CN111439778A - Preparation method of nano-grade gallium oxide - Google Patents
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Abstract
The invention relates to a preparation method of nano-grade gallium oxide, belonging to the technical field of semiconductor materials and comprising the following steps of S1, A solution preparation, wherein the gallium nitrate solution is diluted to the gallium content of 25-55 g/L and the concentration of free nitric acid of 0.1-10%, then a surfactant is added to obtain the A solution, S2, B solution preparation, the precipitator is prepared into a solution with the mass fraction of 5-15% to obtain the B solution, S3, the bottom solution C solution preparation, the B solution is added into pure water to prepare the bottom solution C solution, the temperature of the bottom solution C solution is 15-40 ℃, S4, precipitation reaction, the A solution and the B solution are simultaneously added into the bottom solution C solution to carry out precipitation reaction, S5, and then the nano-grade ellipsoidal nano-grade gallium oxide is obtained through ageing reaction, centrifugal washing and calcining.
Description
Technical Field
The invention relates to a preparation method of nano-grade gallium oxide, belonging to the technical field of semiconductor materials.
Background
Gallium oxide (Ga)2O3) Is an important wide bandgap semiconductor material with five crystal structures of α -Ga2O3、β-Ga2O3、γ-Ga2O3、-Ga2O3and-Ga2O3Which can be converted into each other under certain conditions β -Ga2O3Is most stable and has a monoclinic structure at room temperature, and the spatial structure is C2/m, a =12.214 Å, b =3.037 Å, C =5.798 Å, β =103.83 degrees2O3Has excellent photoluminescence performance, chemical and thermal stability and other characteristics, and may be used widely in sensitive material, catalyst, photoelectronic material, fluorescent powder and other fields.
In recent years, IGZO (indium gallium zinc oxide) is applied to the field of TFT-L CD displays, so that the number of transistors is reduced, the light transmittance of each pixel is improved, the display has a higher energy efficiency level, and the efficiency is higher.
Currently, IGZO sputtering target materials sold In commercial markets are mainly sintered by solid-phase reaction hot pressing, and In is prepared by2O3ZnO and Ga2O3Mixing the three kinds of powder according to a certain proportion, ball-milling and homogenizing, hot-pressing and sintering and the like to prepare the IGZO target material for sputtering. The preparation method is simple to operate, but the uniformity of mechanical ball milling mixing is influenced by the granularity and the morphology of each powder. In2O3ZnO and Ga2O3The granularity, the shape, the fluidity and the dispersity of the powder play a decisive role in the homogenizing effect and the hot pressing process.
Chinese patent application CN108821329A discloses a method for preparing high purity gallium oxide, which comprises dissolving gallium metal in a mixed solution of sulfuric acid and hydrogen peroxide to obtain gallium sulfate solution, purifying by crystallization to obtain high purity gallium sulfate crystal, and calcining the sulfuric acid crystal to obtain high purity gallium oxide. Although the method can obtain high-purity gallium oxide, sulfur oxide-containing gas is generated in the calcining process, the obtained product is agglomerated, the uniformity of the crushed product is poor, the decomposition temperature of the sulfate is high, and the energy consumption is high.
Chinese patent application CN107010654B discloses a method for preparing monodisperse gallium oxide powder and its high-density ceramic target material. The invention uses more than 99.99% of metal gallium to dissolve in acid, then ammonia water is added for precipitation and aging to obtain white precipitate, and the product is obtained through procedures of washing, filtering, drying, calcining and the like. However, the method has high calcination temperature, the obtained product microscopic particles are easy to agglomerate, and the product uniformity is reduced.
The prior art can not obtain ellipsoidal nano-scale gallium oxide particles, and the obtained gallium oxide particles can not meet the requirements of fluidity and dispersibility.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of nano-scale gallium oxide, and the gallium oxide synthesized by the method has higher fluidity and dispersibility.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of nanoscale gallium oxide comprises the following steps:
s1, preparing a solution A, namely preparing a gallium nitrate solution, diluting the gallium nitrate solution until the gallium content is 25-55 g/L (0.358-0.789 mol/L) and the concentration of free nitric acid is 0.1-10%, and then adding a surfactant to obtain the solution A;
preparing an S2 solution and a B solution: preparing a precipitator into a solution with the mass fraction of 5-15% to obtain a solution B;
s3, preparing a base solution C: adding the solution B into pure water to prepare a base solution C solution, wherein the temperature of the base solution C solution is 15-40 ℃;
s4, precipitation reaction: simultaneously adding the solution A and the solution B into the solution C of the base solution to carry out precipitation reaction;
s5, and then carrying out aging reaction, centrifugal washing and calcination to obtain the nano-grade gallium oxide.
At present, the method commonly adopted in the high-purity gallium oxide industry is to precipitate gallium ions with ammonia water to obtain hydroxyl gallium oxide, and then calcine the hydroxyl gallium oxide to obtain a gallium oxide product. However, the gallium oxide obtained by the method is rod-shaped, and the rod-shaped structure has poor fluidity and dispersibility, so that the uniformity and density of the target are influenced when the target is prepared.
The preparation method aims at synthesizing ellipsoidal gallium oxide with the particle size D90= 700-1000 nm, and the particle size D90= 700-1000 nm is obtained by simultaneously adding the solution A and the solution B into the solution C of the base solution, and simultaneously limiting the reaction temperature, the concentrations of the solution A and the solution B and the feeding speeds of the solution A and the solution B; the shape of the solution is ellipsoidal by limiting the types of the precipitating agents and the concentrations of the solution A and the solution B. The gallium oxide prepared by the invention has higher fluidity and dispersibility than rod-shaped gallium oxide so as to meet the use requirement of a target material. The gallium oxide prepared by the invention has the following characteristics: high specific surface area, BET = 16-20 g/cm2(ii) a High purity (up to 99.995%) and nano-class granularity.
As a preferred embodiment of the preparation method of the present invention, in the step (1), the preparation method of the gallium nitrate solution comprises: dissolving the gallium nitrate crystal in pure water, and then adding nitric acid to obtain a gallium nitrate solution.
As a preferred embodiment of the preparation method, the mass ratio of the metal gallium to the surfactant is (100-200): 1.
AS a preferred embodiment of the preparation method of the present invention, in the step (1), the surfactant is at least one of dodecylbenzene sulfonic acid (L AS), sodium Alkyl Benzene Sulfonate (ABS), α -olefin sulfonate (AOS), and secondary alkyl sodium sulfonate (SAS).
In a preferred embodiment of the preparation method of the present invention, in the step (2), the precipitant is at least one of ammonia water, ammonium bicarbonate and sodium hydroxide.
More preferably, the precipitant is at least one of ammonia water and sodium hydroxide, and the ellipsoidal gallium oxide can be formed by using the precipitant. More preferably, the precipitant is ammonia water, and the ellipsoidal gallium oxide can be formed by using the precipitant, and the post-treatment operation is simple.
In a preferred embodiment of the preparation method of the present invention, in the step (3), the pH of the solution of the base solution C is 7.5 to 9.5.
As a preferable embodiment of the preparation method, in the step (4), the reaction temperature is 15-40 ℃, the volume ratio of the solution of the base solution C to the solution A is 1 (0.5-1.5), the feeding speed of the solution A is 20-50L/min, the feeding speed of the solution B is regulated to maintain the pH value of the system to be 7.5-9.5, the stirring is continued for 1-3 h after the feeding is finished, the temperature in the stirring process is 15-40 ℃, and the pH value is 7.5-9.5.
In the precipitation reaction, the volume ratio of the solution C as the base solution to the solution A is 1 (0.5-1.5), the dosage range of the solution B is not limited, and the pH value of the reaction system is maintained to be 7.5-9.5 by adjusting the speed of the solution B until the solution A is added.
And simultaneously adding the solution A and the solution B into the solution C of the base solution, and maintaining the pH value of the system to be 7.5-9.5 by regulating the feeding speed of the solution B to form a balanced reaction system, so that the control of granularity and morphology is facilitated. In the existing preparation method, the solution B is directly added into the solution A, the concentration of gallium ions is continuously changed, and the formed particles are different in size.
As a preferred embodiment of the preparation method, in the step (5), the temperature of the aging reaction is 75-115 ℃, the pH value is 7.5-9.5, and the time is 0.5-8 h.
As a preferable embodiment of the production method of the present invention, in the step (5), washing is performed until the washing water conductivity is less than 100. mu.S/cm.
As a preferred embodiment of the preparation method, in the step (5), the calcining temperature is 600-900 ℃ and the time is 4-12 h.
Compared with the prior art, the invention has the beneficial effects that: the method prepares the ellipsoidal nano-scale gallium oxide by simultaneously adding the solution A and the solution B into the solution C of the base solution, and simultaneously limiting the reaction temperature, the concentrations of the solution A and the solution B, the feeding speeds of the solution A and the solution B and the types of the precipitating agents. The gallium oxide prepared by the invention has the following characteristics: high specific surface area, BET16= 16-20 g/cm2(ii) a The purity is high and can reach 99.995%; the particle size can reach the nanometer level, and D90 is between 700 and 1000 nm.
Drawings
Fig. 1 is an SEM image of nano gallium oxide prepared in example 1.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1.
A preparation method of nano-scale gallium oxide comprises the following steps:
s1, preparing a gallium nitrate solution, namely adding 300L purified water into a dissolving kettle, heating to 50 ℃, then adding 329.53kg of gallium nitrate nonahydrate crystals with the purity of 99.999%, then adding 191kg of superior grade pure nitric acid with the content of 68%, then adding purified water to a constant volume of 1000L, filtering by a precision filter to obtain a gallium nitrate solution with the gallium content of 55 g/L and the free acidity of 10%, then adding 275g of ABS into the solution, and stirring until the solution is completely dissolved to obtain a solution A;
s2, preparing a precipitant solution, namely adding 1200L purified water into a precipitant storage tank, adding 300kg of high-grade pure ammonia water with the content of 25wt% to form a solution with the mass fraction of 5%, and stirring uniformly to obtain a solution B;
s3, preparing a base solution, namely adding 500L purified water into a reaction kettle, cooling to 15 ℃, adding 0.5L solution B to adjust the pH value to 9.5 to obtain a base solution C;
s4, carrying out precipitation reaction, namely adding the solution A and the solution B into the solution C of the base solution at the same time, controlling the reaction temperature to be 15 ℃, the pH value to be 9.5 and the feeding speed of the solution A to be 20L/min in the feeding process, regulating the feeding speed of the solution B to maintain the pH value of the system to be 9.5, and continuously stirring for 3 hours after the feeding is finished;
s5, aging reaction: heating to 75 ℃, stopping stirring, keeping the temperature at 75 ℃ and aging for 8h, and keeping the pH value of the system at 9.5 in the aging process.
And (3) suction filtration and washing: after the aging reaction is finished, starting stirring to make the slurry uniform, then pumping the slurry into a centrifuge, introducing purified water for washing until the conductivity of the washing water is less than 100 mu S/cm, carrying out high-speed centrifugation, spin-drying and discharging;
and (3) calcining: transferring the dried material to a quartz boat, putting the quartz boat into a tubular atmosphere furnace, introducing mixed gas of nitrogen and oxygen with a certain flow, calcining the quartz boat for 4 hours at 900 ℃, cooling the quartz boat to below 80 ℃, and discharging the quartz boat to obtain 72.5kg of nano gallium oxide with the yield of 98%.
The gallium oxide prepared in this example was sampled to detect impurities, and the ICP-MS test results are shown in table 1, and the laser particle size diagram is shown in fig. 1. As can be seen from Table 1 and FIG. 1, the product had a purity of 99.995%, a particle size D90 of 890 nm and a specific surface BET of 17.2g/cm2。
Table 1 ICP-MS test results for gallium oxide obtained in example 1.
| Impurity element | Na | Mg | Ca | Cr | Mn | Fe | Co | Ni | Cu | Zn | In | Pb |
| Content/ppm | 0.10 | ＜0.1 | 0.13 | ＜0.1 | ＜0.1 | 0.25 | ＜0.1 | ＜0.1 | ＜0.1 | 0.20 | ＜0.1 | 0.18 |
Example 2.
A preparation method of nano-scale gallium oxide comprises the following steps:
s1, preparing a gallium nitrate solution, namely adding 300L purified water into a dissolving kettle, heating to 50 ℃, then adding 149.79kg of gallium nitrate nonahydrate crystals with the purity of 99.999%, then adding 1.5kg of superior grade pure nitric acid with the content of 68%, then adding purified water to reach the constant volume of 1000L, filtering by a precision filter to obtain a gallium nitrate solution with the gallium content of 25 g/L and the free acidity of 0.1%, then adding 250g of ABS into the solution, and stirring until the solution is completely dissolved to obtain a solution A;
s2, preparing a precipitant solution, namely adding 400L of purified water into a precipitant storage tank, adding 600kg of high-grade pure ammonia water with the content of 25wt% to form a solution with the mass fraction of 15%, and stirring uniformly to obtain a solution B;
s3, preparing a base solution, namely adding 1500L purified water into a reaction kettle, heating to 40 ℃, adding 0.8L solution B to adjust the pH value to 7.5 to obtain a base solution C;
s4, carrying out precipitation reaction, namely adding the solution A and the solution B into the solution C of the base solution at the same time, controlling the reaction temperature to be 40 ℃, the pH value to be 7.5 and the feeding speed of the solution A to be 50L/min in the feeding process, regulating the feeding speed of the solution B to maintain the pH value of the system to be 7.5, and continuously stirring for 1h after the feeding is finished;
s5, aging reaction: heating to 115 ℃, stopping stirring, keeping the temperature at 115 ℃ and aging for 0.5h, and keeping the pH value of the system at 7.5 in the aging process.
And (3) suction filtration and washing: and after the aging reaction is finished, starting stirring to make the slurry uniform, then pumping the slurry into a centrifuge, introducing purified water for washing until the conductivity of the washing water is less than 100 mu S/cm, carrying out high-speed centrifugation, spin-drying and discharging.
And (3) calcining: transferring the dried material to a quartz boat, putting the quartz boat into a tubular atmosphere furnace, introducing mixed gas of nitrogen and oxygen with a certain flow, calcining the quartz boat for 12 hours at the temperature of 600 ℃, cooling the quartz boat to the temperature below 80 ℃, and discharging the quartz boat to obtain 33.28kg of nano-scale gallium oxide with the yield of 99%.
The gallium oxide prepared in this example was sampled to detect impurities, and the ICP-MS test results are shown in table 2, with a laser particle size distribution diagram highly similar to that of fig. 1. As can be seen from Table 2, the product had a purity of 99.995%, a particle size D90 of 790 nm and a specific surface BET of 16.7g/cm2。
Table 2 ICP-MS test results for gallium oxide obtained in example 2.
| Impurity element | Na | Mg | Ca | Cr | Mn | Fe | Co | Ni | Cu | Zn | In | Pb |
| Content/ppm | 0.10 | ＜0.1 | 0.15 | ＜0.1 | ＜0.1 | 0.19 | ＜0.1 | ＜0.1 | ＜0.1 | 0.23 | ＜0.1 | 0.12 |
Example 3.
A preparation method of nano-scale gallium oxide comprises the following steps:
s1, preparing a gallium nitrate solution, namely adding 300L purified water into a dissolving kettle, heating to 50 ℃, then adding 239.66kg of gallium nitrate nonahydrate crystals with the purity of 99.999%, then adding 88kg of superior grade pure nitric acid with the content of 68%, then adding the purified water to a constant volume of 1000L, filtering by a precision filter to obtain a gallium nitrate solution with the gallium content of 40 g/L and the free acidity of 5.0%, then adding 266g of ABS into the solution, and stirring until the solution is completely dissolved to obtain a solution A;
s2, preparing a precipitant solution, namely adding 600L purified water into a precipitant storage tank, adding 400kg of high-grade pure ammonia water with the content of 25wt% to form a solution with the mass fraction of 10%, and stirring uniformly to obtain a solution B;
s3, preparing a base solution, namely adding 1000L purified water into a reaction kettle, cooling to 25 ℃, adding 1L solution B to adjust the pH value to 8.0 to obtain a base solution C;
s4, carrying out precipitation reaction, namely adding the solution A and the solution B into the solution C of the base solution at the same time, controlling the reaction temperature to be 25 ℃, the pH value to be 8.0 and the feeding speed of the solution A to be 30L/min in the feeding process, regulating the feeding speed of the solution B to maintain the pH value of the system to be 8.0, and continuously stirring for 2 hours after the feeding is finished;
s5, aging reaction: heating to 85 ℃, stopping stirring, keeping the temperature at 85 ℃, and aging for 4 hours, wherein the pH value of the system is kept at 8.5 in the aging process.
And (3) suction filtration and washing: and after the aging reaction is finished, starting stirring to make the slurry uniform, then pumping the slurry into a centrifuge, introducing purified water for washing until the conductivity of the washing water is less than 100 mu S/cm, carrying out high-speed centrifugation, spin-drying and discharging.
And (3) calcining: transferring the dried material to a quartz boat, putting the quartz boat into a tubular atmosphere furnace, introducing mixed gas of nitrogen and oxygen with a certain flow, calcining the quartz boat for 10 hours at 700 ℃, cooling the quartz boat to below 80 ℃, and discharging the quartz boat to obtain 51.95kg of nano gallium oxide with the yield of 96.6 percent.
The gallium oxide prepared in this example was sampled to detect impurities, and the ICP-MS test results are shown in table 3, with a laser particle size distribution diagram highly similar to that of fig. 1. As can be seen from Table 3, the product had a purity of 99.995%, a particle size D90 of 910 nm and a specific surface BET of 16.2g/cm2。
Table 3 ICP-MS test results for gallium oxide obtained in example 3.
| Impurity element | Na | Mg | Ca | Cr | Mn | Fe | Co | Ni | Cu | Zn | In | Pb |
| Content/ppm | ＜0.1 | ＜0.1 | 0.13 | ＜0.1 | ＜0.1 | 0.25 | ＜0.1 | ＜0.1 | ＜0.1 | 0.20 | ＜0.1 | 0.18 |
In summary, compared with the prior art, the invention has the beneficial effects that: the method prepares the ellipsoidal nano-scale gallium oxide by simultaneously adding the solution A and the solution B into the solution C of the base solution, and simultaneously limiting the reaction temperature, the concentrations of the solution A and the solution B, the feeding speeds of the solution A and the solution B and the types of the precipitating agents. The gallium oxide prepared by the invention has the following characteristics: high specific surface area, BET16= 16-20 g/cm2(ii) a The purity is high and can reach 99.995%; the particle size can reach the nanometer level, and D90 is between 700 and 1000 nm.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A preparation method of nano-scale gallium oxide is characterized by comprising the following steps:
s1, preparing a solution A, namely preparing a gallium nitrate solution, diluting the gallium nitrate solution until the content of gallium is 25-55 g/L and the concentration of free nitric acid is 0.1-10%, and then adding a surfactant to obtain the solution A;
preparing an S2 solution and a B solution: preparing a precipitator into a solution with the mass fraction of 5-15% to obtain a solution B;
s3, preparing a base solution C: adding the solution B into pure water to prepare a base solution C solution, wherein the temperature of the base solution C solution is 15-40 ℃;
s4, precipitation reaction: simultaneously adding the solution A and the solution B into the solution C of the base solution to carry out precipitation reaction;
s5, and then carrying out aging reaction, centrifugal washing and calcination to obtain the nano-grade gallium oxide.
2. The method according to claim 1, wherein in S1, the gallium nitrate solution is prepared by: gallium nitrate crystals are dissolved in purified water, and then nitric acid is added to adjust the free acid content of the solution.
3. The preparation method according to claim 2, wherein the mass ratio of the metal gallium to the surfactant is (100-200): 1.
4. the method according to claim 1, wherein in the step (1), the surfactant is at least one of dodecylbenzene sulfonic acid, sodium alkylbenzenesulfonate, α -olefin sulfonate, and secondary sodium alkyl sulfonate.
5. The method according to claim 1, wherein in the step (2), the precipitant is at least one of ammonia water, ammonium bicarbonate and sodium hydroxide.
6. The method according to claim 1, wherein in the step (3), the pH of the solution of the base solution C is 7.5 to 9.5.
7. The preparation method according to claim 1, wherein in the step (4), the reaction temperature is 15-40 ℃, the volume ratio of the solution of the base solution C to the solution A is 1 (0.5-1.5), the feeding speed of the solution A is 20-50L/min, the feeding speed of the solution B is regulated to maintain the pH value of the system to be 7.5-9.5, the stirring is continued for 1-3 h after the feeding is finished, the temperature in the stirring process is 15-40 ℃, and the pH value is 7.5-9.5.
8. The method according to claim 1, wherein in the step (5), the aging reaction is carried out at a temperature of 75 to 115 ℃ and a pH of 7.5 to 9.5 for a period of 0.5 to 8 hours.
9. The production method according to claim 1, wherein in the step (5), washing is carried out until the washing water conductivity is less than 100. mu.S/cm.
10. The method according to claim 1, wherein in the step (5), the calcining temperature is 600 to 900 ℃ and the calcining time is 4 to 12 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114408970A (en) * | 2022-01-25 | 2022-04-29 | 重庆邮电大学 | Preparation method of hollow mesoporous carbon-doped gallium sesquioxide nanospheres and product thereof |
| CN116332224A (en) * | 2023-03-22 | 2023-06-27 | 广东长信精密设备有限公司 | Spherical gallium oxide and preparation process thereof |
-
2020
- 2020-05-21 CN CN202010435973.3A patent/CN111439778A/en active Pending
Non-Patent Citations (1)
| Title |
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| 柯文明等: ""沉淀法制备超高致密度GZO陶瓷靶材用纳米氧化镓"", 《中国陶瓷》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114408970A (en) * | 2022-01-25 | 2022-04-29 | 重庆邮电大学 | Preparation method of hollow mesoporous carbon-doped gallium sesquioxide nanospheres and product thereof |
| CN114408970B (en) * | 2022-01-25 | 2023-07-18 | 重庆邮电大学 | Preparation method of hollow mesoporous carbon-doped gallium trioxide nanospheres and product thereof |
| CN116332224A (en) * | 2023-03-22 | 2023-06-27 | 广东长信精密设备有限公司 | Spherical gallium oxide and preparation process thereof |
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