CN114293263A - Protection device and method for preventing surface decomposition and impurity incorporation under high-temperature thermal annealing - Google Patents
Protection device and method for preventing surface decomposition and impurity incorporation under high-temperature thermal annealing Download PDFInfo
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- CN114293263A CN114293263A CN202111655564.5A CN202111655564A CN114293263A CN 114293263 A CN114293263 A CN 114293263A CN 202111655564 A CN202111655564 A CN 202111655564A CN 114293263 A CN114293263 A CN 114293263A
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Abstract
The invention discloses a protection device and a method for preventing surface decomposition and impurity incorporation under high-temperature thermal annealing, wherein the device comprises a cup body and a pressure applying structure, the pressure applying structure is used for clamping a wafer in the cup body and applying pressure not less than 1.96N to the wafer, the melting points of the pressure applying structure and the cup body are both more than 1600 ℃, and the materials of the pressure applying structure and the cup body are inert materials. Adopt the annealing device of this application, when carrying out high temperature thermal annealing, when the little air bubble that exists between two wafers takes place the inflation under high temperature, can extrude the expanded bubble through the clamping-force of applying pressure structure and cup to two wafers, still can weaken the surface separation that the sample warpage leads to under the high temperature simultaneously, the design of cup can effectively block when high temperature thermal annealing, impurity in the annealing furnace body is to wafer sample diffusion, under the high temperature thermal annealing of alleviating, the impurity of furnace body is to the pollution problem of wafer sample material, thereby improve the crystal quality and the product yield of material.
Description
Technical Field
The invention relates to the technical field of semiconductor integrated circuit manufacturing, in particular to a protection device and a method for preventing surface decomposition and impurity incorporation under high-temperature thermal annealing.
Background
The annealing process is an important ring of modern semiconductor process and is commonly used for metal electrode alloy, interface passivation, doping activation, recrystallization, crystal solid phase reaction and the like. Annealing refers to placing a semiconductor material in a high temperature environment for heat treatment to change the properties of the semiconductor surface or the bulk. In the preparation of a new generation of wide bandgap semiconductor, especially an aluminum nitride (AlN) material, a high temperature thermal annealing process is one of the important means for improving the crystallization quality of the AlN material. Because of the high covalent bond energy and high melting point (2750 ℃), an AlN substrate with low dislocation density cannot be prepared by a single crystal pulling method. Currently, AlN single crystal material is commonly grown on a heterogeneous substrate such as sapphire, silicon carbide, etc. by Metal Organic Chemical Vapor Deposition (MOCVD), Hydride Vapor Phase Epitaxy (HVPE), or Physical Vapor Transport (PVT). AlN materials grown on foreign substrates are limited by large lattice mismatch and thermal mismatch, and generally have a lattice mismatch as high as 108-109cm-2The dislocation density of (a) seriously affects its further applications.
In order to further improve the crystallization quality of AlN materials, people have developed a high-temperature thermal annealing treatment technique, i.e., the prepared AlN wafer is placed in a high-temperature annealing furnace, and the temperature is raised to over 1600 ℃ so that the AlN crystal lattice is rearranged and dislocation slips, thereby achieving the purpose of reducing the dislocation density of the materials. Due to the high annealing temperature, the surface of the AlN material is decomposed at high temperature, and the surface of the annealed material is rapidly degraded, so that the performance of the material is seriously influenced.
In order to solve the problem, in the prior art, a protective gas nitrogen is introduced into the cavity to weaken the surface decomposition of the AlN material at high temperature. However, due to the large thermal mismatch between the AlN epitaxial layer and the sapphire substrate, the wafer may be significantly warped at high temperature, so that the sample surface tightly attached at normal temperature is separated and exposed to the environment, and the exposed portion may have a severe surface decomposition phenomenon at high temperature, which seriously affects the yield of the product, and also makes impurities such as carbon, oxygen, and the like more easily incorporated, thereby reducing the overall performance of the material. On the other hand, contamination in the furnace body is also a current problem in high-temperature thermal annealing treatment of AlN materials. The graphite, tungsten alloy or silicon-molybdenum materials adopted by the prior furnace body can cause pollution to the AlN material.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a protection device for preventing surface decomposition and impurity incorporation in high-temperature thermal annealing. The method can effectively solve the problems of surface decomposition and impurity incorporation of the AlN material due to air bubbles and sample warping under high-temperature thermal annealing, and improve the crystallization quality and the product yield of the AlN material. The annealing device of the present invention is mainly used for high-temperature thermal annealing treatment of AlN materials, but is not limited to AlN materials, and can be applied to new-generation semiconductor materials such as aluminum gallium nitride (AlGaN), Boron Nitride (BN), gallium oxide (GaO), and diamond.
According to an aspect of the application, a protection device for preventing the decomposition of the lower surface and the incorporation of impurities in high-temperature thermal annealing is provided, and the protection device comprises a cup body and a pressure applying structure, wherein the pressure applying structure is used for clamping two wafers which are oppositely covered on the front surface in the cup body, the melting points of the pressure applying structure and the cup body are both more than 1600 ℃, and the pressure applying structure and the cup body are made of inert materials.
Adopt the annealing device of this application, when carrying out high temperature thermal annealing, when the little air bubble that exists between two wafers takes place the inflation under high temperature, can extrude the expanded bubble through the clamping-force of applying pressure structure and cup to two wafers, still can weaken the surface separation that the sample warpage leads to under the high temperature simultaneously, the design of cup can effectively block when high temperature thermal annealing, impurity in the annealing furnace body is to wafer sample diffusion, under alleviating high temperature thermal annealing, the impurity of furnace body is to the pollution problem of wafer sample material, thereby can effectively improve the crystal quality and the product yield of material.
In some embodiments, a channel is provided between the pressure applying structure and the cup for allowing a shielding gas outside the cup to contact the wafer inside the cup when the wafer is clamped.
Therefore, the protective gas introduced during the high-temperature thermal annealing can smoothly flow to the periphery of the wafer, so that the surface decomposition of the wafer at high temperature is reduced.
In some embodiments, the channel may include a first space provided between the pressure exerting structure and the cup.
Therefore, the pressure applying structure and the cup body are kept at a certain interval by the arrangement, so that the surface decomposition of the wafer at high temperature can be further weakened by introducing protective gas into the device, and the crystallization quality and the product yield of the material are further improved.
In some embodiments, the pressing structure may include a pressing portion and a top cover configured to completely cover a rim of the cup body, the pressing portion being disposed at a bottom of the top cover.
Therefore, the top cover can be arranged to further prevent impurities in the annealing furnace body from diffusing to the wafer sample, so that the problem of pollution of the impurities of the furnace body to the wafer sample material under high-temperature thermal annealing is solved.
In some embodiments, the channel may include a first space provided between the pressure exerting structure and the cup and a second space provided between the overcap and the top of the cup.
From this, can all keep having certain interval between structure and the cup of exerting pressure, between top cap and the cup through setting up like this to be favorable to when letting in protective gas, protective gas enters into near wafer sample material and cladding wafer sample material, thereby improves protective gas's protective effect, further improves the crystallization quality and the product yield of material.
In some embodiments, the edge of the lid may extend with a lip toward the cup.
Therefore, through the arrangement, impurities in the annealing furnace body can be further effectively prevented from diffusing to the wafer sample through the side cover, and the problem of pollution of the impurities of the furnace body to the wafer sample material under high-temperature thermal annealing is further relieved.
In some embodiments, the channel may further include a third space provided between the lid and the cup.
From this, can be through setting up like this for also be provided with certain interval between side cover and the cup, can be favorable to protective gas's entering, improve protective gas's protecting effect.
In some embodiments, the length of the lid is no less than the size of the second gap and no greater than the height of the cup.
Therefore, the blocking effect of the side cover on the diffusion of the impurities in the annealing furnace body to the wafer sample is further enhanced through the arrangement, and the problem of pollution of the impurities in the furnace body to the wafer sample material under high-temperature thermal annealing is solved.
In some embodiments, the pressing structure includes a pressing portion which is a pressing block, and the pressing block clamps the wafer on the bottom of the inner side of the cup body.
Therefore, the complexity of the pressing structure can be effectively simplified through the arrangement, and if the pressing structure comprises parts made of various different materials, the crystallization quality and the product yield of a wafer sample can be possibly influenced when high-temperature thermal annealing is carried out.
In some embodiments, the pressure part is a pressure block integrally formed with the top cover and the side cover, the pressure block clamps the two wafers with front surfaces oppositely covered at the bottom of the inner side of the cup body, and the pressure block, the top cover, the side cover and the cup body are made of one or more materials selected from corundum materials, tungsten metal materials, boron nitride materials and silicon carbide materials.
Therefore, the complexity of the pressing structure can be effectively simplified through the integrally formed cover body-pressure block structure, and meanwhile, the purity of the device can be ensured by adopting the cup body and the cover body-pressure block structure which are made of corundum materials or tungsten metal materials with excellent high-temperature property and mechanical strength, the use stability of the device can be ensured, and the crystallization quality and the product yield of a wafer sample can be ensured.
According to another aspect of the present application, there is provided a method for preventing decomposition of a surface and incorporation of impurities under high temperature thermal annealing, which employs the above-mentioned protection device for preventing decomposition of a surface and incorporation of impurities under high temperature thermal annealing, comprising
The wafers with the cross section area not larger than the area of the pressure surface of the pressure structure are covered oppositely by two pairs of front surfaces to form a group, and the group is completely covered and clamped on the inner side of the cup body through the pressure structure;
putting the protection device into an annealing furnace for high-temperature thermal annealing treatment at 1400-2000 ℃ for 1-20 hours, and introducing protection gas;
and after naturally cooling to room temperature, taking out the whole protection device, and taking out the wafer.
By adopting the method, when high-temperature thermal annealing is carried out, when the micro air bubbles existing between the two wafers expand at high temperature, the expanded air bubbles can be extruded out by the clamping force of the pressure applying structure and the cup body on the two wafers, and meanwhile, the surface separation caused by warping of the sample at high temperature can be weakened.
Drawings
Fig. 1 is a schematic structural view of a cup body of an apparatus for preventing decomposition of a lower surface and incorporation of impurities in high temperature thermal annealing according to an embodiment of the present invention, in which fig. a is a sectional structural view, and fig. B is a top structural view;
FIG. 2 is a schematic view of the overall structure of the apparatus for preventing surface decomposition and impurity incorporation during high temperature thermal annealing according to one embodiment of the present invention;
FIG. 3 is a schematic structural diagram of an auxiliary alignment structure added to a pressing part of the apparatus for preventing surface decomposition and impurity incorporation during high temperature thermal annealing according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of a pressing structure of an apparatus for preventing decomposition of a lower surface and incorporation of impurities during high temperature thermal annealing and a structure of a wafer clamped by a cup according to an embodiment of the present invention;
FIG. 5 is a schematic view of a pressing structure and a wafer clamping state of a cup of an apparatus for preventing decomposition of a lower surface and incorporation of impurities in high temperature thermal annealing according to another embodiment of the present invention;
fig. 6 is a schematic structural view of a cup according to a second embodiment, in which fig. a is a sectional structural view and fig. B is a top structural view;
FIG. 7 is a schematic diagram of the overall structure of example two;
FIG. 8 is a flow chart of preventing surface decomposition and impurity incorporation during high temperature thermal annealing in accordance with one embodiment of the present invention;
description of reference numerals: 1. a cup body; 2. a pressure applying structure; 21. a pressing part; 211. a pressure block; 212. briquetting; 213. an auxiliary alignment structure; 3. a top cover; 4. a side cover; 5. a channel; 51. a first interval; 52. a second interval; 53. a third interval.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
It is further noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The protection device for preventing surface decomposition and impurity incorporation in high-temperature thermal annealing in the embodiment of the invention is used for carrying out high-temperature thermal annealing on the semiconductor material of the new generation. The new-generation semiconductor material includes AlN material, aluminum gallium nitride (AlGaN), Boron Nitride (BN), gallium oxide (GaO), diamond, and the like, which is not limited by the embodiments of the present invention. The present invention will be described by way of example with AlN material as an implementation example.
Referring to fig. 1 and 2, fig. 1 and 2 schematically illustrate a protection device structure for preventing surface decomposition and impurity incorporation under high temperature thermal annealing according to an embodiment of the present invention.
The protection device for preventing the decomposition of the lower surface and the incorporation of impurities in the high-temperature thermal annealing comprises a cup body 1 and a pressing structure 2, wherein the pressing structure 2 is used for clamping two AlN samples with front surfaces oppositely covered in the cup body 1 and applying pressure of not less than 1.96N. Wherein, the components of the cup body 1 and the pressure applying structure 2 are both required to be high temperature resistant materials, because the device is used for high temperature thermal annealing, the high temperature resistant shape of the materials is required to be higher than the temperature required during annealing, taking an AlN sample as an example, when the AlN sample is subjected to high temperature thermal annealing, the AlN sample needs to be placed in a high temperature annealing furnace, the temperature is raised to more than 1600 ℃, so that the materials of the cup body 1 and the pressure applying structure 2 are required to be capable of withstanding the high temperature of more than 1600 ℃, meanwhile, the materials of the cup body 1 and the pressure applying structure 2 are also required to be materials which are not easy to react with the materials of the wafer, so as to avoid the influence on the crystallization quality and the product yield of the wafer during annealing, and therefore, the materials of the cup body 1 and the pressure applying structure 2 are selected within the range, and the preparation materials can specifically adopt corundum materials, tungsten metal materials, One or more materials of a boron nitride material and a silicon carbide material. Referring to fig. 1, the cup body 1 includes a cup opening, the structure of the cup body 1 is not particularly limited, and may be a cylindrical cup body 1, or may be a polygonal cup body 1, and the inclination of the wall of the cup body 1 does not have a corresponding requirement, and may be inclined from bottom to top toward the outer side of the cup body 1, may be inclined from bottom to top toward the inner side of the cup body 1, or may be not inclined, and the shape and style of the cup body 1 do not affect the effect. For the placing mode of the two AlN samples, the front surface in the front surface opposite covering refers to a surface of the AlN sample where the AlN epitaxial layer is located, the other surface is a substrate, such as a sapphire substrate, and the front surface opposite covering refers to that the front surfaces of the two AlN samples are opposite, and the front surface of one AlN sample is attached to the front surface of the other AlN sample, so that the front surfaces of the two AlN samples are opposite to cover each other. Referring to fig. 2, the pressing structure 2 and the cup 1 are preferably configured to have a larger size than the AlN sample when the AlN sample is clamped, so that the AlN sample can be completely covered, the clamping effect can be improved, and a certain warpage resistance can be achieved. By clamping the two AlN samples in the cup body 1 in a manner of covering the front surfaces of the AlN samples oppositely and then carrying out high-temperature thermal annealing, when micro air bubbles existing between the two AlN samples expand at high temperature, the expanded air bubbles can be extruded out, and meanwhile, the surface separation caused by the warping of the samples at high temperature can be weakened.
Referring to fig. 4 and 5, the specific clamping positions of the two AlN samples in the cup body 1 may be on the inner side wall of the cup body 1 or the bottom of the inner side of the cup body 1, and the height of the side surface of the cup body 1 is preferably set to a structural pattern which can ensure the AlN samples to be coated inside the cup body 1, so as to ensure the barrier effect of the side surface of the cup body 1 on impurities diffused to the AlN samples in the annealing furnace body during high-temperature thermal annealing, and correspondingly, the pressing structure 2 is preferably set to a structural pattern which extends into the cup body 1. The pressing structure 2 specifically includes a pressing portion 21, and referring to fig. 4, if the clamping position is set on the inner side wall of the cup body 1, the cup body 1 can be clamped on the inner side wall of the cup body 1 stably by the polygonal cup body structure, so that two AlN samples can be clamped on the inner side wall of the cup body 1 stably, and at this time, the pressing portion 21 can be designed according to the number of the side edges of the cup body 1, so as to maximize the utilization of the inner side wall of the cup body 1. Correspondingly, the pressing part 21 may be designed to include a housing and a pushing pressing block 212 in threaded connection with the housing, and the two AlN samples are clamped between the pressing block 212 and the inner side wall of the cup body 1 in a threaded manner, so as to achieve the corresponding technical effect of extruding the expanded bubbles, where the surface of the pressing block 212 for clamping the AlN sample is a clamping surface; referring to fig. 5, if the clamping position is set at the bottom inside the cup body 1, the pressing portion 21 may be simplified correspondingly, for example, the pressing portion 21 may be a single pressure block 211, and the pressure block 211 may clamp two AlN samples between the pressure block 211 and the bottom of the cup body 1 by gravity through its own weight, so as to achieve the corresponding technical effect of extruding out the expanded bubbles, where the bottom surface of the pressure block 211 is the clamping surface. The weight of the pressure block 211 cannot be too light, otherwise the desired ideal effect cannot be achieved, and specifically, the weight of the pressure block 211 is preferably greater than 200G, i.e., the pressure applied to the wafer by the pressing structure 2 is preferably 1.96N, where the 1.96N is calculated by the gravitational constant G of 9.8N/kg. The simplification of splenium 21 is favorable to the stability in use of device, also can guarantee the purity of device, if splenium 21 contains the spare part of multiple different materials, then probably will appear the condition of releasing impurity or the unstable condition of structure when carrying out high temperature thermal annealing to crystal quality and yields to the AlN sample cause the influence.
Referring to fig. 4 and 5, in some embodiments, a channel 5 for contacting the protective gas outside the cup body 1 with the AlN sample inside the cup body 1 when the AlN sample is clamped may be provided between the pressure applying structure 2 and the cup body 1, and the arrow in fig. 4 and 5 indicates the flow direction of the protective gas flowing through the channel 5 to the surroundings of the AlN sample. Specifically, referring to fig. 4 and 5, the channel 5 may include a first space 51 left between the press 21 and the cup 1. Wherein, when the clamping position of the AlN sample is on the inner sidewall of the cup body 1, referring to fig. 4, the first gap 51 may be a gap between the inner sidewall of the cup body 1 and the pressing part 21; when the clamped position of the AlN sample is the bottom inside the cup body 1, referring to fig. 5, the first gap 51 may be a gap composed of a gap between the inner side surface of the cup body 1 and the pressing portion 21 and a gap between the bottom of the pressing portion 21 and the bottom inside the cup body 1. With this arrangement, the protective gas (e.g., nitrogen gas) introduced during the high-temperature thermal annealing can be better flowed through the first gap 51 to the periphery of the clamped AlN sample, and the AlN sample is coated, so that the surface decomposition of the AlN sample at high temperature is reduced, and further the crystallization quality and the product yield of the material can be further improved. Wherein the first space 51 is preferably set to be not less than 5mm to ensure the circulation of the shielding gas, the first space 51 is set according to the size specification of the cup 1 and the pressing structure 2, and the larger the size of the cup 1 and the pressing structure 2 is, the larger the first space 51 left by the cup 1 and the pressing structure 2 should be to ensure the circulation of the shielding gas. Referring to fig. 3, correspondingly, in order to enable the pressing portion 21 to ensure the interval size of the first interval 51 when clamping the AlN sample, an auxiliary alignment structure 213 may be additionally disposed on the side surface of the pressing portion 21 to ensure that the pressing portion 21 can keep the first interval 51 with a sufficiently large interval when clamping the AlN sample, and the pressing portion 21 may be located at the center of the cup body 1 to avoid the first interval 51 with different sizes. Specifically, the auxiliary alignment structure 213 may be protruding rods disposed on the side surface of the pressing portion 21, the number of the protruding rods is at least two, and the protruding rods are uniformly disposed on the outer side surface of the pressing portion 21, and the protruding rods are abutted against the inner side surface of the cup body 1 to ensure the size of the first gap 51 and ensure the circulation of the shielding gas.
With continued reference to fig. 5, in some embodiments, the pressing structure 2 may further include a top cover 3, the pressing portion 21 is disposed at the bottom of the top cover 3, and the top cover 3 is used to block the impurities in the annealing furnace body from diffusing to the AlN sample in the cup body 1, so as to alleviate the problem of contamination of the AlN sample by the impurities in the furnace body during the high-temperature thermal annealing. When the pressure applying portion 21 is the pressure block 211, the pressure generated by the top cover 3 and the pressure block 211 on the AlN sample needs to be considered, so that the weight of the pressure block 211 can be adjusted according to the weight of the top cover 3. Specifically, the top lid 3 may preferably be provided in a form capable of completely covering the rim of the cup body 1, thereby effectively blocking impurities in the annealing furnace body. The top cover 3 can be set to be the horizontally top cover 3, also can set to be the toper or other shape styles, and the shape is not influenced to the effect, and the size of top cover 3 can be bigger than the rim of a cup, and it can be better to block the effect like this to be favorable to guaranteeing crystallization instruction and the yields of AlN sample. The arrangement of the top cover 3 can be combined with the first gap 51 of the channel 5 between the pressure applying structure 2 and the cup body 1, and a corresponding second gap 52 is reserved between the top cover 3 and the cup mouth, so that the effect of blocking impurities in the annealing furnace body can be achieved, and the effect of ensuring the circulation of the protective gas of the channel 5 can also be achieved. Wherein the second interval 52 is similar to the first interval 51 and is preferably set to be not less than 5mm, the second interval 52 is also set according to the size specification of the cup 1 and the pressing structure 2, and the larger the size of the cup 1 and the pressing structure 2 is, the larger the second interval 52 is left. Specifically, in the example where the AlN sample is held on the inner surface of the cup body 1, since the pressing portion 21 is also subjected to a corresponding holding force when holding the AlN sample, the gap between the top cover 3 and the cup rim can be adjusted by adjusting the holding position of the AlN sample in the cup body 1, or the bottom of the pressing structure 2 is abutted against the bottom of the cup body 1, and the height of the pressing structure 2 is made 5mm or more higher than the inner height of the cup body 1, and it is also possible to ensure that the top cover 3 is 5mm or more higher than the cup rim. In the example where the AlN sample is held at the bottom of the cup body 1, the AlN sample is held between the pressure block 21 and the bottom of the cup body 1, and the specification of the held wafer sample is different in the actual use process, so that the size of the gap between the top cover 3 and the cup mouth after the wafer sample is held cannot be used as the setting standard of the second gap 52, and therefore, the height of the pressure applying portion 21 is made to be more than 5mm higher than the internal height of the cup body 1 to ensure that the second gap 52 is not less than 5mm in the held state, thereby achieving the effect of ensuring the circulation of the shielding gas. For the stability in use of the device and the purity of the device, the top cover 3 and the pressing portion 21 can be integrally formed, so that the influence on the crystallization quality and the yield of the AlN sample due to the impurity release or unstable structure during high-temperature thermal annealing is avoided.
With continued reference to fig. 5, in some embodiments, a side cover 4 may further extend from the edge of the top cover 3 toward the cup body 1, and the side cover 4 is used to further block the impurities in the annealing furnace body from diffusing into the AlN sample in the cup body 1, thereby further alleviating the problem of contamination of the AlN sample by the impurities in the furnace body during the high-temperature thermal annealing process. Similarly to the top cover 3, when the pressing portion 21 is the pressure block 211, the pressure generated by the top cover 3, the side cover 4 and the pressure block 211 on the AlN sample needs to be considered, so that the weight of the pressure block 211 can be adjusted according to the weight of the top cover 3 and the side cover 4. The side cover 4 may be the side cover 4 which is vertically downward, or may be inclined toward the middle of the top cover 3 or inclined toward the outside of the top cover 3, and the shape of the side cover 4 does not have a great influence on the operation effect thereof, while the length of the side cover 4 has a relatively great influence on the operation effect thereof, so that it is required that the length of the side cover 4 is set to a space size not smaller than the second space 52. Specifically, the length of side cover 4 preferably sets up to be not less than 10mm correspondingly, can not be greater than the height of cup 1 simultaneously, and the effect of blockking of impurity in can effectual assurance side cover 4 to the annealing stove body can be set up like this. The length of the side cover 4 is set in relation to the size of the actual integrated device, and the larger the size of the integrated device is, the longer the length of the side cover 4 should be set. Correspondingly, in order to avoid shielding the second space 52 between the top cover 3 and the cup mouth from affecting the circulation of the shielding gas, preferably, the channel 5 may further include a third space 53 left between the side cover 4 and the outer side wall of the cup body 1, so that the channel 5 is formed into a zigzag shape, wherein the third space 53 is similar to the first space 51 and the second space 52, and is preferably set to be not less than 5mm, specifically, the third space 53 is set to be related to the size specification of the whole device, and the larger the size specification of the whole device is, the larger the third space 53 should be. Illustratively, the edge cover 4 may be disposed parallel to the outer sidewall of the cup body 1, so as to further prevent impurities in the annealing furnace body from diffusing to the AlN sample in the cup body 1 while ensuring the circulation of the protective gas, thereby improving the crystallization quality and yield of the AlN sample. For the stability in use of device and the purity nature of assurance device, side cover 4, top cap 3 and pressurize portion 21 can set up to integrated into one piece to avoid the condition of the release impurity that appears when carrying out high temperature thermal annealing or the unstable condition of structure, thereby cause the influence to the crystallization quality and the yields of AlN sample.
Referring to fig. 8, according to another aspect of the present application, there is provided a method for preventing surface decomposition and impurity incorporation under high temperature thermal annealing using the above protection device, which can be implemented by the following steps when performing high temperature thermal annealing:
step S1: the wafers with the cross section area not larger than the area of the pressure applying surface of the pressure applying structure 2 are covered with two pairs of front surfaces oppositely to form a group, and the group is completely covered and clamped at the inner side of the cup body 1 through the pressure applying structure 2;
step S2: putting the protection device into an annealing furnace for high-temperature thermal annealing treatment at 1400-2000 ℃ for 1-20 hours, and introducing protection gas;
step S3: and after naturally cooling to room temperature, taking out the whole protection device, and taking out the wafer.
In step S1, taking the pressing portion 21 as the pressure block 211 and clamping the AlN wafer on the bottom surface inside the cup body 1 as an example, it is preferable to adopt an AlN wafer having a cross-sectional area not larger than the area of the pressing surface of the pressing structure 2 (i.e., the area of the bottom surface of the pressure block 211) as a processing target of the protection apparatus, because a better anti-warp effect can be achieved. If the area of the pressure applying surface of the pressure applying structure 2 is large, multiple groups of two-by-two AlN wafers can be placed at the same time, so that the annealing efficiency is improved. When the pressing structure 2 includes the top cover 3, the side cover 4 and the channel 5, when the pressure block 211 is used for clamping the AlN wafer, a first gap 51 is left between the pressure block 211 and the inner side wall of the cup body 1, so that a protective gas can flow into the vicinity of the AlN wafer through the channel 5 and cover the AlN wafer when high-temperature thermal annealing is performed, surface decomposition of the AlN sample at high temperature can be reduced, and further, the crystallization quality and the product yield of the material can be further improved.
In step S2, the annealing temperature and the annealing time are different, and taking the AlN wafer as an example, the annealing temperature for the AlN wafer is 1600 ℃ to 1750 ℃, and the high-temperature thermal annealing time is 1 hour to 3 hours.
According to the protection device provided by the invention, when high-temperature thermal annealing is carried out, when micro air bubbles existing between two wafers expand at high temperature, the expanded air bubbles can be extruded out by the clamping force of the pressing structure 2 and the cup body 1 on the two wafers, and meanwhile, the surface separation caused by warping of a sample at high temperature can be weakened, so that the crystallization quality and the product yield of the material are improved.
Two specific embodiments of the protection device of the present invention are given below for exemplary reference.
Example 1
Referring to fig. 1 and 2, the pressing portion 21 is a pressing block 211, and the pressing portion 21, the top cover 3, and the side cover 4 are integrally formed. The cup body 1, the pressure block 211, the top cover 3 and the side cover 4 are all made of corundum materials, and the melting point of the corundum materials is up to 2000-2030 ℃. The cup body 1 is a cylindrical cup body 1, the inner diameter is 54mm, and the height is 20 mm. The top cover 3 is designed for a horizontal top cover 3, the edge cover 4 is designed for a vertical edge cover 4, the diameter of the pressure block 211 is 34mm, i.e. the first distance 51 is 5mm, and the vertical height of the pressure block 211 is 25 mm. Pressure block 211 sets up in the middle part of top cap 3 bottom surface, and when not having the centre gripping to have the wafer material, and make pressure block 211 align to place in the middle of cup 1, second interval 52 between top cap 3 and the rim of a cup is 5mm, and the distance between the lateral surface of side cover 4 and the rim of a cup is 5mm, and the length of side cover 4 is 10 mm.
Example two
Referring to fig. 6 and 7, the pressing coupling part 21 is a pressing block 211, and the pressing part 21, the top cover 3, and the side cover 4 are integrally formed. The cup body 1, the pressure block 211, the top cover 3 and the side cover 4 are all made of tungsten metal, the tungsten metal is refractory metal with the highest melting point, and generally, the metal with the melting point higher than 1650 ℃ and a certain reserve and the metal with the melting point higher than the melting point (1852 ℃) of zirconium are called refractory metal. The cup body 1 is a quadrilateral cup body 1, the side length of the inner side is 110mm, and the height is 50 mm. The top cover 3 is designed to be a horizontal top cover 3, the side cover 4 is designed to be a vertical side cover 4, the pressure block 21 is also quadrilateral, the side length is 45mm, namely the first interval 51 is 32.5mm, and the vertical height of the pressure block 211 is 60 mm. Pressure block 211 sets up in the middle part of top cap 3 bottom surface, and when not having the centre gripping to have the wafer material, and make pressure block 211 align to place in the middle of cup 1, second interval 52 between top cap 3 and the rim of a cup is 10mm, and the distance between the lateral surface of side cover 4 and the rim of a cup is 10mm, and the length of side cover 4 is 20 mm.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present application, and not to limit the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions in the embodiments of the present application.
Claims (10)
1. Prevent the protection device that surface decomposition and impurity merged into under the high temperature thermal annealing, its characterized in that: the wafer pressing device comprises a cup body and a pressing structure, wherein the pressing structure is used for clamping a wafer in the cup body and applying pressure not less than 1.96N to the wafer, the melting points of the pressing structure and the cup body are both more than 1600 ℃, and the pressing structure and the cup body are made of inert materials.
2. The protection device for preventing surface decomposition and impurity incorporation under high-temperature thermal annealing according to claim 1, wherein: and a channel for enabling the protective gas outside the cup body to be in contact with the wafer inside the cup body when the wafer is clamped is arranged between the pressure applying structure and the cup body.
3. The protection device for preventing surface decomposition and impurity incorporation under high temperature thermal annealing according to claim 2, wherein: the pressing structure comprises a pressing part, and the channel comprises a first interval arranged between the pressing part and the cup body.
4. The protection device for preventing surface decomposition and impurity incorporation under high temperature thermal annealing according to claim 2, wherein: the pressure applying structure comprises a pressure applying part and a top cover, the pressure applying part is used for clamping the wafer in the cup body, the top cover is arranged to be capable of completely covering the cup opening of the cup body, and the pressure applying part is arranged at the bottom of the top cover.
5. The protection device for preventing surface decomposition and impurity incorporation under high temperature thermal annealing according to claim 4, wherein: the channel includes a first space provided between the pressure portion and the cup and a second space provided between the top cap and the top of the cup.
6. The protection device for preventing surface decomposition and impurity incorporation under high-temperature thermal annealing according to claim 5, wherein: the edge of top cap has the side cover towards cup direction extension, and the passageway still includes the third interval that is equipped with between side cover and the cup.
7. The protection device for preventing surface decomposition and impurity incorporation under high-temperature thermal annealing according to claim 6, wherein: the length of the side cover is not less than the interval size of the second interval and not more than the height of the cup body.
8. The protection device for preventing surface decomposition and impurity incorporation under high temperature thermal annealing according to any one of claims 1 to 7, wherein: the pressure applying structure comprises a pressure applying part which is a pressure block, and the pressure block clamps the wafer at the bottom of the inner side of the cup body.
9. The protection device for preventing surface decomposition and impurity incorporation under high-temperature thermal annealing according to claim 6, wherein: the pressure block, the top cover, the side cover and the cup body are made of one or a plurality of materials selected from corundum materials, tungsten metal materials, boron nitride materials and silicon carbide materials.
10. A method for preventing decomposition of a surface and incorporation of impurities under high temperature thermal annealing, which comprises using the protection device for preventing decomposition of a surface and incorporation of impurities under high temperature thermal annealing as claimed in any one of claims 1 to 9, the method comprising
The wafers with the cross section area not larger than the area of the pressure surface of the pressure structure are covered oppositely by two pairs of front surfaces to form a group, and the group is completely covered and clamped on the inner side of the cup body through the pressure structure;
putting the protection device into an annealing furnace for high-temperature thermal annealing treatment at 1400-2000 ℃ for 1-20 hours, and introducing protection gas;
and after naturally cooling to room temperature, taking out the whole protection device, and taking out the wafer.
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| JPH09199508A (en) * | 1995-11-14 | 1997-07-31 | Japan Energy Corp | Heat treatment method for GaAs substrate and substrate holder for heat treatment |
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Application publication date: 20220408 |