Aluminum zinc oxide target and method for producing the same

Abstract

The application belongs to the technical field of new materials, and discloses a preparation method of an aluminum zinc oxide target material. Molten aluminum and zinc mixed metal liquid and inert gas are mixed and prepared into a spray, the spray is mixed with oxygen to perform an oxidation reaction, and an aluminum zinc oxide powder is prepared. The aluminum zinc oxide target material is prepared by using the aluminum zinc oxide powder. The method uses a molten metal liquid spray oxidation method to prepare the aluminum zinc oxide powder. The related production equipment only needs one-time investment and can be used for a long time. No additional expensive reagent is needed, and the production cost is low and the process is simple.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of new materials, in particular to an aluminum zinc oxide target material and a preparation method thereof. BACKGROUND

[0002] Transparent conductive oxide as an important optoelectronic information material, has been widely used in the fields of light emitting devices, thin film solar cells, surface acoustic wave devices, sensors, flat panel liquid crystal displays and infrared reflectors. At present, the most widely used is indium tin oxide (ITO), however, In is a scarce resource, expensive and toxic, so it is urgent to find a material to replace ITO. The transparent conductive aluminum zinc oxide film has excellent infrared reflection characteristics in the infrared region, and the metal aluminum zinc is widely available and low in price, and has better stability than ITO in H plasma, and has broad application prospects in the fields of thin film solar cells, flat panel displays, infrared reflective window films and heat reflectors. At present, China advocates energy saving and emission reduction, and aluminum zinc oxide coated glass has excellent infrared reflection performance, which can reduce a large part of energy loss when used on building glass, thereby achieving the purpose of energy saving. Therefore, it is of great significance to carry out research on transparent high-conductive near-infrared reflective aluminum zinc oxide film;

[0003] TW201925094A discloses a silver-doped aluminum zinc oxide composite target material and a preparation method thereof, which adopts a precipitation method to prepare a precursor, and then sintering to form an aluminum zinc oxide nano target material.

[0004] CN118561591A discloses a zinc tin oxide target material and a preparation method thereof, which also adopts a precipitation method to prepare a precursor, and then sintering to form an aluminum zinc oxide target material.

[0005] The above-mentioned process using the precipitation method has the following problems: the process is relatively complex, a precipitating agent and operations such as precipitation and washing are required, the process is relatively complex, and the production cost is relatively large.

[0006] The technical problem solved by the present application is how to further reduce the preparation difficulty of the aluminum zinc oxide target material while ensuring its ultra-low resistivity. SUMMARY

[0007] The purpose of the present application is to provide a preparation method of an aluminum zinc oxide target material, which adopts a molten metal liquid spray oxidation method to prepare an aluminum zinc oxide powder, and the related production equipment only needs one-time investment and can be used for a long time without additional expensive reagents, so that the production cost is low and the process is simple.

[0008] Meanwhile, the present application also provides an aluminum zinc oxide target material prepared based on the method.

[0009] To achieve the above-mentioned purpose, the present application discloses:

[0010] A preparation method of an aluminum zinc oxide target, a molten aluminum zinc mixed metal liquid and an inert gas are mixed and prepared into a spray, the spray is mixed with oxygen to perform an oxidation reaction to prepare an aluminum zinc oxide powder; and the aluminum zinc oxide target is prepared using the aluminum zinc oxide powder.

[0011] In the prior art, the spray oxidation method is generally suitable for light metals such as potassium and sodium; for example, a method for preparing super-potassium superoxide powder by a spray oxidation method of metal potassium, with the publication number CN107879361A and the invention name of a method for preparing super-potassium superoxide powder by a spray oxidation method of metal potassium, uses the spray oxidation method to prepare super-potassium superoxide; and the mixing of the metal liquid and air is realized by an inner and outer nested spray pipe.

[0012] In the research of the present application, it is found that when the melt with zinc as the main material is sprayed to prepare an oxide, the following problems exist: 1. the nozzle is blocked, and the pre-mixed oxygen-containing gas causes part of the metal to be oxidized in advance, especially the precipitate generated after the reaction of aluminum and oxygen is easy to float on the metal liquid and accumulate at the nozzle position, accelerating the blocking condition; 2. compared with potassium, the density of zinc is more than 8 times that of potassium, and it is difficult to form a relatively uniform spray with the high-density metal liquid; and uniform spray is a prerequisite for full oxidation.

[0013] Through research, the present application mixes an inert gas into the melt before forming the spray and reacting with oxygen, disperses bubbles in the metal melt, reduces the density of the metal liquid, so that the metal liquid can contact with oxygen in the form of small droplets when forming the spray, improves the oxidation effect, and does not form oxide blocking material at the nozzle position.

[0014] In the above preparation method, the weight ratio of aluminum to zinc in the metal liquid is 0.5-2:98-99.5.

[0015] The weight ratio of aluminum to zinc is required by the target material of the present application, and in actual production, the ratio of aluminum to zinc can be flexibly adjusted according to the composition requirements of the target material.

[0016] As a further extension of the present application, the oxidation of other heavier metal elements can also use the technical solution of the present application, and the amount of inert gas added to the spray melt is flexibly adjusted according to the density of the metal element to make the final spray density reach the expected target, forming a relatively dispersed and small droplet spray.

[0017] In the above preparation method, the melting temperature of the metal liquid is 900-1100 DEG C.

[0018] In the present application, the melting point of zinc is 419 DEG C, the melting point of aluminum is 660 DEG C, the present application controls the melting temperature of the metal liquid in the range of 300-500 DEG C higher than the melting point of aluminum, which can ensure that the temperature of the metal liquid is high enough, on the one hand, it can balance the temperature reduction caused by the heat absorption of inert gas; on the other hand, it can make the spray exist in the molten state in the oxidation chamber for more time, avoid rapid solidification, and improve the oxidation effect.

[0019] In the preparation method, the volume ratio of the metal liquid to the inert gas is 1:1-2.

[0020] In the present application, the volume of the inert gas refers to the volume under standard conditions (standard atmospheric pressure, 298K temperature); when the temperature is increased to 1100 DEG C, the volume will be increased by 4 times, which can reduce the density of the mixture formed by the metal liquid and the inert gas to 10-20% of the density of the metal liquid, and improve the atomization effect of the spray.

[0021] In some embodiments of the present application, the volume ratio of the metal liquid to the inert gas is 1:1, 1:1.5, 1:2.

[0022] In the preparation method, the spray speed of the mixture formed by the metal liquid and the inert gas is 18-22 ml / min; the flow rate of oxygen is 40 L / min-50 L / min.

[0023] In the preparation method, the oxidation reaction is carried out in the oxidation chamber, and the oxygen is injected into the oxidation chamber.

[0024] In the preparation method, the method for preparing the aluminum zinc oxide target material from the aluminum zinc oxide powder is:

[0025] The aluminum zinc oxide powder is formed, cold isostatic pressed, and sintered, so that the aluminum zinc oxide target material is obtained, wherein the sintering temperature is 1280 DEG C-1350 DEG C.

[0026] Meanwhile, the present application also discloses an aluminum zinc oxide target material, which is prepared by the method.

[0027] The present application has at least the following beneficial effects:

[0028] The present application adopts the method of molten metal liquid spray oxidation to prepare the aluminum zinc oxide powder, the related production equipment only needs one-time investment and can be used for a long time, without additional expensive reagents, and the production cost is low and the process is simple.

[0029] The process of the present application has the following process points:

[0030] 1. In the melting stage, nitrogen and metal liquid are mixed to avoid early oxidation of the metal liquid and block the spray pipeline;

[0031] 2. In the oxidation stage, the ratio of the molten metal and the inert gas needs to be controlled so that the molten metal is spread in the form of spray to facilitate the full progress of the oxidation reaction. DETAILED DESCRIPTION

[0032] The present application will be described in detail below with reference to the embodiments of the present application. In the description of the present application, it should be noted that the specific conditions not mentioned in the embodiments are conducted according to the conventional conditions or the conditions recommended by the manufacturers. The reagents or instruments not mentioned by the manufacturers are the conventional products that can be purchased in the market.

[0033] Example 1

[0034] (1) 0.26 kg of aluminum ingot and 39.74 kg of zinc ingot were added into a nitrogen gas melting chamber and heated to 900°C, and then the aluminum ingot and the zinc ingot were melted and mixed thoroughly;

[0035] (2) The mixed molten aluminum-zinc liquid was mixed with high-pressure nitrogen gas to form a gas-liquid mixture, and the gas-liquid mixture was flowed into an oxidation chamber at 850°C at a rate of 20 ml / min; the volume ratio of the molten aluminum-zinc liquid to the high-pressure nitrogen gas was prepared according to the nitrogen gas volume ratio under the conditions of 1 atmosphere and 298K; the nitrogen gas volume ratio under the conditions of 1 atmosphere and 298K was 1:1.5; and the pressure of the high-pressure nitrogen gas was 3 atmospheres;

[0036] (3) The gas-liquid mixture flowed into the oxidation chamber was scattered in the form of spray, and oxygen was introduced into the oxidation chamber at a rate of 40 L / min;

[0037] (4) The oxidized oxide powder was collected and cooled to room temperature to obtain an aluminum zinc oxide powder with a powder particle size D90 of 0.259 μm;

[0038] (5) The aluminum zinc oxide powder obtained in step (4) was subjected to hydraulic forming, cold isostatic pressing, and sintering at 1280°C to obtain an aluminum zinc oxide target material with a relative density of 99.1% and an electrical resistivity of 1.76 mΩ.cm.

[0039] Example 2

[0040] (1) 0.53 kg of aluminum ingot and 39.47 kg of zinc ingot were added into a nitrogen gas melting chamber and heated to 1000°C, and then the aluminum ingot and the zinc ingot were melted and mixed thoroughly;

[0041] (2) The mixed molten aluminum-zinc liquid is mixed with high-pressure nitrogen gas to form a gas-liquid mixture, and the gas-liquid mixture is flowed into an oxidation chamber at 900°C at a rate of 20 ml / min; the volume ratio of the molten aluminum-zinc liquid to nitrogen gas under the conditions of 1 atmosphere and 298K is 1:1; the pressure of the high-pressure nitrogen gas is 5 atmospheres;

[0042] (3) The gas-liquid mixture flowed into the oxidation chamber is dispersed in a jet shape, and oxygen gas is introduced into the oxidation chamber at a rate of 45 L / min;

[0043] (4) The oxidized oxide powder is collected and cooled to room temperature to obtain an aluminum-zinc oxide powder with a powder particle size D90 of 0.245 μm;

[0044] (5) The aluminum-zinc oxide powder obtained in step (4) is subjected to hydraulic forming, cold isostatic pressing, and sintering at 1320°C to obtain an aluminum-zinc oxide target material with a relative density of 99.3% and an electrical resistivity of 0.57 mΩ.cm.

[0045] Example 3

[0046] (1) 0.80 kg of aluminum ingot and 39.20 kg of zinc ingot are added to a nitrogen gas melting chamber and heated to 1100°C, and the aluminum ingot and the zinc ingot are melted and mixed thoroughly;

[0047] (2) The mixed molten aluminum-zinc liquid is mixed with high-pressure nitrogen gas to form a gas-liquid mixture, and the gas-liquid mixture is flowed into an oxidation chamber at 950°C at a rate of 20 ml / min; the volume ratio of the molten aluminum-zinc liquid to nitrogen gas under the conditions of 1 atmosphere and 298K is 1:2; the pressure of the high-pressure nitrogen gas is 4 atmospheres;

[0048] (3) The gas-liquid mixture flowed into the oxidation chamber is dispersed in a jet shape, and oxygen gas is introduced into the oxidation chamber at a rate of 50 L / min;

[0049] (4) The oxidized oxide powder is collected and cooled to room temperature to obtain an aluminum-zinc oxide powder with a powder particle size D90 of 0.288 μm;

[0050] (5) The aluminum-zinc oxide powder obtained in step (4) is subjected to hydraulic forming, cold isostatic pressing, and sintering at 1350°C to obtain an aluminum-zinc oxide target material with a relative density of 99.1% and an electrical resistivity of 1.92 mΩ.cm.

[0051] Example 4

[0052] The procedure of Example 3 is substantially the same, except that in step (1), the temperature for heating and melting is 800°C.

[0053] Comparative Example 1

[0054] (1) 0.26 kg of aluminum ingot and 39.74 kg of zinc ingot were added to an oxygen melting chamber and heated to 900°C, and after the aluminum ingot and the zinc ingot were melted, they were mixed thoroughly;

[0055] (2) The mixed molten aluminum-zinc liquid was mixed with high-pressure oxygen, and then flowed into an oxidation chamber at 850°C at a rate of 20 ml / min; the amount of oxygen was the same as the amount of nitrogen in Example 1;

[0056] (3) The gas-liquid mixture flowing into the oxidation chamber was dispersed in a jet shape, and oxygen was introduced into the oxidation chamber at a rate of 40 L / min;

[0057] (4) The oxidized oxide powder was collected and cooled to room temperature to obtain an aluminum zinc oxide powder having a powder particle size D90 of 383.4 μm;

[0058] (5) The aluminum zinc oxide powder obtained in step (4) was subjected to hydraulic forming, cold isostatic pressing, and sintering at 1280°C to obtain an aluminum zinc oxide target material having a relative density of 97.2% and an electrical resistivity of 4.25 mΩ.cm;

[0059] During production, the nozzle was often blocked and needed to be cleaned, resulting in downtime.

[0060] Comparative Example 2

[0061] (1) 0.53 kg of aluminum ingot and 39.47 kg of zinc ingot were added to a nitrogen melting chamber and heated to 1000°C, and after the aluminum ingot and the zinc ingot were melted, they were mixed thoroughly;

[0062] (2) The mixed molten aluminum-zinc liquid was mixed with high-pressure nitrogen, and then flowed into an oxidation chamber at 900°C at a rate of 20 ml / min; the amount of nitrogen was the same as the amount of nitrogen in Example 2;

[0063] (3) The gas-liquid mixture flowing into the oxidation chamber was dispersed in a jet shape, and oxygen was introduced into the oxidation chamber at a rate of 10 L / min;

[0064] (4) The oxidized oxide powder was collected and cooled to room temperature to obtain a mixed powder of aluminum zinc oxide and aluminum zinc alloy, which did not meet the requirements.

[0065] Performance Test

[0066] The test items included relative density and electrical resistivity.

[0067] The test method for relative density was: relative density = density (drainage method) / true density (immersion method)

[0068] The test method for electrical resistivity was: four-probe method

[0069] The test results are shown in Table 1 below;

[0070] Table 1 test results

[0071] Case Relative density (%) Resistivity (mΩ.cm) Example 1 99.1 1.76 Example 2 99.3 0.57 Example 3 99.1 1.92 Example 4 98.2 8.48 Comparative Example 1 97.2 4.25 Comparative Example 2 / /

[0072] Result analysis:

[0073] 1. From Examples 1 to 3, it can be seen that by reasonably controlling the use of nitrogen and using the method of spray oxidation, the relative density can be effectively improved and the resistivity can be reduced.

[0074] 2. From Example 3 and Example 4, it can be seen that the temperature of the melt is relatively important. When the melt temperature is low, the temperature decreases rapidly when mixed with nitrogen, and after spraying, it cannot exist in liquid state for a long time for oxidation, and will quickly solidify. At the same time, the decrease of temperature can also make the oxide layer float on the surface of the droplet, reducing the reaction degree of oxygen and metal liquid.

[0075] 3. From Example 1 and Comparative Example 1, it can be seen that the use of inert gas can avoid nozzle blockage on the one hand, and can effectively control the particle size of the oxide powder on the other hand. The possible reason for the increase of the particle size of the oxide powder is that the oxygen is consumed in advance to form the oxide, and the spray fineness is not enough, resulting in the increase of the particle size.

[0076] 4. From Example 2 and Comparative Example 2, it can be seen that sufficient oxygen supply is the key to prepare qualified products.

[0077] It is apparent to those skilled in the art that the present application is not limited to the details of the foregoing exemplary embodiments, and that the present application can be implemented in other specific forms without departing from the spirit or essential characteristics of the present application. Therefore, the embodiments should be considered in all respects as illustrative and not restrictive, and the scope of the present application should be defined by the appended claims rather than the above description, and it is intended to include all changes falling within the meaning and scope of equivalents of the claims.

Claims

1. A method of producing an aluminum zinc oxide target material, characterized by, The molten aluminum-zinc mixed metal liquid and inert gas are mixed and prepared into a spray, the spray is mixed with oxygen to perform an oxidation reaction, and an aluminum zinc oxide powder is prepared; and an aluminum zinc oxide target is prepared by using the aluminum zinc oxide powder. The weight ratio of aluminum to zinc in the metal liquid is 0.5-2:98-99.

5. The melting temperature of the metal liquid is 900-1100 DEG C. The volume ratio of the metal liquid to inert gas is 1:1-2. The spray speed of the mixture of the metal liquid and inert gas is 18-22 mL / min, and the flow rate of oxygen is 40 L / min-50 L / min.

2. The production method according to claim 1, characterized by, The oxidation reaction is performed in an oxidation chamber, and the oxygen is injected into the oxidation chamber.

3. The preparation method according to claim 1, characterized in that, The method for preparing the aluminum zinc oxide target by using the aluminum zinc oxide powder is as follows: The aluminum zinc oxide powder is formed, cold isostatic pressed, and sintered, and the aluminum zinc oxide target is obtained, wherein the sintering temperature is 1280 DEG C-1350 DEG C.