CN113690128A - A kind of cleaning method of indium phosphide wafer - Google Patents
A kind of cleaning method of indium phosphide wafer Download PDFInfo
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- CN113690128A CN113690128A CN202110994873.9A CN202110994873A CN113690128A CN 113690128 A CN113690128 A CN 113690128A CN 202110994873 A CN202110994873 A CN 202110994873A CN 113690128 A CN113690128 A CN 113690128A
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
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Abstract
本发明属于半导体晶片加工技术领域，公开了一种磷化铟晶片的清洗方法。该清洗方法，先采用有机溶剂去除磷化铟晶片表面的有机物，然后依次采用碱液、酸液和碱液对磷化铟晶片进行清洗。本发明提供的清洗方法，依次去除大颗粒物、小颗粒物和金属残留杂质，能够有效去除大直径磷化铟晶片上的微纳米级杂质颗粒，使大直径磷化铟晶片残留80nm的粒子数密度小于0.2颗/厘米2；在边缘去除2mm情况下，4英寸的磷化铟晶片残留80nm的粒子小于340颗，6英寸的磷化铟晶片残留80nm的粒子小于450颗。
The invention belongs to the technical field of semiconductor wafer processing, and discloses a cleaning method for an indium phosphide wafer. In the cleaning method, the organic solvent is first used to remove the organic substances on the surface of the indium phosphide wafer, and then the indium phosphide wafer is cleaned with an alkali solution, an acid solution and an alkali solution in sequence. The cleaning method provided by the invention sequentially removes large particles, small particles and residual metal impurities, which can effectively remove the micro-nano impurity particles on the large-diameter indium phosphide wafer, so that the particle number density of the remaining 80 nm of the large-diameter indium phosphide wafer is less than 0.2 particles/cm 2 ; when the edge is removed by 2mm, less than 340 particles of 80 nm remain on a 4-inch indium phosphide wafer, and less than 450 particles of 80 nm remain on a 6-inch indium phosphide wafer.
Description
Technical Field
The invention belongs to the technical field of semiconductor wafer processing, and particularly relates to a method for cleaning an indium phosphide wafer.
Background
InP is one of important III-V group compound semiconductor materials, and due to the advantages of InP, InP can be widely applied to many technical fields such as lasers, light emitting diodes, detectors, optical amplifiers, optical communication, microwave devices, millimeter wave devices, radiation-resistant solar cells and the like, and cannot be replaced. The diameter of the InP wafers will directly impact the cost of manufacturing electronic components, which is calculated to be about 8 times more cost effective using 4 inch wafers than using 2 inch wafers. Therefore, the method has important significance for exploring the growth of the high-quality large-diameter InP single crystal and realizing the industrialization thereof.
The InP wafer processing is to make the grown InP single crystal rod pass through a diamond wire with cutting fluid, and realize the separation process from the InP single crystal rod to the wafer by controlling the tension of the steel wire and the reciprocating motion of the high-speed positive and negative rhythmic steel wire. The wafer which is separately finished is put into a grinding disc, hard abrasive particles and the relative motion process formed by the wafer and the grinding disc are utilized to damage the surface of the wafer, staggered cracks are formed on the surface of the wafer, the cracks extend to the lower part of the surface, and the abrasive materials break the wafer slightly under the action of tangential impact force to form a new damage layer. And then coating wax with certain adhesive force on the back surface of the formed new damage layer grinding wafer to fix the wafer on a ceramic disc, and flattening the surface of the wafer by adopting a chemical mechanical polishing technology. The process is that under the condition of certain pressure and polishing liquid, the wafer makes planetary relative motion with respect to the polishing disk, and chemical-mechanical balance is achieved through the organic combination of the corrosion among the grinding particles, the oxidant and the wafer in the polishing liquid, so as to obtain the atomic roughness and the chemical surface state. At this time, a large amount of oxide and unsaturated dangling bonds exist on the wafer surface, and the unsaturated dangling bonds are in an unstable state and tend to bond with surrounding molecules or atoms, which is called "adsorption". The adsorption of impurities on the wafer surface is divided into physical adsorption and chemical adsorption. During polishing and chemical cleaning, the adsorption of the substrate surface adsorbs particles or impurities in the surrounding environment and chemical agents mainly by van der waals, electrostatic and chemical bonding forces. The particles or impurities adsorbed on the surface of the wafer form non-radiative recombination centers, which affect the epitaxial quality.
Through the above wafer processing process, the particles adsorbed on the surface of the cmp wafer are various and complicated. Chemical states of the detected residual impurities include various organics composed of C, H, O according to the wafer surface chemistry; binary oxide or ternary oxide consisting of In, P and O; residual impurities of metal adsorbed on the surface of the wafer, mainly including impurities of Si, S, Cl, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu and Zn are polluted; and chemical matching deviation generated by the unavoidable thermal stress action of the InP material in the growth process, impurity contamination absorbed by deep-level in-situ point defects such as component segregation and the like. The particles are classified according to the sizes of the adsorbed foreign particles, including micro-sized foreign particles (large particles) and nano-sized foreign particles (small particles). The method has the advantages of large quantity of nano-scale impurity particles, strong adsorption force and high removal difficulty, and at present, no good cleaning method exists, especially for impurities adsorbed on the surface of a large-diameter indium phosphide wafer.
Therefore, it is desirable to provide a method for cleaning an InP wafer, which can effectively remove the micro-nano-scale impurity particles on the large-diameter (4-6 inches) InP wafer.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides a method for cleaning an indium phosphide wafer, which can effectively remove micro-nano impurity particles on a large-diameter (4-6 inches) indium phosphide wafer.
The invention conception is as follows: the invention designs a cleaning process aiming at the large-diameter (4-6 inches) indium phosphide wafer, and changes the mode of cleaning by acid or alkali alone in the traditional method. According to the method, organic solvent is adopted to remove organic matters remained on the surface of the indium phosphide wafer, and then the processes of alkali washing, acid washing and alkali washing are sequentially carried out to remove large particles, small particles and metal residual impurities. The method can effectively remove micro-nano impurity particles on large-diameter (4-6 inches) indium phosphide wafers.
The invention provides a method for cleaning an indium phosphide wafer.
Specifically, the method for cleaning the indium phosphide wafer comprises the following steps: removing organic matters remained on the surface of the indium phosphide wafer by using an organic solvent, and then cleaning the indium phosphide wafer by sequentially using an alkali solution, an acid solution and an alkali solution;
the lye comprises weak alkali. The pH value of the weak base solution is more than 7 and less than 12. If the pH value is greater than 12, the wafer surface is damaged, which is not favorable for cleaning.
Preferably, the lye further comprises at least one of an oxidizing agent, a surfactant or a solvent.
Preferably, the weak base is ammonia and/or tetramethylammonium hydroxide (TMAH).
Preferably, when the weak base is ammonia water, an oxidant and a solvent are selected to be used in a matching way, and the mass ratio of the ammonia water to the oxidant to the solvent is (1-2): 0-2): 8-15; further preferably, the mass ratio of the ammonia water to the oxidant to the solvent is (1-2): 0-2): 8-15.
More preferably, when the weak base is ammonia water, an oxidant, a surfactant and a solvent are selected for matching use, and the mass ratio of the ammonia water to the oxidant, the surfactant and the solvent is (1-2): 8-15; most preferably, the mass ratio of the ammonia water to the oxidant, the surfactant and the solvent is (1-2): 8-12.
When the weak base is tetramethylammonium hydroxide, a solvent is selected for matching use, and the mass ratio of the tetramethylammonium hydroxide to the solvent is (0.5-3): (80-120); more preferably, the mass ratio of the tetramethylammonium hydroxide to the solvent is (0.5-2): (90-110).
Preferably, the surfactant may be anionic surfactant, cationic surfactant, nonionic surfactant and zwitterionic surfactant, such as stearyl-dodecyl-phenol polyoxyethylene ether, fatty acid, sodium dodecylbenzenesulfonate, quaternary ammonium compound, lecithin, betaine, fatty glyceride, sorbitan fatty acid, etc.
Preferably, the organic solvent is selected from at least one of ethanol, acetone, isopropanol, trichloroethylene or carbon tetrachloride.
Preferably, ultrasonic waves are assisted when the organic solvent is adopted to remove the residual wax on the surface of the indium phosphide wafer; more preferably, the ultrasonic wave has a wavelength of 0 to 40 kHZ.
The organic matter remained on the surface of the indium phosphide wafer is mainly wax and is distributed on the back surface of the indium phosphide wafer in a large amount.
Preferably, the acid solution comprises an acid, an oxidant and a solvent. Further preferably, the mass ratio of the acid to the oxidant to the solvent is (1-5): (0.5-2): (8-15); more preferably, the mass ratio of the acid to the oxidant to the solvent is (2-5): (0.5-1): (8-12).
Preferably, the acid is selected from at least one of citric acid, hydrochloric acid, hydrofluoric acid or sulfuric acid.
Preferably, the oxidant is hydrogen peroxide.
Preferably, the solvent is water.
Preferably, the cleaning process with acid solution is as follows: cleaning by sequentially adopting an acid liquid a, an acid liquid b and an acid liquid c, wherein the acid liquid a contains citric acid, an oxidizing agent and water, the acid liquid b contains hydrochloric acid, an oxidizing agent and water, and the acid liquid c contains hydrofluoric acid, an oxidizing agent and deionized water.
Preferably, megasonic waves are used for assisting in cleaning the indium phosphide wafer by adopting alkali liquor and acid liquor; further preferably, the wavelength of the megasonic wave is 0 to 40 kHZ.
More specifically, the method for cleaning the indium phosphide wafer comprises the following steps:
firstly, carrying out ultrasonic treatment for 3-60min at 0-60 ℃ by adopting an organic solvent to remove organic matters remained on the surface of the indium phosphide wafer, and drying the wafer; cleaning with alkali solution A at 0-20 deg.C for 1-60s with megasonic wave, and drying the wafer; cleaning with acid solution at 10-40 deg.C for 3-180s with megasonic wave, and drying the wafer; finally, cleaning the wafer for 1 to 60 seconds by megasonic waves with alkali liquor B at the temperature of between 0 and 20 ℃, and drying the wafer to finish cleaning.
The invention also provides application of the cleaning method in preparation of the indium phosphide wafer.
Compared with the prior art, the invention has the following beneficial effects:
according to the cleaning method provided by the invention, organic matters remained on the surface of the indium phosphide wafer are removed by adopting an organic solvent, and then large particles, small particles and metal residual impurities are removed in sequence through the processes of alkali cleaning, acid cleaning and alkali cleaning. The method can effectively removeRemoving micro-nano impurity particles on a large-diameter (4-6 inches) indium phosphide wafer to ensure that the residual 80nm particle number density of the large-diameter (4-6 inches) indium phosphide wafer is less than 0.2 particles/cm2(ii) a Under the condition of edge removal of 2mm, the residual 80nm particles of the 4-inch indium phosphide wafer are less than 340 particles, and the residual 80nm particles of the 6-inch indium phosphide wafer are less than 450 particles.
Drawings
Fig. 1 is a process flow diagram of the cleaning method provided in example 1.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The starting materials, reagents or apparatuses used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.
Example 1
A method for cleaning an indium phosphide wafer comprises the following steps:
(1) removing wax by using an organic solvent: the indium phosphide wafer (4 inches) is firstly subjected to ultrasonic treatment in acetone for 10min and then is subjected to ultrasonic treatment in ethanol for 10min, the ultrasonic treatment is carried out in isopropanol for 10min, the temperature of each ultrasonic treatment is controlled between 30 and 40 ℃, and the ultrasonic frequency is 20 kHZ. And after ultrasonic treatment, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(2) Cleaning with alkali liquor A: placing the indium phosphide wafer subjected to wax removal in the step (1) in a weak base solution for megacorrosion for 30s, wherein the megacorrosion frequency is 100MHZ, and the weak base solution comprises the following components: ammonia water, hydrogen peroxide, sodium dodecyl benzene sulfonate and deionized water in the weight ratio of 1 to 10, and the temperature of the weak base solution is controlled to be 15 ℃. And after the megacorrosion, washing the indium phosphide wafer by using deionized water, wherein the temperature of the deionized water is controlled to be 10-25 ℃, and the conductivity of the deionized water is 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(3) Cleaning with acid liquor: and (3) placing the indium phosphide wafer cleaned by the weak base in the step (2) in a solution containing citric acid for megasonic cleaning for 30s, wherein the megasonic cleaning frequency is 100 MHz. The solution containing citric acid consists of citric acid, hydrogen peroxide and deionized water in the weight ratio of 3 to 1 to 10. The temperature of the solution of citric acid was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s. The InP wafer was then megasonically cleaned in a solution containing hydrochloric acid at a megasonic frequency of 100MHz for 30 s. The solution containing hydrochloric acid consists of hydrochloric acid, hydrogen peroxide and deionized water in a ratio of 3:1: 10. The temperature of the solution containing hydrochloric acid was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s. The InP wafer is then cleaned in hydrofluoric acid containing solution for 30 sec at megasonic frequency of 100 MHz. The hydrofluoric acid-containing solution comprises hydrofluoric acid, hydrogen peroxide and deionized water in a ratio of 3:1: 10. The temperature of the hydrofluoric acid containing solution was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(4) Cleaning with alkali liquor B: placing the indium phosphide wafer cleaned by the acid liquor in the step (3) in a weak base solution for megacorrosion for 30s, wherein the megacorrosion frequency is 100MHZ, and the weak base solution comprises the following components: the ratio of tetramethylammonium hydroxide to deionized water is 1:100, and the temperature of the weak base solution is controlled to be 15 ℃. And after the megacorrosion, washing the indium phosphide wafer by using deionized water, wherein the temperature of the deionized water is controlled to be 10-25 ℃, and the conductivity of the deionized water is 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
Fig. 1 is a process flow diagram of the cleaning method, in fig. 1, an alkali liquor a is composed of ammonia water, hydrogen peroxide, sodium dodecyl benzene sulfonate and deionized water, an alkali liquor B is composed of tetramethylammonium hydroxide and deionized water, citric acid represents a solution containing citric acid, HCl is a solution containing hydrochloric acid, and HF is a solution containing hydrofluoric acid.
Example 2
A method for cleaning an indium phosphide wafer comprises the following steps:
(1) removing wax by using an organic solvent: the indium phosphide wafer (4 inches) is firstly subjected to ultrasonic treatment in acetone for 10min and then is subjected to ultrasonic treatment in ethanol for 10min, the ultrasonic treatment is carried out in isopropanol for 10min, the temperature of each ultrasonic treatment is controlled between 30 and 40 ℃, and the ultrasonic frequency is 20 kHZ. And after ultrasonic treatment, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(2) Cleaning with alkali liquor A: placing the indium phosphide wafer subjected to wax removal in the step (1) in a weak base solution for megacorrosion for 30s, wherein the megacorrosion frequency is 100MHZ, and the weak base solution comprises the following components: the ratio of tetramethylammonium hydroxide to deionized water is 1:100, and the temperature of the weak base solution is controlled to be 15 ℃. And after the megacorrosion, washing the indium phosphide wafer by using deionized water, wherein the temperature of the deionized water is controlled to be 10-25 ℃, and the conductivity of the deionized water is 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(3) Cleaning with acid liquor: and (3) placing the indium phosphide wafer cleaned by the weak base in the step (2) in a solution containing citric acid for megasonic cleaning for 30s, wherein the megasonic cleaning frequency is 100 MHz. The solution containing citric acid consists of citric acid, hydrogen peroxide and deionized water in the weight ratio of 3 to 1 to 10. The temperature of the solution of citric acid was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s. The InP wafer was then megasonically cleaned in a solution containing hydrochloric acid at a megasonic frequency of 100MHz for 30 s. The solution containing hydrochloric acid consists of hydrochloric acid, hydrogen peroxide and deionized water in a ratio of 3:1: 10. The temperature of the solution containing hydrochloric acid was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s. The InP wafer is then cleaned in hydrofluoric acid containing solution for 30 sec at megasonic frequency of 100 MHz. The hydrofluoric acid-containing solution comprises hydrofluoric acid, hydrogen peroxide and deionized water in a ratio of 3:1: 10. The temperature of the hydrofluoric acid containing solution was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(4) Cleaning with alkali liquor B: placing the indium phosphide wafer cleaned by the acid liquor in the step (3) in a weak base solution for megacorrosion for 30s, wherein the megacorrosion frequency is 100MHZ, and the weak base solution comprises the following components: ammonia water, hydrogen peroxide and deionized water in the ratio of 1 to 10, and the temperature of the weak base solution is controlled to be 15 ℃. And after the megacorrosion, washing the indium phosphide wafer by using deionized water, wherein the temperature of the deionized water is controlled to be 10-25 ℃, and the conductivity of the deionized water is 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
Example 3
A method for cleaning an indium phosphide wafer comprises the following steps:
(1) removing wax by using an organic solvent: the indium phosphide wafer (4 inches) is firstly subjected to ultrasonic treatment in isopropanol for 10min, and then is subjected to ultrasonic treatment in acetone for 10min, wherein the ultrasonic treatment is carried out in ethanol for 10min, the temperature of each ultrasonic treatment is controlled between 30 and 40 ℃, and the ultrasonic frequency is 30 kHZ. And after ultrasonic treatment, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(2) Cleaning with alkali liquor A: placing the indium phosphide wafer subjected to wax removal in the step (1) in a weak base solution for megacorrosion for 30s, wherein the megacorrosion frequency is 100MHZ, and the weak base solution comprises the following components: ammonia water, hydrogen peroxide, sodium dodecyl benzene sulfonate and deionized water in the weight ratio of 2 to 1 to 2 to 12, and the temperature of the weak base solution is controlled to be 15 ℃. And after the megacorrosion, washing the indium phosphide wafer by using deionized water, wherein the temperature of the deionized water is controlled to be 10-25 ℃, and the conductivity of the deionized water is 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(3) Cleaning with acid liquor: and (3) placing the indium phosphide wafer cleaned by the weak base in the step (2) in a solution containing citric acid for megasonic cleaning for 30s, wherein the megasonic cleaning frequency is 100 MHz. The solution containing citric acid consists of citric acid, hydrogen peroxide and deionized water in the weight ratio of 3 to 1 to 10. The temperature of the solution of citric acid was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s. The indium phosphide wafer was then megasonically cleaned in a solution containing hydrochloric acid at a megasonic frequency of 150MHZ for 30 seconds. The solution containing hydrochloric acid consists of hydrochloric acid, hydrogen peroxide and deionized water in a ratio of 3:1: 10. The temperature of the solution containing hydrochloric acid was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s. The InP wafer is then megasonically cleaned in a hydrofluoric acid containing solution for 30 seconds at a megasonic frequency of 150 MHz. The hydrofluoric acid-containing solution comprises hydrofluoric acid, hydrogen peroxide and deionized water in a ratio of 3:1: 10. The temperature of the hydrofluoric acid containing solution was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(4) Cleaning with alkali liquor B: placing the indium phosphide wafer cleaned by the acid liquor in the step (3) in a weak base solution for megacorrosion for 30s, wherein the megacorrosion frequency is 150MHZ, and the weak base solution comprises the following components: the ratio of tetramethylammonium hydroxide to deionized water is 1:100, and the temperature of the weak base solution is controlled to be 15 ℃. And after the megacorrosion, washing the indium phosphide wafer by using deionized water, wherein the temperature of the deionized water is controlled to be 10-25 ℃, and the conductivity of the deionized water is 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
Example 4
A method for cleaning an indium phosphide wafer comprises the following steps:
(1) removing wax by using an organic solvent: the indium phosphide wafer (4 inches) is firstly subjected to ultrasonic treatment in acetone for 10min and then is subjected to ultrasonic treatment in ethanol for 10min, the ultrasonic treatment is carried out in isopropanol for 10min, the temperature of each ultrasonic treatment is controlled between 30 and 40 ℃, and the ultrasonic frequency is 20 kHZ. And after ultrasonic treatment, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(2) Cleaning with alkali liquor A: placing the indium phosphide wafer subjected to wax removal in the step (1) in a weak base solution for megacorrosion for 30s, wherein the megacorrosion frequency is 100MHZ, and the weak base solution comprises the following components: ammonia water, hydrogen peroxide, sodium dodecyl benzene sulfonate and deionized water in the weight ratio of 1 to 10, and the temperature of the weak base solution is controlled to be 15 ℃. And after the megacorrosion, washing the indium phosphide wafer by using deionized water, wherein the temperature of the deionized water is controlled to be 10-25 ℃, and the conductivity of the deionized water is 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(3) Cleaning with acid liquor: and (3) placing the indium phosphide wafer cleaned by the weak base in the step (2) in a solution containing hydrochloric acid for megasonic cleaning for 30s, wherein the megasonic cleaning frequency is 100 MHZ. The solution containing hydrochloric acid consists of hydrochloric acid, hydrogen peroxide and deionized water in a ratio of 3:1: 10. The temperature of the solution containing hydrochloric acid was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s. The InP wafer was then megasonically cleaned in a hydrofluoric acid containing solution for 30 seconds at a megasonic frequency of 100 MHz. The hydrofluoric acid-containing solution comprises hydrofluoric acid, hydrogen peroxide and deionized water in a ratio of 3:1: 10. The temperature of the hydrofluoric acid containing solution was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s. The InP wafer is then megasonically cleaned in a solution containing citric acid for 30 seconds at a megasonic frequency of 100 MHz. The solution containing citric acid consists of citric acid, hydrogen peroxide and deionized water in the weight ratio of 3 to 1 to 10. The temperature of the solution of citric acid was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(4) Cleaning with alkali liquor B: placing the indium phosphide wafer cleaned by the acid liquor in the step (3) in a weak base solution for megacorrosion for 30s, wherein the megacorrosion frequency is 100MHZ, and the weak base solution comprises the following components: the ratio of tetramethylammonium hydroxide to deionized water is 1:100, and the temperature of the weak base solution is controlled to be 15 ℃. And after the megacorrosion, washing the indium phosphide wafer by using deionized water, wherein the temperature of the deionized water is controlled to be 10-25 ℃, and the conductivity of the deionized water is 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
Example 5
Example 5 differs from example 1 in that: a 6 inch indium phosphide wafer was cleaned.
Comparative example 1
Comparative example 1 differs from example 1 in that: only adopting alkali liquor A and alkali liquor B to clean.
Specifically, the method for cleaning the indium phosphide wafer comprises the following steps:
(1) removing wax by using an organic solvent: the indium phosphide wafer (4 inches) is firstly subjected to ultrasonic treatment in acetone for 10min and then is subjected to ultrasonic treatment in ethanol for 10min, the ultrasonic treatment is carried out in isopropanol for 10min, the temperature of each ultrasonic treatment is controlled between 30 and 40 ℃, and the ultrasonic frequency is 20 kHZ. And after ultrasonic treatment, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(2) Cleaning with alkali liquor A: placing the indium phosphide wafer subjected to wax removal in the step (1) in a weak base solution for megacorrosion for 30s, wherein the megacorrosion frequency is 100MHZ, and the weak base solution comprises the following components: ammonia water, hydrogen peroxide, sodium dodecyl benzene sulfonate and deionized water in the weight ratio of 1 to 10, and the temperature of the weak base solution is controlled to be 15 ℃. And after the megacorrosion, washing the indium phosphide wafer by using deionized water, wherein the temperature of the deionized water is controlled to be 10-25 ℃, and the conductivity of the deionized water is 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(3) Cleaning with alkali liquor B: putting the indium phosphide wafer cleaned by the alkali liquor A in the step (2) into a weak alkali solution for megaly corroding for 30s, wherein the megaly frequency is 100MHZ, and the weak alkali solution comprises the following components: the ratio of tetramethylammonium hydroxide to deionized water is 1:100, and the temperature of the weak base solution is controlled to be 15 ℃. And after the megacorrosion, washing the indium phosphide wafer by using deionized water, wherein the temperature of the deionized water is controlled to be 10-25 ℃, and the conductivity of the deionized water is 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
Comparative example 2
Comparative example 2 differs from example 1 in that: and only using acid liquor for cleaning.
Specifically, the method for cleaning the indium phosphide wafer comprises the following steps:
(1) removing wax by using an organic solvent: the indium phosphide wafer (4 inches) is firstly subjected to ultrasonic treatment in acetone for 10min and then is subjected to ultrasonic treatment in ethanol for 10min, the ultrasonic treatment is carried out in isopropanol for 10min, the temperature of each ultrasonic treatment is controlled between 30 and 40 ℃, and the ultrasonic frequency is 20 kHZ. And after ultrasonic treatment, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(2) Cleaning with acid liquor: and (2) placing the indium phosphide wafer subjected to wax removal in the step (1) in a solution containing citric acid, and cleaning for 30s at megasonic frequency of 100 MHz. The solution containing citric acid consists of citric acid, hydrogen peroxide and deionized water in the weight ratio of 3 to 1 to 10. The temperature of the solution of citric acid was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s. The InP wafer was then megasonically cleaned in a solution containing hydrochloric acid at a megasonic frequency of 100MHz for 30 s. The solution containing hydrochloric acid consists of hydrochloric acid, hydrogen peroxide and deionized water in a ratio of 3:1: 10. The temperature of the solution containing hydrochloric acid was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s. The InP wafer is then cleaned in hydrofluoric acid containing solution for 30 sec at megasonic frequency of 100 MHz. The hydrofluoric acid-containing solution comprises hydrofluoric acid, hydrogen peroxide and deionized water in a ratio of 3:1: 10. The temperature of the hydrofluoric acid containing solution was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
Comparative example 3
Comparative example 3 differs from example 4 in that: and only using acid liquor for cleaning.
Specifically, the method for cleaning the indium phosphide wafer comprises the following steps:
(1) removing wax by using an organic solvent: the indium phosphide wafer (4 inches) is firstly subjected to ultrasonic treatment in acetone for 10min and then is subjected to ultrasonic treatment in ethanol for 10min, the ultrasonic treatment is carried out in isopropanol for 10min, the temperature of each ultrasonic treatment is controlled between 30 and 40 ℃, and the ultrasonic frequency is 20 kHZ. And after ultrasonic treatment, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(2) Cleaning with acid liquor: and (2) putting the indium phosphide wafer subjected to wax removal in the step (1) into a solution containing hydrochloric acid, and carrying out megasonic cleaning for 30s, wherein the megasonic frequency is 100 MHZ. The solution containing hydrochloric acid consists of hydrochloric acid, hydrogen peroxide and deionized water in a ratio of 3:1: 10. The temperature of the solution containing hydrochloric acid was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s. The InP wafer was then megasonically cleaned in a hydrofluoric acid containing solution for 30 seconds at a megasonic frequency of 100 MHz. The hydrofluoric acid-containing solution comprises hydrofluoric acid, hydrogen peroxide and deionized water in a ratio of 3:1: 10. The temperature of the hydrofluoric acid containing solution was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s. The InP wafer is then megasonically cleaned in a solution containing citric acid for 30 seconds at a megasonic frequency of 100 MHz. The solution containing citric acid consists of citric acid, hydrogen peroxide and deionized water in the weight ratio of 3 to 1 to 10. The temperature of the solution of citric acid was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, wherein the temperature of the deionized water is controlled to be 10-25 ℃, and the conductivity of the deionized water is 18 megaohm per centimeter. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
Comparative example 4 differs from example 1 in that: washing is carried out without alkali liquor A.
Specifically, the method for cleaning the indium phosphide wafer comprises the following steps:
(1) removing wax by using an organic solvent: the indium phosphide wafer (4 inches) is firstly subjected to ultrasonic treatment in acetone for 10min and then is subjected to ultrasonic treatment in ethanol for 10min, the ultrasonic treatment is carried out in isopropanol for 10min, the temperature of each ultrasonic treatment is controlled between 30 and 40 ℃, and the ultrasonic frequency is 20 kHZ. And after ultrasonic treatment, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(2) Cleaning with acid liquor: and (2) placing the indium phosphide wafer subjected to wax removal in the step (1) in a solution containing citric acid, and cleaning for 30s at megasonic frequency of 100 MHz. The solution containing citric acid consists of citric acid, hydrogen peroxide and deionized water in the weight ratio of 3 to 1 to 10. The temperature of the solution of citric acid was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s. The InP wafer was then megasonically cleaned in a solution containing hydrochloric acid at a megasonic frequency of 100MHz for 30 s. The solution containing hydrochloric acid consists of hydrochloric acid, hydrogen peroxide and deionized water in a ratio of 3:1: 10. The temperature of the solution containing hydrochloric acid was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s. The InP wafer is then cleaned in hydrofluoric acid containing solution for 30 sec at megasonic frequency of 100 MHz. The hydrofluoric acid-containing solution comprises hydrofluoric acid, hydrogen peroxide and deionized water in a ratio of 3:1: 10. The temperature of the hydrofluoric acid containing solution was 25 ℃. And after megaly cleaning, washing the indium phosphide wafer by using deionized water, controlling the temperature of the deionized water to be 10-25 ℃, and controlling the conductivity of the deionized water to be 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
(3) Cleaning with alkali liquor B: placing the indium phosphide wafer cleaned by the acid liquor in the step (2) in a weak base solution for megacorrosion for 30s, wherein the megacorrosion frequency is 100MHZ, and the weak base solution comprises the following components: the ratio of tetramethylammonium hydroxide to deionized water is 1:100, and the temperature of the weak base solution is controlled to be 15 ℃. And after the megacorrosion, washing the indium phosphide wafer by using deionized water, wherein the temperature of the deionized water is controlled to be 10-25 ℃, and the conductivity of the deionized water is 18 megaohm.cm. After rinsing, the wafer was spin-dried at a high speed of 3000rad/min for 60 s.
Product effectiveness testing
The surface graininess of the cleaned indium phosphide wafers of examples 1-5 and comparative examples 1-4 were tested, respectively.
The test method comprises the following steps: the whole surface of a sample is scanned by laser, defects (particles, scratches, pits, water stains, traces and the like) are classified through signals collected by detectors of 4 channels (a scattered light channel, a reflected light channel, a phase shift channel and a Z channel), the number of each defect is counted, the corresponding defect size is measured, and finally the whole surface defect is given. Measurement conditions were as follows: the edges were removed by 2 mm. Table 1 shows the measurement results. The table shows the particles having a particle size of 1.0. mu.m, 0.5. mu.m, 0.3. mu.m, 0.2. mu.m, 0.08 μm and the Total number of particles (Total) on the surface of the cleaned indium phosphide wafer of examples 1 to 5 and comparative examples 1 to 4.
TABLE 1 results of particle size testing
As can be seen from the examples, the indium phosphide wafers cleaned by the method provided by the invention had a small number of particles per particle size and a small total number of particles per particle size. From the comparative example, it can be seen that when no acid solution treatment or no two-time alkali solution treatment is adopted, the number of particles and the total number of particles at each particle size are increased sharply, and the residual quantity of particles on the surface of the large-size indium phosphide wafer obviously does not meet the quality requirement.
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