CN111900200A - Diamond-based gallium nitride composite wafer and bonding preparation method thereof - Google Patents
Diamond-based gallium nitride composite wafer and bonding preparation method thereof Download PDFInfo
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Abstract
一种金刚石基氮化镓复合晶片及其键合制备方法,该晶片具有氮化镓/成核层/碳化硅/金属中间层/金刚石衬底、氮化镓/金属中间层/金刚石衬底、氮化镓/陶瓷膜层/金属中间层/金刚石衬底等结构,主要制备步骤为:减薄氮化镓的碳化硅衬底,或者将碳化硅衬底完全剥离并减薄氮化镓层;对碳化硅衬底或氮化镓层及金刚石的待键合表面进行抛光和氩等离子体处理;在碳化硅衬底待键合表面沉积金属缓冲层及金膜,或者在氮化镓层待键合表面沉积金属缓冲层和金膜或沉积陶瓷膜层、金属缓冲层和金膜,在金刚石待键合表面沉积金属缓冲层和金膜;先进行氮化镓与金刚石的预键合,再进行二次键合;对金刚石基氮化镓复合晶片进行退火处理。本发明能提高键合强度。
A diamond-based gallium nitride composite wafer and a bonding preparation method thereof, the wafer has gallium nitride/nucleation layer/silicon carbide/metal intermediate layer/diamond substrate, gallium nitride/metal intermediate layer/diamond substrate, For structures such as gallium nitride/ceramic film layer/metal intermediate layer/diamond substrate, the main preparation steps are: thinning the silicon carbide substrate of gallium nitride, or completely peeling off the silicon carbide substrate and thinning the gallium nitride layer; Polish and argon plasma treatment on the surface to be bonded of silicon carbide substrate or gallium nitride layer and diamond; deposit metal buffer layer and gold film on the to-be-bonded surface of silicon carbide substrate, or on the gallium nitride layer to be bonded Deposit metal buffer layer and gold film or deposit ceramic film, metal buffer layer and gold film on the bonding surface, deposit metal buffer layer and gold film on the diamond surface to be bonded; first perform pre-bonding of gallium nitride and diamond, and then carry out Secondary bonding; annealing GaN-on-diamond composite wafers. The present invention can improve the bond strength.
Description
技术领域technical field
本发明属于半导体与集成电路技术领域,具体涉及一种金刚石基氮化镓复合晶片及其键合制备方法,可应用于微波射频器件和电力电子器件的制作。The invention belongs to the technical field of semiconductors and integrated circuits, in particular to a diamond-based gallium nitride composite wafer and a bonding preparation method thereof, which can be applied to the manufacture of microwave radio frequency devices and power electronic devices.
背景技术Background technique
氮化镓作为第三代半导体材料,与硅和砷化镓材料相比,具有禁带宽度大、击穿场强高、饱和电子速度大、耐高温以及抗辐射能力强等特点,非常适合于高温大功率器件、高频微波器件、紫外和核辐射探测器件的制作,在通信、电力电子等技术领域均具有极高的应用价值。然而,严重的自热效应和低热导率限制了氮化镓器件固有优势的完全发挥,成为制约氮化镓器件进一步向高频、大功率方向发展的技术瓶颈。As a third-generation semiconductor material, gallium nitride has the characteristics of large band gap, high breakdown field strength, high saturation electron velocity, high temperature resistance and radiation resistance compared with silicon and gallium arsenide materials. It is very suitable for The production of high-temperature and high-power devices, high-frequency microwave devices, and ultraviolet and nuclear radiation detection devices has extremely high application value in technical fields such as communications and power electronics. However, the severe self-heating effect and low thermal conductivity limit the full play of the inherent advantages of GaN devices, and become the technical bottleneck restricting the further development of GaN devices in the direction of high frequency and high power.
金刚石具有很高的热导率,是碳化硅(氮化镓器件常用衬底材料之一)热导率的近五倍,用金刚石作为衬底材料可有效降低氮化镓器件的热阻,显著降低AlGaN/GaN结区温度。近年来国际上已开展的研究表明,采用金刚石衬底的氮化镓器件(金刚石基氮化镓复合器件)与以碳化硅为衬底的氮化镓器件(碳化硅基氮化镓复合器件)相比,由于散热问题的解决,器件输出功率密度、功率附加效率和可靠性均得到明显提高,并使模组尺寸进一步减小。因此,采用金刚石衬底是解决氮化镓器件热管理问题的一种有效方法。金刚石基氮化镓复合器件正发展成为高频和大功率半导体器件的一项主流技术。Diamond has a high thermal conductivity, which is nearly five times that of silicon carbide (one of the commonly used substrate materials for gallium nitride devices). Using diamond as a substrate material can effectively reduce the thermal resistance of gallium nitride devices. Lower AlGaN/GaN junction temperature. In recent years, international research has shown that gallium nitride devices using diamond substrates (GaN-on-diamond composite devices) and GaN devices using silicon carbide as substrates (GaN-on-SiC composite devices) In contrast, due to the solution of the heat dissipation problem, the output power density, power added efficiency and reliability of the device have been significantly improved, and the size of the module has been further reduced. Therefore, the use of diamond substrates is an effective method to solve the thermal management problem of GaN devices. GaN-on-diamond composite devices are developing into a mainstream technology for high-frequency and high-power semiconductor devices.
目前制备金刚石基氮化镓复合器件主要有三种方法,分别是在氮化镓表面外延生长金刚石、在金刚石表面外延生长氮化镓以及氮化镓与金刚石的键合。对于前两种方法,由于氮化镓与金刚石的热膨胀系数之间有较大失配,在较高温度下进行金刚石或氮化镓的外延生长,外延层中存在较大应力,容易引起晶片翘曲;此外,氮化镓与金刚石的晶格常数也存在较大差异,难以生长出高质量的氮化镓或金刚石外延层。与前两种采用金刚石或氮化镓外延生长方法制备金刚石基氮化镓复合器件不同,第三种方法采用的是氮化镓与金刚石的键合技术,该方法的优点是可以分别采用各自最佳的工艺制备出高质量的氮化镓和金刚石,键合可以在较低温度甚至室温下进行,避免了两种材料由于热膨胀系数和晶格常数失配所带来的问题。采用键合法制备金刚石基氮化镓复合器件,降低界面热阻、减少键合空洞率及提高键合强度是获得高键合质量的关键。At present, there are three main methods for preparing GaN-on-diamond composite devices, namely, epitaxial growth of diamond on the surface of gallium nitride, epitaxial growth of gallium nitride on the surface of diamond, and bonding of gallium nitride and diamond. For the first two methods, due to the large mismatch between the thermal expansion coefficients of gallium nitride and diamond, the epitaxial growth of diamond or gallium nitride at a higher temperature will cause a large stress in the epitaxial layer, which is easy to cause the wafer to warp. In addition, the lattice constants of gallium nitride and diamond are also quite different, making it difficult to grow high-quality gallium nitride or diamond epitaxial layers. Different from the first two methods to prepare GaN-on-diamond composite devices by epitaxial growth of diamond or gallium nitride, the third method uses the bonding technology of gallium nitride and diamond. The optimal process can produce high-quality gallium nitride and diamond, and the bonding can be carried out at lower temperature or even room temperature, avoiding the problems caused by the mismatch of thermal expansion coefficient and lattice constant between the two materials. Using the bonding method to fabricate GaN-on-diamond composite devices, reducing the interface thermal resistance, reducing the bonding void ratio and improving the bonding strength are the keys to obtain high bonding quality.
发明内容SUMMARY OF THE INVENTION
本发明的目的在于针对氮化镓器件制备存在的问题,提供一种金刚石基氮化镓复合晶片及其键合制备方法,能有效降低氮化镓与金刚石的界面热阻、减少键合空洞率并提高键合强度,从而制备出高性能的金刚石基氮化镓复合晶片,提升氮化镓器件优势的发挥。The purpose of the present invention is to solve the problems existing in the preparation of gallium nitride devices, to provide a diamond-based gallium nitride composite wafer and a bonding preparation method thereof, which can effectively reduce the interface thermal resistance between gallium nitride and diamond, and reduce the bonding void ratio. And improve the bonding strength, so as to prepare high-performance GaN-on-diamond composite wafers, and improve the play of the advantages of GaN devices.
为了实现上述目的,本发明采用如下的技术方案:In order to achieve the above object, the present invention adopts the following technical scheme:
一种金刚石基氮化镓复合晶片,具有以下a)、b)和c)中的任意一种结构:A gallium nitride-on-diamond composite wafer having any one of the following a), b) and c) structures:
a)依次由氮化镓、成核层、碳化硅、金属中间层、金刚石衬底形成的多层结构;a) a multilayer structure formed by gallium nitride, nucleation layer, silicon carbide, metal intermediate layer, and diamond substrate in sequence;
b)依次由氮化镓、金属中间层、金刚石衬底形成的多层结构;b) a multilayer structure formed by gallium nitride, a metal intermediate layer, and a diamond substrate in sequence;
c)依次由氮化镓、陶瓷膜层、金属中间层、金刚石衬底形成的多层结构,所述陶瓷膜层的材料为氮化铝或碳化硅;c) a multi-layer structure formed by gallium nitride, a ceramic film layer, a metal intermediate layer, and a diamond substrate in sequence, and the material of the ceramic film layer is aluminum nitride or silicon carbide;
所述的金属中间层具有依次设置的金属缓冲层、金膜层及金属缓冲层三层结构;所述金属缓冲层的材料为钨、钼或铝。The metal intermediate layer has a three-layer structure of a metal buffer layer, a gold film layer and a metal buffer layer arranged in sequence; the material of the metal buffer layer is tungsten, molybdenum or aluminum.
作为本发明金刚石基氮化镓复合晶片的一种优选方案,所述的结构a)、b)和c)中金刚石衬底的厚度为100-2000微米;金属缓冲层的厚度为1-20纳米;金膜层的厚度为5-200纳米;所述的结构a)中碳化硅的层厚为5-80微米;所述的结构b)中氮化镓的层厚为1-3微米;所述的结构c)中氮化镓的层厚为1-3微米,陶瓷膜层的厚度为1-15纳米。As a preferred solution of the diamond-based gallium nitride composite wafer of the present invention, the thickness of the diamond substrate in the structures a), b) and c) is 100-2000 microns; the thickness of the metal buffer layer is 1-20 nanometers The thickness of the gold film layer is 5-200 nanometers; the layer thickness of silicon carbide in the described structure a) is 5-80 micrometers; the layer thickness of gallium nitride in the described structure b) is 1-3 micrometers; In the aforementioned structure c), the thickness of the gallium nitride layer is 1-3 micrometers, and the thickness of the ceramic film layer is 1-15 nanometers.
本发明还提供一种金刚石基氮化镓复合晶片的键合制备方法,包括以下步骤:The present invention also provides a bonding preparation method of a diamond-based gallium nitride composite wafer, comprising the following steps:
1)用粘接剂将碳化硅衬底氮化镓的氮化镓外延层一侧的表面与临时载片粘接在一起;1) bonding the surface of the gallium nitride epitaxial layer on the silicon carbide substrate gallium nitride with the temporary carrier with an adhesive;
2)将碳化硅衬底减薄;或者将碳化硅衬底完全剥离,去除成核层,将氮化镓外延层减薄;2) thinning the silicon carbide substrate; or completely peeling off the silicon carbide substrate, removing the nucleation layer, and thinning the gallium nitride epitaxial layer;
3)对已减薄的碳化硅衬底表面或已减薄的氮化镓外延层的表面进行抛光,并对金刚石表面进行抛光,使碳化硅衬底或氮化镓外延层及金刚石抛光面的粗糙度低于要求值;3) Polish the surface of the thinned silicon carbide substrate or the surface of the thinned gallium nitride epitaxial layer, and polish the diamond surface, so that the silicon carbide substrate or the gallium nitride epitaxial layer and the diamond polished surface are polished. The roughness is lower than the required value;
4)先后用丙酮、乙醇和去离子水对氮化镓和金刚石进行超声波清洗;4) ultrasonically clean gallium nitride and diamond with acetone, ethanol and deionized water successively;
5)以碳化硅衬底或氮化镓外延层的抛光面为氮化镓的待键合表面,以金刚石的抛光面为金刚石的待键合表面,对氮化镓和金刚石的待键合表面进行氩等离子体处理;5) The polishing surface of the silicon carbide substrate or the gallium nitride epitaxial layer is the surface to be bonded of gallium nitride, the polished surface of diamond is the surface to be bonded of diamond, and the surface to be bonded of gallium nitride and diamond is Argon plasma treatment;
6)在已减薄碳化硅衬底的氮化镓待键合表面相继沉积金属缓冲层和金膜层,或者是在已减薄氮化镓外延层的氮化镓待键合表面相继沉积金属缓冲层和金膜层或相继沉积陶瓷膜层、金属缓冲层和金膜层;在金刚石的待键合表面相继沉积金属缓冲层和金膜层;6) successively deposit a metal buffer layer and a gold film layer on the surface to be bonded of gallium nitride of the thinned silicon carbide substrate, or successively deposit metal on the surface to be bonded of gallium nitride of the thinned epitaxial layer of gallium nitride Buffer layer and gold film layer or successively deposit ceramic film layer, metal buffer layer and gold film layer; successively deposit metal buffer layer and gold film layer on the surface to be bonded of diamond;
7)将氮化镓的待键合表面与金刚石的待键合表面相对放置并使它们相互接触,施加压力进行氮化镓与金刚石的第一次键合,即预键合;7) Place the surface to be bonded of gallium nitride and the surface to be bonded of diamond relative to each other and make them contact each other, and apply pressure to carry out the first bonding of gallium nitride and diamond, that is, pre-bonding;
8)施加压力对预键合在一起的氮化镓与金刚石进行第二次键合;8) applying pressure to bond the pre-bonded gallium nitride and diamond for the second time;
9)去除金刚石衬底氮化镓表面的粘接剂和临时载片,制备出金刚石基氮化镓复合晶片;9) removing the adhesive and the temporary carrier on the gallium nitride surface of the diamond substrate to prepare a gallium nitride-on-diamond composite wafer;
10)对金刚石基氮化镓复合晶片进行退火处理,完成制备。10) annealing the diamond-based gallium nitride composite wafer to complete the preparation.
作为本发明键合制备方法的一种优选方案,步骤1)所述的粘接剂为光刻胶、苯并环丁烯或502胶;所述临时载片的材料为硅、氧化铝、碳化硅、石英或金刚石,临时载片的表面粗糙度不高于10纳米。As a preferred solution of the bonding preparation method of the present invention, the adhesive described in step 1) is photoresist, benzocyclobutene or 502 glue; the material of the temporary carrier is silicon, alumina, carbonized Silicon, quartz or diamond, the surface roughness of the temporary slide is not higher than 10 nm.
作为本发明键合制备方法的一种优选方案,步骤2)采用机械研磨的方法将碳化硅衬底减薄至5-80微米;或者继续采用感应耦合等离子刻蚀法刻蚀掉剩余的碳化硅衬底,去除成核层,并将氮化镓外延层减薄至1-3微米;As a preferred solution of the bonding preparation method of the present invention, step 2) using mechanical grinding to thin the silicon carbide substrate to 5-80 microns; or continuing to use inductively coupled plasma etching to etch away the remaining silicon carbide Substrate, remove the nucleation layer, and thin the GaN epitaxial layer to 1-3 microns;
步骤3)所述粗糙度的要求值为2纳米;Step 3) The required value of the roughness is 2 nanometers;
步骤6)氮化镓和金刚石的待键合表面所沉积金属缓冲层的厚度分别为1-20纳米,氮化镓和金刚石的待键合表面所沉积金膜层的厚度分别为2.5-100纳米,氮化镓的待键合表面所沉积陶瓷膜层的厚度为1-15纳米。Step 6) The thickness of the metal buffer layer deposited on the surfaces to be bonded of gallium nitride and diamond is 1-20 nanometers, respectively, and the thickness of the gold film layer deposited on the surfaces to be bonded of gallium nitride and diamond is 2.5-100 nanometers, respectively , the thickness of the ceramic film layer deposited on the surface to be bonded of the gallium nitride is 1-15 nanometers.
作为本发明键合制备方法的一种优选方案,步骤5)所述的氩等离子体处理中采用的氩等离子体通过气体放电产生,放电功率为30-200W,氩等离子体的处理时间为0.5-20分钟。As a preferred solution of the bonding preparation method of the present invention, the argon plasma used in the argon plasma treatment described in step 5) is generated by gas discharge, the discharge power is 30-200W, and the treatment time of the argon plasma is 0.5-200W. 20 minutes.
作为本发明键合制备方法的一种优选方案,步骤7)在氮化镓和金刚石的待键合表面沉积完各膜层后,在不暴露大气条件下,采用机械加压方式进行氮化镓与金刚石的第一次键合,或者是从镀膜腔体中取出氮化镓和金刚石,在室温和大气环境条件下采用手工加压或重物加压方式快速进行氮化镓与金刚石的第一次键合,施加的压强为0.2-2MPa,加压时间为1-3分钟。As a preferred solution of the bonding preparation method of the present invention, in step 7) after each film layer is deposited on the surface to be bonded of gallium nitride and diamond, the gallium nitride is subjected to mechanical pressure without exposing to the atmosphere. The first bonding with diamond, or taking out gallium nitride and diamond from the coating cavity, the first bonding of gallium nitride and diamond is carried out quickly by manual pressure or heavy object pressure at room temperature and atmospheric conditions. For secondary bonding, the applied pressure is 0.2-2MPa, and the pressing time is 1-3 minutes.
作为本发明键合制备方法的一种优选方案,步骤8)对氮化镓与金刚石进行第二次键合时,氮化镓和金刚石的温度低于150℃,施加的压强为0.5-10MPa,加压时间为1-20分钟。As a preferred solution of the bonding preparation method of the present invention, in step 8) when gallium nitride and diamond are bonded for the second time, the temperature of gallium nitride and diamond is lower than 150 ° C, and the applied pressure is 0.5-10 MPa, Pressurization time is 1-20 minutes.
作为本发明键合制备方法的一种优选方案,步骤9)去除粘接剂和临时载片的方式为:放入丙酮溶液中,采用超声波振动加速粘接剂的溶解。As a preferred solution of the bonding preparation method of the present invention, the method of removing the adhesive and the temporary carrier sheet in step 9) is: put it into an acetone solution, and use ultrasonic vibration to accelerate the dissolution of the adhesive.
作为本发明键合制备方法的一种优选方案,步骤10)所述的退火处理在真空环境中或在高纯氮气气氛中进行,退火温度为100-200℃,退火时间为10-60分钟。As a preferred solution of the bonding preparation method of the present invention, the annealing treatment in step 10) is performed in a vacuum environment or in a high-purity nitrogen atmosphere, the annealing temperature is 100-200° C., and the annealing time is 10-60 minutes.
相较于现有技术,本发明金刚石基氮化镓复合晶片具有如下的有益效果:Compared with the prior art, the present invention has the following beneficial effects:
现有技术通常采用钛、铬膜层作为金薄膜粘接层的缓冲层,利用钛或铬膜与碳化硅、氮化镓、金刚石、金薄膜等材料间具有较强的结合力,以提高金薄膜与碳化硅、氮化镓、金刚石的结合强度。但是钛和铬的热导率很低,分别约为21.9W/m·K和93.7W/m·K,用它们作为缓冲层会增加氮化镓与金刚石间的热阻。本发明复合晶片采用钨、钼、铝作为缓冲层,这些金属膜层不仅与碳化硅、氮化镓、金刚石之间有很好的结合力,而且具有较高的热导率(分别约为174W/m·K、138W/m·K、237W/m·K),用它们作为缓冲层可减小氮化镓与金刚石间的热阻,有利于降低氮化镓器件热点区域的温度。此外,对于本发明采用的将氮化镓外延层减薄后与金刚石进行键合的方案,为了防止金属纳米粘接层中金属原子扩散进入氮化镓而降低器件性能,在减薄了的氮化镓外延层的待键合表面先沉积一层薄的具有较高热导率的氮化铝或碳化硅陶瓷膜层,然后再沉积金属缓冲层和金薄膜,用陶瓷膜层阻挡金属原子进入氮化镓,能够避免金属粘接层的存在对氮化镓器件性能带来的不利影响。In the prior art, titanium and chromium films are usually used as the buffer layer of the gold film bonding layer, and the titanium or chromium films have strong bonding force with silicon carbide, gallium nitride, diamond, gold films and other materials to improve the gold film. The bonding strength of the film to silicon carbide, gallium nitride, and diamond. However, the thermal conductivity of titanium and chromium is very low, about 21.9W/m·K and 93.7W/m·K, respectively, and using them as buffer layers will increase the thermal resistance between gallium nitride and diamond. The composite wafer of the present invention adopts tungsten, molybdenum and aluminum as buffer layers. These metal film layers not only have good bonding force with silicon carbide, gallium nitride and diamond, but also have high thermal conductivity (about 174W respectively). /m·K, 138W/m·K, 237W/m·K), using them as a buffer layer can reduce the thermal resistance between gallium nitride and diamond, which is beneficial to reduce the temperature of the hot spot area of the gallium nitride device. In addition, for the scheme of bonding the gallium nitride epitaxial layer with diamond after thinning, in order to prevent the metal atoms in the metal nano-bonding layer from diffusing into the gallium nitride and reducing the device performance, the thinned nitrogen A thin layer of aluminum nitride or silicon carbide ceramic film with high thermal conductivity is first deposited on the surface to be bonded of the gallium nitride epitaxial layer, and then a metal buffer layer and a gold film are deposited, and the ceramic film layer is used to block metal atoms from entering nitrogen gallium nitride can avoid the adverse effect of the presence of the metal bonding layer on the performance of the gallium nitride device.
本发明采用了两种技术方案来制备金刚石基氮化镓复合晶片。第一种方案是保留氮化镓的5-80微米厚度的碳化硅衬底,将碳化硅衬底表面作为键合面与金刚石进行键合。这种方案的优点是制备工艺相对简单,键合成功率高,但缺点是由于存在碳化硅衬底及氮化镓外延层较厚,制备出的金刚石基氮化镓复合器件的热阻较高。第二种方案是完全剥离掉碳化硅衬底及成核层,并将氮化镓减薄至1-3微米,将减薄的氮化镓的表面作为键合面与金刚石进行键合。采用该方案制备出的金刚石基氮化镓复合器件的热点区域与金刚石衬底的距离较近,有利于器件散热,但其缺点是制备工艺复杂,技术难度较大,制作成本较高。因此,这两种技术方案各有优缺点,可以根据不同的实际需要来选择不同的技术方案。The present invention adopts two technical solutions to prepare a diamond-based gallium nitride composite wafer. The first solution is to retain a silicon carbide substrate with a thickness of 5-80 microns of gallium nitride, and use the surface of the silicon carbide substrate as a bonding surface to bond with diamond. The advantage of this scheme is that the preparation process is relatively simple and the bonding power is high, but the disadvantage is that the thermal resistance of the prepared GaN-on-diamond composite device is high due to the existence of the silicon carbide substrate and the thick gallium nitride epitaxial layer. The second solution is to completely peel off the silicon carbide substrate and the nucleation layer, thin the gallium nitride to 1-3 microns, and use the surface of the thinned gallium nitride as the bonding surface to bond with the diamond. The distance between the hot spot area and the diamond substrate of the GaN-on-diamond composite device prepared by this scheme is relatively close, which is beneficial to the heat dissipation of the device. Therefore, these two technical solutions have their own advantages and disadvantages, and different technical solutions can be selected according to different actual needs.
与现有技术相比,本发明金刚石基氮化镓复合晶片的键合制备方法具有如下有益效果:现有的晶片键合技术通常采用在晶片的键合表面沉积完金属粘接层后,从镀膜机中取出晶片,再放入键合设备中进行加压键合。由于从镀膜机中取出晶片到将晶片放入键合设备通常需要较长的时间,在此期间金属粘接层表面会吸附较多的气体(如水蒸气)甚至沾染一些灰尘颗粒,影响氮化镓与金刚石键合界面两侧金原子的相互扩散及形成金属键,从而降低了键合质量。本发明将氮化镓与金刚石的键合分两步进行,即在氮化镓和金刚石的待键合表面沉积完各膜层后,在不暴露大气条件下,施加压力进行氮化镓与金刚石的预键合,或者是从溅射镀膜机腔体中取出氮化镓和金刚石,快速地施加压力进行氮化镓与金刚石的预键合,然后再将预键合在一起的氮化镓与金刚石放入键合设备中,进行氮化镓与金刚石的第二次键合。采用预键合方式可以避免金属纳米粘接层表面暴露在空气中或尽量缩短暴露在空气中的时间,减少气体和灰尘颗粒吸附对金属纳米粘接层表面造成的污染,以保证氮化镓和金刚石的待键合面上的两个新鲜的金膜表面能充分地相互接触。此后,为了增加键合强度,再将预键合的样品放入键合设备中进行二次键合,由于两个相互接触的金膜表面很清洁,二次键合只需要施加较低的压力即能够实现具有低空洞率和高键合强度的键合。本发明在沉积金属纳米粘接层之前,用氩等离子体处理待键合表面,能够较彻底地清洁氮化镓及金刚石的待键合表面,增强碳化硅衬底或氮化镓外延层及金刚石衬底与金属纳米粘接层之间的结合力。为增强基于金属纳米粘接层的氮化镓与金刚石键合的粘接强度,本发明对键合完成的金刚石基氮化镓复合晶片进行退火处理,从而增强了金/金键合界面两侧金原子的相互扩散,提高氮化镓与金刚石的键合强度。Compared with the prior art, the bonding preparation method of the diamond-based gallium nitride composite wafer of the present invention has the following beneficial effects: The wafer is taken out from the coating machine and put into the bonding equipment for pressure bonding. Since it usually takes a long time to remove the wafer from the coating machine and put the wafer into the bonding equipment, during this period, the surface of the metal bonding layer will absorb more gas (such as water vapor) and even be contaminated with some dust particles, which will affect the gallium nitride. The interdiffusion of gold atoms on both sides of the bonding interface with diamond and the formation of metal bonds reduce the bonding quality. In the present invention, the bonding of gallium nitride and diamond is carried out in two steps, that is, after each film layer is deposited on the surfaces to be bonded of gallium nitride and diamond, pressure is applied to carry out gallium nitride and diamond without exposing to the atmosphere. pre-bonding, or take out gallium nitride and diamond from the cavity of the sputter coater, quickly apply pressure to pre-bond gallium nitride and diamond, and then pre-bond gallium nitride and diamond together The diamond is put into the bonding equipment for the second bonding of gallium nitride and diamond. Using the pre-bonding method can avoid the surface of the metal nano-bonding layer from being exposed to the air or minimize the exposure time to the air, and reduce the pollution caused by the adsorption of gas and dust particles on the surface of the metal nano-bonding layer, so as to ensure that the gallium nitride and the The two fresh gold film surfaces on the to-be-bonded surface of the diamond can sufficiently contact each other. After that, in order to increase the bonding strength, the pre-bonded samples are put into the bonding equipment for secondary bonding. Since the surfaces of the two gold films in contact with each other are very clean, the secondary bonding only needs to apply lower pressure. That is, bonding with low void ratio and high bonding strength can be realized. In the present invention, the surfaces to be bonded are treated with argon plasma before the metal nano-bonding layer is deposited, so that the surfaces to be bonded of gallium nitride and diamond can be cleaned thoroughly, and the silicon carbide substrate or the epitaxial layer of gallium nitride and the diamond can be strengthened. The bonding force between the substrate and the metal nanobond layer. In order to enhance the bonding strength between gallium nitride and diamond based on the metal nano-bonding layer, the present invention performs annealing treatment on the bonded diamond-based gallium nitride composite wafer, thereby enhancing the gold atoms on both sides of the gold/gold bonding interface. The interdiffusion of gallium nitride and diamond improves the bonding strength.
本发明从工艺过程以及结构特征上进行改进,采用本发明金刚石基氮化镓复合晶片以及相应的键合制备方法可以实现高性能金刚石基氮化镓器件的制备。The invention improves the technological process and structural features, and can realize the preparation of high-performance diamond-based gallium nitride devices by using the diamond-based gallium nitride composite wafer and the corresponding bonding preparation method of the present invention.
附图说明Description of drawings
图1本发明基于金属纳米层的氮化镓与金刚石键合方法的工艺流程图;Fig. 1 is the process flow chart of the bonding method of gallium nitride and diamond based on metal nanolayer of the present invention;
图2实施例1采用本发明键合方法制备出的金刚石基氮化镓复合晶片的一种结构(氮化镓/成核层/碳化硅(5-80微米)/金属缓冲层/金膜/金属缓冲层/金刚石)示意图;Figure 2 Example 1 A structure of a GaN-on-diamond composite wafer prepared by the bonding method of the present invention (gallium nitride/nucleation layer/silicon carbide (5-80 microns)/metal buffer layer/gold film/ Metal buffer layer/diamond) schematic diagram;
图3实施例2采用本发明键合方法制备出的金刚石基氮化镓复合晶片的一种结构(即氮化镓(1-3微米)/金属缓冲层/金膜/金属缓冲层/金刚石)示意图;Figure 3 Example 2 A structure of a GaN-on-diamond composite wafer prepared by the bonding method of the present invention (ie, gallium nitride (1-3 microns)/metal buffer layer/gold film/metal buffer layer/diamond) schematic diagram;
图4实施例3采用本发明键合方法制备出的金刚石基氮化镓复合晶片的一种结构(即氮化镓(1-3微米)/陶瓷膜层/金属缓冲层/金膜/金属缓冲层/金刚石)示意图;Figure 4 Example 3 A structure of a GaN-on-diamond composite wafer prepared by the bonding method of the present invention (ie, gallium nitride (1-3 microns)/ceramic film layer/metal buffer layer/gold film/metal buffer layer/diamond) schematic diagram;
图5经过表面抛光的金刚石衬底的原子力显微镜图;Fig. 5 is the atomic force microscope image of the diamond substrate through surface polishing;
图6金刚石衬底上沉积了钼缓冲层和金薄膜的原子力显微镜图;Fig. 6 AFM image of molybdenum buffer layer and gold thin film deposited on diamond substrate;
图7经过表面抛光的氮化镓层的原子力显微镜图;Figure 7 is an atomic force microscope image of a surface-polished gallium nitride layer;
图8氮化镓层上沉积了钼缓冲层和金薄膜的原子力显微镜图;Fig. 8 AFM image of the molybdenum buffer layer and the gold thin film deposited on the gallium nitride layer;
图9本发明键合法制备的氮化镓/成核层/碳化硅(5-80微米)/金属缓冲层/金膜/金属缓冲层/金刚石多层结构的金刚石基氮化镓复合晶片形貌图;Fig. 9 Morphology of GaN-on-diamond composite wafer prepared by bonding method of the present invention/nucleation layer/silicon carbide (5-80 microns)/metal buffer layer/gold film/metal buffer layer/diamond multilayer structure picture;
图10本发明键合法制备的氮化镓(1-3微米)/金属缓冲层/金膜/金属缓冲层/金刚石多层结构的金刚石基氮化镓复合晶片形貌图;Figure 10 is a topography of a GaN-on-diamond composite wafer with a gallium nitride (1-3 micron)/metal buffer layer/gold film/metal buffer layer/diamond multilayer structure prepared by the bonding method of the present invention;
图11本发明键合法制备的金刚石基氮化镓复合晶片的超声波扫描显微镜图。Fig. 11 is an ultrasonic scanning microscope image of the GaN-on-diamond composite wafer prepared by the bonding method of the present invention.
附图中:1—氮化镓外延层,2—成核层,3—碳化硅衬底,4—金刚石衬底,11—金属缓冲层,12—金膜,13—陶瓷膜层。In the drawings: 1—gallium nitride epitaxial layer, 2—nucleation layer, 3—silicon carbide substrate, 4—diamond substrate, 11—metal buffer layer, 12—gold film, 13—ceramic film layer.
具体实施方式Detailed ways
下面结合附图以及实施例对本发明做进一步的详细说明。The present invention will be further described in detail below with reference to the accompanying drawings and embodiments.
为了解决高频、大功率氮化镓器件的散热问题,将氮化镓器件与具有高热导率的金刚石衬底相结合,本发明采用了一种基于金属纳米层的键合方法来制备金刚石基氮化镓复合晶片,该晶片具有氮化镓/成核层/碳化硅/金属中间层/金刚石衬底、氮化镓/金属中间层/金刚石衬底、氮化镓/陶瓷膜层/金属中间层/金刚石衬底等结构。本发明提出的制备方法分两步进行氮化镓与金刚石的键合,即在氮化镓和金刚石的待键合表面沉积完各膜层后,在不暴露大气条件下,采用机械加压方式进行氮化镓与金刚石的预键合,或者是从镀膜腔体中取出氮化镓和金刚石,在室温和大气环境条件下采用手工加压或重物加压方式快速进行氮化镓与金刚石的预键合,然后用键合设备进行氮化镓与金刚石的二次键合。采用预键合方式可以避免金属纳米粘接层表面暴露在空气中或尽量缩短暴露在空气中的时间,减少气体和灰尘颗粒吸附对金属纳米粘接层表面的污染,以保证两个新鲜的金膜表面相互接触。为了增加键合强度,将经过预键合的样品放入键合设备中进行二次键合,由于两个相互接触的金膜表面很清洁,二次键合只需要施加较低的压力即能够获得低键合空洞率和高粘接强度。在沉积金属缓冲层前,用氩等离子体处理待键合表面,可以清洁待键合表面,增强碳化硅衬底或氮化镓外延层以及金刚石与金属缓冲层之间的结合力,以提高键合质量。采用钨、钼、铝作为缓冲层,这些金属膜层不仅能够与碳化硅、氮化镓、金刚石及金薄膜之间有很好的结合力,而且具有较高的热导率,用它们作为缓冲层有利于降低氮化镓器件热点区域的温度。此外,对于本发明采用的将氮化镓外延层减薄后再与金刚石键合的方案,为了防止金属纳米层中金属原子扩散进入氮化镓而降低器件性能,在减薄了的氮化镓外延层的待键合表面先沉积一层薄的氮化铝或碳化硅陶瓷膜层,然后再沉积金属缓冲层和金薄膜,用陶瓷膜层阻挡金属原子进入氮化镓。为了进一步增加氮化镓与金刚石的粘接强度,对键合完成的金刚石衬底氮化镓进行退火处理,以增强金/金键合界面两侧金原子的相互扩散。In order to solve the heat dissipation problem of high-frequency and high-power gallium nitride devices, the gallium nitride device is combined with a diamond substrate with high thermal conductivity, and the present invention adopts a bonding method based on metal nanolayers to prepare diamond substrates Gallium nitride composite wafer with gallium nitride/nucleation layer/silicon carbide/metal interlayer/diamond substrate, gallium nitride/metal interlayer/diamond substrate, gallium nitride/ceramic film layer/metal interlayer layer/diamond substrate, etc. The preparation method proposed by the present invention performs the bonding of gallium nitride and diamond in two steps, that is, after each film layer is deposited on the surfaces to be bonded of gallium nitride and diamond, and under the condition of not exposing to the atmosphere, a mechanical pressing method is adopted. Carry out pre-bonding of gallium nitride and diamond, or take out gallium nitride and diamond from the coating cavity, and use manual pressure or heavy object pressure to quickly carry out gallium nitride and diamond at room temperature and atmospheric conditions. Pre-bonding, and then secondary bonding of gallium nitride and diamond with bonding equipment. Using the pre-bonding method can avoid the surface of the metal nano-adhesive layer from being exposed to the air or minimize the exposure time to the air, and reduce the contamination of the surface of the metal nano-adhesion layer by the adsorption of gas and dust particles, so as to ensure two fresh gold The membrane surfaces are in contact with each other. In order to increase the bonding strength, the pre-bonded samples are put into the bonding equipment for secondary bonding. Since the surfaces of the two gold films in contact with each other are very clean, the secondary bonding only needs to apply a lower pressure. Obtain low bond voids and high bond strength. Before depositing the metal buffer layer, the surface to be bonded is treated with argon plasma, which can clean the surface to be bonded and enhance the bonding force between the silicon carbide substrate or the gallium nitride epitaxial layer and the diamond and the metal buffer layer to improve the bond combined quality. Tungsten, molybdenum and aluminum are used as buffer layers. These metal films not only have good bonding force with silicon carbide, gallium nitride, diamond and gold films, but also have high thermal conductivity. Use them as buffer layers. The layer is beneficial to reduce the temperature of the hot spot region of the gallium nitride device. In addition, for the scheme of thinning the gallium nitride epitaxial layer and then bonding it with diamond, in order to prevent the metal atoms in the metal nanolayer from diffusing into the gallium nitride and reducing the device performance, the thinned gallium nitride is used in the thinned gallium nitride. A thin aluminum nitride or silicon carbide ceramic film layer is deposited on the surface to be bonded of the epitaxial layer, and then a metal buffer layer and a gold film are deposited, and the ceramic film layer is used to block the metal atoms from entering the gallium nitride. In order to further increase the bonding strength between gallium nitride and diamond, the bonded diamond substrate gallium nitride is annealed to enhance the mutual diffusion of gold atoms on both sides of the gold/gold bonding interface.
故采用本发明的一种金刚石基氮化镓复合晶片及其键合制备方法能够制备出低空洞率、高键合强度的金刚石基氮化镓复合晶片,能有效解决高频、大功率氮化镓器件的散热问题。Therefore, the diamond-based gallium nitride composite wafer and the bonding preparation method of the present invention can prepare a diamond-based gallium nitride composite wafer with low void ratio and high bonding strength, and can effectively solve the problem of high-frequency and high-power gallium nitride devices. cooling problem.
实施例1Example 1
参见图1和图2,本发明制备的金刚石基氮化镓复合晶片具有氮化镓/成核层/碳化硅(5-80微米)/金属缓冲层/金膜/金属缓冲层/金刚石的结构,具体制备方法包括以下步骤:1 and 2, the GaN-on-diamond composite wafer prepared by the present invention has the structure of gallium nitride/nucleation layer/silicon carbide (5-80 microns)/metal buffer layer/gold film/metal buffer layer/diamond , the specific preparation method comprises the following steps:
1)用光刻胶将碳化硅衬底氮化镓的氮化镓外延层的表面与硅片(临时载片)粘接在一起;1) The surface of the gallium nitride epitaxial layer of the silicon carbide substrate gallium nitride and the silicon wafer (temporary carrier) are bonded together with photoresist;
2)采用机械研磨将碳化硅衬底减薄至40微米;2) Using mechanical grinding to thin the silicon carbide substrate to 40 microns;
3)对碳化硅衬底和金刚石进行表面抛光,使碳化硅衬底和金刚石的抛光面的粗糙度低于2纳米;3) Surface polishing is performed on the silicon carbide substrate and the diamond, so that the roughness of the polished surface of the silicon carbide substrate and the diamond is less than 2 nanometers;
4)先后用丙酮、乙醇和去离子水对氮化镓和金刚石进行超声波清洗;4) ultrasonically clean gallium nitride and diamond with acetone, ethanol and deionized water successively;
5)将氮化镓和金刚石放入溅射镀膜机中,将碳化硅衬底和金刚石的抛光面作为待键合表面,对待键合表面进行氩等离子体处理,等离子体放电功率为50W,处理时间为5分钟;5) Put the gallium nitride and diamond into the sputtering coater, use the polished surface of the silicon carbide substrate and the diamond as the surface to be bonded, and carry out argon plasma treatment on the surface to be bonded, and the plasma discharge power is 50W. The time is 5 minutes;
6)采用溅射沉积法,在碳化硅衬底和金刚石的待键合表面相继沉积2纳米厚的钨缓冲层和10纳米厚的金薄膜;6) adopt sputtering deposition method, successively deposit 2 nanometer thick tungsten buffer layer and 10 nanometer thick gold film on the surface to be bonded of silicon carbide substrate and diamond;
7)在碳化硅衬底和金刚石的待键合表面沉积完钨缓冲层和金薄膜后,在不暴露大气条件下,将碳化硅衬底的待键合表面与金刚石衬底的待键合表面相对放置并使它们相互接触,采用机械加压方式进行氮化镓与金刚石的预键合,施加压强为0.3MPa的压力并保持3分钟;7) After the tungsten buffer layer and the gold thin film are deposited on the surfaces to be bonded of the silicon carbide substrate and the diamond, the surface to be bonded of the silicon carbide substrate and the surface to be bonded of the diamond substrate are not exposed to the atmosphere. Place them relative to each other and make them in contact with each other, use mechanical pressure to pre-bond gallium nitride and diamond, apply a pressure of 0.3MPa and keep it for 3 minutes;
8)将预键合后的氮化镓与金刚石放入键合设备中,对氮化镓与金刚石施加5MPa压强并保持5分钟,进行第二次键合,将氮化镓与金刚石衬底键合在一起;8) Put the pre-bonded gallium nitride and diamond into the bonding equipment, apply a pressure of 5 MPa to the gallium nitride and diamond and keep it for 5 minutes, carry out the second bonding, and bond the gallium nitride and the diamond substrate combine together;
9)将粘接在临时载片上的金刚石衬底氮化镓放入盛有丙酮溶液的容器中,并采用超声波振动来加速粘接剂的溶解,去除金刚石衬底氮化镓表面的粘接剂和临时载片,制备出金刚石基氮化镓复合晶片;9) Put the diamond substrate gallium nitride bonded on the temporary carrier into a container filled with acetone solution, and use ultrasonic vibration to accelerate the dissolution of the adhesive to remove the adhesive on the surface of the diamond substrate gallium nitride and a temporary slide to prepare a GaN-on-diamond composite wafer;
10)在真空环境中对金刚石基氮化镓复合晶片进行退火处理,退火温度为150℃,退火时间为40分钟。10) The gallium nitride-on-diamond composite wafer is annealed in a vacuum environment, the annealing temperature is 150° C., and the annealing time is 40 minutes.
实施例2Example 2
参见图1和图3,本发明制备的金刚石基氮化镓复合晶片具有氮化镓(1-3微米)/金属缓冲层/金膜/金属缓冲层/金刚石的结构,具体制备方法包括以下步骤:Referring to FIG. 1 and FIG. 3 , the GaN-on-diamond composite wafer prepared by the present invention has the structure of gallium nitride (1-3 microns)/metal buffer layer/gold film/metal buffer layer/diamond, and the specific preparation method includes the following steps :
1)用苯并环丁烯(BCB)将碳化硅衬底氮化镓的氮化镓外延层的表面与碳化硅晶片(临时载片)粘接在一起;1) Using benzocyclobutene (BCB) to bond the surface of the gallium nitride epitaxial layer of the silicon carbide substrate gallium nitride to the silicon carbide wafer (temporary carrier);
2)采用机械研磨将碳化硅衬底减薄至30微米,然后采用感应耦合等离子刻蚀法,刻蚀掉剩余的碳化硅衬底,去除成核层,并将氮化镓外延层减薄至2微米;2) The silicon carbide substrate is thinned to 30 microns by mechanical grinding, and then the remaining silicon carbide substrate is etched by inductively coupled plasma etching, the nucleation layer is removed, and the gallium nitride epitaxial layer is thinned to 2 microns;
3)对氮化镓外延层和金刚石进行表面抛光,使氮化镓和金刚石的抛光面的粗糙度低于2纳米;3) Surface polishing of the gallium nitride epitaxial layer and diamond, so that the roughness of the polished surface of gallium nitride and diamond is less than 2 nanometers;
4)先后用丙酮、乙醇和去离子水对氮化镓和金刚石进行超声波清洗;4) ultrasonically clean gallium nitride and diamond with acetone, ethanol and deionized water successively;
5)将氮化镓和金刚石放入溅射镀膜机中,将氮化镓和金刚石的抛光面作为待键合表面,对待键合表面进行氩等离子体处理,等离子体放电功率为100W,处理时间为2分钟;5) Put gallium nitride and diamond into a sputtering coater, use the polished surface of gallium nitride and diamond as the surface to be bonded, and perform argon plasma treatment on the surface to be bonded, the plasma discharge power is 100W, and the treatment time for 2 minutes;
6)采用溅射沉积法,在氮化镓和金刚石的待键合表面相继沉积3纳米厚的钼缓冲层和15纳米厚的金薄膜;6) adopt the sputtering deposition method to successively deposit a 3-nanometer thick molybdenum buffer layer and a 15-nanometer thick gold film on the surfaces to be bonded of gallium nitride and diamond;
7)从溅射镀膜机中取出氮化镓和金刚石,在1分钟时间内快速将氮化镓的待键合表面与金刚石衬底的待键合表面相对放置并使之相互接触,采用重物加压方式对氮化镓与金刚石施加0.5MPa压强并保持2分钟进行第一次键合,即预键合;7) Take out gallium nitride and diamond from the sputtering coater, quickly place the to-be-bonded surface of gallium nitride and the to-be-bonded surface of the diamond substrate relative to each other within 1 minute and make them contact each other, using heavy objects The pressure method applies 0.5MPa pressure to the gallium nitride and diamond and keeps it for 2 minutes for the first bonding, that is, pre-bonding;
8)将预键合后的氮化镓与金刚石放入键合设备中,对氮化镓与金刚石施加10MPa压强并保持3分钟,进行第二次键合,将氮化镓与金刚石衬底键合在一起;8) Put the pre-bonded gallium nitride and diamond into the bonding equipment, apply a pressure of 10 MPa to the gallium nitride and diamond and keep it for 3 minutes, carry out the second bonding, and bond the gallium nitride and the diamond substrate combine together;
9)将粘接在临时载片上的金刚石衬底氮化镓放入盛有丙酮溶液的容器中,并采用超声波振动来加速粘接剂的溶解,去除金刚石衬底氮化镓表面的粘接剂和临时载片,制备出金刚石基氮化镓复合晶片;9) Put the diamond substrate gallium nitride bonded on the temporary carrier into a container filled with acetone solution, and use ultrasonic vibration to accelerate the dissolution of the adhesive to remove the adhesive on the surface of the diamond substrate gallium nitride and a temporary slide to prepare a GaN-on-diamond composite wafer;
10)在高纯氮气环境中对金刚石基氮化镓复合晶片进行退火处理,退火温度为180℃,退火时间为20分钟。10) The gallium nitride-on-diamond composite wafer is annealed in a high-purity nitrogen environment, the annealing temperature is 180° C., and the annealing time is 20 minutes.
实施例3Example 3
参见图1和图4,本发明制备的金刚石基氮化镓复合晶片具有氮化镓(1-3微米)/陶瓷膜层/金属缓冲层/金膜/金属缓冲层/金刚石的结构,具体制备方法包括以下步骤:Referring to FIG. 1 and FIG. 4 , the GaN-on-diamond composite wafer prepared by the present invention has the structure of gallium nitride (1-3 microns)/ceramic film layer/metal buffer layer/gold film/metal buffer layer/diamond. The method includes the following steps:
1)用502胶将碳化硅衬底氮化镓的氮化镓外延层的表面与石英片(临时载片)粘接在一起;1) Use 502 glue to bond the surface of the gallium nitride epitaxial layer of the silicon carbide substrate gallium nitride to the quartz wafer (temporary carrier);
2)采用机械研磨将碳化硅衬底减薄至50微米,然后采用感应耦合等离子刻蚀法,刻蚀掉剩余的碳化硅衬底,去除成核层,并将氮化镓外延层减薄至3微米;2) The silicon carbide substrate is thinned to 50 microns by mechanical grinding, and then the remaining silicon carbide substrate is etched by inductively coupled plasma etching, the nucleation layer is removed, and the gallium nitride epitaxial layer is thinned to 3 microns;
3)对氮化镓外延层和金刚石进行表面抛光,使氮化镓和金刚石的抛光面的粗糙度低于2纳米;3) Surface polishing of the gallium nitride epitaxial layer and diamond, so that the roughness of the polished surface of gallium nitride and diamond is less than 2 nanometers;
4)先后用丙酮、乙醇和去离子水对氮化镓和金刚石进行超声波清洗;4) ultrasonically clean gallium nitride and diamond with acetone, ethanol and deionized water successively;
5)将氮化镓和金刚石放入溅射镀膜机中,将氮化镓和金刚石的抛光面作为待键合表面,对待键合表面进行氩等离子体处理,等离子体放电功率为150W,处理时间为1分钟;5) Put gallium nitride and diamond into a sputtering coater, use the polished surface of gallium nitride and diamond as the surface to be bonded, and perform argon plasma treatment on the surface to be bonded, the plasma discharge power is 150W, and the treatment time is 1 minute;
6)采用溅射沉积法,在氮化镓待键合表面相继沉积2纳米厚的氮化铝膜、4纳米厚的铝缓冲层和50纳米厚的金薄膜,在金刚石待键合表面相继沉积4纳米厚的铝缓冲层和50纳米厚的金薄膜;6) Using the sputtering deposition method, successively deposit a 2-nanometer-thick aluminum nitride film, a 4-nanometer-thick aluminum buffer layer and a 50-nanometer-thick gold film on the surface to be bonded of gallium nitride, and successively deposit on the surface to be bonded of diamond 4nm thick aluminum buffer layer and 50nm thick gold film;
7)从溅射镀膜机中取出氮化镓和金刚石,在1分钟时间内快速将氮化镓的待键合表面与金刚石衬底的待键合表面相对放置并使它们相互接触,采用手工加压方式对氮化镓与金刚石施加1MPa压强并保持1分钟进行第一次键合,即预键合;7) Take out the gallium nitride and diamond from the sputtering coater, quickly place the surface to be bonded of the gallium nitride and the surface to be bonded of the diamond substrate relative to each other and make them contact each other within 1 minute. Apply 1MPa pressure to gallium nitride and diamond and hold for 1 minute for the first bonding, that is, pre-bonding;
8)将预键合后的氮化镓与金刚石放入键合设备中,对氮化镓与金刚石施加8MPa压强并保持4分钟,进行第二次键合,将氮化镓与金刚石衬底键合在一起;8) Put the pre-bonded gallium nitride and diamond into the bonding equipment, apply a pressure of 8 MPa to the gallium nitride and diamond and keep it for 4 minutes, carry out the second bonding, and bond the gallium nitride and the diamond substrate combine together;
9)将粘接在临时载片上的金刚石衬底氮化镓放入盛有丙酮溶液的容器中,并采用超声波振动来加速粘接剂的溶解,去除金刚石衬底氮化镓表面的粘接剂和临时载片,制备出金刚石基氮化镓复合晶片;9) Put the diamond substrate gallium nitride bonded on the temporary carrier into a container filled with acetone solution, and use ultrasonic vibration to accelerate the dissolution of the adhesive to remove the adhesive on the surface of the diamond substrate gallium nitride and a temporary slide to prepare a GaN-on-diamond composite wafer;
10)在高纯氮气环境中对金刚石基氮化镓复合晶片进行退火处理,退火温度为120℃,退火时间为60分钟。10) The gallium nitride-on-diamond composite wafer is annealed in a high-purity nitrogen environment, the annealing temperature is 120° C., and the annealing time is 60 minutes.
实施例4Example 4
参见图1和图4,本发明制备的金刚石基氮化镓复合晶片具有氮化镓(1-3微米)/陶瓷膜层/金属缓冲层/金膜/金属缓冲层/金刚石的结构,具体制备方法包括以下步骤:Referring to FIG. 1 and FIG. 4 , the GaN-on-diamond composite wafer prepared by the present invention has the structure of gallium nitride (1-3 microns)/ceramic film layer/metal buffer layer/gold film/metal buffer layer/diamond. The method includes the following steps:
1)用光刻胶将碳化硅衬底氮化镓的氮化镓外延层的表面与金刚石晶(临时载片)片粘接在一起;1) The surface of the gallium nitride epitaxial layer of the silicon carbide substrate gallium nitride and the diamond crystal (temporary carrier) sheet are bonded together with photoresist;
2)采用机械研磨将碳化硅衬底减薄至10微米,然后采用感应耦合等离子刻蚀法,刻蚀掉剩余的碳化硅衬底,去除成核层,并将氮化镓外延层减薄至1.5微米;2) The silicon carbide substrate is thinned to 10 microns by mechanical grinding, and then the remaining silicon carbide substrate is etched by inductively coupled plasma etching, the nucleation layer is removed, and the gallium nitride epitaxial layer is thinned to 1.5 microns;
3)对氮化镓和金刚石进行表面抛光,使氮化镓和金刚石的抛光面的粗糙度低于2纳米;3) Surface polishing of gallium nitride and diamond, so that the roughness of the polished surface of gallium nitride and diamond is less than 2 nanometers;
4)先后用丙酮、乙醇和去离子水对氮化镓和金刚石进行超声波清洗;4) ultrasonically clean gallium nitride and diamond with acetone, ethanol and deionized water successively;
5)将氮化镓和金刚石放入溅射镀膜机中,将氮化镓和金刚石的抛光面作为待键合表面,对待键合表面进行氩等离子体处理,等离子体放电功率为80W,处理时间为3分钟;5) Put gallium nitride and diamond into a sputtering coater, use the polished surface of gallium nitride and diamond as the surface to be bonded, and perform argon plasma treatment on the surface to be bonded, the plasma discharge power is 80W, and the treatment time for 3 minutes;
6)采用溅射沉积法,在氮化镓待键合表面相继沉积3纳米厚的碳化硅膜、5纳米厚的钨缓冲层和8纳米厚的金薄膜,在金刚石的待键合表面相继沉积5纳米厚的钨缓冲层和8纳米厚的金薄膜;6) Using the sputtering deposition method, successively deposit a 3-nanometer-thick silicon carbide film, a 5-nanometer-thick tungsten buffer layer and an 8-nanometer-thick gold film on the surface to be bonded of gallium nitride, and successively deposit on the surface to be bonded of diamond 5nm thick tungsten buffer layer and 8nm thick gold film;
7)从溅射镀膜机中取出氮化镓和金刚石,在1分钟时间内快速将氮化镓的待键合表面与金刚石衬底的待键合表面相对放置并使它们相互接触,采用重物加压方式对氮化镓与金刚石施加1.5MPa压强并保持1分钟进行第一次键合,即预键合;7) Take out the gallium nitride and diamond from the sputtering coater, quickly place the surface to be bonded of the gallium nitride and the surface to be bonded of the diamond substrate relative to each other within 1 minute and make them contact each other, using a heavy object The pressure method applies 1.5MPa pressure to the gallium nitride and diamond and keeps it for 1 minute for the first bonding, that is, pre-bonding;
8)将预键合后的氮化镓与金刚石放入键合设备中,对氮化镓与金刚石施加3MPa压强并保持10分钟,进行第二次键合,将氮化镓与金刚石衬底键合在一起;8) Put the pre-bonded gallium nitride and diamond into the bonding equipment, apply a pressure of 3 MPa to the gallium nitride and diamond and keep it for 10 minutes, carry out the second bonding, and bond the gallium nitride and the diamond substrate combine together;
9)将粘接在临时载片上的金刚石衬底氮化镓放入盛有丙酮溶液的容器中,并采用超声波振动来加速粘接剂的溶解,去除金刚石衬底氮化镓表面的粘接剂和临时载片,制备出金刚石基氮化镓复合晶片;9) Put the diamond substrate gallium nitride bonded on the temporary carrier into a container filled with acetone solution, and use ultrasonic vibration to accelerate the dissolution of the adhesive to remove the adhesive on the surface of the diamond substrate gallium nitride and a temporary slide to prepare a GaN-on-diamond composite wafer;
10)在真空环境中对金刚石基氮化镓复合晶片进行退火处理,退火温度为200℃,退火时间为10分钟。10) Perform annealing treatment on the GaN-on-diamond composite wafer in a vacuum environment, the annealing temperature is 200° C., and the annealing time is 10 minutes.
参见图5、图6、图7和图8,可以看出,经过表面抛光的金刚石衬底和氮化镓层都有很低的表面粗糙度,分别为0.509纳米和0.265纳米,即使在它们的键合面上沉积了钼缓冲层和金薄膜后,表面粗糙度仍然很低,分别为0.685纳米和0.438纳米,有利于实现氮化镓与金刚石的高质量键合。Referring to Fig. 5, Fig. 6, Fig. 7 and Fig. 8, it can be seen that both the polished diamond substrate and the gallium nitride layer have very low surface roughness, 0.509 nm and 0.265 nm, respectively, even at their After depositing a molybdenum buffer layer and a gold thin film on the bonding surface, the surface roughness is still very low, 0.685 nm and 0.438 nm, respectively, which is conducive to the realization of high-quality bonding of gallium nitride and diamond.
图9和图10分别是用键合法制备的具有氮化镓/成核层/碳化硅(5-80微米)/金属缓冲层/金膜/金属缓冲层/金刚石结构和氮化镓(1-3微米)/金属缓冲层/金膜/金属缓冲层/金刚石结构的金刚石基氮化镓复合晶片形貌,这两个样品都达到了10MPa以上的键合强度。Figures 9 and 10 are the structures with gallium nitride/nucleation layer/silicon carbide (5-80 microns)/metal buffer layer/gold film/metal buffer layer/diamond structure and gallium nitride (1- 3 μm)/metal buffer layer/gold film/metal buffer layer/diamond structure of the GaN-on-diamond composite wafer morphology, both samples achieved a bonding strength of more than 10MPa.
图11是一个用键合法制备的金刚石基氮化镓复合晶片的超声波扫描显微镜照片,可以明显地看出,氮化镓与金刚石的键合界面无任何空洞存在。Fig. 11 is an ultrasonic scanning microscope photograph of a GaN-on-diamond composite wafer prepared by bonding method. It can be clearly seen that there is no void in the bonding interface between GaN and diamond.
本发明实现了基于金属纳米中间层的金刚石基氮化镓复合晶片结构,采用分两步键合的氮化镓与金刚石键合方法,能够减小键合空洞率,增加键合强度,并降低氮化镓与金刚石间的热阻,达到提高氮化镓与金刚石键合质量的目的,可制备出高性能金刚石基氮化镓器件。The invention realizes a diamond-based gallium nitride composite wafer structure based on a metal nano-intermediate layer, adopts a two-step bonding method of gallium nitride and diamond bonding, can reduce the bonding void rate, increase the bonding strength, and reduce the The thermal resistance between gallium nitride and diamond can improve the bonding quality of gallium nitride and diamond, and can prepare high-performance GaN-on-diamond devices.
以上所述仅仅是本发明的较佳实施例,并不用以对本发明的技术方案进行任何限制,本领域技术人员应当理解的是,在不脱离本发明精神和原则的前提下,该技术方案还可以进行若干简单的修改和替换,这些修改和替换也均会落入权利要求书所涵盖的保护范围。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the technical solutions of the present invention. Those skilled in the art should understand that, without departing from the spirit and principles of the present invention, the technical solutions also Several simple modifications and substitutions can be made, and these modifications and substitutions will also fall within the protection scope covered by the claims.
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| CN116084024A (en) * | 2022-12-12 | 2023-05-09 | 咸阳职业技术学院 | Gallium oxide and diamond wafer based on metal bonding layer and bonding method thereof |
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| CN119764179A (en) * | 2024-12-23 | 2025-04-04 | 西安电子科技大学芜湖研究院 | A wafer integration method for improving the bonding strength between gallium nitride and diamond |
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