CN111170746B - Method for preparing silicon oxynitride powder in air atmosphere - Google Patents
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Abstract
The invention discloses a method for preparing silicon oxynitride powder in an air atmosphere. According to the method, silicon powder is used as a raw material, silicon powder accumulation bodies with different particle sizes and thicknesses are subjected to nitrogen oxidation synthesis under the conditions of normal pressure and high temperature, and then an upper-layer micro-sintered state and a small amount of side products are removed to obtain a finished product of the silicon oxynitride powder. Compared with the prior art, the invention not only ensures that impurities such as silicon oxide, silicon nitride and the like generated by the nitrogen oxidation reaction are easy to separate from the silicon oxynitride, thereby greatly improving the product purity, but also has very high yield, and utilizes normal pressure air as nitrogen and oxygen sources, thereby saving the cost, ensuring that the preparation method has simple process, easy operation and low cost, and is suitable for industrial large-scale production.
Description
Technical Field
The invention relates to the technical field of preparation of inorganic nonmetal powder materials, in particular to a method for preparing silicon oxynitride powder in an air atmosphere.
Background
Silicon oxynitride (Si)2N2O) is widely applied to high-temperature structural materials and refractory materials because of the excellent thermal shock resistance, high-temperature strength, high-temperature oxidation resistance and low thermal expansion coefficient. In the prior art, there are many methods for preparing silicon oxynitride powder, wherein a direct nitrogen oxidation reaction of silicon powder in a nitrogen-oxygen mixed gas or a direct nitrogen oxidation reaction of silicon powder is adopted, and the direct nitrogen oxidation of silicon powder is not only low in cost but also capable of avoiding impurity pollution, and is one of the more common methods.
However, as the literature is bright, etc. the conditions of gas phase nitridation and oxynitridation of crystalline silicon micropowder (materials science and engineering report 2010,28(3):416-2And O2The reaction has a kinetic competition relationship, and the nitrogen oxide product has obvious gradient, namely the generated product sequentially comprises silicon oxide, a mixed layer of the silicon oxide and the silicon oxide nitride, nitrogen oxide from top to bottomThe gradient phenomena of a silicon layer, a mixed layer of silicon oxynitride and silicon nitride, a silicon nitride layer, residual silicon and the like easily cause small gradient distance of a pure silicon oxynitride phase along the direction of reaction gas flow if the proportion of oxygen and nitrogen and the oxygen partial pressure are not well controlled, so that the prepared finished product of the nitrogen oxide usually contains cristobalite and a silicon nitride byproduct phase or residual silicon and is difficult to obtain a pure-phase silicon oxynitride product sample, thereby causing low yield of silicon oxynitride powder. In addition, in the literature, a mixed gas of nitrogen and oxygen in a micro-positive pressure flowing state is used as an oxygen and nitrogen source, and when most of oxygen is consumed on the upper layer of the silicon material accumulation body, oxygen can still be rapidly supplemented into the accumulation body, so that the amount of upper silicon powder required to be consumed is greatly increased. Therefore, it is necessary to develop a silicon oxynitride synthesized by direct nitrogen oxidation reaction, which can improve the purity of silicon oxynitride product and reduce the loss of silicon powder.
Disclosure of Invention
On the basis of overcoming the defects of the prior art, the invention provides a method for preparing silicon oxynitride powder under an air atmosphere, which takes silicon powder as a raw material, carries out oxynitride synthesis under the condition of high temperature of 1350-1500 ℃ by using silicon powder accumulation bodies with different grain diameters and thicknesses and using nitrogen and oxygen mixed gas of air under normal pressure and static state as an oxygen and nitrogen source, and then removes an upper micro-sintered state and a small amount of edges to obtain a silicon oxynitride powder finished product.
In order to realize the purpose, the technical scheme is as follows:
on the one hand, the method for preparing the silicon oxynitride powder in the air atmosphere comprises the following steps:
(1) charging: loosely loading the silicon powder I into a ceramic sagger, wherein the loose thickness is 15-100 mm, and covering the silicon powder II on the accumulated body of the silicon powder I, and the covering thickness is 5-15 mm;
(2) nitrogen oxidation synthesis reaction: placing the ceramic sagger in the step (1) in a uniform temperature zone of a high-temperature furnace, rapidly heating to 1000 ℃ at a heating rate of 10-20 ℃/min, then heating to 1350-1500 ℃ at a heating rate of 2-5 ℃/min, preserving heat for 2-4 h for nitrogen oxidation synthesis, then cooling to room temperature along with the furnace, and discharging;
(3) obtaining a finished product: after the synthetic reaction of the nitrogen oxide, the lower layer product is white and fluffy, the powder for covering the upper layer is in a micro-sintered state, and the upper layer micro-sintered product and a small amount of product at the contact part of the edge part and the ceramic sagger are removed to obtain the finished product of the silicon oxynitride powder.
Furthermore, in the step 1, the average grain diameter of the silicon powder I is 0.5-2 μm.
Further, in the step 1, the oxygen content of the silicon powder I is less than 2%.
Furthermore, the average particle size of the silicon powder II in the step 1 is 10-30 μm.
In another aspect, a silicon oxynitride powder prepared by the above preparation method is provided.
The invention has the following positive effects:
1. according to the invention, the large-particle silicon powder (II) is covered on the small-particle silicon powder (I) accumulation body, and the large-particle silicon powder (II) is oxidized into a micro-sintering state in the rapid heating process, so that the porosity can be reduced, the oxygen partial pressure of the lower silicon powder (I) accumulation body can be in the interval range of silicon oxynitride thermodynamic equilibrium, and the yield of silicon oxynitride can be improved. Meanwhile, micro-sintered-state heterogeneous products formed by the large-particle silicon powder (II) accumulation body on the upper layer are easier to separate from white fluffy silicon oxynitride generated by oxidation of the small-particle silicon powder (I) accumulation body on the lower layer, so that the situation that in the prior art, silicon oxide, silicon nitride and other heterogeneous phases generated by directly performing nitrogen oxidation reaction on silicon powder with the same particle size are more and cannot be separated from the silicon oxynitride is greatly changed.
In addition, the particle size, the thickness and the like of the upper layer silicon powder and the lower layer silicon powder are adjusted within a reasonable process condition range, so that the proportion of oxygen and nitrogen required by the lower layer silicon powder (I) accumulation body is ensured, the controllable adjustment of the proportion of oxygen and nitrogen is realized, the proportion of producing silicon oxynitride is improved, and the product purity is improved.
Therefore, the invention adopts the direct nitrogen oxidation method to synthesize the finished product of the silicon oxynitride powder, the product is fluffy and easy to crush, the purity and the yield of the product are greatly improved, the product only contains the silicon oxynitride phase detected by an X-ray powder diffractometer, the oxygen content in the product is 15.9 to 16.3 percent detected by an oxygen-nitrogen analyzer, and the yield is over 91 percent (calculated by the amount of the silicon powder (I)).
2. The invention adopts the nitrogen-oxygen mixed gas of air under normal pressure static state to replace the nitrogen-oxygen mixed gas of micro-positive pressure circulating air as the oxygen and nitrogen source, firstly, the condition that oxygen can still be rapidly supplemented into the accumulation body at the lower layer after most of oxygen is consumed at the upper layer of the silicon material accumulation body is reduced, thereby reducing the loss of large-particle silicon powder (II) at the upper layer and saving the cost. Secondly, air is used as a nitrogen source and an oxygen source, and the cost is saved by directly adopting nitrogen and oxygen; thirdly, the requirement on equipment by adopting the normal pressure condition is further reduced.
Drawings
FIG. 1 is an XRD spectrum of a silicon oxynitride powder in example 1 of the present invention.
Detailed Description
The present invention is further described in the following examples, which should not be construed as limiting the scope of the invention, but rather as providing the following examples which are set forth to illustrate and not limit the scope of the invention.
Example 1
Taking silicon powder (I) with the average particle diameter of 1.12 mu m and the oxygen content of 1.51 percent, and loosely loading the silicon powder (I) into a ceramic sagger, wherein the loose loading thickness is 60 mm; then, large-particle silicon powder (II) with an average particle size of 15 μm is covered on the accumulated body of the silicon powder (I) to a thickness of 5 mm. Placing the ceramic sagger in a uniform temperature zone of a high-temperature furnace, heating to 1000 ℃ at a heating rate of 10 ℃/min, subsequently heating to 1380 ℃ at a heating rate of 5 ℃/min, and preserving heat for 3.5 hours to carry out nitrogen oxidation synthesis reaction; and then cooling to room temperature along with the furnace and discharging. After the synthetic reaction of the nitrogen oxide, the lower layer product is white and fluffy, the powder for covering the upper layer is in a micro-sintered state, and the upper layer micro-sintered product and a small amount of product at the contact part of the edge part and the ceramic sagger are removed to obtain the finished product of the silicon oxynitride powder.
The obtained silicon oxynitride powder finished product is fluffy and easy to crush, the product purity is high, only a silicon oxynitride phase is contained in the product detected by an X-ray powder diffractometer, and an X-ray diffraction powder diagram is shown in an attached figure 1. The oxygen content in the product was found to be 16.1% by an oxygen nitrogen analyzer. The yield of the silicon oxynitride powder was 93% (calculated based on the amount of silicon powder (I)).
Example 2
Taking silicon powder (I) with the average particle diameter of 1.93 mu m and the oxygen content of 0.91 percent, and loosely loading the silicon powder (I) into a ceramic sagger, wherein the loose loading thickness is 40 mm; then, large-particle silicon powder (II) with an average particle size of 15 μm is covered on the accumulated body of the silicon powder (I) to a thickness of 20 mm. Placing the ceramic sagger in a uniform temperature zone of a high-temperature furnace, heating to 1000 ℃ at a heating rate of 20 ℃/min, subsequently heating to 1420 ℃ at a heating rate of 4 ℃/min, and preserving heat for 4 hours to carry out a nitrogen oxidation synthesis reaction; and then cooling to room temperature along with the furnace and discharging. After the synthetic reaction of the nitrogen oxide, the lower layer product is white and fluffy, the powder for covering the upper layer is in a micro-sintered state, and the upper layer micro-sintered product and a small amount of product at the contact part of the edge part and the ceramic sagger are removed to obtain the finished product of the silicon oxynitride powder.
The obtained finished product of the silicon oxynitride powder is fluffy and easy to crush, the product purity is high, and only a silicon oxynitride phase is contained in the product detected by an X-ray powder diffractometer. The oxygen content in the product was 15.9% as determined by an oxygen nitrogen analyzer. The yield of the silicon oxynitride powder was 92% (calculated on the amount of silicon powder (I)).
Example 3
Taking silicon powder (I) with the average particle diameter of 0.68 mu m and the oxygen content of 1.96 percent, and loosely filling the silicon powder (I) into a ceramic sagger, wherein the loose filling thickness is 100 mm; then, large-particle silicon powder (II) with an average particle size of 24 μm is covered on the accumulated body of the silicon powder (I) to a thickness of 10 mm. Placing the ceramic sagger in a uniform temperature zone of a high-temperature furnace, heating to 1000 ℃ at a heating rate of 15 ℃/min, subsequently heating to 1400 ℃ at a heating rate of 5 ℃/min, and preserving heat for 2.5 hours to carry out a nitrogen oxidation synthesis reaction; and then cooling to room temperature along with the furnace and discharging. After the synthetic reaction of the nitrogen oxide, the lower layer product is white and fluffy, the powder for covering the upper layer is in a micro-sintered state, and the upper layer micro-sintered product and a small amount of product at the contact part of the edge part and the ceramic sagger are removed to obtain the finished product of the silicon oxynitride powder.
The obtained finished product of the silicon oxynitride powder is fluffy and easy to crush, the product purity is high, and only a silicon oxynitride phase is contained in the product detected by an X-ray powder diffractometer. The oxygen content in the product was 16.2% as determined by an oxygen nitrogen analyzer. The yield of the silicon oxynitride powder was 95% (calculated based on the amount of silicon powder (I)).
Example 4
Taking silicon powder (I) with the average particle diameter of 0.94 mu m and the oxygen content of 1.04 percent, and loosely loading the silicon powder (I) into a ceramic sagger, wherein the loose loading thickness is 80 mm; then, large-particle silicon powder (II) with an average particle size of 12 μm is covered on the accumulated body of the silicon powder (I) to a thickness of 12 mm. Placing the ceramic sagger in a uniform temperature zone of a high-temperature furnace, heating to 1000 ℃ at a heating rate of 15 ℃/min, then heating to 1480 ℃ at a heating rate of 2 ℃/min, and preserving heat for 2 hours to carry out a nitrogen oxidation synthesis reaction; and then cooling to room temperature along with the furnace and discharging. After the synthetic reaction of the nitrogen oxide, the lower layer product is white and fluffy, the powder for covering the upper layer is in a micro-sintered state, and the upper layer micro-sintered product and a small amount of product at the contact part of the edge part and the ceramic sagger are removed to obtain the finished product of the silicon oxynitride powder.
The obtained finished product of the silicon oxynitride powder is fluffy and easy to crush, the product purity is high, and only a silicon oxynitride phase is contained in the product detected by an X-ray powder diffractometer. The oxygen content in the product was 16.0% as determined by an oxygen nitrogen analyzer. The yield of the silicon oxynitride powder was 95% (calculated based on the amount of silicon powder (I)).
Example 5
Taking silicon powder (I) with the average particle diameter of 1.51 mu m and the oxygen content of 1.31 percent, and loosely loading the silicon powder (I) into a ceramic sagger, wherein the loose loading thickness is 50 mm; then, large-particle silicon powder (II) with an average particle size of 28 μm was coated on the above silicon powder (I) stack to a thickness of 8 mm. Placing the ceramic sagger in a uniform temperature zone of a high-temperature furnace, heating to 1000 ℃ at a heating rate of 20 ℃/min, subsequently heating to 1450 ℃ at a heating rate of 4 ℃/min, and preserving heat for 4 hours to carry out a nitrogen oxidation synthesis reaction; and then cooling to room temperature along with the furnace and discharging. After the synthetic reaction of the nitrogen oxide, the lower layer product is white and fluffy, the powder for covering the upper layer is in a micro-sintered state, and the upper layer micro-sintered product and a small amount of product at the contact part of the edge part and the ceramic sagger are removed to obtain the finished product of the silicon oxynitride powder.
The obtained finished product of the silicon oxynitride powder is fluffy and easy to crush, the product purity is high, and only a silicon oxynitride phase is contained in the product detected by an X-ray powder diffractometer. The oxygen content in the product was 16.2% as determined by an oxygen nitrogen analyzer. The yield of the silicon oxynitride powder was 91% (calculated based on the amount of silicon powder (I)).
Example 6
Taking silicon powder (I) with the average particle diameter of 1.75 mu m and the oxygen content of 1.28 percent, and loosely loading the silicon powder (I) into a ceramic sagger, wherein the loose loading thickness is 55 mm; then, large-particle silicon powder (II) with an average particle size of 18 μm is covered on the accumulated body of the silicon powder (I) to a thickness of 15 mm. Placing the ceramic sagger in a uniform temperature zone of a high-temperature furnace, heating to 1000 ℃ at a heating rate of 12 ℃/min, subsequently heating to 1500 ℃ at a heating rate of 5 ℃/min, and preserving heat for 2 hours to carry out a nitrogen oxidation synthesis reaction; and then cooling to room temperature along with the furnace and discharging. After the synthetic reaction of the nitrogen oxide, the lower layer product is white and fluffy, the powder for covering the upper layer is in a micro-sintered state, and the upper layer micro-sintered product and a small amount of product at the contact part of the edge part and the ceramic sagger are removed to obtain the finished product of the silicon oxynitride powder.
The obtained finished product of the silicon oxynitride powder is fluffy and easy to crush, the product purity is high, and only a silicon oxynitride phase is contained in the product detected by an X-ray powder diffractometer. The oxygen content in the product was found to be 16.3% by an oxygen nitrogen analyzer. The yield of the silicon oxynitride powder was 93% (calculated based on the amount of silicon powder (I)).
From the above examples 1 to 6, it is known that, in contrast to the prior art, for example: bright, etc. the crystalline silicon micro powder is subjected to gas phase nitridation and nitrogen oxidation conditions (material science and engineering bullets, 2010,28(3): 416-: firstly, the product is fluffy and easy to crush; secondly, the purity is greatly improved, an X-ray powder diffractometer is used for detecting the purity, the literature is 84.2%, the product only contains a silicon oxynitride phase, an oxygen analyzer is used for detecting the oxygen content in the product to be 15.9% -16.3%, and the purity of the silicon oxynitride product is further proved to be very high; finally, the yield of the silicon oxynitride powder obtained by the invention is very high, and is more than 91 percent.
Claims (2)
1. A method for preparing silicon oxynitride powder in an air atmosphere is characterized by comprising the following steps:
(1) charging: loosely loading silicon powder I with the average particle size of 0.5-2 mu m and the oxygen content of less than 2% into a ceramic sagger, wherein the loose loading thickness is 15-100 mm, covering silicon powder II with the average particle size of 10-30 mu m on a silicon powder I accumulation body, and covering the silicon powder II with the thickness of 5-15 mm;
(2) nitrogen oxidation synthesis reaction: placing the ceramic sagger in the step (1) in a uniform temperature zone of a high-temperature furnace, rapidly heating to 1000 ℃ at a heating rate of 10-20 ℃/min, then heating to 1350-1500 ℃ at a heating rate of 2-5 ℃/min, preserving heat for 2-4 h for nitrogen oxidation synthesis, then cooling to room temperature along with the furnace, and discharging;
(3) obtaining a finished product: after the synthetic reaction of the nitrogen oxide, the lower layer product is white and fluffy, the powder for covering the upper layer is in a micro-sintered state, and the upper layer micro-sintered product and a small amount of product at the contact part of the edge part and the ceramic sagger are removed to obtain the finished product of the silicon oxynitride powder.
2. A silicon oxynitride powder produced by the production method according to claim 1.
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