Preparation method of high-activity IGZO powder

Abstract

The invention discloses a preparation method of high-activity IGZO powder. The preparation method comprises the following steps: S1, mixing indium salt, zinc salt, gallium salt and deionized water to form a mixed solution; s2, adding organic phosphonate into the mixed solution prepared in the step S1, and stirring; s3, dropwise adding diluted ammonia water, and adjusting the pH value of the solution to 7.5-8.5 to obtain a reaction solution; s4, putting the reaction solution into a reaction kettle, and reacting at 110 DEG C for 8-10 hours; and S5, after the reaction is finished, filtering, washing, drying and roasting to obtain IGZO powder. Compared with the prior art, the preparation method of the high-activity IGZO powder has the advantages that the process is simple, and the IGZO powder with moderate particle size, large specific surface area, high activity and uniform components can be prepared.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of IGZO powder preparation, in particular to a preparation method of high-activity IGZO powder. BACKGROUND

[0002] The amorphous IGZO (indium gallium zinc oxide) thin film is one of the best materials in known oxide semiconductor thin films, has high electron mobility, high light transmittance and other characteristics, and can replace traditional silicon-based thin film transistors to become next-generation technology-driven devices.

[0003] In the prior art, the preparation method of the IGZO powder is mainly solid-state reaction. The solid-state reaction method mainly comprises the following steps: mixing three kinds of pure oxides, uniformly crushing, and then sintering at high temperature to obtain an IGZO target material.

[0004] However, although the method is simple, the current mechanical grinding capacity is limited, so that the three kinds of powders are not uniformly mixed, and the density of the target material is not uniform, and the target material cannot be further used.

[0005] Therefore, it is necessary to explore an IGZO powder preparation method which has low process control difficulty and high uniformity and stability of the prepared product. SUMMARY

[0006] The technical problem to be solved by the application is to overcome the above technical defects, and to provide a preparation method of high-activity IGZO powder which has moderate particle size, large specific surface area, high activity and uniform composition.

[0007] To solve the above technical problems, the technical scheme provided by the application is as follows: a preparation method of high-activity IGZO powder, comprising the following steps:

[0008] S1: mixing indium salt, zinc salt and gallium salt with deionized water to form a mixed solution;

[0009] S2: adding an organic phosphonate to the mixed solution prepared in S1 and stirring;

[0010] S3: adding diluted ammonia water dropwise to adjust the PH of the solution to 7.5-8.5 to obtain a reaction solution;

[0011] S4: placing the reaction solution in a reaction kettle and reacting at 110 DEG C for 8-10 hours;

[0012] S5: after the reaction is completed, filtering, washing with water, drying and calcining to obtain IGZO powder.

[0013] Preferably, the organic phosphonate is a combination of one or more of aminotri-methylene phosphonic acid, hydroxyethylidene diphosphonic acid or ethylenediamine tetra-methylene phosphonic acid.

[0014] Preferably, the indium salt is indium nitrate or indium chloride, the zinc salt is zinc nitrate or zinc acetate, and the gallium salt is gallium nitrate or gallium chloride.

[0015] The molar ratio of the indium salt, the zinc salt, and the gallium salt is 1:1:0.5-2.

[0016] Preferably, the dropping speed of the diluted ammonia water in S3 is 2.5 L / min, and the stirring speed is greater than or equal to 300 rpm when the solution PH is adjusted.

[0017] Preferably, the molar ratio of the organophosphonate to the metal ion in S2 is 0.8-1.5.

[0018] Preferably, an online PH monitor is used in S3 for real-time monitoring.

[0019] Preferably, the average particle size of the IGZO powder in S5 is 4 μm, and the specific surface area is 15 m2 / g.

[0020] Preferably, the drying temperature in S5 is 60-80℃, and the drying time is 4-6 hours.

[0021] The calcination temperature is 800-1300℃, the calcination time is 2-5 hours, and the calcination atmosphere is inert gas.

[0022] Compared with the prior art, the present application has the following advantages: the present application uses an organophosphonate as a chelating agent, which can effectively solve the problem of inconsistent ion precipitation rates in the traditional coprecipitation method, thereby ensuring the uniformity of the IGZO powder composition, reducing the overall control difficulty, and improving the uniformity and stability of the prepared product, thereby facilitating industrialized production and popularization. BRIEF DESCRIPTION OF DRAWINGS

[0023] Figure 1 is a process flow diagram of the preparation method of the high-activity IGZO powder. DETAILED DESCRIPTION

[0024] The present application will be further described in detail below with reference to the accompanying drawings.

[0025] In combination with the accompanying Figure 1 As shown in the drawings, the preparation method of the high-activity IGZO powder comprises the following steps:

[0026] S1: mixing an indium salt, a zinc salt, and a gallium salt with deionized water to form a mixed solution;

[0027] S2: adding an organophosphonate to the mixed solution prepared in S1 and stirring;

[0028] S3: adding diluted ammonia water dropwise, adjusting the solution PH to 7.5-8.5 to obtain a reaction solution;

[0029] S4: The reaction solution is placed in a reaction kettle and reacted at 110°C for 8-10 hours;

[0030] S5: After the reaction, the IGZO powder is obtained by filtering, washing with water, drying and calcining.

[0031] Specifically, a certain amount of organic phosphonate is added to a mixed solution formed by mixing indium salt, zinc salt, gallium salt and deionized water (the ratio of organic phosphonate to metal ions is 0.8-1.5); after stirring uniformly, diluted ammonia water is added dropwise (ammonia water: water = 1:2, dropwise speed: 2.5L / min), the PH value of the mixed solution is adjusted to 7.5-8.5, the reaction solution is placed in a reaction kettle, heated to 110°C and reacted for 8-10h, and after the reaction is completed, the reaction solution is filtered, washed with water, dried, calcined and the like to obtain the target product. After detection, the average particle size of the target product is about 4um, and the specific surface area is about 15㎡ / g.

[0032] The organic phosphonate is a combination of one or more of aminotri(methylene) phosphonic acid, hydroxyethylidene diphosphonic acid or ethylenediamine tetra(methylene) phosphonic acid;

[0033] The indium salt is indium nitrate or indium chloride, the zinc salt is zinc nitrate or zinc acetate, and the gallium salt is gallium nitrate or gallium chloride;

[0034] The molar ratio of the indium salt, zinc salt and gallium salt is 1:1:0.5-2.

[0035] In S2, the molar ratio of the organic phosphonate to the metal ions is 0.8-1.5, in S3, the dropwise speed of the diluted ammonia water is 2.5L / min, the stirring speed is ≥300rpm when adjusting the PH of the solution, and an online PH monitor is used to monitor the PH in real time.

[0036] In S5, the average particle size of the IGZO powder is 4um, the specific surface area is 15㎡ / g, the drying temperature is 60-80°C, the drying time is 4-6 hours, the calcination temperature is 800-1300°C, the calcination time is 2-5 hours, and the calcination atmosphere is inert gas.

[0037] In one of the embodiments:

[0038] Indium nitrate, zinc nitrate and gallium nitrate are mixed according to a molar ratio of 1:1:0.5 with deionized water, stirred until completely dissolved to form a mixed solution; aminotri(methylene) phosphonic acid is added to the above mixed solution, wherein the molar ratio of aminotri(methylene) phosphonic acid to metal ions (indium ions, zinc ions and gallium ions) is 0.8, the mixed solution is stirred for 30 minutes, diluted ammonia water is added dropwise to the mixed solution at a dropwise speed of 2.5L / min, an online PH monitor is used to monitor the PH value of the solution in real time, the stirring speed is adjusted to 300rpm, and the PH value of the solution is adjusted to 7.5 to obtain a reaction solution;

[0039] The reaction solution was put into a reaction kettle and reacted at 110°C for 8 hours. After the reaction was completed, the product was filtered, washed with deionized water three times, then dried at 60°C for 4 hours, and finally calcined at 800°C under an inert gas (nitrogen) atmosphere for 2 hours to obtain an IGZO powder.

[0040] The contents not described in detail in the specification belong to the prior art known to those skilled in the art.

[0041] The scope of protection of the present application is defined by the appended claims and their equivalents, therefore, the following detailed description of the embodiments of the application provided in the drawings is not intended to limit the scope of the application claimed, but merely represents selected embodiments of the application.

[0042] All other embodiments obtained by those skilled in the art based on the embodiments of the present application without creative labor fall within the scope of protection of the present application.

[0043] It should be noted that similar reference numbers and letters represent similar items in the following drawings, therefore, once an item is defined in one drawing, it does not need to be further defined and explained in subsequent drawings.

[0044] The above describes the present application and its embodiments, which are not limited, and the embodiments shown in the drawings are only one of the embodiments of the present application, and the actual structure is not limited thereto. In general, if those skilled in the art are inspired by it, without departing from the purpose of the present application, without creative design, similar structure and embodiments of the technical solution should belong to the protection scope of the present application.

Claims

1. A method for preparing highly active IGZO powder, characterized in that: Includes the following steps: S1: Mix indium salt, zinc salt, gallium salt and deionized water to form a mixed solution; S2: Add organophosphonate to the mixed solution prepared in S1 and stir; S3: Add diluted ammonia water dropwise to adjust the pH of the solution to 7.5-8.5 to obtain the reaction solution; S4: Place the reaction solution into the reaction vessel and react at 110℃ for 8-10 hours; S5: After the reaction is completed, the product is filtered, washed with water, dried and calcined to obtain IGZO powder.

2. The method for preparing highly active IGZO powder according to claim 1, characterized in that: The organophosphonate is one or a combination of aminotrimethylenephosphonic acid, hydroxyethylidene diphosphonic acid, or ethylenediaminetetramethylenephosphonic acid.

3. The method for preparing highly active IGZO powder according to claim 1, characterized in that: The indium salt is indium nitrate or indium chloride, the zinc salt is zinc nitrate or zinc acetate, and the gallium salt is gallium nitrate or gallium chloride; The molar ratio of the indium salt, zinc salt, and gallium salt is 1:1:0.5 to 2.

4. The method for preparing highly active IGZO powder according to claim 1, characterized in that: The ammonia solution in S3 is added at a rate of 2.5 L / min, and the stirring rate is ≥300 rpm when adjusting the pH of the solution.

5. The method for preparing highly active IGZO powder according to claim 3, characterized in that: The molar ratio of organophosphonate to metal ions in S2 is 0.8-1.

5.

6. The method for preparing highly active IGZO powder according to claim 4, characterized in that: The S3 uses an online pH monitor for real-time monitoring.

7. The method for preparing highly active IGZO powder according to claim 1, characterized in that: The IGZO powder in S5 has an average particle size of 4 μm and a specific surface area of ​​15 m² / g.

8. The method for preparing highly active IGZO powder according to claim 1, characterized in that: The drying temperature in S5 is 60-80℃, and the drying time is 4-6 hours; The calcination temperature is 800-1300℃, the calcination time is 2-5 hours, and the calcination atmosphere is an inert gas.

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