Method for improving reaction rate of preparing gallium oxide from metal gallium

Abstract

The embodiment of the invention provides a method for improving the reaction rate of preparing gallium oxide from metal gallium. Comprising the following steps: mixing metal gallium with water to form a reaction mixture; adding an accelerant into the reaction mixture to promote the oxidation reaction of the metal gallium; carrying out chemical reaction on the reaction mixture containing the accelerant under the action of an external physical field to generate hydroxyl gallium oxide powder; and carrying out thermal cracking on the hydroxyl gallium oxide powder in inert gas to obtain gallium oxide powder. By adding the accelerant and utilizing an external physical field, the reaction rate of preparing gallium oxide from metal gallium is effectively improved through a plurality of links and a synergistic effect, the problem of low reaction rate in the prior art is solved, and powerful technical support is provided for efficient preparation of high-purity gallium oxide.

Description

Technical Field

[0001] The present application relates to the technical field of metal oxide material preparation, and in particular to a method for increasing the reaction rate of preparing gallium oxide from metallic gallium. Background Art

[0002] Gallium oxide (Ga2O3), a new fourth-generation ultra-wide bandgap semiconductor material, boasts excellent resistance to high voltage, high temperature, and radiation, and holds significant application value in high-power electronic devices, communications, aerospace, and ultraviolet (UV) solar-blind detection. High-purity gallium oxide powder is the primary raw material for preparing gallium oxide single crystals. Rapid and efficient production of qualified high-purity gallium oxide powder provides a stable raw material supply for the development of the gallium oxide semiconductor industry.

[0003] Existing methods for preparing gallium oxide powders generally suffer from complex processes, long reaction times, and high reagent consumption. For example, the traditional hydrothermal method for preparing gallium metal, due to its high surface tension, makes it difficult to evenly disperse in water, resulting in a slow reaction rate. High temperatures and pressures, as well as vigorous mechanical stirring, are required to achieve high conversion rates, which not only increases energy consumption but also reduces production efficiency. Therefore, developing an efficient, environmentally friendly, and streamlined process for preparing gallium oxide powders with a short reaction time is of great significance. Summary of the Invention

[0004] The present application provides a method for increasing the reaction rate of preparing gallium oxide from metal gallium to solve the following technical problem: how to increase the reaction rate during the process of preparing high-purity gallium oxide by a metal gallium hydrothermal method.

[0005] The present invention provides a method for increasing the reaction rate of preparing gallium oxide from metallic gallium, comprising:

[0006] mixing metallic gallium with water to form a reaction mixture;

[0007] adding a promoter to the reaction mixture;

[0008] Under the action of an external physical field, the reaction mixture containing the promoter undergoes a chemical reaction to generate gallium oxyhydroxide powder;

[0009] In an inert gas, the gallium oxyhydroxide powder is thermally cracked to obtain gallium oxide powder. Optionally, the promoter includes at least one of the following: an oxidant, a catalyst;

[0010] The oxidant comprises at least one of the following: hydrogen peroxide, peroxide, ozone, chlorate, and permanganate;

[0011] The catalyst includes at least one of the following: a metal catalyst and a non-metal catalyst.

[0012] Optionally, the external physical field includes at least one of the following: an ultrasonic field, a pressure field, a magnetic field, and an electric field.

[0013] Optionally, the power of the ultrasonic field is 500-1000W, and the initial pressure of the pressure field is 2-6MPa.

[0014] Optionally, the parameters of the chemical reaction include at least one of the following: reaction temperature of 160 to 220° C., reaction time of 2 to 10 hours, reaction pressure of 2 to 6 MPa, and reaction stirring speed of 800 to 1200 r / min.

[0015] Optionally, the liquid-to-solid ratio of the metal gallium to the water is (4-20):1.

[0016] Optionally, the purity of the metallic gallium is not less than 6N;

[0017] The purity of the gallium oxide powder is not less than 5N.

[0018] Optionally, the temperature of the thermal cracking is 700-950° C., and the time of the thermal cracking is 2-4 hours.

[0019] Optionally, before thermally cracking the gallium oxyhydroxide powder, the method further comprises:

[0020] The gallium oxyhydroxide powder is washed and dried; the drying temperature is 80 to 120° C., and the drying time is 4 to 10 hours.

[0021] The above technical solution provided by the embodiment of the present application has the following advantages compared with the prior art:

[0022] The present embodiment provides a method for increasing the reaction rate of gallium metal to gallium oxide. First, gallium metal and water are mixed to form a reaction mixture. This is a fundamental step in the preparation process and provides the necessary reactant system for subsequent reactions. Next, a promoter is added to the reaction mixture. This key step can significantly accelerate the oxidation reaction rate of gallium metal. The promoter reduces the activation energy of the reaction, allowing the gallium metal to be oxidized more quickly, thereby shortening the oxidation reaction time. Under the influence of an external physical field, the gallium metal and water further react chemically to produce gallium oxyhydroxide powder. The application of an external physical field provides additional energy to the reaction, helping to shift the equilibrium and enable the reaction to proceed more efficiently. For example, the application of an ultrasonic or microwave field can enhance the collision frequency and energy transfer efficiency between reactant molecules, thereby accelerating the reaction process. Finally, the resulting gallium oxyhydroxide powder is thermally cracked to obtain the final gallium oxide powder. The thermal cracking process removes the hydroxyl groups at high temperatures, converting the gallium oxyhydroxide into high-purity gallium oxide. By adding promoters and utilizing external physical fields, starting from multiple links and working synergistically, the reaction rate of preparing gallium oxide from metallic gallium is effectively improved, solving the problem of low reaction rate in existing technologies and providing strong technical support for the efficient preparation of high-purity gallium oxide. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present application and, together with the description, serve to explain the principles of the present application.

[0024] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

[0025] Figure 1 A flow chart of a method for increasing the reaction rate of preparing gallium oxide from metallic gallium provided in an embodiment of the present application. DETAILED DESCRIPTION

[0026] To make the purpose, technical solutions, and advantages of the embodiments of this application more clear, the technical solutions in the embodiments of this application will be clearly and completely described below in conjunction with the drawings in the embodiments of this application. Obviously, the described embodiments are part of the embodiments of this application, not all of the embodiments. Based on the embodiments in this application, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of this application.

[0027] The range descriptions described in this article, such as numerical ranges, ratio ranges, etc., include all possible sub-ranges and single numerical values ​​within the range. For example, the range description of "1 to 6" or "1~6" covers all sub-ranges from 1 to 6 (such as 1 to 3, 2 to 5, etc.) and single numbers (such as 1, 2, 3, 4, 5, 6). Unless otherwise specified, the terms "including", "comprising", etc. used in this article mean "including but not limited to"; relational terms such as "first" and "second" are only used to distinguish different entities or operations, and do not imply an actual sequence or association relationship; "and / or" means that multiple situations can exist alone or at the same time; expressions such as "at least one", "multiple", and "at least one" refer to any combination of corresponding objects, including a combination of single or multiple objects. The proportional relationships involved in the article, such as mass ratios, molar ratios, etc., should be understood as the corresponding relationship between the first and second terms of the proportional formula in the order of description. The raw materials, reagents, instruments and equipment used in this article can be purchased on the market or prepared by existing methods.

[0028] Figure 1 A flow chart of a method for increasing the reaction rate of preparing gallium oxide from metallic gallium is provided for an embodiment of the present application.

[0029] See Figure 1 The present invention provides a method for increasing the reaction rate of preparing gallium oxide from metallic gallium, comprising:

[0030] S1, mixing metallic gallium with water to form a reaction mixture;

[0031] S2, adding a promoter to the reaction mixture,

[0032] S3. Under the action of an external physical field, causing the reaction mixture containing the promoter to undergo a chemical reaction to generate gallium oxyhydroxide powder;

[0033] S4. Thermally cracking the gallium oxyhydroxide powder in an inert gas to obtain gallium oxide powder.

[0034] Gallium metal: A chemical element with a high melting point and high density. Promoter: A substance that accelerates the rate of a chemical reaction, such as an oxidant or catalyst. External physical field: External conditions that influence a chemical reaction through physical means (such as ultrasound, pressure, magnetic field, or electric field). Gallium oxyhydroxide powder: An intermediate product formed by the reaction of gallium metal and water, typically in the form of a nanoscale powder. Thermal cracking is a chemical process that decomposes organic matter at high temperatures to produce smaller molecules or compounds. After gallium metal and water are mixed, a promoter (such as an oxidant or catalyst) is added to accelerate the oxidation reaction of gallium metal, producing gallium oxyhydroxide powder. External physical fields (such as ultrasound and pressure fields) further improve the reaction rate and product uniformity. An inert gas environment effectively isolates the gallium oxyhydroxide precursor from the outside world, reducing the risk of impurity introduction. At the same time, some impurities in the precursor decompose or volatilize at high temperatures, significantly improving the purity of the gallium oxide powder. The thermal cracking process will cause the crystal structure of gallium oxyhydroxide to change from amorphous or low crystallinity to high crystallinity, making the crystal structure more regular and reducing lattice defects. At the same time, the particles undergo a certain degree of recrystallization or sintering, and the particle size distribution is more uniform, which helps to improve the performance consistency of the material. In terms of technical effects: through the synergistic effect of the promoter and the external physical field, the oxidation reaction rate of metallic gallium is significantly improved. The optimized reaction conditions reduce the reaction time and the required high temperature and high pressure conditions, and reduce energy consumption. The gallium oxide powder preparation technology provided in this application is suitable for large-scale industrial production of high-purity gallium oxide powder for use in semiconductors, electronic devices, aerospace and other fields. In terms of optical properties, high-purity, high-crystallinity gallium oxide powder has higher transmittance and less absorption in the ultraviolet light region; in terms of electrical properties, the carrier mobility is improved and the resistivity is reduced; in terms of chemical stability, it is more stable in harsh environments such as high temperature and high humidity, and is not easy to decompose or react chemically with other substances.

[0035] Exemplary:

[0036] Hydrogen peroxide was used as the oxidant, the ultrasonic field power was 800 W, the reaction temperature was 180° C., and the reaction time was 6 hours.

[0037] Ozone was used as the oxidant, the initial pressure of the pressure field was 4 MPa, and the reaction time was 5 hours.

[0038] Chlorate was used as the oxidant, the magnetic field strength was 0.5 T, and the reaction time was 8 hours.

[0039] Permanganate was used as the oxidant, the electric field strength was 1000 V / cm, and the reaction time was 7 hours.

[0040] A combination of hydrogen peroxide and a catalyst was used, the ultrasonic field power was 1000 W, the reaction temperature was 200° C., and the reaction time was 4 hours.

[0041] Peroxide was used as the oxidant, the initial pressure of the pressure field was 3 MPa, and the reaction time was 9 hours.

[0042] Hydrogen peroxide was used, the ultrasonic field power was 600 W, the reaction temperature was 160° C., and the reaction time was 10 hours.

[0043] Ozone was used, the initial pressure of the pressure field was 5 MPa, and the reaction time was 3 hours.

[0044] Chlorate was used, the magnetic field strength was 0.3 T, and the reaction time was 7 hours.

[0045] Permanganate was used, the electric field strength was 800 V / cm, and the reaction time was 6 hours.

[0046] In some embodiments, the promoter includes at least one of the following: an oxidant, a catalyst;

[0047] The oxidant comprises at least one of the following: hydrogen peroxide, peroxide, ozone, chlorate, and permanganate;

[0048] The catalyst includes at least one of the following: a metal catalyst and a non-metal catalyst.

[0049] Oxidants: Chemical substances that can provide oxygen or accept electrons, such as hydrogen peroxide and peroxide. Catalysts: Substances that accelerate the rate of a chemical reaction without being consumed. Oxidants promote the oxidation of gallium metal by providing oxygen or accepting electrons, producing gallium oxyhydroxide. Catalysts accelerate the reaction rate and improve reaction efficiency by reducing the activation energy of the reaction. Hydrogen peroxide has strong oxidizing properties and can quickly oxidize gallium metal to gallium ions. The free radicals produced during the reaction can further promote the oxidation of gallium metal, increasing the reaction rate. The oxygen produced by the decomposition of hydrogen peroxide during the reaction also acts as a stirring agent, making the reaction more uniform. Peroxides, like hydrogen peroxide, also have strong oxidizing properties and can effectively promote the oxidation of gallium metal. However, due to their relatively active chemical properties, the reaction conditions must be carefully controlled during use to avoid side reactions and the introduction of impurities. Ozone is a strong oxidant with stronger oxidizing power than hydrogen peroxide. It can oxidize gallium metal into gallium ions more quickly, thereby increasing the reaction rate. However, due to the poor stability of ozone, the reaction conditions need to be strictly controlled during the reaction to ensure the safety and stability of the reaction. Chlorate can release chlorate ions in aqueous solution and has strong oxidizing properties, which can effectively promote the oxidation reaction of gallium metal. At the same time, chlorate can also form a certain acidic environment during the reaction, further promoting the dissolution and reaction of gallium metal. Permanganate has a strong oxidizing property and can quickly oxidize gallium metal into gallium ions. At the same time, by-products such as manganese dioxide produced during the reaction can also play a certain catalytic role, further increasing the reaction rate. However, since the reduction products of permanganate may have a certain impact on the purity of the product, it is necessary to pay attention to fully washing and purifying the product during use. In this application, catalysts include metal catalysts and non-metallic catalysts. Metal catalysts, such as copper and silver, can reduce the activation energy of the reaction, allowing the reaction to proceed rapidly at lower temperatures and pressures, thereby increasing the reaction rate. At the same time, metal catalysts can also improve the selectivity of the reaction and the purity of the product by adsorbing and activating the reactant molecules. Non-metallic catalysts, such as activated carbon and molecular sieves, have a large specific surface area and a rich pore structure. They can adsorb reactant molecules and increase the probability of collision between them, thereby increasing the reaction rate. In addition, non-metallic catalysts can further promote the reaction by adjusting the pH of the reaction system and other conditions. In terms of technical effects: The use of oxidants and catalysts significantly increases the oxidation reaction rate of metallic gallium. Selecting the right oxidant and catalyst at the same time can avoid the introduction of impurities in the promoter.

[0050] Exemplary:

[0051] Using hydrogen peroxide as the oxidant, the reaction rate increased by about 30%.

[0052] Using peroxide as the oxidant, the reaction rate increased by about 25%.

[0053] Using ozone as the oxidant, the reaction rate increased by about 35%.

[0054] Using chlorate as the oxidant, the reaction rate increased by about 20%.

[0055] Using permanganate as the oxidant, the reaction rate increased by about 40%.

[0056] Using a combination of hydrogen peroxide and a catalyst, the reaction rate increased by about 50%.

[0057] Using the peroxide and catalyst combination, the reaction rate increased by approximately 45%.

[0058] Using the ozone and catalyst combination, the reaction rate increased by about 55%.

[0059] Using the chlorate and catalyst combination, the reaction rate increased by about 30%.

[0060] Using the permanganate and catalyst combination, the reaction rate increased by about 60%.

[0061] In some embodiments, the external physical field includes at least one of the following: an ultrasonic field, a pressure field, a magnetic field, and an electric field.

[0062] External physical fields: These influence the external conditions of a chemical reaction through physical means (such as ultrasound, pressure, magnetic fields, and electric fields). Ultrasonic fields: These utilize the high-frequency vibrations of ultrasound to create a localized high-temperature and high-pressure environment. Pressure fields: These influence the conditions of a chemical reaction by applying pressure. Magnetic fields: These influence the conditions of a chemical reaction by utilizing magnetic fields. Electric fields: These influence the conditions of a chemical reaction by utilizing electric fields. The effect of ultrasound on reaction rates varies at different power levels. At a power of 500W, the reaction rate improves modestly; at a power of 1000W, the reaction rate increases significantly, and the product uniformity improves. This is because higher ultrasound power creates a stronger localized high-temperature and high-pressure environment, leading to higher reaction rates. The effect of pressure on reaction rates also varies at different initial pressures. At an initial pressure of 2MPa, the reaction rate improves modestly; at an initial pressure of 6MPa, the reaction rate increases significantly, resulting in better product quality. This is because higher initial pressures increase the frequency of collisions between reactant molecules, leading to higher reaction rates. The effect of magnetic fields on reaction rates varies at different intensities. When the magnetic field strength is 0.3T, the reaction rate increases slightly; when the magnetic field strength is 0.5T, the reaction rate increases significantly, and the product purity is higher. This is because the higher the magnetic field strength, the greater the impact on the movement of the reactant molecules, and the higher the reaction rate. The effect of the electric field on the reaction rate varies at different intensities. When the electric field strength is 500V / cm, the reaction rate increases slightly; when the electric field strength is 1000V / cm, the reaction rate increases significantly, and the product uniformity improves. This is because the higher the electric field strength, the greater the impact on the movement of the reactant molecules, and the higher the reaction rate. In terms of technical effects: The use of an external physical field significantly increases the oxidation reaction rate of metallic gallium. The use of ultrasonic and pressure fields improves the uniformity of the product.

[0063] Exemplary:

[0064] Using an ultrasonic field with a power of 800W, the reaction rate increased by about 40%.

[0065] Using a pressure field with an initial pressure of 4 MPa, the reaction rate increased by about 35%.

[0066] Using a magnetic field with a strength of 0.5 T, the reaction rate increased by about 30%.

[0067] Using an electric field with a strength of 1000 V / cm, the reaction rate increased by about 45%.

[0068] Using a combination of ultrasonic field and pressure field with a power of 800W and an initial pressure of 4MPa, the reaction rate increased by about 60%.

[0069] Using a combination of ultrasonic and magnetic fields with a power of 600W and an intensity of 0.3T, the reaction rate increased by about 55%.

[0070] Using a combination of ultrasonic and electric fields with a power of 1000W and an intensity of 800V / cm, the reaction rate increased by about 70%.

[0071] Using a combination of pressure and magnetic fields, with an initial pressure of 3 MPa and an intensity of 0.5 T, the reaction rate increased by about 65%.

[0072] Using a combination of pressure and electric fields, with an initial pressure of 5 MPa and an intensity of 1000 V / cm, the reaction rate increased by about 75%.

[0073] Using a combination of magnetic and electric fields with a strength of 0.3 T and an intensity of 800 V / cm, the reaction rate increased by about 50%.

[0074] In some embodiments, the power of the ultrasonic field is 500-1000 W, and the initial pressure of the pressure field is 2-6 MPa.

[0075] Ultrasonic field power: The power of the ultrasonic wave, measured in watts (W). Initial pressure: The pressure applied at the start of the reaction, measured in megapascals (MPa). The higher the ultrasonic power, the stronger the local high-temperature and high-pressure environment generated, and the higher the reaction rate. The higher the initial pressure, the higher the frequency of collisions between reactant molecules, and the higher the reaction rate. Within the power range of 500 to 1000 W, higher ultrasonic field power creates a stronger local high-temperature and high-pressure environment, and the higher the reaction rate. For example, at a power of 500 W, the reaction rate improves modestly; at a power of 1000 W, the reaction rate increases significantly, and the product uniformity improves. Within the initial pressure range of 2 to 6 MPa, higher initial pressure increases the frequency of collisions between reactant molecules and the reaction rate. However, since hydrogen is released during the reaction of metallic gallium with water to form gallium oxyhydroxide, the reaction rate increases in a "volcano-like" manner as the initial pressure increases (above 4 MPa). For example, when the initial pressure is 2 MPa or 6 MPa, the reaction rate is improved to a certain extent; when the initial pressure is 4 MPa, the reaction rate is the fastest and the product quality is better.

[0076] Exemplary:

[0077] The ultrasonic field power is 800W, the initial pressure of the pressure field is 4MPa, and the reaction rate is increased by about 60%.

[0078] The ultrasonic field power is 1000W, the initial pressure of the pressure field is 5MPa, and the reaction rate is increased by about 70%.

[0079] The ultrasonic field power is 600W, the initial pressure of the pressure field is 3MPa, and the reaction rate is increased by about 50%.

[0080] The ultrasonic field power is 900W, the initial pressure of the pressure field is 4MPa, and the reaction rate is increased by about 65%.

[0081] The ultrasonic field power is 700W, the initial pressure of the pressure field is 2MPa, and the reaction rate is increased by about 45%.

[0082] The ultrasonic field power is 1100W, the initial pressure of the pressure field is 6MPa, and the reaction rate is increased by about 75%.

[0083] The ultrasonic field power is 500W, the initial pressure of the pressure field is 2MPa, and the reaction rate is increased by about 35%.

[0084] The ultrasonic field power is 1200W, the initial pressure of the pressure field is 6MPa, and the reaction rate is increased by about 80%.

[0085] The ultrasonic field power is 850W, the initial pressure of the pressure field is 5MPa, and the reaction rate is increased by about 68%.

[0086] The ultrasonic field power is 950W, the initial pressure of the pressure field is 4MPa, and the reaction rate is increased by about 72%.

[0087] In some embodiments, the parameters of the chemical reaction include at least one of the following: a reaction temperature of 160 to 220° C., a reaction pressure of 2 to 6 MPa, and a reaction stirring speed of 800 to 1200 r / min.

[0088] Reaction Temperature: The temperature at which the reaction is carried out, in degrees Celsius (°C). Reaction Time: The time the reaction is carried out, in hours (h). Reaction Pressure: The pressure during the reaction, in megapascals (MPa). Reaction Stirring Speed: The speed of the stirrer during the reaction, in revolutions per minute (r / min).

[0089] Gallium metal (Ga) reacts with water (H2O) to produce gallium hydroxide (GaOOH) and hydrogen (H2). The chemical equation is: Ga + H2O → GaOOH + H2.

[0090] Reaction Mechanism: Gallium metal is an active metal that reacts chemically with water. During the reaction, gallium atoms lose electrons, while hydrogen atoms in water molecules gain electrons, generating hydrogen. Simultaneously, gallium combines with oxygen in the water to form gallium hydroxide (GaOOH). High temperatures (160-220°C) provide sufficient energy to increase the activity of gallium atoms and water molecules, making it easier for chemical bonds to break and recombine. This increases the reaction rate and shortens the reaction time. High pressure (2-6 MPa) increases the frequency of collisions between reactant molecules, facilitating the reaction. It also inhibits hydrogen diffusion, ensuring a more complete reaction. Agitation (800-1200 rpm) ensures thorough mixing of the reactants, preventing localized concentrations from being too high or too low, and ensuring a uniform reaction. This increases the contact area between the reactants, further accelerating the reaction rate.

[0091] Exemplary:

[0092] The reaction temperature is 180° C., the reaction pressure is 4 MPa, the stirring speed is 1000 r / min, and the reaction rate is increased by about 60%.

[0093] The reaction temperature is 200° C., the reaction pressure is 5 MPa, the stirring speed is 1200 r / min, and the reaction rate is increased by about 70%.

[0094] The reaction temperature is 160° C., the reaction pressure is 3 MPa, the stirring speed is 800 r / min, and the reaction rate is increased by about 50%.

[0095] The reaction temperature is 190° C., the reaction pressure is 4 MPa, the stirring speed is 1000 r / min, and the reaction rate is increased by about 65%.

[0096] The reaction temperature is 220° C., the reaction pressure is 4 MPa, the stirring speed is 1200 r / min, and the reaction rate is increased by about 75%.

[0097] The reaction temperature is 170° C., the reaction pressure is 3 MPa, the stirring speed is 900 r / min, and the reaction rate is increased by about 55%.

[0098] The reaction temperature is 210° C., the reaction pressure is 5 MPa, the stirring speed is 1000 r / min, and the reaction rate is increased by about 70%.

[0099] The reaction temperature is 180° C., the reaction pressure is 4 MPa, the stirring speed is 1100 r / min, and the reaction rate is increased by about 60%.

[0100] The reaction temperature is 200° C., the reaction pressure is 4 MPa, the stirring speed is 1200 r / min, and the reaction rate is increased by about 72%.

[0101] The reaction temperature is 190° C., the reaction pressure is 4 MPa, the stirring speed is 1100 r / min, and the reaction rate is increased by about 67%.

[0102] In some embodiments, the liquid-to-solid ratio of the metal gallium to the water is (4-20):1.

[0103] Liquid-to-solid ratio: The mass ratio of liquid water (mass) to solid gallium metal (mass). Maintaining a constant amount of water during the reaction, a lower liquid-to-solid ratio (4-20:1) results in more gallium metal, which can increase the yield of gallium oxyhydroxide powder and improve production efficiency. For example, compared to a liquid-to-solid ratio of 20:1, a liquid-to-solid ratio of 4:1 increases the yield of gallium oxyhydroxide powder obtained in a single reaction by five times, significantly improving production efficiency. Furthermore, since the introduction of background impurities from the equipment system itself is constant during the reaction, reducing the liquid-to-solid ratio and increasing yield can significantly improve product purity.

[0104] Exemplary liquid-to-solid ratios may be 10:1, 15:1, 5:1, 20:1, 8:1, 12:1, 18:1, 6:1, 14:1, 16:1, and the like.

[0105] In some embodiments, the purity of the metallic gallium is not less than 6N;

[0106] The purity of the gallium oxide powder is not less than 5N.

[0107] Gallium metal purity: The purity of gallium metal, the unit is 6N (indicating 99.9999%). Gallium oxide powder purity: The purity of gallium oxide powder, the unit is 5N (indicating 99.999%).

[0108] In some embodiments, the temperature of the thermal cracking is 700-950° C., and the time of the thermal cracking is 2-4 hours.

[0109] Pyrolysis temperature: The temperature at which pyrolysis is carried out, in degrees Celsius (°C). Pyrolysis time: The time during which pyrolysis is carried out, in hours (h).

[0110] Within the temperature range of 700-950°C, higher thermal cracking temperatures facilitate rapid conversion of gallium oxyhydroxide powder and shorten calcination time. Furthermore, the appropriate temperature provides energy for crystal transformation, transforming gallium oxyhydroxide from a low-crystallinity structure to a high-crystallinity gallium oxide. Higher crystallinity results in superior performance, but excessively high temperatures can lead to excessive sintering of the particles, affecting particle size distribution. A thermal cracking time of 2-4 hours facilitates recrystallization, resulting in a regular crystal structure and uniform particle size distribution, while also maintaining production efficiency and reducing unnecessary energy consumption and time costs.

[0111] Exemplary:

[0112] The thermal cracking temperature is 800°C and the thermal cracking time is 3 hours.

[0113] The thermal cracking temperature is 900°C and the thermal cracking time is 2 hours.

[0114] The thermal cracking temperature is 750°C and the thermal cracking time is 4 hours.

[0115] The thermal cracking temperature is 850°C and the thermal cracking time is 3 hours.

[0116] The thermal cracking temperature is 950°C and the thermal cracking time is 2 hours.

[0117] The thermal cracking temperature is 780°C and the thermal cracking time is 3.5 hours.

[0118] The thermal cracking temperature is 880°C and the thermal cracking time is 2.5 hours.

[0119] The thermal cracking temperature is 820°C and the thermal cracking time is 3 hours.

[0120] The thermal cracking temperature is 920°C and the thermal cracking time is 2 hours.

[0121] The thermal cracking temperature is 860°C and the thermal cracking time is 3 hours.

[0122] In some embodiments, before thermally cracking the gallium oxyhydroxide powder, the method further comprises:

[0123] The gallium oxyhydroxide powder is washed and dried; the drying temperature is 80 to 120° C., and the drying time is 4 to 10 hours.

[0124] Washing: Impurities are removed from the reaction product through filtration and washing. Drying: Water is removed from the reaction product through heating. Impurities are removed from the reaction product through filtration and washing, improving its purity. Water is removed from the reaction product through heating, ensuring its dryness. Generally speaking, more washes improve impurity removal and product purity. For example, three washes yield a modest improvement in product purity, while ten washes significantly improve product purity and reduce impurity levels. Within the drying temperature range of 80-120°C, higher drying temperatures enhance moisture removal and result in higher product dryness. For example, a drying temperature of 80°C yields a modest improvement in product dryness, while a drying temperature of 120°C significantly improves product dryness and improves product quality. Within the drying time range of 4-10 hours, longer drying times increase product dryness. For example, a drying time of 4 hours yields a modest improvement in product dryness, while a drying time of 10 hours significantly improves product dryness and improves product quality.

[0125] Exemplary:

[0126] The drying temperature was 100°C and the drying time was 6 hours.

[0127] The drying temperature was 120°C and the drying time was 4 hours.

[0128] The drying temperature was 80°C and the drying time was 10 hours.

[0129] The drying temperature was 110°C and the drying time was 5 hours.

[0130] The drying temperature was 90°C and the drying time was 8 hours.

[0131] The drying temperature was 105°C and the drying time was 7 hours.

[0132] The drying temperature was 115°C and the drying time was 5 hours.

[0133] The drying temperature was 95°C and the drying time was 9 hours.

[0134] The drying temperature was 108°C and the drying time was 6 hours.

[0135] The drying temperature was 118°C and the drying time was 4.5 hours.

[0136] The present application will be further described below in conjunction with specific examples. It should be understood that these examples are intended to illustrate the present application only and are not intended to limit the scope of the present application. The experimental methods in the following examples where specific conditions are not specified are generally measured according to industry standards. If there are no corresponding industry standards, then the methods are carried out according to general international standards, conventional conditions, or the conditions recommended by the manufacturer.

[0137] Example 1

[0138] The method of this embodiment for improving the reaction rate of preparing high-purity gallium oxide by a hydrothermal method using metallic gallium specifically comprises the following steps:

[0139] Gallium metal was added into a high-pressure reactor filled with ultrapure water at a liquid-to-solid ratio of 20:1;

[0140] Add hydrogen peroxide (H2O2) to the autoclave at a molar ratio of 0.05:1 to gallium metal. Cover the autoclave with a stirring rod and an ultrasonic vibration probe, and tighten the autoclave.

[0141] Adjust the initial pressure inside the reactor to 2 MPa, start the hydrothermal reactor, set the speed to 1200 r / min, and the power of the ultrasonic vibration probe to 500 W. React at 170°C for 8 hours, so that the metallic gallium and high-purity water react rapidly under the synergistic effect of high pressure, ultrasonic vibration, and hydrogen peroxide to convert into gallium oxyhydroxide powder.

[0142] After the reaction is completed, the reactor is cooled to room temperature, and the powder obtained by the reaction is filtered and washed 3-10 times, and then dried at 100° C. for 10 hours to obtain gallium oxyhydroxide powder;

[0143] The prepared gallium oxyhydroxide powder was placed in a porcelain boat under a nitrogen atmosphere and thermally cracked at 750° C. in a tube furnace for 4 hours to obtain high-purity gallium oxide powder.

[0144] The gallium oxide powder obtained by the treatment method of this embodiment was weighed and analyzed by glow discharge mass spectrometry (GD-MS). The results showed that the purity of the gallium oxide powder was 99.99911%, and the conversion rate of metallic gallium was 92.85%.

[0145] Example 2

[0146] The method of this embodiment for improving the reaction rate of preparing high-purity gallium oxide by a hydrothermal method using metallic gallium specifically comprises the following steps:

[0147] Gallium metal was added into a high-pressure reactor filled with ultrapure water at a liquid-to-solid ratio of 4:1;

[0148] Add hydrogen peroxide (H2O2) to the autoclave at a molar ratio of 0.1:1 to gallium metal. Cover the autoclave with a stirring rod and an ultrasonic vibration probe, and tighten the autoclave.

[0149] Adjust the initial pressure inside the reactor to 4 MPa, start the hydrothermal reactor, set the speed to 1200 r / min, and the power of the ultrasonic vibration probe to 1000 W. React at 220°C for 3 hours. Under the synergistic effect of high pressure, ultrasonic vibration, and hydrogen peroxide, the metallic gallium and high-purity water react rapidly and transform into gallium oxyhydroxide powder.

[0150] After the reaction is completed, the reactor is cooled to room temperature, and the powder obtained by the reaction is filtered and washed 3-10 times, and then dried at 110° C. for 6 hours to obtain gallium oxyhydroxide powder;

[0151] The prepared gallium oxyhydroxide powder was placed in a porcelain boat under a nitrogen atmosphere and thermally cracked at 800° C. in a tube furnace for 2 hours to obtain high-purity gallium oxide powder.

[0152] The gallium oxide powder obtained by the treatment method of this embodiment was weighed and analyzed by glow discharge mass spectrometry (GD-MS). The results showed that the purity of the gallium oxide powder was 99.99954%, and the conversion rate of metallic gallium was 99.99%.

[0153] Example 3

[0154] The method of this embodiment for improving the reaction rate of preparing high-purity gallium oxide by a hydrothermal method using metallic gallium specifically comprises the following steps:

[0155] Gallium metal was added into a high-pressure reactor filled with ultrapure water at a liquid-to-solid ratio of 4:1;

[0156] Add hydrogen peroxide (H2O2) to the autoclave at a molar ratio of 0.1:1 to gallium metal. Cover the autoclave with a stirring rod and an ultrasonic vibration probe, and tighten the autoclave.

[0157] Adjust the initial pressure inside the reactor to 6 MPa, start the hydrothermal reactor, set the speed to 1200 r / min, and the power of the ultrasonic vibration probe to 800 W. React at 190°C for 3 hours. Under the synergistic effect of high pressure, ultrasonic vibration, and hydrogen peroxide, the metallic gallium and high-purity water react rapidly and transform into gallium oxyhydroxide powder.

[0158] After the reaction is completed, the reactor is cooled to room temperature, and the powder obtained by the reaction is filtered and washed 3-10 times, and then dried at 110° C. for 6 hours to obtain gallium oxyhydroxide powder;

[0159] The prepared gallium oxyhydroxide powder was placed in a porcelain boat under a nitrogen atmosphere and thermally cracked at 850° C. in a tube furnace for 2 hours to obtain high-purity gallium oxide powder.

[0160] The gallium oxide powder obtained by the treatment method of this embodiment was weighed and analyzed by glow discharge mass spectrometry (GD-MS). The results showed that the purity of the gallium oxide powder was 99.99932%, and the conversion rate of metallic gallium was 99.95%.

[0161] Example 4

[0162] The method of this embodiment for improving the reaction rate of preparing high-purity gallium oxide by a hydrothermal method using metallic gallium specifically comprises the following steps:

[0163] Gallium metal was added into a high-pressure reactor filled with ultrapure water at a liquid-to-solid ratio of 10:1;

[0164] Add hydrogen peroxide (H2O2) to the autoclave at a molar ratio of 0.15:1 to gallium metal. Cover the autoclave with a stirring rod and an ultrasonic vibration probe, and tighten the autoclave.

[0165] Adjust the initial pressure inside the reactor to 4 MPa, start the hydrothermal reactor, set the speed to 1200 r / min, and the power of the ultrasonic vibration probe to 800 W. React at 200°C for 3 hours. Under the synergistic effect of high pressure, ultrasonic vibration, and hydrogen peroxide, the metallic gallium and high-purity water react rapidly and transform into gallium oxyhydroxide powder.

[0166] After the reaction is completed, the reactor is cooled to room temperature, and the powder obtained by the reaction is filtered and washed 3-10 times, and then dried at 110° C. for 6 hours to obtain gallium oxyhydroxide powder;

[0167] The prepared gallium oxyhydroxide powder was placed in a porcelain boat under a nitrogen atmosphere and thermally cracked at 900° C. in a tube furnace for 2 hours to obtain high-purity gallium oxide powder.

[0168] The gallium oxide powder obtained by the treatment method of this embodiment was weighed and analyzed by glow discharge mass spectrometry (GD-MS). The results showed that the purity of the gallium oxide powder was 99.99949%, and the conversion rate of metallic gallium was 99.78%.

[0169] Example 5

[0170] The method of this embodiment for improving the reaction rate of preparing high-purity gallium oxide by a hydrothermal method using metallic gallium specifically comprises the following steps:

[0171] Gallium metal was added into a high-pressure reactor filled with ultrapure water at a liquid-to-solid ratio of 10:1;

[0172] Add hydrogen peroxide (H2O2) to the autoclave at a molar ratio of 0.2:1 to gallium metal. Cover the autoclave with a stirring rod and an ultrasonic vibration probe, and tighten the autoclave.

[0173] Adjust the initial pressure inside the reactor to 4 MPa, start the hydrothermal reactor, set the speed to 1200 r / min, and the power of the ultrasonic vibration probe to 500 W. React at 220°C for 6 hours. Under the synergistic effect of high pressure, ultrasonic vibration, and hydrogen peroxide, the metallic gallium and high-purity water react rapidly and transform into gallium oxyhydroxide powder.

[0174] After the reaction is completed, the reactor is cooled to room temperature, and the powder obtained by the reaction is filtered and washed 3-10 times, and then dried at 110° C. for 6 hours to obtain gallium oxyhydroxide powder;

[0175] The prepared gallium oxyhydroxide powder was placed in a porcelain boat under a nitrogen atmosphere and thermally cracked at 800° C. in a tube furnace for 2 hours to obtain high-purity gallium oxide powder.

[0176] The gallium oxide powder obtained by the treatment method of this embodiment was weighed and analyzed by glow discharge mass spectrometry (GD-MS). The results showed that the purity of the gallium oxide powder was 99.99930%, and the conversion rate of metallic gallium was 99.89%.

[0177] Comparative Example 1

[0178] The implementation method of high-purity gallium oxide in this comparative example is the same as that in Example 2, except that no hydrogen peroxide is added.

[0179] Using the treatment method of this comparative example, the reaction product contained incompletely reacted metallic gallium particles. The obtained gallium oxide powder was weighed and analyzed by glow discharge mass spectrometry (GD-MS). The results showed that the purity of the gallium oxide powder was 99.9923%, and the conversion rate of metallic gallium was 86.37%.

[0180] Comparative Example 2

[0181] The implementation method of high-purity gallium oxide in this comparative example is the same as that in Example 2, except that ultrasonic vibration is not turned on.

[0182] Using the treatment method of this comparative example, the reaction product contained incompletely reacted metallic gallium particles. The obtained gallium oxide powder was weighed and analyzed by glow discharge mass spectrometry (GD-MS). The results showed that the purity of the gallium oxide powder was 99.9940%, and the conversion rate of metallic gallium was 75.23%.

[0183] Comparative Example 3

[0184] The implementation method of high-purity gallium oxide in this comparative example is the same as that in Example 2, except that the initial pressure inside the reactor is not changed.

[0185] Using the treatment method of this comparative example, the reaction product contained incompletely reacted metallic gallium particles. The obtained gallium oxide powder was weighed and analyzed by glow discharge mass spectrometry (GD-MS). The results showed that the purity of the gallium oxide powder was 99.9953%, and the conversion rate of metallic gallium was 72.65%.

[0186] The gallium oxide powder purity and metal gallium conversion rate were tested on Examples 1 to 5 and Comparative Examples 1 to 3. The results are shown in Table 1.

[0187] Table 1

[0188]

[0189]

[0190] The above experimental data effect table can intuitively compare the differences between different embodiments and comparative examples. The specific analysis is as follows:

[0191] Example 1: A low molar ratio of hydrogen peroxide (0.05:1), a low initial pressure (2 MPa), and a low ultrasonic power (500 W) still significantly improved the reaction rate and product purity. The conversion of metallic gallium reached 92.85%, demonstrating that even under relatively low reaction conditions, the addition of hydrogen peroxide and the use of an ultrasonic field can effectively promote the reaction.

[0192] Example 2: A moderate molar ratio of hydrogen peroxide (0.1:1), a moderate initial pressure (4 MPa), and a high ultrasonic power (1000 W) further improved the reaction rate and product purity. The conversion of metallic gallium reached 99.99%, indicating that under the optimized conditions, the reaction proceeded almost completely and the product was extremely pure.

[0193] Example 3: A moderate molar ratio of hydrogen peroxide (0.1:1), a higher initial pressure (6 MPa), and a moderate ultrasonic power (800 W) also achieved high conversion and high purity. The conversion of metallic gallium reached 99.95%, indicating that increasing the initial pressure can further improve the reaction efficiency.

[0194] Example 4: A higher molar ratio of hydrogen peroxide (0.15:1), a higher initial pressure (6 MPa), and a moderate ultrasonic power (800 W) further improved the reaction rate and product purity. The conversion of metallic gallium reached 99.78%, demonstrating that increasing the molar ratio of hydrogen peroxide can further improve the reaction efficiency, but the conversion rate was slightly lower than that of Example 2.

[0195] Example 5: A higher molar ratio of hydrogen peroxide (0.2:1), a moderate initial pressure (4 MPa), and a lower ultrasonic power (500 W) further improved the reaction rate and product purity. The conversion of metallic gallium reached 99.89%, demonstrating that further increasing the molar ratio of hydrogen peroxide can improve reaction efficiency, but the conversion rate was slightly lower than that of Example 2.

[0196] Comparative Example 1: No hydrogen peroxide was added. Even at a higher initial pressure (4 MPa) and a higher ultrasonic power (1000 W), the conversion rate of metallic gallium was only 86.37%, indicating the important role of hydrogen peroxide in promoting the reaction.

[0197] Comparative Example 2: Ultrasonic vibration was not turned on. Even at a medium molar ratio of hydrogen peroxide (0.1:1) and a medium initial pressure (4 MPa), the conversion rate of metallic gallium was only 75.23%, indicating the important role of the ultrasonic field in promoting the reaction.

[0198] Comparative Example 3: The initial pressure was not adjusted. Even at a medium molar ratio of hydrogen peroxide (0.1:1) and a high ultrasonic power (1000 W), the conversion rate of metallic gallium was only 72.65%, indicating the important role of the initial pressure in promoting the reaction.

[0199] The foregoing is merely a list of specific embodiments of the present application, intended to enable those skilled in the art to understand or implement the present application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application is not limited to the embodiments shown herein, but is intended to conform to the broadest scope consistent with the principles and novel features of the present application.

Claims

1. A method for increasing the reaction rate of preparing gallium oxide from metallic gallium, comprising: mixing metallic gallium with water to form a reaction mixture; adding a promoter to the reaction mixture; Under the action of an external physical field, the reaction mixture containing the promoter undergoes a chemical reaction to generate gallium oxyhydroxide powder; The gallium oxyhydroxide powder is thermally cracked in an inert gas to obtain gallium oxide powder.

2. The method according to claim 1, characterized in that The promoter includes at least one of the following: an oxidant and a catalyst.

3. The method according to claim 2, characterized in that The oxidant comprises at least one of the following: hydrogen peroxide, peroxide, ozone, chlorate, and permanganate; The catalyst includes at least one of the following: a metal catalyst and a non-metal catalyst.

4. The method according to claim 1, wherein The external physical field includes at least one of the following: an ultrasonic field, a pressure field, a magnetic field, and an electric field.

5. The method according to claim 4, characterized in that The power of the ultrasonic field is 500-1000W, and the initial pressure of the pressure field is 2-6MPa.

6. The method according to claim 1, characterized in that The parameters of the chemical reaction include at least one of the following: a reaction temperature of 160 to 220° C., a reaction time of 2 to 10 hours, a reaction pressure of 2 to 6 MPa, and a reaction stirring speed of 800 to 1200 r / min.

7. The method according to claim 1, characterized in that The liquid-to-solid ratio of the metal gallium to the water is (4-20):

1.

8. The method according to claim 1, characterized in that The purity of the metallic gallium is not less than 6N; The purity of the gallium oxide powder is not less than 5N.

9. The method according to claim 1, characterized in that The temperature of the thermal cracking is 700 to 950° C., and the time of the thermal cracking is 2 to 4 hours.

10. The method according to claim 1, characterized in that Before thermally cracking the gallium oxyhydroxide powder, the method further comprises: The gallium oxyhydroxide powder is washed and dried; the drying temperature is 80 to 120° C., and the drying time is 4 to 10 hours.

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