CN103824903B - Substrate processing method for improving emission compensation temperature measurement accuracy or consistency - Google Patents
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Abstract
一种提高发射补偿测温准确性或一致性的衬底加工方法，涉及LED材料工程技术领域。本发明的方法步骤为：对于探测光波长而透明的衬底，平衬底采用双面抛光处理。将图形化衬底正面图形的表面进行平整和光滑处理，并保持图形结构几何特征的均一性，图形化衬底背面进行再抛光处理。对于探测光波长非透明的衬底，平衬底仅进行正面抛光处理。将图形化衬底正面图形的表面进行平整和光滑处理，并保持图形结构几何特征的均一性。加工后的平衬底或者图形化衬底的弯曲度、翘曲度和总厚度变化均小于15微米。本发明通过对平衬底或者图形化衬底表面的加工处理，使衬底表面均匀性提高，以提升测试精度。
A substrate processing method for improving the accuracy or consistency of emission compensation temperature measurement relates to the technical field of LED material engineering. The method steps of the invention are as follows: for the substrate which is transparent for the detection light wavelength, the flat substrate is treated with double-side polishing. The surface of the front pattern of the patterned substrate is flattened and smoothed, and the uniformity of the geometric characteristics of the pattern structure is maintained, and the back of the patterned substrate is re-polished. For substrates that are not transparent to the probe light wavelength, only the front side of the flat substrate is polished. The surface of the pattern on the front side of the patterned substrate is flattened and smoothed, and the uniformity of the geometric characteristics of the pattern structure is maintained. The curvature, warpage and total thickness variation of the processed flat substrate or patterned substrate are all less than 15 microns. The invention improves the uniformity of the substrate surface by processing the surface of the flat substrate or the patterned substrate to improve the test accuracy.
Description
技术领域technical field
本发明涉及LED材料工程技术领域，特别是能提高采用发射补偿型测温方式准确性或一致性的LED外延材料生长设备上使用的衬底的加工方法。The invention relates to the technical field of LED material engineering, in particular to a method for processing substrates used in LED epitaxial material growth equipment that can improve the accuracy or consistency of emission compensation temperature measurement methods.
背景技术Background technique
有机金属化学气相沉积（英文缩写为MOCVD）设备或技术是目前产业界广泛用于制造化合物半导体的方法。它能够在一定的衬底材料上外延出涵盖Ⅲ-Ⅴ族化合物，如氮化物、磷化物、砷化物等，以及Ⅱ-Ⅵ族化合物，如氧化物、硫化物等的单晶晶体。而这些材料大多是宽禁带半导体，在电子、光电子行业有着丰富多样的用途，比如，采用上述材料制造发光二极管、激光二极管、光电二极管、太阳能光伏电池、场效应晶体管、高电子迁移率晶体管等等。Metal-Organic Chemical Vapor Deposition (MOCVD) equipment or technology is currently a method widely used in the industry to manufacture compound semiconductors. It can epitaxially produce single crystals covering group III-V compounds, such as nitrides, phosphides, arsenides, etc., and group II-VI compounds, such as oxides and sulfides, on certain substrate materials. Most of these materials are wide-bandgap semiconductors, which have a variety of uses in the electronics and optoelectronics industries. For example, the above materials are used to manufacture light-emitting diodes, laser diodes, photodiodes, solar photovoltaic cells, field-effect transistors, high electron mobility transistors, etc. Wait.
在MOCVD设备上，温控系统是其中最重要的组成部分之一，它可大致分为两大模块：温度测量模块和温度控制模块。因为在一定的压强条件下，当各种反应物齐备时，温度主要决定了材料的相变、结晶程度、微结构等物理、化学性质。在某些应用场合中，温控系统对反应温度的测量与控制的准确性或一致性对材料品质、参数良率和产品可复制性有着重要意义。例如，在MOCVD上进行氮化物发光二极管（LED）的多量子阱（MQW）外延结构生长时，最终产品LED器件的发射光谱主波长会随MQW的合成温度灵敏变化。比如MQW的合成温度变化1℃，则LED的主波长将变化2～5纳米左右。而LED产品对主波长的分档规格一般控制在±2.5纳米以下，由此可以看到精确或可重现地控制MQW合成温度对LED主波长良率的重要性。On MOCVD equipment, the temperature control system is one of the most important components, which can be roughly divided into two modules: temperature measurement module and temperature control module. Because under certain pressure conditions, when all kinds of reactants are available, the temperature mainly determines the physical and chemical properties of the material such as phase transition, crystallization degree, and microstructure. In some applications, the accuracy or consistency of the temperature control system's measurement and control of the reaction temperature is of great significance to material quality, parameter yield and product reproducibility. For example, when the multi-quantum well (MQW) epitaxial structure of nitride light-emitting diode (LED) is grown on MOCVD, the dominant wavelength of the emission spectrum of the final product LED device will change sensitively with the synthesis temperature of MQW. For example, if the synthesis temperature of MQW changes by 1°C, the dominant wavelength of the LED will change by about 2 to 5 nanometers. The binning specifications of the dominant wavelength of LED products are generally controlled below ±2.5 nanometers. From this, we can see the importance of accurately or reproducibly controlling the MQW synthesis temperature for the yield of the dominant wavelength of LEDs.
现有技术中，发射补偿型测温方式是MOCVD设备上常见的一种测温方法。该种方法的实体被称为发射补偿型温度计，它是温控系统的测量模块。参看图1，发射补偿型温度计位于MOCVD反应室上部的观察口位置，通过量测目标样品的热辐射强度和反射率来计算目标样品的温度。其计算原理可通过普朗克黑体辐射公式与基尔霍夫辐射定律推导，具体表达式如下：In the prior art, the emission compensation type temperature measurement method is a common temperature measurement method on MOCVD equipment. The entity of this method is called an emission-compensated thermometer, which is the measurement module of the temperature control system. Referring to Figure 1, the emission compensation thermometer is located at the observation port on the upper part of the MOCVD reaction chamber, and the temperature of the target sample is calculated by measuring the thermal radiation intensity and reflectivity of the target sample. Its calculation principle can be derived through Planck’s black body radiation formula and Kirchhoff’s radiation law, and the specific expressions are as follows:
其中，T为样品温度，λ为温度计的探测波长（即测量样品反射率时的光源波长），α t 为样品的吸收率，E t 为样品在λ波长下的热辐射强度，c 1 、c 2 为常数。Among them, T is the sample temperature, λ is the detection wavelength of the thermometer (that is, the wavelength of the light source when measuring the reflectance of the sample), α t is the absorptivity of the sample, E t is the thermal radiation intensity of the sample at λ wavelength, c 1 , c 2 is a constant.
此外，对于波长λ而言是非透明材质的样品，其吸收率和反射率可根据能量守恒定律得到如下关系式：In addition, for a sample that is a non-transparent material for the wavelength λ , its absorptivity and reflectivity can be obtained according to the law of energy conservation as follows:
其中，R t 为被测样品的反射率。Among them, Rt is the reflectance of the tested sample.
公式、中样品的热辐射强度E t 和反射率R t 都通过发射补偿型温度计测量得到，进而通过公式得到样品的温度。formula , Both the thermal radiation intensity E t and the reflectance R t of the sample in the sample are measured by the emission compensation thermometer, and then obtained by the formula Get the temperature of the sample.
通常情况下，样品表面的反射率需要使用半空间的积分球才能准确测量，但是在MOCVD系统上观测外延片的反射率这样的设计却是难于实现的。一种简单的近似做法是在反应室上方预留一个观测口，在某一固定的空间立体角内收集和观测反射率，同时也对热辐射强度进行测量。不过使用这种方法有一定的局限，即若外延片或者衬底样品的表面处于粗糙或易于发生漫反射时，反射率的量测信号将是微弱或误差较大的。这样将造成测试软件的“模式识别”错误或温度计算不准、缺乏一致性和可重现性。只有当样品表面处于理想镜面时，反射率探测才能获得最大的信噪比，并保持较高的精度或一致性。Usually, the reflectance of the sample surface needs to be measured accurately by using a half-space integrating sphere, but it is difficult to realize the design of observing the reflectance of the epitaxial wafer on the MOCVD system. A simple approximation is to reserve an observation port above the reaction chamber to collect and observe the reflectivity within a fixed spatial solid angle, and measure the intensity of thermal radiation at the same time. However, this method has certain limitations, that is, if the surface of the epitaxial wafer or substrate sample is rough or prone to diffuse reflection, the measurement signal of the reflectance will be weak or have large errors. This will cause "pattern recognition" errors of the test software or inaccurate temperature calculations, lack of consistency and reproducibility. Only when the sample surface is a perfect mirror, reflectivity detection can achieve the maximum signal-to-noise ratio and maintain high accuracy or consistency.
发明内容Contents of the invention
针对上述现有技术中存在的发射补偿型温度计适用局限，本发明的目的是提供一种提高发射补偿测温准确性或一致性的衬底加工方法。它通过对平衬底或者图形化衬底表面的加工处理，使衬底表面均匀性提高，以提升测试精度。In view of the application limitations of emission compensation thermometers in the above-mentioned prior art, the purpose of the present invention is to provide a substrate processing method that improves the accuracy or consistency of emission compensation temperature measurement. It improves the uniformity of the substrate surface by processing the surface of the flat substrate or patterned substrate to improve the test accuracy.
为了达到上述发明目的，本发明的技术方案以如下方式实现：In order to achieve the above-mentioned purpose of the invention, the technical solution of the present invention is realized in the following manner:
一种提高发射补偿测温准确性或一致性的衬底加工方法，所述衬底是制备发光二极管产品进行材料生长的承载基板。其步骤为：对于探测光波长透明的衬底，平衬底采用双面抛光处理；然后将平衬底正面进行干法刻蚀工艺，制作金字塔形图形，形成图形化衬底，将图形化衬底正面图形的表面进行平整和光滑处理，并保持图形结构几何特征的均一性，图形化衬底背面进行再抛光处理。对于探测光波长非透明的衬底，平衬底仅进行正面抛光处理。然后将平衬底正面进行干法刻蚀工艺，制作金字塔形图形，形成图形化衬底，将图形化衬底正面图形的表面进行平整和光滑处理，并保持图形结构几何特征的均一性。加工后的平衬底或者图形化衬底的弯曲度、翘曲度和总厚度变化均小于15微米。A substrate processing method for improving the accuracy or consistency of emission compensation temperature measurement, the substrate is a carrier substrate for preparing light-emitting diode products for material growth. The steps are as follows: for a substrate with a transparent wavelength of detection light, the flat substrate is polished on both sides; then the front of the flat substrate is subjected to a dry etching process to produce a pyramid-shaped pattern to form a patterned substrate, and the patterned substrate is The surface of the bottom and front graphics is flattened and smoothed, and the uniformity of the geometric characteristics of the graphic structure is maintained, and the back of the patterned substrate is re-polished. For substrates that are not transparent to the probe light wavelength, only the front side of the flat substrate is polished. Then carry out the dry etching process on the front of the flat substrate to make a pyramid-shaped pattern to form a patterned substrate. The surface of the front pattern of the patterned substrate is flattened and smoothed, and the uniformity of the geometric characteristics of the pattern structure is maintained. The curvature, warpage and total thickness variation of the processed flat substrate or patterned substrate are all less than 15 microns.
在上述衬底加工方法中，所述图形结构包括周期性单元的形状和几何尺寸。In the above substrate processing method, the pattern structure includes the shape and geometric dimensions of the periodic units.
本发明由于采用了上述方法，经过加工处理的衬底更容易形成镜面反射，在使用发射补偿型温度计时可以增强反射信号，提高测温准确性、一致性。Because the method is adopted in the present invention, the processed substrate is more likely to form specular reflection, and the reflection signal can be enhanced when using the emission compensation type thermometer, so as to improve the accuracy and consistency of temperature measurement.
下面结合附图和具体实施方式对本发明做进一步说明。The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.
附图说明Description of drawings
图1为在MOCVD系统上发射补偿型温度计的量测示意图；Fig. 1 is the measurement schematic diagram of emission compensation type thermometer on MOCVD system;
图2为本发明中对于探测光波长透明的平衬底的加工示意图；Fig. 2 is the schematic diagram of the processing of the flat substrate transparent to the probe light wavelength in the present invention;
图3为本发明中对于探测光波长透明的图形化衬底的加工示意图；3 is a schematic diagram of processing a patterned substrate transparent to the probe light wavelength in the present invention;
图4为从发射补偿型温度计出射的探测光线经过粗糙背面衬底的反射光路；Fig. 4 is the reflection optical path of the detection light emitted from the emission compensation type thermometer passing through the rough back substrate;
图5为从发射补偿型温度计出射的探测光线经过本发明加工后衬底的反射光路。Fig. 5 is a reflection optical path of the detection light emitted from the emission compensation thermometer through the processed substrate of the present invention.
具体实施方式detailed description
参看图2和图3，本发明加工方法步骤为：对于探测光波长透明的衬底，平衬底采用双面抛光处理；然后将平衬底正面进行干法刻蚀工艺，制作金字塔形图形，形成图形化衬底，将图形化衬底正面图形的表面进行平整和光滑处理，并保持图形结构几何特征的均一性，图形化衬底背面再进行抛光处理。对于探测光波长非透明的衬底，平衬底仅进行正面抛光处理；然后将平衬底正面进行干法刻蚀工艺，制作金字塔形图形，形成图形化衬底，将图形化衬底正面图形的表面进行平整和光滑处理，并保持图形结构几何特征的均一性。抛光处理后的衬底表面粗糙度越小越好，以易于形成镜面发射。图形结构包括周期性单元的形状和几何尺寸。Referring to Fig. 2 and Fig. 3, the processing method step of the present invention is: for the substrate that probe light wavelength is transparent, flat substrate adopts double-sided polishing process; Then carry out dry etching process to the front of flat substrate, make pyramid figure, A patterned substrate is formed, the surface of the patterned substrate is flattened and smoothed, and the uniformity of the geometric characteristics of the patterned structure is maintained, and the back of the patterned substrate is polished. For the non-transparent substrate of the detection light wavelength, only the front side of the flat substrate is polished; then the front side of the flat substrate is subjected to a dry etching process to make a pyramid-shaped pattern to form a patterned substrate, and the front side of the patterned substrate is patterned The surface is smoothed and smoothed, and the uniformity of the geometric characteristics of the graphic structure is maintained. The smaller the surface roughness of the polished substrate, the better, so as to facilitate the formation of specular emission. The graph structure includes the shape and geometry of the periodic units.
下面以2英寸图形化蓝宝石衬底为例，说明本发明的一种具体实施方式。A specific embodiment of the present invention will be described below by taking a 2-inch patterned sapphire substrate as an example.
第一步，先将蓝宝石单晶延 c面0.2°偏角（偏向m面）方向切割成2英寸大小的Wafer，平边所对应的平面即是蓝宝石晶胞的a面，且平边对c轴的张角为30°。此外，Wafer的厚度在420～440微米范围；弯曲度、翘曲度以及总厚度变化应小于15微米；The first step is to first cut the sapphire single crystal into 2-inch wafers along the c-plane at a 0.2° off-angle (towards the m-plane). The plane corresponding to the flat side is the a-plane of the sapphire unit cell, and the flat side is opposite to the c The opening angle of the shaft is 30°. In addition, the thickness of Wafer is in the range of 420-440 microns; the curvature, warpage and total thickness change should be less than 15 microns;
第二步，对蓝宝石Wafer进行双面抛光处理，抛光的精细度越高越好，即表面粗糙度越小越好。优选地，抛光后的表面粗糙度应至少保持在0.5微米以下；The second step is to perform double-sided polishing on the sapphire wafer. The higher the fineness of the polishing, the better, that is, the smaller the surface roughness, the better. Preferably, the surface roughness after polishing should be kept at least below 0.5 microns;
第三步，选择蓝宝石正面进行干法刻蚀工艺，制作底面直径为2.6微米，高度为1.65微米，周期尺寸为3微米的金字塔形(Pyramid)图形。在该工艺过程中，应优化工艺参数以保证图形尺寸的几何均一性和图形表面的光滑、平整度。或者增添辅助工艺，采用物理或化学方法尽可能降低图形表面的粗糙度。The third step is to select the front side of the sapphire for a dry etching process to produce a pyramid pattern with a bottom diameter of 2.6 microns, a height of 1.65 microns, and a period size of 3 microns. During this process, the process parameters should be optimized to ensure the geometric uniformity of the graphic size and the smoothness and flatness of the graphic surface. Or add an auxiliary process, using physical or chemical methods to reduce the roughness of the graphic surface as much as possible.
经过以上三步制作的图形化蓝宝石衬底在采用发射补偿型温度计的MOCVD系统上进行氮化物LED外延结构的生长时，能提高LED外延片的主波长等参数的均匀性和一致性。When the patterned sapphire substrate produced by the above three steps is grown on the MOCVD system using an emission compensation thermometer for the growth of the nitride LED epitaxial structure, the uniformity and consistency of the dominant wavelength and other parameters of the LED epitaxial wafer can be improved.
以使用蓝宝石衬底在MOCVD上进行氮化物LED结构的外延生长为例，当LED外延片生长到MQW层时，氮化物、蓝宝石衬底及镀有SiC的石墨载盘共同组合成为发射补偿型温度计的测温目标。如果温度计中测量反射率使用的光源波长为930纳米，那么该波长光线对氮化物、蓝宝石衬底，及石石墨盘表层的SiC都是透明的，且此时近似镜面的GaN表面也为反射率和热辐射强度的测量提供了有利条件。假设石墨盘和SiC镀层的表面状况是均匀和不变的，那么衬底表面的状况将主要影响反射率的量测精度或一致性。以平衬底为例，930纳米的光线将在空气与氮化物、氮化物与蓝宝石衬底、蓝宝石衬底与空气之间的三个界面处发生反射和折射。参看图4，图中仅展示了到达衬底背面的反射光光路，倘若此时衬底的背面较粗糙而使光线发生漫反射时，将导致测温目标的反射率下降，由前述公式、计算得到的温度将会比实际值低，由此造成了温度量测误差。反之，如果衬底背面经过抛光处理，那么衬底背表面反射状况的均匀性也随之提高。如图5所示，则更容易形成镜面反射，如此便可增强反射信号，提高测温精度或一致性。类似地可以证明，对于探测波长非透明的衬底，平衬底的正面进行抛光处理或者充分提高图形化衬底表面图形的几何均匀性及表面光滑、平整度也能增加反射率信号强度，同时提高反射率和温度的测量精度或一致性。Taking the epitaxial growth of a nitride LED structure on MOCVD using a sapphire substrate as an example, when the LED epitaxial wafer grows to the MQW layer, the nitride, sapphire substrate and SiC-coated graphite carrier are combined to form an emission compensation thermometer. temperature measurement target. If the wavelength of the light source used to measure the reflectance in the thermometer is 930 nanometers, then the wavelength of light is transparent to the nitride, sapphire substrate, and SiC on the surface of the graphite disk, and the GaN surface, which is approximately a mirror surface, is also reflective. And the measurement of thermal radiation intensity provides favorable conditions. Assuming that the surface conditions of the graphite disk and the SiC coating are uniform and constant, the condition of the substrate surface will mainly affect the measurement accuracy or consistency of the reflectivity. Taking a flat substrate as an example, light at 930 nm will be reflected and refracted at three interfaces between air and nitride, nitride and sapphire substrate, and sapphire substrate and air. Referring to Figure 4, the figure only shows the optical path of the reflected light reaching the back of the substrate. If the back of the substrate is rough at this time and the light is diffusely reflected, the reflectivity of the temperature measurement target will decrease. According to the above formula , The calculated temperature will be lower than the actual value, thus causing a temperature measurement error. Conversely, if the back surface of the substrate is polished, the uniformity of the reflection on the back surface of the substrate will also be improved. As shown in Figure 5, it is easier to form specular reflection, which can enhance the reflection signal and improve the accuracy or consistency of temperature measurement. Similarly, it can be proved that for a non-transparent substrate at the detection wavelength, polishing the front of the flat substrate or fully improving the geometric uniformity, smoothness and flatness of the surface pattern of the patterned substrate can also increase the reflectivity signal intensity, and at the same time Improve the accuracy or consistency of reflectivity and temperature measurements.
上述仅公开了本发明的示范性实施例。对于本领域的相关技术人员依据本发明实例的技术思想，在具体实施方式及应用范围上的改变之处，都应属于本发明的保护范围。The foregoing discloses only exemplary embodiments of the present invention. For those skilled in the art, based on the technical ideas of the examples of the present invention, changes in specific implementation methods and application scopes shall all belong to the protection scope of the present invention.
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| SU1717976A1 (en) * | 1988-10-25 | 1992-03-07 | Восточно-Сибирский технологический институт | Temperature control method |
| US5388909A (en) * | 1993-09-16 | 1995-02-14 | Johnson; Shane R. | Optical apparatus and method for measuring temperature of a substrate material with a temperature dependent band gap |
| RU2148802C1 (en) * | 1999-01-27 | 2000-05-10 | Институт физики полупроводников СО РАН | Device for detection of heat radiation |
| CN1545140A (en) * | 2001-03-28 | 2004-11-10 | ��ʽ���綫֥ | Substrate temperature measurement method |
| CN1608199A (en) * | 2001-12-26 | 2005-04-20 | 沃泰克工业有限公司 | Method and system for measuring temperature and heat treatment |
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| SU1717976A1 (en) * | 1988-10-25 | 1992-03-07 | Восточно-Сибирский технологический институт | Temperature control method |
| US5388909A (en) * | 1993-09-16 | 1995-02-14 | Johnson; Shane R. | Optical apparatus and method for measuring temperature of a substrate material with a temperature dependent band gap |
| RU2148802C1 (en) * | 1999-01-27 | 2000-05-10 | Институт физики полупроводников СО РАН | Device for detection of heat radiation |
| CN1545140A (en) * | 2001-03-28 | 2004-11-10 | ��ʽ���綫֥ | Substrate temperature measurement method |
| CN1608199A (en) * | 2001-12-26 | 2005-04-20 | 沃泰克工业有限公司 | Method and system for measuring temperature and heat treatment |
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