CN112479683A - Preparation method of doped IGZO material - Google Patents
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Abstract
The invention belongs to the technical field of target material manufacturing, and discloses a preparation method of a doped IGZO material. The preparation method comprises the following steps: (1) to ZnO and In2O3、Ga2O3Adding ammonium molybdate solution into the powder, mixing, drying, sieving and heating to obtain IGZO powder; (2) adding a forming agent into the IGZO powder prepared in the step (1), mixing, drying, sieving, forming, removing the forming agent, and sintering to obtain the IGZO material; ZnO and In2O3、Ga2O3The particle size of the powder is 300-800 nm. The IGZO material prepared by the preparation method has the relative density of more than 99.6 percent and the resistivity of less than 9.5 multiplied by 10‑4Omega cm; the IGZO thin film material prepared from the IGZO material has strong stability and high quality. The preparation method is simple and easy to operate.
Description
Technical Field
The invention belongs to the technical field of target material manufacturing, and particularly relates to a preparation method of a doped IGZO material.
Background
The Indium Gallium Zinc Oxide (IGZO) film as a novel semiconductor material has the advantages of high carrier mobility, strong chemical stability, simple preparation process and the like. Therefore, the IGZO thin film is applied to a channel layer material in a new generation Thin Film Transistor (TFT) technology, and the prepared TFT has the characteristics of high-speed driving performance, high resolution, large size, low power consumption and the like.
At present, the IGZO film is mainly prepared by adopting a mode of magnetron sputtering an IGZO ceramic target material. IGZO ceramic powder is volatile at high temperature, densification and sintering are difficult, and increasing the sintering aid is easy to reduce the service performance of IGZO materials. Therefore, while ensuring the excellent photoelectric properties of the IGZO material, the sintering activity of the material is improved by doping, and the reduction of the sintering temperature is an important research direction of the IGZO material. The molybdenum trioxide has a lower melting point, and the doped molybdenum oxide can reduce the densification temperature of the IGZO ceramic, inhibit the growth of grains and facilitate the preparation of fine-grain IGZO targets. By doping a small amount of molybdenum oxide, the light transmittance of the IGZO film is not reduced, the resistivity of the IGZO film is improved, and the stability of the IGZO film material is improved.
At present, the doped IGZO target material is prepared by adding trace element oxide powder into IGZO powder and mixing the powder by adopting a ball milling method. In order to achieve a good mixing effect, long-time ball milling and multiple times of pre-dispersion are needed, and the time for preparing the powder is greatly prolonged. And the micro solid powder is difficult to homogenize by adopting a mechanical ball milling method, and powder is easy to gather at one position, so that the doping elements are not uniform, and the quality of the target material is influenced. More importantly, the ball milling is easy to cause the abrasion of the ball milling medium, new impurities are introduced, and the target material is polluted.
Therefore, it is desirable to provide a method for preparing a micro-doped IGZO material, which can prepare an IGZO material with uniform doping and low resistivity.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides a preparation method of the doped IGZO material, which can be used for preparing the IGZO material with uniform doping and low resistivity.
The conception of the invention is as follows: uniformly mixing raw material powder of an IGZO material and an ammonium molybdate aqueous solution by utilizing the characteristic that ammonium molybdate is dissolved in water, forming an ammonium molybdate coating layer which is uniformly dispersed on the surface of the raw material powder after drying, and then pyrolyzing the ammonium molybdate into MoO by heating3Realization of micro MoO3While ammonium molybdate is pyrolyzed to generate NH thermally dissociated3Can be fully escaped along with heating, and can not introduce new impurities into the raw material powder. In order to prepare an IGZO material having uniform doping and low resistivity, it is also important to control the particle size of the raw material powder.
IGZO is composed of ZnO and In2O3、Ga2O3Three oxides, different from the materials consisting of other ternary or binary oxides, Ga2O3Melting point of (2) and ZnO, In2O3The difference in melting point of (b) is large, and the crystal structure is easily transformed at high temperature, so that the doping is more difficult.
A method of preparing a doped IGZO material, comprising the steps of:
(1) to ZnO and In2O3、Ga2O3Adding ammonium molybdate solution into the powder, mixing, drying, sieving and heating to obtain IGZO powder;
(2) adding a forming agent into the IGZO powder prepared in the step (1), mixing, drying, sieving, forming, removing the forming agent, and sintering to obtain the IGZO material; the ZnO and In2O3、Ga2O3The particle size of the powder is 300-800 nm.
Preferably, the particle size of the IGZO powder is 300-800 nm.
Preferably, In the step (1), the ZnO and In are2O3And Ga2O3The mol ratio of the powder is (1-2): (1-2): (1-8); more preferably, In the step (1), the ZnO or In is2O3And Ga2O3The molar ratio of the powder is 1: 1: (1-8).
Preferably, the IGZO material is doped with molybdenum, and the doping amount of the molybdenum is 0.01-0.2 wt%; further preferably, the doping amount of the molybdenum in the IGZO material is 0.02-0.2 wt%.
Preferably, the concentration of ammonium molybdate in the ammonium molybdate solution in the step (1) is 0.01 to 0.3 wt%; further preferably, the concentration of ammonium molybdate in the ammonium molybdate solution in step (1) is 0.05 to 0.3 wt%.
Preferably, in the step (1), the mixing process is mixing by means of wet milling, and the time of the wet milling is 24-48 h.
Preferably, in the step (1), the heating temperature is 280-380 ℃; further preferably, the temperature of the heating in the step (1) is 300-350 ℃. At which temperature the ammonium molybdate pyrolyzes more fully.
Preferably, in the step (2), the forming agent is polyethylene glycol or polyvinyl alcohol; further preferably, in the step (2), the forming agent is polyethylene glycol.
Preferably, in the step (2), the amount of the forming agent is 0.5 to 5 wt%.
Preferably, in the step (2), the molding process comprises molding and static pressure, the pressure of the molding is 20-40MPa, and the pressure of the static pressure is 200-400 MPa; further preferably, the pressure of the molding is 20-30MPa, and the pressure of the static pressure is 200-300 MPa.
Preferably, in the step (2), the sintering process is sintering at 1300-1500 ℃ and under the oxygen atmosphere at normal pressure for 5-12 h; further preferably, in the step (2), the sintering process is sintering at 1300-1450 ℃ under oxygen atmosphere at normal pressure for 6-10 h.
Specifically, the preparation method of the doped IGZO material comprises the following steps:
(1) according to the molar ratio (1-2): (1-2): (1-8) weighing ZnO and In2O3、Ga2O3Adding the powder into 0.01-0.3 wt% ammonium molybdate solution, wet-grinding for 24-48h, mixing uniformly, drying, sieving with 5000-8000 mesh sieve, heating to 280-380 deg.C to pyrolyze ammonium molybdate into MoO3To prepare IGZO powder;
(2) adding a forming agent polyethylene glycol into the powder prepared in the step (1), wet-grinding, mixing, drying, sieving, then carrying out die pressing under the pressure of 20-40MPa, preparing a green compact under the pressure static pressure of 200-400MPa, removing the forming agent, and sintering at 1300-1500 ℃ and under the oxygen atmosphere for 5-12h at normal pressure to obtain the IGZO material.
The doped IGZO material is prepared by the preparation method, the relative density of the IGZO material is more than 99.6%, and the resistivity of the IGZO material is less than 9.5 multiplied by 10-4Ω·cm。
The doped IGZO material is applied to the field of semiconductors. The target material is mainly used as a target material for sputtering coating, comprises a plane target and a rotating target and is used as an active layer material of a thin film transistor.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, by utilizing the characteristic that ammonium molybdate is dissolved in water, the ammonium molybdate and IGZO powder are mixed, dried and pyrolyzed to obtain MoO3The coated IGZO powder greatly improves the trace MoO3The degree of homogeneity of the powder mixing under doping. And a trace of MoO3The solid solution is dissolved in zinc oxide crystal lattices, and the conductivity and the relative density of the IGZO material can be greatly improved under the condition of not influencing a target material phase. The IGZO material has a relative density of more than 99.6% and a resistivity of less than 9.5 × 10-4Omega cm. The IGZO thin film material prepared from the IGZO material has strong stability and high quality.
(2) The preparation method is simple and easy to operate, and can economically and efficiently prepare the IGZO materials with various complex shapes.
Drawings
FIG. 1 is a flow chart of a process for preparing IGZO powder in an IGZO material according to example 1;
FIG. 2 is a flow chart of the sintering process for preparing IGZO powder in IGZO material in example 1.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The starting materials, reagents or apparatuses used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.
Example 1
A preparation method of a doped IGZO material refers to a preparation process flow chart of IGZO powder in figure 1 and a sintering process flow chart of IGZO powder in figure 2, and comprises the following steps:
(1) according to the mol ratio of 1: 1: 1 weighing ZnO and In2O3、Ga2O3Powder (ZnO, In)2O3、Ga2O3The particle size of the powder is 300-800nm), adding the powder into 0.1 wt% ammonium molybdate aqueous solution, wet-grinding for 36h, uniformly mixing, then drying by hot air, and fully grinding until all the powder passes through a 200-mesh sieve; then heated to 320 ℃ to pyrolyze the ammonium molybdate into MoO3To prepare IGZO powder;
(2) adding 3 wt% of polyethylene glycol into the powder prepared in the step (1), wet-grinding for 24h, uniformly mixing, fully drying, crushing, fully grinding until all the powder passes through a 200-mesh sieve; and then mould pressing is carried out under the pressure of 30MPa, a green body is prepared under the pressure of 350MPa, the temperature is increased to 750 ℃, furnace cooling is carried out for 4h (the forming agent is removed), and then sintering is carried out for 10h under the atmospheric pressure in the oxygen atmosphere at 1380 ℃, thus obtaining the IGZO material. The IGZO material has a relative density of 99.90% and a resistivity of less than 2 × 10-4Ω·cm。
Example 2
A method of preparing a doped IGZO material, comprising the steps of:
(1) according to the mol ratio of 1: 2: 8 weighing ZnO and In2O3、Ga2O3Powder (ZnO, In)2O3、Ga2O3The particle size of the powder is 300-800nm), adding the powder into 0.01 wt% ammonium molybdate aqueous solution, wet-grinding for 24h, uniformly mixing, then drying by hot air, and fully grinding until all the powder passes through a 200-mesh sieve; heating to 320 ℃ to pyrolyze ammonium molybdate into MoO3To prepare IGZO powder;
(2) adding 1 wt% of polyethylene glycol into the powder prepared in the step (1), wet-grinding for 24h, uniformly mixing, fully drying, crushing, fully grinding until all the powder passes through a 200-mesh sieve; and then mould pressing is carried out under the pressure of 20MPa, a green body is prepared under the pressure of 400MPa, the temperature is increased to 750 ℃, furnace cooling is carried out for 4h (forming agent is removed), and then sintering is carried out for 10h under the atmospheric pressure in the oxygen atmosphere at 1380 ℃, thus obtaining the IGZO material. The IGZO material has a relative density of 99.85% and a resistivity of less than 3.5 × 10-4Ω·cm。
Example 3
A method of preparing a doped IGZO material, comprising the steps of:
(1) and (2) according to molar ratio: 1: 5 weighing ZnO and In2O3、Ga2O3Powder (ZnO, In)2O3、Ga2O3The particle size of the powder is 300-800nm), adding the powder into 0.1 wt% ammonium molybdate aqueous solution, wet-grinding for 36h, uniformly mixing, then drying by hot air, and fully grinding until all the powder passes through a 200-mesh sieve; then heated to 320 ℃ to pyrolyze the ammonium molybdate into MoO3To prepare IGZO powder;
(2) adding 5 wt% of polyethylene glycol into the powder prepared in the step (1), wet-grinding for 24h, uniformly mixing, fully drying, crushing, fully grinding until all the powder passes through a 200-mesh sieve; and then carrying out die pressing under the pressure of 40MPa, preparing a green body under the pressure of 200MPa, heating to 750 ℃, keeping the temperature for 4h, carrying out furnace cooling (removing the forming agent), and then sintering at 1420 ℃ under the atmospheric pressure in an oxygen atmosphere for 10h to obtain the IGZO material. The IGZO material has a relative density of 99.82% and a resistivity of less than 3.2 × 10-4Ω·cm。
Example 4
A method of preparing a doped IGZO material, comprising the steps of:
(1) according to the mol ratio of 1: 2: 1 weighing ZnO and In2O3、Ga2O3Powder (ZnO, In)2O3、Ga2O3The particle size of the powder is 300-800nm), adding the powder into 0.1 wt% ammonium molybdate aqueous solution, wet-grinding for 48h, uniformly mixing, then drying by hot air, and fully grinding until the powder is completely groundPassing through a 200-mesh sieve; then heated to 320 ℃ to pyrolyze the ammonium molybdate into MoO3To prepare IGZO powder;
(2) adding 3 wt% of polyethylene glycol into the powder prepared in the step (1), wet-grinding for 24h, uniformly mixing, fully drying, crushing, fully grinding until all the powder passes through a 200-mesh sieve; and then carrying out die pressing under the pressure of 35MPa, preparing a green body under the pressure of 350MPa, heating to 750 ℃, keeping the temperature for 4h, carrying out furnace cooling (removing the forming agent), and then sintering at 1500 ℃ under the oxygen atmosphere for 8h at normal pressure to obtain the IGZO material. The IGZO material has a relative density of 99.80% and a resistivity of less than 4.2 × 10-4Ω·cm。
Example 5
A method of preparing a doped IGZO material, comprising the steps of:
(1) according to the mol ratio of 1: 1: 1 weighing ZnO and In2O3、Ga2O3Powder (ZnO, In)2O3、Ga2O3The particle size of the powder is 300-800nm), adding the powder into 0.1 wt% ammonium molybdate aqueous solution, wet-grinding for 36h, uniformly mixing, then drying by hot air, and fully grinding until all the powder passes through a 200-mesh sieve; then heated to 280 ℃ to pyrolyze the ammonium molybdate into MoO3To prepare IGZO powder;
(2) adding 3 wt% of polyethylene glycol into the powder prepared in the step (1), wet-grinding for 24h, uniformly mixing, fully drying, crushing, fully grinding until all the powder passes through a 200-mesh sieve; and then mould pressing is carried out under the pressure of 30MPa, a green body is prepared under the pressure of 350MPa, the temperature is increased to 750 ℃, furnace cooling is carried out for 4h (the forming agent is removed), and then sintering is carried out for 10h under the atmospheric pressure in the oxygen atmosphere at 1380 ℃, thus obtaining the IGZO material. The IGZO material has a relative density of 99.78% and a resistivity of less than 5.6 × 10-4Ω·cm。
Example 6
A method of preparing a doped IGZO material, comprising the steps of:
(1) according to the mol ratio of 1: 1: 1 weighing ZnO and In2O3、Ga2O3Powder (ZnO, In)2O3、Ga2O3The powder has a particle size of 300-800nm), adding the mixture into 0.1 wt% ammonium molybdate aqueous solution, wet-grinding for 36h, uniformly mixing, then drying by hot air, and fully grinding until all the mixture passes through a 200-mesh sieve; then heated to 350 ℃ to pyrolyze the ammonium molybdate into MoO3To prepare IGZO powder;
(2) adding 3 wt% of polyethylene glycol into the powder prepared in the step (1), wet-grinding for 24h, uniformly mixing, fully drying, crushing, fully grinding until all the powder passes through a 200-mesh sieve; and then mould pressing is carried out under the pressure of 30MPa, a green body is prepared under the pressure of 350MPa, the temperature is increased to 750 ℃, furnace cooling is carried out for 4h (the forming agent is removed), and then sintering is carried out for 10h under the atmospheric pressure in the oxygen atmosphere at 1380 ℃, thus obtaining the IGZO material. The IGZO material has a relative density of 99.76% and a resistivity of less than 7.2 × 10-4Ω·cm。
Example 7
A method of preparing a doped IGZO material, comprising the steps of:
(1) according to the mol ratio of 1: 1: 1 weighing ZnO and In2O3、Ga2O3Powder (ZnO, In)2O3、Ga2O3The particle size of the powder is 300-800nm), adding the powder into 0.1 wt% ammonium molybdate aqueous solution, wet-grinding for 36h, uniformly mixing, then drying by hot air, and fully grinding until all the powder passes through a 200-mesh sieve; then heated to 320 ℃ to pyrolyze the ammonium molybdate into MoO3To prepare IGZO powder;
(2) adding 3 wt% of polyethylene glycol into the powder prepared in the step (1), wet-grinding for 24h, uniformly mixing, fully drying, crushing, fully grinding until all the powder passes through a 200-mesh sieve; and then mould pressing is carried out under the pressure of 45MPa, a green body is prepared under the pressure of 450MPa, the temperature is increased to 750 ℃, furnace cooling is carried out for 4h (forming agent is removed), and then sintering is carried out for 10h under the atmospheric pressure in the oxygen atmosphere at 1380 ℃, thus obtaining the IGZO material. The IGZO material has a relative density of 99.62% and a resistivity of less than 9.4 × 10-4Ω·cm。
Example 8
A method of preparing a doped IGZO material, comprising the steps of:
(1) according to the mol ratio of 1: 1: 1 weighing ZnO and In2O3、Ga2O3Powder (ZnO, In)2O3、Ga2O3The particle size of the powder is 300-800nm), adding the powder into 0.1 wt% ammonium molybdate aqueous solution, wet-grinding for 36h, uniformly mixing, then drying by hot air, and fully grinding until all the powder passes through a 200-mesh sieve; then heated to 320 ℃ to pyrolyze the ammonium molybdate into MoO3To prepare IGZO powder;
(2) adding 3 wt% of polyethylene glycol into the powder prepared in the step (1), wet-grinding for 24h, uniformly mixing, fully drying, crushing, fully grinding until all the powder passes through a 200-mesh sieve; and then mould pressing is carried out under the pressure of 30MPa, a green body is prepared under the pressure of 350MPa, the temperature is increased to 750 ℃, furnace cooling is carried out for 4h (the forming agent is removed), and then sintering is carried out for 10h under the atmospheric pressure in the oxygen atmosphere at 1380 ℃, thus obtaining the IGZO material. The IGZO material has a relative density of 99.75% and a resistivity of less than 6.8 × 10-4Ω·cm。
Comparative example 1
A method of preparing a doped IGZO material, comprising the steps of:
(1) according to the mol ratio of 1: 1: 1 weighing ZnO and In2O3、Ga2O3Powder (ZnO, In)2O3、Ga2O3The particle size of the powder is 2-4 mu m), adding the powder into 0.1 wt% ammonium molybdate solution, wet-grinding for 36h, uniformly mixing, drying by hot air, and fully grinding until the powder passes through a 200-mesh sieve; then heated to 320 ℃ to pyrolyze the ammonium molybdate into MoO3To prepare IGZO powder;
(2) adding 3 wt% of polyethylene glycol into the powder prepared in the step (1), wet-grinding for 24h, uniformly mixing, fully drying, crushing, fully grinding until all the powder passes through a 200-mesh sieve; and then mould pressing is carried out under the pressure of 30MPa, a green body is prepared under the pressure of 350MPa, the temperature is increased to 750 ℃, furnace cooling is carried out for 4h (the forming agent is removed), and then sintering is carried out for 10h under the atmospheric pressure in the oxygen atmosphere at 1380 ℃, thus obtaining the IGZO material. The IGZO material has a relative density of 98.5% and a resistivity of less than 7.5 × 10-3Ω·cm。
Comparative example 2
A method of preparing a doped IGZO material, comprising the steps of:
(1) according to the mol ratio of 1: 1: 1 weighing ZnO and In2O3、Ga2O3Powder (ZnO, In)2O3、Ga2O3The particle size of the powder is 300-800nm), wet grinding is carried out for 36h, the mixture is uniformly mixed, and then the mixture is dried by hot air and fully ground until the mixture completely passes through a 200-mesh sieve, so as to prepare the IGZO powder;
(2) adding 3 wt% of polyethylene glycol into the powder prepared in the step (1), wet-grinding for 24h, uniformly mixing, fully drying, crushing, fully grinding until the powder completely passes through a 200-mesh sieve, then carrying out die pressing under the pressure of 30MPa to prepare a green body under the pressure of 350MPa, heating to 750 ℃, keeping the temperature for 4h, carrying out furnace cooling (removing a forming agent), and then carrying out normal pressure sintering at 1380 ℃ in an oxygen atmosphere for 10h to prepare the IGZO material. The IGZO material has a relative density of 98.1% and a resistivity of less than 9 × 10-2Ω·cm。
Claims (10)
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Application publication date: 20210312 |