CN114959898A - Preparation method of silicon carbide epitaxial wafer for high-voltage and ultrahigh-voltage device - Google Patents
Preparation method of silicon carbide epitaxial wafer for high-voltage and ultrahigh-voltage device Download PDFInfo
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Abstract
The invention provides a preparation method of a silicon carbide epitaxial wafer for a high-voltage and ultrahigh-voltage device, which comprises the following steps: coating a carbon film on the carbon surface of a silicon carbide substrate, placing the silicon carbide substrate in an epitaxial furnace reaction chamber, introducing hydrogen, gradually heating to 1600-1650 ℃, introducing a silicon source, a carbon source and a doping source, growing a buffer layer on the silicon surface of the silicon carbide substrate, adjusting the flow values of various sources, growing an epitaxial layer to a specified thickness, annealing, cooling to room temperature, protecting a wafer, and then removing the carbon film to obtain the silicon carbide epitaxial wafer. The carbon film is coated on the carbon surface of the substrate on the basis of the existing commercial epitaxial furnace, carbon vacancies of the epitaxial layer are supplemented through carbon atom migration of the carbon film in the processes of epitaxy and annealing, carbon vacancy restoration is realized, in addition, annealing process parameters can be adjusted to improve the density of the carbon vacancies, and the service life of a current carrier is prolonged.
Description
Technical Field
The invention belongs to a silicon carbide epitaxial growth method, and particularly relates to a preparation method of a silicon carbide epitaxial wafer for a high-voltage and ultrahigh-voltage device.
Background
The third generation semiconductor silicon carbide material has the advantages of high thermal conductivity, high breakdown field strength, high saturated electron drift rate and the like, can meet the new requirements of modern electronic technology on severe conditions such as high temperature, high power, high voltage, high frequency, radiation resistance and the like, and is also the strategic direction of the semiconductor technology in China in the future. With the continuous popularization and development of the third-generation semiconductor material, the semiconductor material plays a key role in the industries of power electronics, aerospace, new energy, smart power grids, electric vehicles and the like.
Light is irradiated on the surface of the semiconductor, and absorption is caused. Photon absorption simultaneously generates one majority carrier and one minority carrier, referred to as non-equilibrium carriers. In many semiconductor materials, the number of photogenerated non-equilibrium carriers is much less than the majority carriers due to doping that are inherently present in the material. Thus, the number of majority carriers in a semiconductor is substantially unchanged upon illumination, while minority carriers are significantly increased.
The average time of the non-equilibrium carriers from generation to recombination is called the non-equilibrium carrier lifetime (minority carrier lifetime), denoted by τ. It reflects the decay rate of minority carrier concentration. The influence of unbalanced minority carriers is dominant over unbalanced majority carriers, so the lifetime of unbalanced carriers is often referred to as minority carrier lifetime, abbreviated as minority carrier lifetime
Minority carrier lifetime is an important parameter of semiconductor materials and semiconductor devices, and directly reflects the quality of the materials and whether the characteristics of the devices meet requirements. In addition, the minority carrier lifetime is also a key factor influencing the characteristics of high-voltage bipolar power devices such as SiC IGBTs, and for bipolar semiconductor devices which mainly operate by means of minority carrier transport (mainly diffusion), in order to ensure that the minority carrier recombination in the base region is as little as possible (so as to obtain a large current amplification factor), the longer the minority carrier lifetime of the base region is, the better the minority carrier lifetime is. For IGBT switching devices, the direct effect of minority carrier lifetime reduction is to reduce the conductance modulation effect. Therefore, the service life of minority carriers is prolonged, which is an important requirement for manufacturing high-voltage ultrahigh-voltage devices and has important significance for the development of semiconductor devices.
In order to reduce conduction loss when manufacturing a high-voltage ultra-high device, conductivity modulation based on injection of minority carriers needs to be generated by prolonging the carrier lifetime of a drift layer, so that the conduction voltage is reduced. Therefore, in order to extend the carrier lifetime of the drift layer, it is necessary to reduce crystal defects which are present in the epitaxial film and cause the lifetime to be shortened. For example, as being present in an n-type SiC epitaxial film, so-called Z 1/2 Center and EH 6/7 The central point defect is the major crystal defect that results in a shortened carrier lifetime. The literature (n.t. son, et al, phys.rev.lett.109(2012)187603) refers to these Z' s 1/2 Center and EH 6/7 The center is a crystal defect caused by a carbon (C) vacancy in the SiC epitaxial film. Therefore, in order to reduce crystal defects in the SiC epitaxial film, it is necessary to form the SiC epitaxial film with few carbon vacancies. As a method for reducing carbon vacancies in SiC epitaxial films, it has been proposed to form a SiC epitaxial film by chemical vapor deposition and then further perform carbon ion implantationAnd high-temperature annealing heat treatment or long-time high-temperature sacrificial oxidation.
The method of high-temperature annealing after carbon implantation is easy to introduce new defects in the process of high-energy carbon ion implantation; in severe cases, the damaged layer on the surface of the epitaxial layer can not be repaired after long-time annealing, so that the using effect of the device is influenced, and meanwhile, the effect is not ideal enough for the thick-layer silicon carbide epitaxy due to the limitation of the carbon injection depth.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a silicon carbide epitaxial wafer for a high-voltage and ultra-high-voltage device, which realizes effective repair of carbon vacancies during in-situ growth, thereby achieving the purpose of prolonging the carrier lifetime of a silicon carbide epitaxial layer.
The invention provides a preparation method of a silicon carbide epitaxial wafer for a high-voltage and ultrahigh-voltage device, which comprises the following steps:
coating a carbon film on the carbon surface of a silicon carbide substrate, placing the silicon carbide substrate in an epitaxial furnace reaction chamber, introducing hydrogen, gradually heating to 1600-1650 ℃, introducing a silicon source, a carbon source and a doping source, growing a buffer layer on the silicon surface of the silicon carbide substrate, adjusting the flow values of various sources, growing an epitaxial layer to a specified thickness, annealing, cooling to room temperature, performing silicon surface blue film protection on a wafer, and removing the carbon film to obtain the silicon carbide epitaxial wafer for the high-pressure and ultrahigh-pressure device.
In the present invention, the silicon carbide substrate is selected from silicon carbide in which the silicon plane is biased toward the <11-20> direction by 1 ° to 8 °.
In the present invention, the carbon film has a thickness of 50 to 500. mu.m.
In the invention, the flow rate of the hydrogen is 80-120L/min, and the pressure of the introduced hydrogen to the reaction chamber is 80-200 mbar.
And after the reaction chamber reaches the set temperature of 1600-1650 ℃, opening air inlet valves of a precursor silicon source, a carbon source and a doping source, introducing various sources into an exhaust gas path, setting the flow of various sources through mass flow to meet the flow requirement required by a growth buffer layer, keeping other parameters unchanged, and carrying out in-situ hydrogen etching treatment on the silicon carbide substrate for 5-15 minutes.
In the invention, before introducing a silicon source, a carbon source and a doping source, in-situ hydrogen etching treatment is carried out on the silicon carbide substrate for 5-15 min.
In the present invention, the rate of growth of the buffer layer is 10 microns/hour; C/Si is more than or equal to 0.8 and less than or equal to 1.4 when the buffer layer grows;
the thickness of the buffer layer is 0.5-10 μm, and the doping concentration is 1-5 × 10 18 cm -3 。
In the present invention, the rate of growth of the epitaxial layer is greater than 80 microns/hour. Adjusting the flow values of various sources before the epitaxial layer grows, specifically comprising the following steps: and transferring the silicon source, the carbon source and the doping source to an exhaust gas path, keeping the pressure, the growth temperature and the hydrogen flow in the reaction chamber unchanged, and gradually changing the flow of each source to the flow value required by rapid growth within 30 seconds.
In the invention, the epitaxial layer can be a drift layer with the thickness of 70-100 microns required by 6500V and 10KV high-voltage devices.
In the present invention, the carbon film is produced by vapor deposition;
or coating photoresist and drying.
In the invention, the silicon source is selected from silane, dichlorosilane or trichlorosilane;
the carbon source is selected from methane, ethylene or propane.
In the present invention, the dopant source is selected from N 2 And/or TMA (trimethylaluminum).
In the invention, after an epitaxial layer is grown to a specified thickness, a silicon source, a carbon source and a doping source are transferred to an exhaust gas path, the pressure, the growth temperature and the hydrogen flow rate of a reaction chamber are kept unchanged, annealing is carried out until the temperature reaches 900 ℃, the whole epitaxial wafer is placed on a slide, argon is introduced, and the temperature is reduced to the room temperature.
In the invention, the annealing process specifically comprises the following steps: and preserving the heat for 10-30 minutes at 1400-1600 ℃. The time of the annealing process can be prolonged according to the experimental effect, so that a better carbon vacancy repairing effect is obtained. In the invention, the temperature of the reaction cavity is slowly reduced to 900 ℃, after the temperature is reduced to room temperature, the wafer is taken out, the front surface of the epitaxial layer is covered with a film for protection, the carbon film on the back surface of the epitaxial layer is polished off, and the carbon film is ground off.
The invention provides a preparation method of a silicon carbide epitaxial wafer for a high-voltage and ultrahigh-voltage device, which comprises the following steps: coating a carbon film on the carbon surface of a silicon carbide substrate, placing the silicon carbide substrate in a reaction chamber of an existing commercial epitaxial furnace, introducing hydrogen, gradually heating to 1600-1650 ℃, introducing a silicon source, a carbon source and a doping source, growing a buffer layer on the silicon surface of the silicon carbide substrate, adjusting the flow values of various sources, growing an epitaxial layer to a specified thickness, annealing, cooling to room temperature, performing blue film protection on the silicon surface of a wafer, and removing the carbon film on the back of the epitaxial wafer to obtain the required silicon carbide epitaxial wafer for the high-pressure and ultrahigh-pressure device.
The method is based on the existing commercial epitaxial furnace, and the carbon film is coated on the carbon surface of the substrate, so that the carbon vacancy of the epitaxial layer is supplemented through the carbon atom migration of the carbon film in the epitaxial and annealing processes, thereby realizing the purpose of repairing the carbon vacancy, and in addition, the annealing process parameters can be adjusted to improve the carbon vacancy density and prolong the service life of a current carrier.
Drawings
FIG. 1 is a schematic diagram of the fabrication of a high minority carrier lifetime silicon carbide epitaxial wafer for a high voltage ultra high voltage device;
fig. 2 is a schematic view of carbon film coating before manufacturing of the high minority carrier lifetime silicon carbide epitaxial wafer for the high-voltage and ultrahigh-voltage device according to the embodiment of the invention.
Detailed Description
In order to further illustrate the present invention, the following will describe in detail the preparation method of the silicon carbide epitaxial wafer for a high-voltage and ultra-high-voltage device provided by the present invention with reference to the examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) Selecting a silicon carbide substrate with the inclination of <11-20> direction and 4 degrees, and uniformly growing a carbon film on the carbon surface of the silicon carbide substrate.
The carbon film is prepared by carbonizing photoresist;
(2) placing the processed silicon carbide substrate in a graphite base, conveying the silicon carbide substrate into a reaction cavity by using a mechanical arm, introducing hydrogen into the reaction chamber, gradually increasing the hydrogen flow to 80-120L/min, setting the pressure of the reaction chamber to be 80-200 mbar, and gradually heating the reaction chamber to 1600-1650 ℃;
(3) after the set temperature is reached, opening air inlet valves of a precursor silicon source, a carbon source and a doping source, introducing various sources into an exhaust air path, setting the flow of various sources through mass flow to meet the flow requirement required by the growth of the buffer layer in the step (4), keeping other parameters unchanged, and carrying out in-situ hydrogen etching treatment on the silicon carbide substrate for 5-15 minutes;
(4) controlling the flow ratio of the silicon source and the hydrogen, controlling the flow of the carbon source to meet the condition that the molar ratio of C/Si is more than or equal to 0.8 and less than or equal to 1.4, introducing the silicon source, the carbon source and the doping source with set flow into the reaction chamber, and growing at the growth thickness of 0.5-10 microns and the doping concentration of 1-5 multiplied by 10 microns at the rate of less than 10 microns/hour 18 cm -3 The high doping concentration buffer layer;
(5) transferring a silicon source, a carbon source and a doping source to an exhaust gas path, keeping the pressure, the growth temperature and the hydrogen flow of a reaction chamber unchanged, and gradually changing the flow of various sources to a flow value required by rapid growth within 30 seconds;
(6) controlling the flow ratio of a silicon source and hydrogen, C/Si, introducing the silicon source, a carbon source and a doping source with set flow into a reaction chamber, growing an epitaxial layer at a speed of more than 80 microns/hour according to the epitaxial thickness required by the voltage grade of a high-voltage and ultrahigh-voltage device, for example, a drift layer with the thickness of 70-100 microns required by 6500V and 10KV high-voltage devices, and adjusting the flow of the doping source to ensure that the doping concentration of the drift layer meets the design doping concentration of the device;
(7) after the drift layer with the specified thickness grows, transferring a silicon source, a carbon source and a doping source to an exhaust gas path, keeping the pressure, the growth temperature and the hydrogen flow of a reaction chamber unchanged, slowly reducing the temperature of the reaction chamber until the temperature reaches 900 ℃, placing an epitaxial wafer to a slide glass, introducing argon, cooling to room temperature, and taking out the wafer;
(8) and (4) sticking a film on the front surface of the epitaxial wafer for protection, polishing the back surface of the carbon, and grinding off the coated carbon film.
The above method can reduce Z which is a cause of shortening the lifetime and is generated by carbon vacancy in the silicon carbide single crystal epitaxial film 1/2 Center and EH 6/7 And a center, thereby extending the carrier lifetime of the silicon carbide single crystal film.
From the above embodiments, the method provided by the invention adopts a method for manufacturing a silicon carbide epitaxial wafer with a high minority carrier lifetime for a high-voltage and ultrahigh-voltage device, and mainly adopts the steps of uniformly coating a carbon film on a carbon surface before epitaxy; and then, epitaxially growing an epitaxial layer required by the high-pressure ultrahigh-pressure device, and finally, carrying out high-temperature annealing treatment on the obtained epitaxial wafer, wherein the purpose of eliminating carbon vacancies is achieved by utilizing the migration of carbon atoms under thermodynamic equilibrium conditions among the carbon film, the silicon carbide substrate and the epitaxial layer in the epitaxial process and the annealing process, so that the effective repair of the carbon vacancies in the in-situ growth process is realized, and the purpose of prolonging the service life of carriers of the silicon carbide epitaxial layer is fulfilled. The epitaxial material grown by the epitaxial method provided by the invention does not need to utilize the post treatment of ion injection or high-temperature oxidation after the epitaxy is finished, the aim of repairing the carbon vacancy can be realized in the epitaxial reaction process in the existing commercial epitaxial furnace, and the annealing process parameters can be adjusted according to the service life of the current carrier or the density of the carbon vacancy, so that the aim of improving the manufacturing of the epitaxial wafer with the high minority carrier lifetime for the high-voltage and ultrahigh-voltage device is realized.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a silicon carbide epitaxial wafer for a high-voltage and ultrahigh-voltage device comprises the following steps:
coating a carbon film on the carbon surface of a silicon carbide substrate, placing the silicon carbide substrate in an epitaxial furnace reaction chamber, introducing hydrogen, gradually heating to 1600-1650 ℃, introducing a silicon source, a carbon source and a doping source, growing a buffer layer on the silicon surface of the silicon carbide substrate, adjusting the flow values of various sources, growing an epitaxial layer to a specified thickness, annealing, cooling to room temperature, performing silicon surface blue film protection on a wafer, and removing the carbon film to obtain the silicon carbide epitaxial wafer for the high-pressure and ultrahigh-pressure device.
2. The production method according to claim 1, wherein the silicon carbide substrate is selected from silicon carbide in which a silicon plane is biased toward a <11-20> direction by 1 ° to 8 °.
3. The method according to claim 1, wherein the flow rate of the hydrogen gas is 80 to 120L/min, and the pressure of the hydrogen gas introduced into the reaction chamber is 80 to 200 mbar.
4. The preparation method of claim 1, wherein the silicon carbide substrate is subjected to in-situ hydrogen etching for 5-15 min before the silicon source, the carbon source and the doping source are introduced.
5. The method of claim 1, wherein the buffer layer is grown at a rate of 10 μm/hr;
the thickness of the buffer layer is 0.5-10 μm, and the doping concentration is 1-5 × 10 18 cm -3 。
6. The method of claim 1, wherein the epitaxial layer is grown at a rate greater than 80 microns/hour.
7. The production method according to claim 1, wherein the carbon film is produced by sputtering or vapor deposition;
or coating photoresist and drying.
8. The preparation method according to claim 1, wherein the silicon source is selected from silane, dichlorosilane or trichlorosilane;
the carbon source is selected from methane, ethylene or propane.
9. The method of claim 1, wherein after the epitaxial layer is grown to a predetermined thickness, the silicon source, the carbon source and the dopant source are transferred to an exhaust gas path, the pressure, the growth temperature and the hydrogen flow rate in the reaction chamber are maintained unchanged, annealing is performed until 900 ℃, the entire epitaxial wafer is placed on the wafer, argon is introduced, and the temperature is reduced to room temperature.
10. The preparation method according to claim 1, wherein the annealing process specifically comprises: and preserving the heat for 10-30 minutes at 1400-1600 ℃.
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