阅读说明：本技术 一种制备ito粉末的工艺 (Process for preparing ITO powder ) 是由 唐安泰 于 2020-12-15 设计创作，主要内容包括：本发明公开了一种制备ITO粉末的工艺,所述ITO粉末原料为金属铟,金属铟与硝酸混合配制成硝酸铟,并与四氯化锡进行混合,随后进行沉淀制备工艺；所述制备工艺分为：添加沉淀剂和添加剂阶段、加热搅拌阶段、洗净过滤阶段、烘干研磨阶段和煅烧阶段,冲洗罐中通入去离子水,去离子水对氢氧化铟和氢氧化锡沉淀物进行冲洗,并且冲洗水通过循环管再次通入冲洗罐中,所述循环管中部加设过滤器,所述过滤器中配备有可拆卸式滤网,便于进行更换,所述煅烧操作采用分级煅烧,煅烧炉中采用分段式隔板,提高混合粉末的离散程度,加快混合粉末的煅烧速度。本发明可对冲洗水进行循环使用,降低水资源的浪费,并且采取震荡式煅烧,加快煅烧的速度。(The invention discloses a process for preparing ITO powder, wherein the raw material of the ITO powder is metal indium, the metal indium is mixed with nitric acid to prepare indium nitrate, the indium nitrate is mixed with stannic chloride, and then the precipitation preparation process is carried out; the preparation process comprises the following steps: adding a precipitator and an additive, heating and stirring, cleaning and filtering, drying and grinding and calcining, introducing deionized water into a washing tank, washing indium hydroxide and tin hydroxide precipitates by the deionized water, introducing the washing water into the washing tank again through a circulating pipe, additionally arranging a filter in the middle of the circulating pipe, wherein a detachable filter screen is arranged in the filter, so that the replacement is convenient, the calcination operation adopts fractional calcination, and a sectional type partition plate is adopted in a calcination furnace, so that the dispersion degree of mixed powder is improved, and the calcination speed of the mixed powder is accelerated. The invention can recycle the washing water, reduces the waste of water resources, and accelerates the calcining speed by adopting the oscillation type calcining.)

1. A process for preparing ITO powder is characterized in that: the ITO powder raw material is metal indium, the metal indium is mixed with nitric acid to prepare indium nitrate, the indium nitrate is mixed with stannic chloride, and then a precipitation preparation process is carried out;

the preparation process comprises the following steps: adding a precipitator and an additive, heating and stirring, cleaning and filtering, drying and grinding and calcining;

after the raw materials are prepared, adding a precipitator and an additive, wherein the precipitator is urea and the additive is ammonium sulfate; adding deionized water after the precipitant and the additive are added, and mixing to prepare indium tin salt aqueous solution;

adding the indium tin salt aqueous solution into a heating kettle, wherein an electric stirring rod is arranged in the heating kettle, and the heating kettle is heated after being electrified and drives the electric stirring rod to heat and stir the indium tin salt aqueous solution in the heating kettle;

after heating and stirring, urea is heated and uniformly decomposed to generate ammonia water, the ammonia water and an indium tin salt aqueous solution generate a chemical reaction to generate indium hydroxide and tin hydroxide, the indium hydroxide and the tin hydroxide are not dissolved in water, and a precipitate is generated;

in the cleaning and filtering stage, deionized water is adopted for washing, filtering is carried out, and impurities such as chloride ions, sulfate ions and the like are taken out to obtain a milky colloidal indium hydroxide and tin hydroxide mixture;

in the drying and grinding stage, the washed indium hydroxide and tin hydroxide are taken out and placed in a drying furnace, and the drying furnace dries the indium hydroxide and tin hydroxide precipitates;

in the calcination stage, indium hydroxide and tin hydroxide powder are placed in a calcination furnace for calcination, the calcination temperature is controlled at 600-1000 ℃, the temperature in the preheating stage is controlled at 500-600 ℃, the preheating is carried out for 1h, and then the high-temperature heating stage is carried out, and the temperature is raised to 800-1000 ℃.

2. The process of claim 1 for preparing an ITO powder, wherein: the temperature of the heating kettle for heating the indium tin salt aqueous solution is controlled between 70 ℃ and 100 ℃, the rotating speed of the electric stirring rod is 1000r/min, and the heating kettle and the electric stirring rod are controlled by independent controllers.

3. The process of claim 1 for preparing an ITO powder, wherein: the indium tin salt aqueous solution is heated and stirred and then is conveyed to a washing tank, meanwhile, the redundant indium tin salt aqueous solution is separated from indium hydroxide and tin hydroxide, and the indium hydroxide and the tin hydroxide are separated into the washing tank;

deionized water is introduced into the washing tank, indium hydroxide and tin hydroxide precipitates are washed by the deionized water, the washing water is introduced into the washing tank again through a circulating pipe, a filter is additionally arranged in the middle of the circulating pipe, and a detachable filter screen is arranged in the filter, so that the filter is convenient to replace;

the sparge water through the filter screen is filtered the back, and the sparge water lets in the washing jar once more, the washing jar is equipped with the puddler, washes indium hydroxide and tin hydroxide precipitate comprehensively, and the recycling of sparge water, the quantity of reducible deionized water, the circulating pipe upper end is connected with control valve and flowmeter, control washing speed and demonstration water flow.

4. The process of claim 1 for preparing an ITO powder, wherein: the drying temperature in the drying and grinding stage is controlled to be about 100 ℃; and after drying, removing water in the indium hydroxide and tin hydroxide precipitate, putting the indium hydroxide and tin hydroxide precipitate into a grinding machine, and grinding the indium hydroxide and tin hydroxide to obtain nano-scale indium hydroxide and tin hydroxide mixed powder.

5. The process of claim 1 for preparing an ITO powder, wherein: the calcination operation adopts staged calcination, a sectional type partition plate is adopted in the calcination furnace, a vibration motor is additionally arranged on the sectional type partition plate, the indium hydroxide and tin hydroxide mixed powder vibrates on the sectional type partition plate, and the calcination furnace uniformly calcines the mixed powder, so that the discrete degree of the mixed powder is improved, and the calcination speed of the mixed powder is accelerated.

Technical Field

The invention relates to the technical field of ITO target preparation, in particular to a process for preparing ITO powder.

Background

The ITO target is a mixture of indium oxide and tin dioxide, which is an important raw material for preparing an ITO film, and the ITO target is mainly used for manufacturing ITO film transparent conductive glass, which is a main material for manufacturing flat liquid crystal display and has wide application in the electronic industry and the information industry. The ITO target is made by calcining ITO powder, so the quality of the ITO powder determines the quality of the ITO target.

Through mass search, Chinese patent of invention CN103771497A in the prior art discloses a process for preparing ITO powder, which comprises dissolving indium in nitric acid, adding excessive ammonia water, and stirring; adding tin tetrachloride into the solution, heating and stirring to obtain indium tin hydroxide precipitation solution; heating and concentrating the precipitation solution to obtain indium tin hydroxide colloid; grinding the colloid; calcining the grinded colloid to obtain an indium-tin mixture; the mixture was dried to obtain ITO powder. The invention adopts a new concentration process to prepare the ITO precursor, and then combines a wet grinding method to prepare the nano-grade ITO powder, thereby providing a new process for preparing the ITO powder, which not only has low preparation cost, but also has simple process.

In conclusion, in the production process of the conventional ITO powder, a homogeneous coprecipitation method is mostly adopted, deionized water washing and calcination are required in the homogeneous coprecipitation method process, and the required equipment is simple, so that the process has the remarkable advantage, but a large amount of water resource waste is caused in the deionized water washing process, the calcination efficiency is low, the process period is long, and the process cannot be suitable for large-scale production.

Disclosure of Invention

The present invention is directed to a process for preparing ITO powder to solve the problems set forth in the background art.

In order to achieve the purpose, the invention provides the following technical scheme: a process for preparing ITO powder comprises the steps of mixing indium metal as a raw material of the ITO powder with nitric acid to prepare indium nitrate, mixing the indium nitrate with stannic chloride, and then carrying out a precipitation preparation process;

the preparation process comprises the following steps: adding a precipitator and an additive, heating and stirring, cleaning and filtering, drying and grinding and calcining;

after the raw materials are prepared, adding a precipitator and an additive, wherein the precipitator is urea and the additive is ammonium sulfate; adding deionized water after the precipitant and the additive are added, and mixing to prepare indium tin salt aqueous solution;

adding the indium tin salt aqueous solution into a heating kettle, wherein an electric stirring rod is arranged in the heating kettle, and the heating kettle is heated after being electrified and drives the electric stirring rod to heat and stir the indium tin salt aqueous solution in the heating kettle;

after heating and stirring, urea is heated and uniformly decomposed to generate ammonia water, the ammonia water and an indium tin salt aqueous solution generate a chemical reaction to generate indium hydroxide and tin hydroxide, the indium hydroxide and the tin hydroxide are not dissolved in water, and a precipitate is generated;

in the cleaning and filtering stage, deionized water is adopted for washing, filtering is carried out, and impurities such as chloride ions, sulfate ions and the like are taken out to obtain a milky colloidal indium hydroxide and tin hydroxide mixture;

in the drying and grinding stage, the washed indium hydroxide and tin hydroxide are taken out and placed in a drying furnace, and the drying furnace dries the indium hydroxide and tin hydroxide precipitates;

in the calcination stage, indium hydroxide and tin hydroxide powder are placed in a calcination furnace for calcination, the calcination temperature is controlled at 600-1000 ℃, the temperature in the preheating stage is controlled at 500-600 ℃, the preheating is carried out for 1h, and then the high-temperature heating stage is carried out, and the temperature is raised to 800-1000 ℃.

Preferably, the heating temperature of the heating kettle for heating the indium tin salt aqueous solution is controlled between 70 ℃ and 100 ℃, the rotating speed of the electric stirring rod is 1000r/min, and the heating kettle and the electric stirring rod are controlled by independent controllers.

Preferably, the indium tin salt aqueous solution is heated and stirred and then is conveyed to a washing tank, meanwhile, the redundant indium tin salt aqueous solution is separated from the indium hydroxide and the tin hydroxide, and the indium hydroxide and the tin hydroxide are separated into the washing tank;

deionized water is introduced into the washing tank, indium hydroxide and tin hydroxide precipitates are washed by the deionized water, the washing water is introduced into the washing tank again through a circulating pipe, a filter is additionally arranged in the middle of the circulating pipe, and a detachable filter screen is arranged in the filter, so that the filter is convenient to replace;

the sparge water through the filter screen is filtered the back, and the sparge water lets in the washing jar once more, the washing jar is equipped with the puddler, washes indium hydroxide and tin hydroxide precipitate comprehensively, and the recycling of sparge water, the quantity of reducible deionized water, the circulating pipe upper end is connected with control valve and flowmeter, control washing speed and demonstration water flow.

Preferably, the drying temperature is controlled to be about 100 ℃; and after drying, removing water in the indium hydroxide and tin hydroxide precipitate, putting the indium hydroxide and tin hydroxide precipitate into a grinding machine, and grinding the indium hydroxide and tin hydroxide to obtain nano-scale indium hydroxide and tin hydroxide mixed powder.

Preferably, the calcination operation is a step calcination, a sectional partition plate is used in the calcination furnace, a vibration motor is additionally arranged on the sectional partition plate, the mixed powder of indium hydroxide and tin hydroxide vibrates on the sectional partition plate, and the calcination furnace uniformly calcines the mixed powder, so that the discrete degree of the mixed powder is improved, and the calcination speed of the mixed powder is accelerated.

Compared with the prior art, the invention has the beneficial effects that: in the process of cleaning indium hydroxide and tin hydroxide by using deionized water, the deionized water is recycled, a detachable filter screen is arranged in a circulating pipe through which the deionized water circulates, so that the deionized water cleaning device is convenient to replace, the recycling of the deionized water is effectively improved, the waste of water resources is reduced, in addition, in the calcining process, the calcining operation is adopted for graded calcining, a sectional type partition plate is adopted in the calcining furnace, a vibrating motor is additionally arranged on the sectional type partition plate, the mixed powder of the indium hydroxide and the tin hydroxide vibrates on the sectional type partition plate, and the calcining furnace uniformly calcines the mixed powder, so that the dispersion degree of the mixed powder is improved, the calcining speed of the mixed powder is accelerated, the process progress is accelerated, the process cycle time is reduced, and the device is.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", and the like indicate orientations or positional relationships only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.

In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "connected," and the like are to be construed broadly, such as "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.

The invention provides three embodiments: a process for preparing ITO powder, ITO powder raw materials are metal indium, metal indium is mixed with nitric acid to prepare indium nitrate, and mix with stannic chloride, carry on the preparation method of precipitation subsequently;

the preparation process comprises the following steps: adding precipitant and additive, heating and stirring, washing and filtering, drying and grinding and calcining.

The first embodiment is as follows:

after the preparation of the raw materials is finished, adding a precipitator and an additive, wherein the precipitator is urea and the additive is ammonium sulfate;

after the precipitant and the additive are added, adding the deionized water and mixing to prepare the indium tin salt aqueous solution.

Adding the indium tin salt aqueous solution into a heating kettle, wherein an electric stirring rod is arranged in the heating kettle, heating the heating kettle after electrifying, and driving the electric stirring rod to heat and stir the indium tin salt aqueous solution in the heating kettle;

after heating and stirring, the urea is heated and uniformly decomposed to generate ammonia water, the ammonia water and the indium tin salt aqueous solution generate chemical reaction to generate indium hydroxide and tin hydroxide, and the indium hydroxide and the tin hydroxide are insoluble in water and generate precipitate.

The temperature of the heating kettle for heating the indium tin salt aqueous solution is controlled between 70 ℃ and 100 ℃, the rotating speed of the electric stirring rod is 1000r/min, and the heating kettle and the electric stirring rod are controlled by independent controllers.

And in the cleaning and filtering stage, deionized water is adopted for washing, filtering is carried out, and impurities such as chloride ions, sulfate ions and the like are taken out, so that a milky colloidal indium hydroxide and tin hydroxide mixture is obtained.

The indium tin salt aqueous solution is heated and stirred and then is transmitted to a washing tank, meanwhile, the redundant indium tin salt aqueous solution is separated from indium hydroxide and tin hydroxide, and the indium hydroxide and the tin hydroxide are separated into the washing tank;

example two:

deionized water is introduced into the washing tank, indium hydroxide and tin hydroxide precipitates are washed by the deionized water, the washing water is introduced into the washing tank again through a circulating pipe, a filter is additionally arranged in the middle of the circulating pipe, and a detachable filter screen is arranged in the filter, so that the filter is convenient to replace;

the washing water passing through the filter screen is filtered, the washing water is introduced into the washing tank again, the washing tank is provided with a stirring rod, indium hydroxide and tin hydroxide precipitates are comprehensively washed, the washing water is recycled, the using amount of deionized water can be reduced, and the upper end of the circulating pipe is connected with a control valve and a flowmeter to control the washing speed and display the water flow.

Example three:

in the drying and grinding stage, the washed indium hydroxide and tin hydroxide are taken out and placed in a drying furnace, the drying furnace dries the indium hydroxide and tin hydroxide precipitates, and the drying temperature is controlled to be about 100 ℃;

and after drying, removing water in the indium hydroxide and tin hydroxide precipitate, putting the indium hydroxide and tin hydroxide precipitate into a grinding machine, and grinding the indium hydroxide and tin hydroxide to obtain nano-scale indium hydroxide and tin hydroxide mixed powder.

In the calcining stage, indium hydroxide and tin hydroxide powder are placed in a calcining furnace for calcining;

the calcination temperature is controlled to be 600-1000 ℃, wherein the temperature in the preheating stage is controlled to be 500-600 ℃, the preheating is carried out for 1h, and then the high-temperature heating stage is carried out, and the temperature is raised to be 800-1000 ℃;

the calcination operation adopts staged calcination, a sectional type partition plate is adopted in the calcination furnace, a vibration motor is additionally arranged on the sectional type partition plate, the indium hydroxide and tin hydroxide mixed powder vibrates on the sectional type partition plate, and the calcination furnace uniformly calcines the mixed powder, so that the discrete degree of the mixed powder is improved, and the calcination speed of the mixed powder is accelerated.

It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.