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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- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
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- H01L29/2003—Nitride compounds
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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Abstract
A diamond-based gallium nitride composite wafer and bonding preparation method thereof, the wafer has gallium nitride/nucleation layer/carborundum/metal intermediate layer/diamond substrate, gallium nitride/ceramic membrane layer/metal intermediate layer/diamond substrate and other structures, the main preparation steps are: thinning the silicon carbide substrate of the gallium nitride, or completely stripping the silicon carbide substrate and thinning the gallium nitride layer; polishing the silicon carbide substrate or the gallium nitride layer and the surface to be bonded of the diamond and performing argon plasma treatment; depositing a metal buffer layer and a gold film on the surface to be bonded of the silicon carbide substrate, or depositing the metal buffer layer and the gold film or depositing a ceramic film layer, the metal buffer layer and the gold film on the surface to be bonded of the gallium nitride layer, and depositing the metal buffer layer and the gold film on the surface to be bonded of the diamond; firstly, pre-bonding gallium nitride and diamond, and then carrying out secondary bonding; and annealing the diamond-based gallium nitride composite wafer. The invention can improve the bonding strength.
Description
Technical Field
The invention belongs to the technical field of semiconductors and integrated circuits, and particularly relates 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.
Background
Gallium nitride as the third generation semiconductor material has the characteristics of large forbidden bandwidth, high breakdown field strength, high saturated electron speed, high temperature resistance, strong radiation resistance and the like compared with silicon and gallium arsenide materials, is very suitable for manufacturing high-temperature high-power devices, high-frequency microwave devices and ultraviolet and nuclear radiation detection devices, and has extremely high application value in the technical fields of communication, power electronics and the like. However, the serious self-heating effect and low thermal conductivity limit the full play of the inherent advantages of the gallium nitride device, and become a technical bottleneck for restricting the further development of the gallium nitride device to high frequency and high power.
The diamond has high thermal conductivity which is nearly five times of that of silicon carbide (one of common substrate materials of gallium nitride devices), and the diamond serving as the substrate material can effectively reduce the thermal resistance of the gallium nitride devices and obviously reduce the junction temperature of AlGaN/GaN. The international research in recent years shows that, compared with a gallium nitride device (silicon carbide-based gallium nitride composite device) using a diamond substrate as a substrate, the gallium nitride device (diamond-based gallium nitride composite device) using a diamond substrate has the advantages that the output power density, the power addition efficiency and the reliability of the device are obviously improved due to the solution of the heat dissipation problem, and the size of the module is further reduced. Therefore, the adoption of the diamond substrate is an effective method for solving the heat management problem of the gallium nitride device. Diamond-based gallium nitride composite devices are being developed as a mainstream technology for high-frequency and high-power semiconductor devices.
At present, three methods are mainly used for preparing a diamond-based gallium nitride composite device, 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 former two methods, because of the large mismatch between the thermal expansion coefficients of gallium nitride and diamond, the epitaxial growth of diamond or gallium nitride is carried out at a high temperature, and the wafer warpage is easily caused because of the large stress in the epitaxial layer; in addition, the lattice constants of gallium nitride and diamond are also greatly different, and it is difficult to grow a high-quality gallium nitride or diamond epitaxial layer. Different from the former two methods of preparing the diamond-based gallium nitride composite device by adopting diamond or gallium nitride epitaxial growth, the third method adopts a gallium nitride and diamond bonding technology, and has the advantages that high-quality gallium nitride and diamond can be prepared by respectively adopting respective optimal processes, bonding can be carried out at lower temperature or even room temperature, and the problem caused by mismatch of thermal expansion coefficients and lattice constants of the two materials is avoided. The key to obtain high bonding quality is to reduce the interface thermal resistance, reduce the bonding voidage and improve the bonding strength by adopting a bonding method to prepare the diamond-based gallium nitride composite device.
Disclosure of Invention
The invention aims to solve the problems in the preparation of a gallium nitride device, and provides a diamond-based gallium nitride composite wafer and a bonding preparation method thereof, which can effectively reduce the interface thermal resistance of gallium nitride and diamond, reduce the bonding voidage and improve the bonding strength, thereby preparing the high-performance diamond-based gallium nitride composite wafer and promoting the exertion of the advantages of the gallium nitride device.
In order to achieve the purpose, the invention adopts the following technical scheme:
a diamond-based gallium nitride composite wafer having a structure of any one of the following a), b) and c):
a) the multilayer structure is formed by gallium nitride, a nucleating layer, silicon carbide, a metal intermediate layer and a diamond substrate in sequence;
b) a multilayer structure formed by gallium nitride, a metal intermediate layer and a diamond substrate in sequence;
c) the multilayer structure is formed by gallium nitride, a ceramic film layer, a metal intermediate layer and a diamond substrate in sequence, wherein the ceramic film layer is made of aluminum nitride or silicon carbide;
the metal middle layer is provided with a metal buffer layer, a gold film layer and a metal buffer layer which are sequentially arranged; the metal buffer layer is made of tungsten, molybdenum or aluminum.
As a preferable scheme of the diamond-based gallium nitride composite wafer, 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 thickness of the layer of the silicon carbide in the structure a) is 5-80 microns; the thickness of the gallium nitride layer in the structure b) is 1-3 microns; the thickness of the gallium nitride layer in the structure c) is 1-3 microns, and the thickness of the ceramic film layer is 1-15 nanometers.
The invention also provides a bonding preparation method of the diamond-based gallium nitride composite wafer, which comprises the following steps:
1) bonding the surface of one side of the gallium nitride epitaxial layer of the gallium nitride of the silicon carbide substrate and the temporary slide glass together by using an adhesive;
2) thinning the silicon carbide substrate; or completely stripping the silicon carbide substrate, removing the nucleating layer and thinning the gallium nitride epitaxial layer;
3) polishing the surface of the thinned silicon carbide substrate or the surface of the thinned gallium nitride epitaxial layer, and polishing the surface of the diamond to ensure that the roughness of the silicon carbide substrate or the gallium nitride epitaxial layer and the diamond polishing surface is lower than a required value;
4) sequentially carrying out ultrasonic cleaning on gallium nitride and diamond by using acetone, ethanol and deionized water;
5) taking the polished surface of the silicon carbide substrate or the gallium nitride epitaxial layer as the surface to be bonded of the gallium nitride, taking the polished surface of the diamond as the surface to be bonded of the diamond, and carrying out argon plasma treatment on the surfaces to be bonded of the gallium nitride and the diamond;
6) sequentially depositing a metal buffer layer and a gold film layer on the to-be-bonded surface of the gallium nitride of the thinned silicon carbide substrate, or sequentially depositing a metal buffer layer and a gold film layer or sequentially depositing a ceramic film layer, a metal buffer layer and a gold film layer on the to-be-bonded surface of the gallium nitride of the thinned epitaxial layer of the gallium nitride; sequentially depositing a metal buffer layer and a gold film layer on the surface to be bonded of the diamond;
7) placing the surface to be bonded of the gallium nitride and the surface to be bonded of the diamond oppositely and making the surfaces to be bonded of the gallium nitride and the diamond contact with each other, and applying pressure to perform primary bonding, namely pre-bonding, of the gallium nitride and the diamond;
8) applying pressure to bond the gallium nitride and the diamond which are bonded together for the second time;
9) removing the adhesive and the temporary slide glass on the surface of the diamond substrate gallium nitride to prepare a diamond-based gallium nitride composite wafer;
10) and annealing the diamond-based gallium nitride composite wafer to finish the preparation.
As a preferable scheme of the bonding preparation method of the invention, the adhesive in step 1) is photoresist, benzocyclobutene or 502 glue; the temporary slide is made of silicon, aluminum oxide, silicon carbide, quartz or diamond, and the surface roughness of the temporary slide is not higher than 10 nanometers.
As a preferable scheme of the bonding preparation method, step 2) adopts a mechanical grinding method to thin the silicon carbide substrate to 5-80 microns; or continuously etching the residual silicon carbide substrate by adopting an inductive coupling plasma etching method, removing the nucleating layer, and thinning the gallium nitride epitaxial layer to 1-3 microns;
step 3) the required value of the roughness is 2 nanometers;
and 6) the thicknesses of the metal buffer layers deposited on the surfaces to be bonded of the gallium nitride and the diamond are respectively 1-20 nanometers, the thicknesses of the gold film layers deposited on the surfaces to be bonded of the gallium nitride and the diamond are respectively 2.5-100 nanometers, and the thickness of the ceramic film layer deposited on the surface to be bonded of the gallium nitride is 1-15 nanometers.
In a preferred embodiment of the bonding preparation method of the present invention, the argon plasma used in the argon plasma treatment in step 5) is generated by gas discharge, the discharge power is 30 to 200W, and the treatment time of the argon plasma is 0.5 to 20 minutes.
As a preferred scheme of the bonding preparation method, step 7) after depositing each film layer on the surfaces to be bonded of the gallium nitride and the diamond, performing the first bonding of the gallium nitride and the diamond by adopting a mechanical pressurization mode under the condition of not exposing the atmosphere, or taking the gallium nitride and the diamond out of a coating cavity, and rapidly performing the first bonding of the gallium nitride and the diamond by adopting a manual pressurization or weight pressurization mode under the conditions of room temperature and atmospheric environment, wherein the applied pressure is 0.2-2MPa, and the pressurization time is 1-3 minutes.
As a preferable scheme of the bonding preparation method, in the step 8), when the gallium nitride and the diamond are bonded for the second time, the temperature of the gallium nitride and the diamond is lower than 150 ℃, the applied pressure is 0.5-10MPa, and the pressurizing time is 1-20 minutes.
As a preferable scheme of the bonding preparation method of the invention, the mode of removing the adhesive and the temporary slide in the step 9) is as follows: putting the mixture into an acetone solution, and accelerating the dissolution of the adhesive by adopting ultrasonic vibration.
As a preferable scheme of the bonding preparation method, the annealing treatment in the step 10) is carried out in a vacuum environment or in a high-purity nitrogen atmosphere, the annealing temperature is 100-200 ℃, and the annealing time is 10-60 minutes.
Compared with the prior art, the diamond-based gallium nitride composite wafer has the following beneficial effects:
in the prior art, a titanium film layer and a chromium film layer are generally used as buffer layers of a gold film bonding layer, and stronger bonding force between the titanium film or the chromium film and materials such as silicon carbide, gallium nitride, diamond, a gold film and the like is utilized to improve the bonding strength between the gold film and the silicon carbide, the gallium nitride and the diamond. However, the thermal conductivity of titanium and chromium is low, about 21.9W/mK and 93.7W/mK, respectively, and their use as buffer layers increases the thermal resistance between gallium nitride and diamond. The composite wafer of the invention adopts tungsten, molybdenum and aluminum as buffer layers, the metal film layers not only have good bonding force with silicon carbide, gallium nitride and diamond, but also have higher thermal conductivity (respectively about 174W/m.K, 138W/m.K and 237W/m.K), and the thermal resistance between the gallium nitride and the diamond can be reduced by using the metal film layers as the buffer layers, thereby being beneficial to reducing the temperature of a hot spot area of a gallium nitride device. In addition, for the scheme of bonding the thinned gallium nitride epitaxial layer and the diamond, in order to prevent metal atoms in the metal nano bonding layer from diffusing into the gallium nitride to reduce the performance of the device, a thin aluminum nitride or silicon carbide ceramic film layer with high thermal conductivity is deposited on the surface to be bonded of the thinned gallium nitride epitaxial layer, then a metal buffer layer and a gold film are deposited, the ceramic film layer is used for preventing the metal atoms from entering the gallium nitride, and the adverse effect of the existence of the metal bonding layer on the performance of the gallium nitride device can be avoided.
The invention adopts two technical schemes to prepare the diamond-based gallium nitride composite wafer. The first scheme is to reserve a silicon carbide substrate with the thickness of 5-80 microns of gallium nitride and bond the surface of the silicon carbide substrate with diamond as a bonding surface. The scheme has the advantages of relatively simple preparation process and high bonding success rate, but has the defect that the thermal resistance of the prepared diamond-based gallium nitride composite device is high due to the existence of the silicon carbide substrate and the thicker gallium nitride epitaxial layer. The second scheme is to strip off the silicon carbide substrate and the nucleation layer completely, thin the gallium nitride to 1-3 microns, and bond the surface of the thinned gallium nitride as a bonding surface with diamond. The diamond-based gallium nitride composite device prepared by the scheme has the advantages that the distance between the hot spot region of the diamond-based gallium nitride composite device and the diamond substrate is short, the heat dissipation of the device is facilitated, but the preparation process is complex, the technical difficulty is high, and the manufacturing cost is high. Therefore, the two technical schemes have advantages and disadvantages respectively, and different technical schemes can be selected according to different actual requirements.
Compared with the prior art, the bonding preparation method of the diamond-based gallium nitride composite wafer has the following beneficial effects: the existing wafer bonding technology generally adopts the steps that after a metal bonding layer is deposited on the bonding surface of a wafer, the wafer is taken out of a coating machine and then put into bonding equipment for pressure bonding. Since a long time is usually required from the time of taking out the wafer from the coater to the time of putting the wafer into the bonding equipment, more gas (such as water vapor) and even some dust particles are adsorbed on the surface of the metal bonding layer during the long time, and the mutual diffusion of the gold atoms on two sides of the bonding interface of the gallium nitride and the diamond and the formation of metal bonds are influenced, thereby reducing the bonding quality. The bonding of gallium nitride and diamond is carried out in two steps, namely after depositing each film layer on the surfaces of the gallium nitride and the diamond to be bonded, applying pressure to pre-bond the gallium nitride and the diamond under the condition of not exposing the atmosphere, or taking the gallium nitride and the diamond out of a cavity of a sputtering film plating machine, rapidly applying pressure to pre-bond the gallium nitride and the diamond, and then putting the pre-bonded gallium nitride and the diamond into bonding equipment to carry out secondary bonding of the gallium nitride and the diamond. The pre-bonding mode can avoid the surface of the metal nano bonding layer from being exposed in the air or shorten the time of the surface of the metal nano bonding layer to be exposed in the air as much as possible, and reduce the pollution of the gas and dust particle adsorption to the surface of the metal nano bonding layer, so as to ensure that the surfaces of two fresh gold films on the surfaces to be bonded of the gallium nitride and the diamond can be fully contacted with each other. And then, in order to increase the bonding strength, the pre-bonded sample is put into a bonding device for secondary bonding, and the secondary bonding only needs to apply lower pressure to realize bonding with low voidage and high bonding strength because the surfaces of the two gold films which are in contact with each other are very clean. According to the invention, before the metal nano bonding layer is deposited, the argon plasma is used for treating the surface to be bonded, so that the surface to be bonded of gallium nitride and diamond can be thoroughly cleaned, and the bonding force between the silicon carbide substrate or the gallium nitride epitaxial layer and the metal nano bonding layer as well as between the diamond substrate and the metal nano bonding layer is enhanced. In order to enhance the bonding strength of bonding between the gallium nitride and the diamond based on the metal nano bonding layer, the invention carries out annealing treatment on the bonded diamond-based gallium nitride composite wafer, thereby enhancing the mutual diffusion of gold atoms at two sides of a gold/gold bonding interface and improving the bonding strength of the gallium nitride and the diamond.
The invention improves the technical process and the structural characteristics, and the preparation of the high-performance diamond-based gallium nitride device can be realized by adopting the diamond-based gallium nitride composite wafer and the corresponding bonding preparation method.
Drawings
FIG. 1 is a process flow diagram of the gallium nitride and diamond bonding method based on a metal nanolayer according to the present invention;
fig. 2 example 1 is a schematic diagram of a structure (gan/nucleation layer/sic (5-80 μm)/metal buffer layer/au film/metal buffer layer/diamond) of a diamond-based gan composite wafer prepared by the bonding method of the present invention;
fig. 3 example 2 is a schematic diagram of a structure (i.e. gan (1-3 μm)/metal buffer layer/au film/metal buffer layer/diamond) of a diamond-based gan composite wafer prepared by the bonding method of the present invention;
fig. 4 is a schematic diagram of a structure (i.e. gallium nitride (1-3 microns)/ceramic film layer/metal buffer layer/gold film/metal buffer layer/diamond) of a diamond-based gallium nitride composite wafer prepared by the bonding method of the present invention in example 3;
FIG. 5 is an atomic force microscope photograph of a diamond substrate subjected to surface polishing;
FIG. 6 is an atomic force microscope image of a diamond substrate with a molybdenum buffer layer and a gold thin film deposited thereon;
FIG. 7 is an atomic force microscope image of a surface polished gallium nitride layer;
FIG. 8 is an atomic force microscope image of a molybdenum buffer layer and a gold thin film deposited on a gallium nitride layer;
FIG. 9 is a diagram showing the morphology of a diamond-based GaN composite wafer with a GaN/nucleation layer/SiC (5-80 μm)/metal buffer layer/Au film/metal buffer layer/diamond multilayer structure prepared by the bonding method of the present invention;
FIG. 10 is a diagram showing the morphology of a diamond-based GaN composite wafer with a multilayer structure of GaN (1-3 μm)/metal buffer layer/gold film/metal buffer layer/diamond prepared by the bonding method of the present invention;
FIG. 11 is an ultrasonic scanning microscope image of a diamond-based gallium nitride composite wafer prepared by the bonding method of the present invention.
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.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
In order to solve the heat dissipation problem of high-frequency and high-power gallium nitride devices, the gallium nitride devices are combined with diamond substrates with high heat conductivity, the invention adopts a bonding method based on metal nano layers to prepare diamond-based gallium nitride composite wafers, and the wafers have structures of gallium nitride/nucleation layers/silicon carbide/metal intermediate layers/diamond substrates, gallium nitride/ceramic film layers/metal intermediate layers/diamond substrates and the like. The preparation method provided by the invention comprises the steps of bonding gallium nitride and diamond in two steps, namely after depositing each film layer on the surface to be bonded of the gallium nitride and the diamond, pre-bonding the gallium nitride and the diamond by adopting a mechanical pressurization mode under the condition of not exposing the atmosphere, or taking the gallium nitride and the diamond out of a coating cavity, rapidly pre-bonding the gallium nitride and the diamond by adopting a manual pressurization or weight pressurization mode under the conditions of room temperature and atmospheric environment, and then carrying out secondary bonding of the gallium nitride and the diamond by using bonding equipment. The pre-bonding mode can avoid the surface of the metal nano bonding layer from being exposed in the air or shorten the time of the surface of the metal nano bonding layer exposed in the air as much as possible, and reduce the pollution of the adsorption of gas and dust particles on the surface of the metal nano bonding layer so as to ensure that the surfaces of two fresh gold films are mutually contacted. In order to increase the bonding strength, the sample subjected to the pre-bonding is placed into a bonding device for secondary bonding, and because the surfaces of two gold films which are in contact with each other are clean, the secondary bonding only needs to apply lower pressure to obtain low bonding void ratio and high bonding strength. Before the metal buffer layer is deposited, the argon plasma is used for treating the surface to be bonded, so that the surface to be bonded can be cleaned, and the bonding force between the silicon carbide substrate or the gallium nitride epitaxial layer and the diamond and the metal buffer layer is enhanced, so that the bonding quality is improved. The tungsten, the molybdenum and the aluminum are used as buffer layers, the metal film layers not only can have good bonding force with silicon carbide, gallium nitride, diamond and gold films, but also have high thermal conductivity, and the metal film layers are used as the buffer layers to be beneficial to reducing the temperature of a hot spot area of a gallium nitride device. In addition, for the scheme of bonding the thinned gallium nitride epitaxial layer and the diamond, in order to prevent metal atoms in the metal nano layer from diffusing into the gallium nitride to reduce the performance of the device, a thin aluminum nitride or silicon carbide ceramic film layer is deposited on the surface to be bonded of the thinned gallium nitride epitaxial layer, then a metal buffer layer and a gold film are deposited, and the ceramic film layer is used for preventing the metal atoms from entering the gallium nitride. In order to further increase the bonding strength of the gallium nitride and the diamond, annealing treatment is carried out on the gallium nitride of the diamond substrate after bonding so as to enhance the mutual diffusion of gold atoms on two sides of a gold/gold bonding interface.
Therefore, the diamond-based gallium nitride composite wafer with low voidage and high bonding strength can be prepared by adopting the diamond-based gallium nitride composite wafer and the bonding preparation method thereof, and the heat dissipation problem of high-frequency and high-power gallium nitride devices can be effectively solved.
Example 1
Referring to fig. 1 and 2, the diamond-based gallium nitride composite wafer prepared by the invention has a structure of gallium nitride/nucleation layer/silicon carbide (5-80 microns)/metal buffer layer/gold film/metal buffer layer/diamond, and the specific preparation method comprises the following steps:
1) bonding the surface of the gallium nitride epitaxial layer of the gallium nitride on the silicon carbide substrate and a silicon wafer (temporary slide glass) by using photoresist;
2) thinning the silicon carbide substrate to 40 microns by adopting mechanical grinding;
3) polishing the surfaces of the silicon carbide substrate and the diamond to ensure that the roughness of the polished surfaces of the silicon carbide substrate and the diamond is lower than 2 nanometers;
4) sequentially carrying out ultrasonic cleaning on gallium nitride and diamond by using acetone, ethanol and deionized water;
5) putting gallium nitride and diamond into a sputtering film plating machine, taking the polished surfaces of the silicon carbide substrate and the diamond as surfaces to be bonded, and carrying out argon plasma treatment on the surfaces to be bonded, wherein the plasma discharge power is 50W, and the treatment time is 5 minutes;
6) depositing a tungsten buffer layer with the thickness of 2 nanometers and a gold film with the thickness of 10 nanometers on the surfaces to be bonded of the silicon carbide substrate and the diamond in sequence by adopting a sputtering deposition method;
7) after depositing the tungsten buffer layer and the gold film on the surfaces to be bonded of the silicon carbide substrate and the diamond, placing the surface to be bonded of the silicon carbide substrate and the surface to be bonded of the diamond substrate oppositely and making the surfaces to be bonded of the silicon carbide substrate and the diamond substrate contact with each other under the condition of not exposing the atmosphere, performing pre-bonding of gallium nitride and the diamond by adopting a mechanical pressurization mode, and applying pressure of 0.3MPa and keeping the pressure for 3 minutes;
8) putting the pre-bonded gallium nitride and diamond into bonding equipment, applying 5MPa pressure to the gallium nitride and the diamond, keeping for 5 minutes, performing secondary bonding, and bonding the gallium nitride and the diamond substrate together;
9) placing the diamond substrate gallium nitride bonded on the temporary slide glass into a container containing acetone solution, accelerating the dissolution of the adhesive by adopting ultrasonic vibration, and removing the adhesive on the surface of the diamond substrate gallium nitride and the temporary slide glass to prepare a diamond-based gallium nitride composite wafer;
10) and annealing the diamond-based gallium nitride composite wafer in a vacuum environment, wherein the annealing temperature is 150 ℃, and the annealing time is 40 minutes.
Example 2
Referring to fig. 1 and 3, the diamond-based gallium nitride composite wafer prepared by the invention has a structure of gallium nitride (1-3 microns)/metal buffer layer/gold film/metal buffer layer/diamond, and the specific preparation method comprises the following steps:
1) bonding the surface of the gallium nitride epitaxial layer of the gallium nitride of the silicon carbide substrate with a silicon carbide wafer (temporary carrier) by benzocyclobutene (BCB);
2) thinning the silicon carbide substrate to 30 microns by adopting mechanical grinding, then etching the rest silicon carbide substrate by adopting an inductive coupling plasma etching method, removing the nucleating layer, and thinning the gallium nitride epitaxial layer to 2 microns;
3) polishing the surfaces of the gallium nitride epitaxial layer and the diamond to ensure that the roughness of the polished surfaces of the gallium nitride and the diamond is lower than 2 nanometers;
4) sequentially carrying out ultrasonic cleaning on gallium nitride and diamond by using acetone, ethanol and deionized water;
5) putting gallium nitride and diamond into a sputtering film plating machine, taking the polished surfaces of the gallium nitride and the diamond as surfaces to be bonded, and carrying out argon plasma treatment on the surfaces to be bonded, wherein the plasma discharge power is 100W, and the treatment time is 2 minutes;
6) adopting a sputtering deposition method to sequentially deposit a molybdenum buffer layer with the thickness of 3 nanometers and a gold film with the thickness of 15 nanometers on the surfaces to be bonded of the gallium nitride and the diamond;
7) taking out the gallium nitride and the diamond from the sputtering film plating machine, rapidly and oppositely placing the surface to be bonded of the gallium nitride and the surface to be bonded of the diamond substrate within 1 minute and enabling the surfaces to be bonded of the gallium nitride and the diamond substrate to be in contact with each other, applying 0.5MPa pressure to the gallium nitride and the diamond by adopting a weight pressurizing mode, and keeping for 2 minutes to carry out first bonding, namely pre-bonding;
8) putting the pre-bonded gallium nitride and diamond into bonding equipment, applying 10MPa pressure to the gallium nitride and the diamond, keeping for 3 minutes, performing secondary bonding, and bonding the gallium nitride and the diamond substrate together;
9) placing the diamond substrate gallium nitride bonded on the temporary slide glass into a container containing acetone solution, accelerating the dissolution of the adhesive by adopting ultrasonic vibration, and removing the adhesive on the surface of the diamond substrate gallium nitride and the temporary slide glass to prepare a diamond-based gallium nitride composite wafer;
10) and annealing the diamond-based gallium nitride composite wafer in a high-purity nitrogen environment at 180 ℃ for 20 minutes.
Example 3
Referring to fig. 1 and 4, the diamond-based gallium nitride composite wafer prepared by the invention has a structure of gallium nitride (1-3 microns)/ceramic film layer/metal buffer layer/gold film/metal buffer layer/diamond, and the specific preparation method comprises the following steps:
1) adhering the surface of the gallium nitride epitaxial layer of the gallium nitride on the silicon carbide substrate and a quartz plate (temporary slide glass) together by using 502 glue;
2) thinning the silicon carbide substrate to 50 microns by adopting mechanical grinding, then etching the rest silicon carbide substrate by adopting an inductive coupling plasma etching method, removing the nucleating layer, and thinning the gallium nitride epitaxial layer to 3 microns;
3) polishing the surfaces of the gallium nitride epitaxial layer and the diamond to ensure that the roughness of the polished surfaces of the gallium nitride and the diamond is lower than 2 nanometers;
4) sequentially carrying out ultrasonic cleaning on gallium nitride and diamond by using acetone, ethanol and deionized water;
5) putting gallium nitride and diamond into a sputtering film plating machine, taking the polished surfaces of the gallium nitride and the diamond as surfaces to be bonded, and carrying out argon plasma treatment on the surfaces to be bonded, wherein the plasma discharge power is 150W, and the treatment time is 1 minute;
6) adopting a sputtering deposition method to sequentially deposit an aluminum nitride film with the thickness of 2 nanometers, an aluminum buffer layer with the thickness of 4 nanometers and a gold film with the thickness of 50 nanometers on the surface to be bonded of the gallium nitride, and sequentially depositing the aluminum buffer layer with the thickness of 4 nanometers and the gold film with the thickness of 50 nanometers on the surface to be bonded of the diamond;
7) taking out the gallium nitride and the diamond from the sputtering film plating machine, rapidly and oppositely placing the surface to be bonded of the gallium nitride and the surface to be bonded of the diamond substrate within 1 minute and enabling the surfaces to be bonded of the gallium nitride and the diamond substrate to be in contact with each other, applying 1MPa pressure to the gallium nitride and the diamond by adopting a manual pressurization mode, and keeping the pressure for 1 minute to carry out first bonding, namely pre-bonding;
8) putting the pre-bonded gallium nitride and diamond into bonding equipment, applying 8MPa pressure to the gallium nitride and the diamond, keeping for 4 minutes, performing secondary bonding, and bonding the gallium nitride and the diamond substrate together;
9) placing the diamond substrate gallium nitride bonded on the temporary slide glass into a container containing acetone solution, accelerating the dissolution of the adhesive by adopting ultrasonic vibration, and removing the adhesive on the surface of the diamond substrate gallium nitride and the temporary slide glass to prepare a diamond-based gallium nitride composite wafer;
10) and annealing the diamond-based gallium nitride composite wafer in a high-purity nitrogen environment at 120 ℃ for 60 minutes.
Example 4
Referring to fig. 1 and 4, the diamond-based gallium nitride composite wafer prepared by the invention has a structure of gallium nitride (1-3 microns)/ceramic film layer/metal buffer layer/gold film/metal buffer layer/diamond, and the specific preparation method comprises the following steps:
1) bonding the surface of the gallium nitride epitaxial layer of the gallium nitride on the silicon carbide substrate and a diamond crystal (temporary slide glass) sheet together by using photoresist;
2) thinning the silicon carbide substrate to 10 microns by adopting mechanical grinding, then etching the rest silicon carbide substrate by adopting an inductive coupling plasma etching method, removing the nucleating layer, and thinning the gallium nitride epitaxial layer to 1.5 microns;
3) polishing the surfaces of the gallium nitride and the diamond to ensure that the roughness of the polished surfaces of the gallium nitride and the diamond is lower than 2 nanometers;
4) sequentially carrying out ultrasonic cleaning on gallium nitride and diamond by using acetone, ethanol and deionized water;
5) putting gallium nitride and diamond into a sputtering film plating machine, taking the polished surfaces of the gallium nitride and the diamond as surfaces to be bonded, and carrying out argon plasma treatment on the surfaces to be bonded, wherein the plasma discharge power is 80W, and the treatment time is 3 minutes;
6) depositing a silicon carbide film with the thickness of 3 nanometers, a tungsten buffer layer with the thickness of 5 nanometers and a gold film with the thickness of 8 nanometers on the surface to be bonded of the gallium nitride in sequence by adopting a sputtering deposition method, and depositing the tungsten buffer layer with the thickness of 5 nanometers and the gold film with the thickness of 8 nanometers on the surface to be bonded of the diamond in sequence;
7) taking out the gallium nitride and the diamond from the sputtering film plating machine, rapidly and oppositely placing the surface to be bonded of the gallium nitride and the surface to be bonded of the diamond substrate within 1 minute and enabling the surfaces to be bonded of the gallium nitride and the diamond substrate to be in contact with each other, applying 1.5MPa pressure to the gallium nitride and the diamond by adopting a weight pressurizing mode, and keeping the pressure for 1 minute to carry out first bonding, namely pre-bonding;
8) putting the pre-bonded gallium nitride and diamond into bonding equipment, applying 3MPa pressure to the gallium nitride and the diamond, keeping for 10 minutes, performing secondary bonding, and bonding the gallium nitride and the diamond substrate together;
9) placing the diamond substrate gallium nitride bonded on the temporary slide glass into a container containing acetone solution, accelerating the dissolution of the adhesive by adopting ultrasonic vibration, and removing the adhesive on the surface of the diamond substrate gallium nitride and the temporary slide glass to prepare a diamond-based gallium nitride composite wafer;
10) and annealing the diamond-based gallium nitride composite wafer in a vacuum environment, wherein the annealing temperature is 200 ℃, and the annealing time is 10 minutes.
Referring to fig. 5, 6, 7 and 8, it can be seen that the diamond substrate and the gallium nitride layer after surface polishing both have very low surface roughness, 0.509 nm and 0.265 nm, respectively, and even after the molybdenum buffer layer and the gold thin film are deposited on their bonding surfaces, the surface roughness is still very low, 0.685 nm and 0.438 nm, respectively, which is beneficial to achieving high-quality bonding of gallium nitride and diamond.
Fig. 9 and 10 show the morphology of a diamond-based gallium nitride composite wafer having a gallium nitride/nucleation layer/silicon carbide (5-80 μm)/metal buffer layer/gold film/metal buffer layer/diamond structure and a gallium nitride (1-3 μm)/metal buffer layer/gold film/metal buffer layer/diamond structure, respectively, prepared by a bonding method, and both samples achieved a bonding strength of 10MPa or more.
Fig. 11 is an ultrasonic scanning microscope photograph of a diamond-based gallium nitride composite wafer prepared by a bonding method, and it is apparent that no void exists at the bonding interface of gallium nitride and diamond.
The invention realizes the structure of the diamond-based gallium nitride composite wafer based on the metal nano intermediate layer, adopts the bonding method of gallium nitride and diamond by two-step bonding, can reduce the bonding voidage, increase the bonding strength, reduce the thermal resistance between the gallium nitride and the diamond, achieve the purpose of improving the bonding quality of the gallium nitride and the diamond, and can prepare a high-performance diamond-based gallium nitride device.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical solution of the present invention, and it should be understood by those skilled in the art that the technical solution can be modified and replaced by a plurality of simple modifications and replacements without departing from the spirit and principle of the present invention, and the modifications and replacements will fall into the protection scope covered by the claims.
Claims (10)
1. A diamond-based gallium nitride composite wafer characterized by having any one of the following structures a), b) and c):
a) the multilayer structure is formed by gallium nitride, a nucleating layer, silicon carbide, a metal intermediate layer and a diamond substrate in sequence;
b) a multilayer structure formed by gallium nitride, a metal intermediate layer and a diamond substrate in sequence;
c) the multilayer structure is formed by gallium nitride, a ceramic film layer, a metal intermediate layer and a diamond substrate in sequence, wherein the ceramic film layer is made of aluminum nitride or silicon carbide;
the metal middle layer is provided with a metal buffer layer, a gold film layer and a metal buffer layer which are sequentially arranged; the metal buffer layer is made of tungsten, molybdenum or aluminum.
2. The diamond-based gallium nitride composite wafer according to claim 1, wherein: 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 thickness of the layer of the silicon carbide in the structure a) is 5-80 microns; the thickness of the gallium nitride layer in the structure b) is 1-3 microns; the thickness of the gallium nitride layer in the structure c) is 1-3 microns, and the thickness of the ceramic film layer is 1-15 nanometers.
3. A bonding preparation method of a diamond-based gallium nitride composite wafer is characterized by comprising the following steps:
1) bonding the surface of one side of the gallium nitride epitaxial layer of the gallium nitride of the silicon carbide substrate and the temporary slide glass together by using an adhesive;
2) thinning the silicon carbide substrate; or completely stripping the silicon carbide substrate, removing the nucleating layer and thinning the gallium nitride epitaxial layer;
3) polishing the surface of the thinned silicon carbide substrate or the surface of the thinned gallium nitride epitaxial layer, and polishing the surface of the diamond to ensure that the roughness of the silicon carbide substrate or the gallium nitride epitaxial layer and the diamond polishing surface is lower than a required value;
4) sequentially carrying out ultrasonic cleaning on gallium nitride and diamond by using acetone, ethanol and deionized water;
5) taking the polished surface of the silicon carbide substrate or the gallium nitride epitaxial layer as the surface to be bonded of the gallium nitride, taking the polished surface of the diamond as the surface to be bonded of the diamond, and carrying out argon plasma treatment on the surfaces to be bonded of the gallium nitride and the diamond;
6) sequentially depositing a metal buffer layer and a gold film layer on the to-be-bonded surface of the gallium nitride of the thinned silicon carbide substrate, or sequentially depositing a metal buffer layer and a gold film layer or sequentially depositing a ceramic film layer, a metal buffer layer and a gold film layer on the to-be-bonded surface of the gallium nitride of the thinned epitaxial layer of the gallium nitride; sequentially depositing a metal buffer layer and a gold film layer on the surface to be bonded of the diamond;
7) placing the surface to be bonded of the gallium nitride and the surface to be bonded of the diamond oppositely and making the surfaces to be bonded of the gallium nitride and the diamond contact with each other, and applying pressure to perform primary bonding, namely pre-bonding, of the gallium nitride and the diamond;
8) applying pressure to bond the gallium nitride and the diamond which are bonded together for the second time;
9) removing the adhesive and the temporary slide glass on the surface of the diamond substrate gallium nitride to prepare a diamond-based gallium nitride composite wafer;
10) and annealing the diamond-based gallium nitride composite wafer to finish the preparation.
4. The bonding preparation method of the diamond-based gallium nitride composite wafer according to claim 3, wherein: the adhesive in the step 1) is photoresist, benzocyclobutene or 502 glue;
the temporary slide is made of silicon, aluminum oxide, silicon carbide, quartz or diamond, and the surface roughness of the temporary slide is not higher than 10 nanometers.
5. The bonding preparation method of the diamond-based gallium nitride composite wafer according to claim 3, wherein: step 2) thinning the silicon carbide substrate to 5-80 microns by adopting a mechanical grinding method; or continuously etching the residual silicon carbide substrate by adopting an inductive coupling plasma etching method, removing the nucleating layer, and thinning the gallium nitride epitaxial layer to 1-3 microns;
step 3) the required value of the roughness is 2 nanometers;
and 6) the thicknesses of the metal buffer layers deposited on the surfaces to be bonded of the gallium nitride and the diamond are respectively 1-20 nanometers, the thicknesses of the gold film layers deposited on the surfaces to be bonded of the gallium nitride and the diamond are respectively 2.5-100 nanometers, and the thickness of the ceramic film layer deposited on the surface to be bonded of the gallium nitride is 1-15 nanometers.
6. The bonding preparation method of the diamond-based gallium nitride composite wafer according to claim 3, wherein: the argon plasma adopted in the argon plasma treatment in the step 5) is generated by gas discharge, the discharge power is 30-200W, and the treatment time of the argon plasma is 0.5-20 minutes.
7. The bonding preparation method of the diamond-based gallium nitride composite wafer according to claim 3, wherein: and 7) after depositing all film layers on the surfaces to be bonded of the gallium nitride and the diamond, performing primary bonding of the gallium nitride and the diamond by adopting a mechanical pressurization mode under the condition of not exposing the atmosphere, or taking the gallium nitride and the diamond out of the coating cavity, and rapidly performing primary bonding of the gallium nitride and the diamond by adopting a manual pressurization or weight pressurization mode under the conditions of room temperature and the atmosphere, wherein the applied pressure is 0.2-2MPa, and the pressurization time is 1-3 minutes.
8. The bonding preparation method of the diamond-based gallium nitride composite wafer according to claim 3, wherein: and 8) during the second bonding of the gallium nitride and the diamond, the temperature of the gallium nitride and the diamond is lower than 150 ℃, the applied pressure is 0.5-10MPa, and the pressurizing time is 1-20 minutes.
9. The bonding preparation method of the diamond-based gallium nitride composite wafer according to claim 3, wherein the manner of removing the adhesive and the temporary carrier in step 9) is as follows: putting the mixture into an acetone solution, and accelerating the dissolution of the adhesive by adopting ultrasonic vibration.
10. The bonding preparation method of the diamond-based gallium nitride composite wafer according to claim 3, wherein the annealing treatment of step 10) is performed in a vacuum environment or in a nitrogen atmosphere, the annealing temperature is 100-200 ℃, and the annealing time is 10-60 minutes.
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