S2分离出幂级数形式中与透明超薄膜厚度dT相关的参量T1和T2:S2 separates out the parameters T 1 and T 2 related to the thickness d T of the transparent ultrathin film in the form of a power series:
S3计算幂级数形式的实部与虚部平方的斜率R,根据斜率R计算的具体值:S3 calculates the slope R of the square of the real part and the imaginary part in the form of a power series, and calculates according to the slope R The specific value of:
假设周围介质、超薄膜以及基底都是透明的情况下,式(4)中常数项和三次项为实数,线性项为虚数,对公式(4)分离实部Reρ1和虚部Imρ1得到:Assuming that the surrounding medium, ultra-thin film and substrate are all transparent, the constant term and the cubic term in equation (4) are real numbers, and the linear term is an imaginary number. For equation (4), the real part Reρ 1 and the imaginary part Imρ 1 are separated to obtain:
根据式(11)得:将及式(5)~(7)代入式(10)中化简得:According to formula (11), we get: Will And formulas (5)-(7) are substituted into formula (10) and simplified to get:
从上述公式(12)可以看出Reρ1和(Imρ1)2间存在线性关系,R表示斜率。From the above formula (12), it can be seen that there is a linear relationship between Reρ 1 and (Imρ 1 ) 2 , and R represents the slope.
其中:in:
根据式(8)和(9)得:According to formulas (8) and (9), we get:
具体的,斜率R采用下式计算:Specifically, the slope R is calculated by the following formula:
其中,Reρ0和Reρ1分别为事先测得的基底椭偏比ρ0的实部和透明超薄膜椭偏比ρ1的实部,Imρ0和Imρ1分别为基底椭偏比ρ0的虚部和透明超薄膜椭偏比ρ1的虚部。Wherein, Reρ 0 and Reρ 1 are respectively the real part of the substrate ellipsometry ratio ρ 0 and the real part of the transparent ultra-thin film ellipsometry ratio ρ 1 , respectively, and Imρ 0 and Imρ 1 are respectively the imaginary base ellipsometry ratio ρ 0 part and the imaginary part of the ellipsometry ratio ρ1 of the transparent ultrathin film.
通过式(13)可得:By formula (13), it can be obtained:
将式(15)计算获得的R及事先测量获得的基底折射率ns、周围介质折射率n0、入射光的入射角θ0和入射光进入基底的折射角θ1代入式(16)中计算获得 Substitute the R calculated from the formula (15) and the refractive index ns of the substrate, the refractive index n 0 of the surrounding medium, the incident angle θ 0 of the incident light and the refraction angle θ 1 of the incident light entering the substrate into the formula (16). Calculated
S4将步骤S3计算的具体值代入式(14)中求解出透明超薄膜的折射率nT,再根据透明超薄膜的折射率nT计算透明超薄膜的厚度。S4 will be calculated in step S3 The specific value is substituted into the formula (14) to obtain the refractive index n T of the transparent ultra-thin film, and then the thickness of the transparent ultra-thin film is calculated according to the refractive index n T of the transparent ultra-thin film.
一般情况下,对具体透明超薄膜材料,其折射率的大致范围可通过文献初步预估,然后判断其与基底折射率的关系,再选择对应计算公式进行精确计算,其中,当透明超薄膜折射率小于基底折射率时:In general, for a specific transparent ultra-thin film material, the approximate range of its refractive index can be preliminarily estimated from the literature, and then determine the relationship between it and the refractive index of the substrate, and then select the corresponding calculation formula for accurate calculation. When the ratio is less than the substrate refractive index:
当透明超薄膜折射率大于基底折射率时:When the refractive index of the transparent ultra-thin film is greater than that of the substrate:
另外,当获得的透明超薄膜椭偏比ρ1和基底椭偏比ρ0相等时,即说明透明超薄膜折射率等于基底折射率,由于基底折射率已知,则无需计算透明超薄膜折射率。In addition, when the obtained transparent ultra-thin film ellipsometry ratio ρ 1 and substrate ellipsometry ratio ρ 0 are equal, that is to say that the transparent ultra-thin film refractive index is equal to the substrate refractive index, because the substrate refractive index is known, then there is no need to calculate the transparent ultra-thin film refractive index .
当然,有时不好判断透明薄膜折射率与基底折射率的关系,因为预估的透明薄膜折射率为一个范围,基底折射率可能在这范围内,故难以确定两者之间的关系,此时可以同时计算两组折射率和厚度,然后利用错误解计算出的厚度不符合物理条件(即为负数)对两组解进行排除。Of course, sometimes it is not easy to judge the relationship between the refractive index of the transparent film and the refractive index of the substrate, because the estimated refractive index of the transparent film is within a range, and the refractive index of the substrate may be within this range, so it is difficult to determine the relationship between the two. Two sets of refractive indices and thicknesses can be calculated at the same time, and then the two sets of solutions can be excluded by using the thickness calculated by the wrong solution that does not meet the physical conditions (ie, a negative number).
具体而言,利用式(17a)和(17b)分别计算出两个折射率,再根据两个折射率利用式(18)分别计算出两个厚度,其中厚度大于零的对应的折射率为正确解,厚度小于零的对应的折射率为错误解,予以排除。Specifically, two indices of refraction are calculated using equations (17a) and (17b), respectively, and two thicknesses are calculated using equation (18) according to the two indices of refraction, where the corresponding indices of refraction whose thickness is greater than zero are correct. solution, the corresponding refractive index with thickness less than zero is an incorrect solution and is excluded.
具体的,根据透明超薄膜的折射率nT采用下式计算透明超薄膜的厚度:Specifically, according to the refractive index n T of the transparent ultra-thin film, the thickness of the transparent ultra-thin film is calculated by the following formula:
其中,ρ1为事先测得的透明超薄膜的椭偏比,Imρ1指的是透明超薄膜椭偏比ρ1的虚部,ρ1'计算公式为:即将计算获得的透明超薄膜的折射率nT及事先测量获得的基底折射率ns、周围介质折射率n0、入射光的入射角θ0和入射光进入基底的折射角θ1代入式(5)中计算获得ρ1'。若透明超薄膜的折射率nT与基底折射率相等,则透明超薄膜的厚度无法通过上述公式求出,可更换其他基底来进行测量分析,但这种情况很少发生,自然界中很少有材料的折射率相同,且折射率会随着波长的变化而改变,两种材料的折射率在整个波段内不会完全相同。Wherein, ρ 1 is the ellipsometry ratio of the transparent ultra-thin film measured in advance, Imρ 1 refers to the imaginary part of the ellipsometry ratio ρ 1 of the transparent ultra-thin film, and the calculation formula of ρ 1 ' is: The refractive index n T of the transparent ultra-thin film to be calculated and the refractive index n s of the substrate obtained by the previous measurement, the refractive index n 0 of the surrounding medium, the incident angle θ 0 of the incident light and the refraction angle θ 1 of the incident light entering the substrate are substituted into the formula ( 5) to obtain ρ 1 '. If the refractive index n T of the transparent ultra-thin film is equal to the refractive index of the substrate, the thickness of the transparent ultra-thin film cannot be calculated by the above formula, and other substrates can be replaced for measurement and analysis, but this situation rarely occurs, and rarely occurs in nature. Materials have the same index of refraction, and the index of refraction varies with wavelength, and the index of refraction of two materials will not be exactly the same over the entire wavelength band.
以下为具体实施例,为了更清楚的阐述本发明所述透明超薄膜折射率及厚度快速测量方法的实施过程,本实施例中优选采用光谱型椭偏仪对玻璃基底上的氧化铝超薄膜进行测量,通过公式(17a)、(17b)和公式(18)计算氧化铝的折射率和厚度,具体如下:The following are specific examples. In order to more clearly describe the implementation process of the method for rapidly measuring the refractive index and thickness of the transparent ultra-thin film of the present invention, in this embodiment, a spectral ellipsometer is preferably used to conduct the ultra-thin alumina film on the glass substrate. Measure, calculate the refractive index and thickness of alumina by formula (17a), (17b) and formula (18), as follows:
(1)选择测量的波长范围,选取测量的波长范围为Γ=[600,1000]nm;(1) Select the wavelength range for measurement, and select the wavelength range for measurement as Γ=[600,1000] nm;
(2)选定测量入射角,入射角选择没有特殊要求,一般椭偏仪可以测量的角度均可,本次入射角选择θ0=60°;(2) Select the incident angle for measurement. There is no special requirement for the selection of the incident angle. Generally, any angle that can be measured by the ellipsometer can be used. This time, the incident angle is selected as θ 0 =60°;
(3)确定所用玻璃基底和周围介质的光学常数,准确确定基底的光学常数是后续精确计算氧化铝超薄膜厚度的前提,对于光学常数比较稳定的基底材料可以直接使用文献参考值,为了保证计算结果的准确性也可以使用椭偏仪测量玻璃基底的椭偏参数,拟合得到其光学常数。透明基底会存在基底背面反射的非相干光,干扰测量结果,一般采用对基底进行打磨处理或者进行折射率匹配使测量光进入匹配材料来消除非相干光的干扰,在60°入射角下对玻璃基底进行椭偏测量,玻璃基底的折射率可利用柯西(Cauchy)模型拟合得到,周围介质为空气,其折射率n0=1,玻璃基底的折射率ns(λ)如图2所示;(3) Determine the optical constants of the glass substrate and the surrounding medium. Accurate determination of the optical constants of the substrate is the premise for the subsequent accurate calculation of the thickness of the ultra-alumina ultra-thin film. For the substrate materials with relatively stable optical constants, the reference value of literature can be used directly. The accuracy of the results can also be measured by using an ellipsometer to measure the ellipsometry parameters of the glass substrate, and its optical constants can be obtained by fitting. The transparent substrate will have incoherent light reflected from the back of the substrate, which will interfere with the measurement results. Generally, the substrate is polished or the index of refraction is matched to make the measurement light enter the matching material to eliminate the interference of the incoherent light. The substrate is measured by ellipsometry. The refractive index of the glass substrate can be obtained by fitting the Cauchy model. The surrounding medium is air, and its refractive index n 0 =1. The refractive index of the glass substrate ns (λ) is shown in Figure 2. Show;
(4)利用椭偏仪测量超薄氧化铝薄膜和空白基底的椭偏参数:(4) Using an ellipsometer to measure the ellipsometric parameters of the ultra-thin alumina thin film and blank substrate:
光以选定的60°角度入射,测量待测样品的椭偏参数(λ)和空白基底的椭偏参数ρsubstrate(λ);测量装置示意图如图4所示,所用椭偏仪由光源1、起偏臂2、样品台3、检偏臂4、探测器5等组成,待测样品6放置在样品台3上;光自光源1出射经起偏臂2变为偏振光,照射到待测样品6上,偏振光与待测样品6作用,偏振态发生改变,反射光经过检偏臂4后被探测器5接收,上述为通过椭偏仪探测椭偏参数的基本过程;The light is incident at a selected angle of 60°, and the ellipsometry parameters of the sample to be measured are measured (λ) and the ellipsometry parameter ρ substrate (λ) of the blank substrate; the schematic diagram of the measurement device is shown in Figure 4. The ellipsometer used consists of a light source 1, a polarizing arm 2, a sample stage 3, an analyzer arm 4, and a detector 5 The sample 6 to be tested is placed on the sample stage 3; the light emitted from the light source 1 is transformed into polarized light through the polarizing arm 2, and irradiated on the sample to be tested 6, the polarized light interacts with the sample to be tested 6, and the polarization state changes , the reflected light is received by the detector 5 after passing through the analyzer arm 4, and the above is the basic process of detecting the ellipsometric parameters by the ellipsometer;
(5)计算待测超薄氧化铝的折射率(λ):(5) Calculate the refractive index of the ultra-thin alumina to be measured (λ):
利用第(4)步测量数据,采用以下公式计算:Using the measured data in step (4), use the following formula to calculate:
查看网上光学常数数据库,玻璃基底的折射率在1.5附近,氧化铝的折射率在1.7附近,由于对应波长下的氧化铝超薄膜折射率大于基底折射率,故(λ)采用下式计算:Looking at the online optical constant database, the refractive index of the glass substrate is around 1.5, and the refractive index of alumina is around 1.7. (λ) is calculated using the following formula:
其中,进入基底的折射角θ1通过计算。where the angle of refraction θ 1 entering the substrate passes through calculate.
图5为在入射角60°、入射光波长在600-1000nm范围内时,计算得到的玻璃基底上氧化超薄膜的折射率;Figure 5 is the calculated refractive index of the ultra-thin oxide film on the glass substrate when the incident angle is 60° and the incident light wavelength is in the range of 600-1000nm;
(6)计算待测超薄氧化铝的厚度d:(6) Calculate the thickness d of the ultra-thin alumina to be tested:
由于选择了光谱椭偏测量,因此在每个波长点下都可以计算得到一个厚度值d(λ):Since spectral ellipsometry is selected, a thickness value d(λ) can be calculated at each wavelength point:
图6是在入射角60°、入射光波长在600-1000nm范围内时,计算得到的玻璃基底上氧化超薄膜的厚度。从图6中可以看出所得结果在不同波长下会有一定变化,这是由于二阶公式近似导致的结果不准确,但是该误差是在亚纳米量级,通过对厚度取均值得到氧化铝的最终厚度d为10.23nm,本发明以椭偏参数为基础数据进行计算可以避免单波长测量下测量系统随机误差导致的测量结果误差。Figure 6 shows the calculated thickness of the ultra-thin oxide film on the glass substrate when the incident angle is 60° and the incident light wavelength is in the range of 600-1000 nm. It can be seen from Figure 6 that the obtained results will vary at different wavelengths. This is due to the inaccuracy of the results caused by the approximation of the second-order formula, but the error is in the sub-nanometer level. The final thickness d is 10.23 nm, and the present invention calculates based on the ellipsometry parameter, which can avoid the measurement result error caused by the random error of the measurement system under single-wavelength measurement.
上述实施例仅以玻璃基底上的氧化铝薄膜为例,对于其余种类的透明超薄膜材料或不同的透明基底类型也可以依照同种方法进行折射率和厚度测量。The above embodiment only takes the aluminum oxide film on the glass substrate as an example, and the refractive index and thickness measurement can also be performed according to the same method for other types of transparent ultra-thin film materials or different types of transparent substrates.
本发明所提供的透明超薄膜折射率和厚度快速测量方法避免了传统建模拟合情况下透明超薄膜折射率未知使得厚度和折射率相互耦合,无法准确唯一确定透明超薄膜折射率和厚度的难题,可实现透明超薄膜折射率和厚度的快速准确测量和计算,原理简单,易于操作。The method for fast measurement of the refractive index and thickness of the transparent ultra-thin film provided by the invention avoids the fact that the refractive index of the transparent ultra-thin film is unknown in the traditional modeling fitting situation, which makes the thickness and the refractive index coupled with each other, and cannot accurately and uniquely determine the refractive index and thickness of the transparent ultra-thin film. It can realize fast and accurate measurement and calculation of the refractive index and thickness of transparent ultra-thin films. The principle is simple and easy to operate.
本发明方法并不局限于上述具体实施方式,本领域一般技术人员根据本发明公开的内容,可以采用其它多种具体实施方式实施本发明,如换用其他能够测量偏振信息的仪器或者换用其他透明或吸收很少的基底,因此,凡是采用本发明的设计方法原理和思路,做一些简单的变化或更改的设计,都落入本发明保护的范围。The method of the present invention is not limited to the above-mentioned specific embodiments. Those skilled in the art can use other specific embodiments to implement the present invention according to the content disclosed in the present invention, such as using other instruments capable of measuring polarization information or using other The substrate is transparent or absorbs little. Therefore, any simple change or modification of the design using the principles and ideas of the design method of the present invention falls within the protection scope of the present invention.
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