CN108002428B - Preparation method of ITO (indium tin oxide) particles for evaporation and ITO particles prepared by method - Google Patents
Preparation method of ITO (indium tin oxide) particles for evaporation and ITO particles prepared by method Download PDFInfo
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Abstract
The invention provides a preparation method of ITO particles for vapor deposition, which comprises the following steps in a pressureless sintering furnace: (1) heating the ITO blank to 240 ℃ at a heating rate of 10-100 ℃/h in an oxygen flowing environment, then heating to 600 ℃ at a heating rate of 10-30 ℃/h, and preserving heat for 1-4 h after the heating is finished; (2) heating to 1300-1500 ℃ at a heating rate of 100-200 ℃/h in an oxygen flowing environment, and carrying out non-pressure oxygen sintering for 1-10 h. The preparation method of the invention simplifies the control conditions of powder preparation, is beneficial to independently controlling the powder quality, simplifies the processes of molding, degreasing and sintering, and belongs to the first preparation method of ITO particles in China. The invention also provides ITO particles, which meet the technical index requirements of a vacuum evaporation method, have uniform structures and are not easy to crack.
Description
Technical Field
The invention belongs to the technical field of semiconductor material preparation, and particularly relates to a preparation method of ITO particles for preparing a transparent conductive film by an evaporation method and the ITO particles prepared by the method.
Background
There are many methods for producing transparent conductive thin film materials, among which magnetron sputtering is the most widely used method. The magnetron sputtering method is mainly applied to the manufacture of LCD and solar cell thin film materials. In the process of semiconductor production technology, the magnetron sputtering method can cause serious damage to the semiconductor surface, so that the vacuum evaporation coating method is generally adopted when preparing the transparent conductive film of a semiconductor Light Emitting Diode (LED), an Organic Light Emitting Diode (OLED) and a Polymer Light Emitting Diode (PLED).
Vacuum evaporation coating, namely a method for depositing a certain substance on a solid surface to form a film by heating and evaporating the substance. Faraday was first proposed in 1857 by m. The transparent conductive film is prepared by using a vacuum evaporation method, the process is simpler, and the prepared film has the advantages of less influence of deposition conditions and higher transmittance of the film. Y.H.Aliyu et al, 1995, reported a structure in which Indium Tin Oxide (ITO) was deposited as a current spreading layer on an MOCVD-prepared AIGaInP epitaxial layer by a thermal evaporation deposition method.
Indium tin oxide ITO is widely used in the field of transparent electrodes of optoelectronic devices. This is because indium tin oxide ITO has high conductivity and visible light transmittance, and compared with other transparent conductive thin films, the ITO thin film also has good chemical stability, thermal stability, good adhesion to a substrate, and good pattern processing characteristics, and is an ideal material for manufacturing a transparent electrode.
At present, the semiconductor LED becomes a new generation illumination light source in the 2l century due to the advantages of high electro-optic conversion efficiency, long service life, environmental protection and the like. The ITO film in the LED is mainly prepared by adopting an electron beam heating vacuum evaporation method, namely, a high-energy electron beam is utilized to bombard the surface of a mixed raw material of indium and tin oxide to sublimate the mixed raw material, and then the mixed raw material is deposited on a substrate in a cold condition to form an ITO film. The method has the advantages of less process parameters needing to be strictly controlled, relatively easy operation and control of the film growth, no generation of a plurality of uncontrollable impurities in the prepared film, strictly controllable growth rate of the film and suitability for large-scale industrial production. With the gradual maturity of the semiconductor technology, the development of the LED device is continuously developed towards the direction of high efficiency and high brightness, the market application is wider and wider, and the demand on ITO evaporation particles is more and more. Meanwhile, the ITO film prepared by vacuum evaporation can also be widely applied to the fields of OLED (organic light emitting diode), PLED (polymer light emitting diode) and the like.
At present, the preparation method of the ITO evaporation particles is a normal pressure sintering method and a pressure sintering method. The former adopts a common high-temperature sintering furnace which is electrically heated and can be filled with oxidizing gas, the equipment is simple, but the oxygen content of atmosphere can not be controlled or detected in the sintering process, the product quality (such as oxygen loss rate and the like) of ITO evaporation particles can not be ensured, and the controllable precision of the equipment is poor; in addition, the normal pressure sintering furnace has larger hearth, smaller air flow and larger temperature difference in the furnace, and has larger influence on the density and microstructure (such as grain size) of the ITO particles, so the common normal pressure sintering method brings hidden quality trouble to the mass production of the ITO particles. The latter can solve the problem of oxygen partial pressure and the problem of furnace temperature uniformity, but the biggest problem is that the sintering furnace has pressure, which forms hidden danger to production safety; in addition, the equipment investment is larger than that of a normal pressure sintering furnace, and the production cost is not favorably controlled. Therefore, research and design of a preparation method of ITO particles for evaporation, which has a simple process, is safe and reliable and can ensure the product quality, is urgently needed.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background art, and provide a preparation method of ITO particles for evaporation and the ITO particles prepared by the method.
In order to realize the purpose of the invention, the technical scheme of the invention is as follows:
a preparation method of ITO particles for evaporation comprises the following steps in a pressureless sintering furnace: (1) heating the ITO blank to 240 ℃ at a heating rate of 10-100 ℃/h in an oxygen flowing environment, then heating to 600 ℃ at a heating rate of 10-30 ℃/h, and preserving heat for 1-4 h after the heating is finished; (2) and heating to 1300-1500 ℃ at a heating rate of 100-200 ℃/h in an oxygen flowing environment, and carrying out non-pressure oxygen sintering for 1-10 h to obtain the ITO particles.
The preparation method adopts pressureless sintering treatment, namely sintering is carried out by adopting a large-flow atmosphere sintering furnace with an oxygen content monitor and a pressure induction detection meter, and the pressure meter shows 0 during sintering. The process of the step (1) is a degreasing process, in order to remove the organic additive completely and prevent the cracking of the particles, the heating rate should not exceed 100 ℃/h, the organic additive starts to decompose after 240 ℃, and can be basically and completely removed after 400 ℃, so the heating rate and the heat preservation time are controlled within the range of the invention. The process of the step (2) is a pressureless oxygen sintering treatment process, and because the organic additive is removed completely, in order to prevent the degreased ITO green body from cracking, the core part and the external contraction rate of the green body are consistent, and meanwhile, the temperature rise rate and the heat preservation time need to be controlled within the range of the invention in consideration of the sintering activity of the powder and the energy conservation and environmental protection of the production process.
According to the preparation method, degreasing treatment is carried out in an oxygen atmosphere, so that gas consumption can be reduced, organic additives are decomposed and reacted more fully, pores of an ITO blank are prevented from increasing after degreasing is finished, air is prevented from entering the pores and being adsorbed, and the phenomenon that nitrogen impurities exceed the standard during vacuum coating due to the fact that ITO particles belong to oxides and nitrogen atoms contained in adsorbed air lack effective diffusion channels and are difficult to eliminate during sintering is avoided. In addition, the preparation method of the invention carries out degreasing and pressureless oxygen sintering in the same sintering furnace, thereby further avoiding the defect caused by the air entering the pores and being adsorbed.
In the above method for preparing ITO particles for vapor deposition, preferably, in the step (1), the temperature is raised to 220 ℃ at a temperature raising rate of 60-100 ℃/h, then the temperature is raised to 600 ℃ at a temperature raising rate of 10-30 ℃/h, and the temperature is maintained for 1-2 h after the temperature raising is finished.
In the preparation method of the ITO particles for vapor deposition, preferably, the flow rate of oxygen in the pressureless sintering furnace is 5-50L/min. The oxygen flow control is in the scope of the invention, which can further prevent the cracking of the green body during the degreasing or sintering process.
In the above method for producing ITO particles for vapor deposition, the ITO green body is preferably prepared by adding In2O3Powder and SnO2The powder is mixed, added with water and a dispersing agent to prepare slurry, and then is prepared by ball milling and mixing, spray granulation and metal mould pressing and forming.
In Using the present invention2O3Powder and SnO2The ITO green body is prepared by a powder mixing mode, on one hand, the component proportion of indium and tin can be conveniently adjusted, and the problem that the electrical property of an ITO film is reduced due to large fluctuation of the component proportion of ITO particles generated in the process of preparing ITO powder by a coprecipitation method is avoided; on the other hand, in (OH) can be overcome3And Sn (OH)4The problem of large difference of pH value required by two hydroxides in precipitation reaction; by separately preparing In2O3Powder and SnO2The powder can independently control the grain growth of the powder, and the granularity range of the blank required by production is conveniently regulated and controlled, so that a proper blank with good sintering activity is obtained.
In the above method for producing ITO particles for vapor deposition, the In is preferably2O3BET specific surface area of powderIs 4m2/g～40m2(ii)/g, the average particle diameter is 20 to 200 nm; the SnO2The BET specific surface area of the powder was 2m2/g～20m2(iv) per gram, the average particle diameter is 40 to 400 nm. The main component for preparing the ITO particles is In2O3Powder and SnO2Powder of In2O3The sintering activity of the powder determines the sintering temperature of the particles, while SnO2The addition of powder can ensure the density of the sintered ITO particles, so In needs to be added2O3Powder and SnO2The BET specific surface area and the average particle diameter of the powder are controlled within the range of the present invention.
In the above method for producing ITO particles for vapor deposition, the In is preferably2O3The BET specific surface area of the powder was 12m2/g～14m2(iv)/g, said SnO2The BET specific surface area of the powder was 10m2/g～12m2/g。
In the above method for producing ITO particles for vapor deposition, the In is preferably2O3Powder and SnO2The mass ratio of the powder is (85-98): (15-2), the solid content of the slurry is 30-75 wt%, and ZrO is adopted in the ball milling process2Ball milling and mixing are carried out by taking the ball as a grinding medium, and slurry and ZrO are controlled2The mass ratio of the balls is 1 (1-5), the ball milling rotating speed is 10-100 r/min, and the grinding time is 1-20 h. To make In2O3Powder and SnO2The powder can be uniformly mixed, and ZrO can be ensured simultaneously2The service life of the ball is prolonged, the Zr content of ITO particles is prevented from exceeding the standard, and the process condition of ball milling treatment is controlled within the scope of the invention.
Preferably, the preparation method of the ITO particles for evaporation comprises the step of performing compression molding on an ITO blank by using a steel die or a hard alloy die, wherein the diameter of the die is 8-34 mm, the molding pressure is 10-30 MPa, and the pressure maintaining time is 0.5-2 min. Because the vacuum coating equipment has certain requirements on the size of the ITO particles, and because the shrinkage rate of the ITO particles during sintering is 11-13%, the diameter of a die and the technological conditions of pressing treatment need to be controlled within the range of the invention, so that the ITO target with the diameter of 7-30 mm can be obtained.
In the preparation method of the ITO particles for vapor deposition, preferably, the dispersant is an aqueous solution of polyacrylate, and the mass fraction of the dispersant is 10-80 wt%; the spray granulation is centrifugal spray granulation or jet spray granulation, a binder is required to be added in the spray granulation process, and the binder is a polyvinyl alcohol aqueous solution, and the mass fraction of the binder is 2-20 wt%. After spray granulation, the powder particles are smooth and spherical, the particle size of the powder spherical particles is 15-105 mu m, wherein the content of 30-70 mu m is more than 60%.
As a general inventive concept, the present invention also provides an ITO particle prepared according to the above preparation method, the ITO particle having an indium oxide single-phase structure, tin being completely dissolved in an indium oxide lattice, the ITO particle having a grain size of 5 μm to 15 μm, wherein 5 μm to 10 μm of the grain size is 80% or more, a relative density of 55 to 65%, and a purity of 99% or more.
Compared with the prior art, the invention has the advantages that:
the method is different from the traditional preparation method, adopts a degreasing and sintering integrated mode in the same equipment, enables the ITO green body to be directly heated and sintered without moving after degreasing, and avoids the phenomena of sintering cracking, corner deletion and the like caused by damage in the moving process of the degreased ITO green body. The method adopts pressureless oxygen sintering, is different from ordinary normal pressure or pressureless sintering, has low requirements on equipment, can effectively control the decomposition of ITO particle oxides, control the oxygen loss rate, stably control the technical indexes such as particle relative density, grain size and the like, can monitor in the whole process in the production process, and ensures the stability of the production quality of the ITO particles.
In general, the ITO particle preparation method simplifies the powder preparation control conditions, is beneficial to independently controlling the powder quality, simplifies the forming and degreasing sintering processes, belongs to the first time in the domestic ITO particle preparation method, and is suitable for industrial production. The ITO particles prepared by the method meet the technical index requirements of a vacuum evaporation method, have uniform structure and are not easy to crack.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a flowchart of a process for producing ITO particles for vapor deposition in example 1 of the present invention;
FIG. 2 is a view showing the morphology of ITO powder particles for vapor deposition prepared in example 1 of the present invention;
FIG. 3 is a phase structure XRD pattern of ITO particles for vapor deposition prepared in example 1 of the present invention;
FIG. 4 is a Scanning Electron Microscope (SEM) cross-sectional view of ITO particles for evaporation prepared in example 1 of the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
The ITO powder particle size distribution is detected by a Mastersizer 3000 particle size analyzer, the grain size of the ITO particles is detected by a scanning electron microscope, the phase structure is detected by an X-ray diffractometer, and the size is measured by a micrometer.
Comparative example 1:
weigh 9500 g of In2O3Powder, 500 g SnO2Powder, 3586 g of pure water and 200 g of dispersing agent are filled into a ball millIn the method, ZrO is filled according to the mass ratio of slurry to balls of 1:22Rolling the ball at a rotating speed of 50 r/min for 12 h; adding 600 g of binder, stirring for 60min, and then carrying out spray granulation; loading the ITO powder into a steel die or a hard alloy die with the diameter of 27.5mm, and maintaining the pressure at 25MPa for 1min to press the ITO powder into a wafer-shaped ITO green body; placing the mixture into a pressureless oxygen atmosphere sintering furnace, heating to 600 ℃ at a heating rate of 60 ℃/h for removing glue, and preserving heat for 1h after heating is finished, wherein the oxygen flow is 20L/min; heating to 1500 ℃ at the heating rate of 200 ℃/h for pressureless oxygen sintering, wherein the sintering time is 5h, and the oxygen flow is 20L/min; the ITO particles obtained finally cracked and were dark green in color, and had a relative density of 74.7% according to the size method. The phase structure is an indium oxide single-phase structure through XRD detection, and the section SEM shows that the grain size is 5-15 mu m.
Comparative example 2:
the preparation of the ITO green body is the same as that of the comparative example 1, the ITO green body is put into a pressureless oxygen atmosphere sintering furnace and is heated to 400 ℃ at the heating rate of 60 ℃/h, and then is heated to 600 ℃ at the heating rate of 30 ℃/h, and the temperature is kept for 1h, wherein the oxygen flow is 20L/min; then heating to 1450 ℃ at the heating rate of 200 ℃/h, and preserving the heat for 5h, wherein the oxygen flow is 20L/min; the ITO particles obtained finally are cracked and green in color, and the relative density is 63.5% according to a size method. The phase structure is an indium oxide single-phase structure through XRD detection, and the section SEM shows that the grain size is 5-15 mu m.
Example 1:
according to the process flow shown In FIG. 1, 9500 g of In were weighed2O3Powder (average particle size 65nm, BET 12.80 m)2Per g), 500 g SnO2Powder (average particle size 70nm, BET 12.50 m)2The preparation method comprises the following steps of (1)/g), 3586 g of pure water and 200 g of dispersing agent are mixed to prepare slurry, wherein the dispersing agent is an aqueous solution of polyacrylate, and the mass fraction of the aqueous solution is 40 wt%; charging the slurry into a ball mill, and charging ZrO according to the mass ratio of the slurry to the ball of 1:22Rolling the ball at a rotating speed of 50 r/min for 12 h; adding 600 g of binder, stirring for 60min, and then carrying out spray granulation, wherein the binder is a polyvinyl alcohol aqueous solution, and the mass fraction of the binder is 10 wt%; loading ITO powder into steel die or hard alloy die with diameter of 27.5mm, and pressing at 25MPaKeeping the pressure for 1min under force to press the ITO green body into a wafer shape; loading the ITO green body into a pressureless oxygen atmosphere sintering furnace, heating to 200 ℃ at the heating rate of 60 ℃/h, heating to 600 ℃ at the heating rate of 30 ℃/h, and keeping the temperature for 1h, wherein the oxygen flow is 20L/min; heating to 1430 ℃ at the heating rate of 120 ℃/h for pressureless oxygen sintering, wherein the sintering time is 5h, and the oxygen flow is 20L/min, so as to obtain ITO particles; the ITO particles are intact, have the morphology structure shown in figure 2, are light green in color, have the purity of 99.99 percent and have the relative density of 60.8 percent according to a size method; the XRD pattern of the phase structure of the ITO particles is shown in FIG. 3, and the phase structure is an indium oxide single-phase structure; the Scanning Electron Microscope (SEM) cross-section of the ITO particles is shown in FIG. 4, which shows that the grain size is 5-10 μm.
Example 2:
the preparation of the ITO green body is the same as that of the example 1, the ITO green body is put into a pressureless oxygen atmosphere sintering furnace, the temperature is firstly heated to 200 ℃ at the heating rate of 100 ℃/h, then the temperature is heated to 600 ℃ at the heating rate of 30 ℃/h, the temperature is kept for 1h, and the oxygen flow is 50L/min; then heating to 1400 ℃ at the heating rate of 200 ℃/h for pressureless oxygen sintering, wherein the sintering time is 5h, and the oxygen flow is 50L/min; the obtained ITO particles are intact, the color is light green, the purity is 99.99 percent, and the relative density is 55.8 percent according to a size method. The phase structure is an indium oxide single-phase structure through XRD detection, and the section SEM shows that the grain size is 5-10 mu m.
Example 3:
weigh 9800 g of In2O3Powder (average particle diameter 60nm, BET 13.60 m)2Per g), 200 g SnO2Powder (average particle diameter 85nm, BET 10.35 m)2And/g), 3586 g of pure water and 200 g of dispersing agent are put into a ball mill, and are ball-milled, mixed, granulated and molded into an ITO green body according to the method of example 1, and the ITO green body is put into a pressureless oxygen atmosphere sintering furnace and is sintered according to the degreasing sintering method of example 1. The prepared ITO particles are intact, the color is light green, the purity is 99.99 percent, and the relative density is 61.7 percent according to a size method. The phase structure is an indium oxide single-phase structure through XRD detection, and the section SEM shows that the grain size is 5-8 mu m.
Example 4:
weighing 9000 g of In2O3Powder (average particle size 67nm, BET 12.54 m)2Per g), 1000 g SnO2Powder (average particle size 70nm, BET 12.48 m)2And/g), 3586 g of pure water and 200 g of dispersing agent are put into a ball mill, and are ball-milled, mixed, granulated and molded into an ITO green body according to the method of example 1, and the ITO green body is put into a pressureless oxygen atmosphere sintering furnace and sintered according to the degreasing sintering method of example 1. The prepared ITO particles are intact, the color is light green, the purity is 99.99 percent, and the relative density is 62.3 percent according to a size method. The phase structure is an indium oxide single-phase structure through XRD detection, and the section SEM shows that the grain size is 5-10 mu m.
Example 5:
8500 g of In is weighed2O3Powder (average particle size 65nm, BET 12.60 m)2Per g), 1500 g SnO2Powder (average particle size 82nm, BET 10.60 m)2And/g), 3586 g of pure water and 200 g of dispersing agent are put into a ball mill, and are subjected to ball milling mixing, granulation and molding in the method of example 1 to prepare an ITO green body, and the ITO green body is put into a pressureless oxygen atmosphere sintering furnace and is sintered in the degreasing sintering method in the example 1. The prepared ITO particles are intact, the color is light green, the purity is 99.99 percent, and the relative density is 58.2 percent according to a size method. The phase structure is an indium oxide single-phase structure through XRD detection, and the section SEM shows that the grain size is 5-10 mu m.
As shown in Table 1, the performance index pairs of the ITO particles prepared in the comparative examples 1-2 and the examples 1-5 are shown in Table 1, and it can be known from Table 1 that the ITO particles prepared by the preparation method disclosed by the invention are uniform in structure and not easy to crack, and meet the technical index requirements of a vacuum evaporation method.
TABLE 1 comparison of Performance indices of ITO particles prepared in comparative examples 1 to 2 and examples 1 to 5
Claims (5)
1. A method for preparing ITO particles for vapor deposition, wherein the ITO particles have an indium oxide single-phase structure, tin is completely dissolved in indium oxide lattices in a solid solution mode, the grain size of the ITO particles is 5-15 mu m, the particles with the size of 5-10 mu m account for more than 80%, the relative density is 55-65%, and the purity is more than 99%, and the method is characterized by comprising the following steps of: (1) heating the ITO blank to 240 ℃ at a heating rate of 10-100 ℃/h in an oxygen flowing environment, then heating to 600 ℃ at a heating rate of 10-30 ℃/h, and preserving heat for 1-4 h after the heating is finished; (2) heating to 1300-1500 ℃ at a heating rate of 100-200 ℃/h in an oxygen flowing environment for pressureless oxygen sintering for 1-10 h to obtain ITO particles;
the oxygen flow in the pressureless sintering furnace is 5-50L/min;
the ITO green body is prepared by mixing In2O3Powder and SnO2Mixing the powder, adding water and a dispersing agent to prepare slurry, and then carrying out ball milling mixing, spray granulation and metal mold compression molding in sequence to obtain the powder;
said In2O3The BET specific surface area of the powder was 12m2/g~14m2(ii)/g, the average particle diameter is 20 to 200 nm; the SnO2The BET specific surface area of the powder was 10m2/g~12m2(iv) per gram, the average particle diameter is 40 to 400 nm.
2. The method as claimed in claim 1, wherein in the step (1), the ITO particles are heated to 200-220 ℃ at a heating rate of 60-100 ℃/h, then heated to 500-600 ℃ at a heating rate of 10-30 ℃/h, and then kept warm for 1-2 h after the heating is finished.
3. The method for producing ITO particles for vapor deposition according to claim 1, wherein In is2O3Powder and SnO2The mass ratio of the powder is (85-98): (15-2), the solid content of the slurry is 30-75 wt%, and ZrO is adopted in the ball milling process2The ball is used as a grinding medium to carry out ball milling and mixing,control slurry and ZrO2The mass ratio of the balls is 1 (1-5), the ball milling rotating speed is 10-100 r/min, and the grinding time is 1-20 h.
4. A method for producing ITO particles for vapor deposition according to claim 1, wherein the ITO green body is press-molded using a steel die or a cemented carbide die, wherein the diameter of the die is 8 to 34mm, the molding pressure is 10 to 30MPa, and the holding pressure is 0.5 to 2 min.
5. The method for producing ITO particles for vapor deposition according to claim 1, wherein the dispersant is an aqueous solution of polyacrylate, and the mass fraction of the dispersant is 10 to 80 wt%; and a binder is required to be added in the spray granulation process, wherein the binder is a polyvinyl alcohol aqueous solution, and the mass fraction of the binder is 2-20 wt%.
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