CN113105246B - Method for rapidly preparing pure-phase AlON fine powder by one-step temperature rise carbon thermal reduction nitridation - Google Patents
Method for rapidly preparing pure-phase AlON fine powder by one-step temperature rise carbon thermal reduction nitridation Download PDFInfo
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Abstract
The invention relates to a method for rapidly preparing pure-phase AlON fine powder by one-step heating and carbon thermal reduction nitridation, belonging to the technical field of ceramic powder preparation. A method for rapidly preparing pure-phase AlON fine powder by one-step temperature rise carbon thermal reduction nitridation comprises the steps of firstly, heating alpha-Al 2 O 3 Ball milling the powder, and then carrying out ball milling on the alpha-Al 2 O 3 Adding the powder and glucose powder into water to obtain alpha-Al 2 O 3 And glucose; the obtained slurry is hydrothermally synthesized into alpha-Al in a reaction kettle 2 O 3 C, washing and drying the mixed powder; drying the alpha-Al 2 O 3 the/C mixed powder is placed in a carbon furnace to synthesize pure-phase AlON powder in nitrogen atmosphere; and (3) insulating the pure-phase AlON powder in an air environment at 600-680 ℃ for 2-6 h to remove residual C, thus obtaining the AlON powder. The powder synthesized by the method is pure-phase AlON, the primary particle size of the powder is small, and the particle refinement is easy to realize through common ball milling, so that AlON fine powder is obtained.
Description
Technical Field
The invention relates to a method for rapidly preparing pure-phase AlON fine powder by one-step heating and carbon thermal reduction nitridation, belonging to the technical field of ceramic powder preparation.
Background
AlON transparent ceramic not only has excellent light transmission, but also has better mechanical property, is a structural function integrated material with good comprehensive performance, can be widely used in various fields such as national defense and safety, energy and information, and is known as one of the most promising transparent ceramic materials in the 21 st century.
The preparation of the AlON transparent ceramic mainly comprises two ways: one is Al 2 O 3 And the AlN powder and the AlON powder are directly subjected to high-temperature solid-phase reaction, and the AlON powder is firstly prepared and then is subjected to densification sintering. In general andin recent years, the preparation of transparent ceramics by first synthesizing the AlON powder and then sintering the AlON powder is favored by researchers. Therefore, the preparation of the high-purity, superfine and high-activity AlON powder becomes a key influencing the research and development of the AlON transparent ceramic.
Among three main methods for synthesizing AlON, namely solid-phase reaction, aluminothermic reduction nitridation and carbothermic reduction nitridation, the carbothermic reduction nitridation method has the advantages of high product purity, small granularity and easiness in realizing batch production. Therefore, many studies have been made in recent years on the carbothermic reduction of the nitrogen compound AlON powder. For example: qiang Liu et Al at Jiangsu university as gamma-Al 2 O 3 And carbon black as raw materials, and performing carbothermal reduction nitridation by two-step temperature rise, namely firstly raising the temperature to 1550 ℃ and preserving the temperature for 1h, and then continuing raising the temperature to 1750 ℃ and preserving the temperature for 2h to obtain pure-phase AlON powder, wherein the particle sizes of the powder after ball milling for 12h and 24h are respectively 3.36 mu m and 1.38 mu m (Ceramics International 42(2016) 8290-8295); yingying Wang at the university of Jinan, with Al 2 O 3 And carbon black are taken as raw materials, and D is synthesized by combining 10 ℃/min with 3 ℃/min and adopting two-stage heat preservation (the temperature at 1550 ℃ is preserved for 1h + the temperature at 1750 ℃ is preserved for 2h) 50 AlON powder 45.32 μm, ball milled for 6h by liquid nitrogen, the particle size is reduced to 3.08 μm (Ceramics International 44(2018) 471-; dalian maritime university uses Al 2 O 3 And activated carbon as raw materials, heating to 1550 ℃ at a speed of 10-30 ℃/min for 1h, then continuously heating to 1750 ℃ for 1h, ball-milling the synthesized AlON powder at 170rpm for 24h to obtain powder with bimodal particle size distribution and particle size range of 1-8 mu m (Ceramics International 41 (2015)) 3992-3998, a method for preparing pure-phase AlON transparent ceramic powder in batches, 201210338387.2, and a method for preparing gamma-AlON transparent ceramic powder, 201410038534.3.
In order to prepare fine-grained AlON powder, researchers adopt a thermal cracking method to prepare Al 2 O 3 And performing carbothermal reduction and nitridation on the/C core-shell structure precursor to synthesize AlON powder. These studies generally used gamma-Al 2 O 3 As raw material, the carbothermic reduction nitridation process needs two-step heat preservation, and the total heat preservation is carried outThe time is usually more than or equal to 3 h. Xihai Jin et Al use nano gamma-Al 2 O 3 Preparing Al 2 O 3 UFR core-shell structure precursor, and then obtaining Al by thermal cracking at 800 DEG C 2 O 3 Synthesizing AlON powder by utilizing two-step carbon thermal reduction nitridation (keeping the temperature at 1550 ℃ for 2h and then continuing to rise to 1700-1720 ℃ for 2h), wherein the particle size of the powder subjected to ball milling for 2h is less than 0.9 mu m (J.Am.Ceram.Soc.95(2012) 2801-; Gamma-Al of 50nm is used by Valid Sabaghi 2 O 3 Thermal cracking with PAN at 800 ℃ for 2h to obtain Al 2 O 3 a/C core-shell structure, then preserving heat at 1550 ℃ for 2h, then preserving heat at 1750 ℃ for 1h, and carrying out carbothermal reduction nitridation, wherein the synthesized AlON powder is rod-shaped, has the length of 2-3 mu m and the width of submicron (Ceramics International 45(2019) 3350-3358).
As can be seen, Al with a core-shell structure is synthesized by a carbon coating technology 2 O 3 The method is an effective technical approach for obtaining fine-particle AlON powder by mixing the/C powder and then carrying out carbothermal reduction nitridation. However, thermal cracking of the precursor proceeds at high temperature to form Al having a core-shell structure 2 O 3 Harmful substances can be released in the/C process, the subsequent carbothermic reduction nitridation process still has the problems of long heat preservation time, low efficiency and high energy consumption, and the synthesized powder has large primary particle size and is not beneficial to the subsequent fine powder preparation and the densification sintering of transparent ceramics. Therefore, a technology for preparing the AlON fine powder, which is simple, easy, energy-saving, environment-friendly, efficient and low-cost, needs to be explored, and if the preparation of the AlON fine powder can be realized under the condition of low equipment requirement, the research and development process of the AlON transparent ceramic can be further promoted.
Disclosure of Invention
The invention aims to provide a catalyst based on alpha-Al 2 O 3 And a method for rapidly preparing pure-phase AlON fine powder by one-step heating of glucose powder and carbothermal reduction nitridation. The method firstly reduces alpha-Al by ball milling 2 O 3 The combination among powder particles improves the specific surface area and the dispersibility of the powder, and then glucose is used as a carbon source for hydro-thermal synthesis of carbon-coated Al 2 O 3 The core-shell structure is mixed with the powder, and then the pure-phase AlON fine powder is rapidly prepared by further heating and carbon thermal reduction nitridation. TheThe powder synthesized by the method is pure-phase AlON, the primary particle size of the powder is small, and the particle refinement is easy to realize through common ball milling, so that AlON fine powder is obtained. The method has the advantages of stable quality of raw materials, low price, low cost and Al 2 O 3 The temperature of the preparation process of the/C core-shell structure mixed powder is low, the requirement on equipment is not high, the process is simple and easy to implement, the process is environment-friendly, the temperature rise speed range in the carbothermic nitridation process is wide (10-50 ℃/min), a one-step temperature rise process is adopted (heat preservation is not needed before the synthesis temperature is reached), the powder synthesis temperature is not high (1700-. Therefore, the method has the characteristics of short time, high efficiency and low energy consumption in the carbothermic reduction nitridation process, and the product is single-phase AlON, has small primary particle size, weak combination among particles and easy particle refinement, and is favorable for improving the purity of powder. The whole process is simple and easy to implement, low in cost, energy-saving and environment-friendly, and the industrialization of pure-phase AlON fine powder is easy to realize.
A method for rapidly preparing pure-phase AlON fine powder by one-step temperature-rise carbon thermal reduction nitridation comprises the following process steps: firstly, alpha-Al is added 2 O 3 Ball milling the powder, and then carrying out ball milling on the alpha-Al 2 O 3 Adding the powder and glucose powder into water according to the mass ratio of 1.8: 1-1: 1 to obtain alpha-Al 2 O 3 And glucose; the obtained slurry is put into a reaction kettle for 24 hours of heat preservation at 180 ℃ to hydrothermally synthesize alpha-Al 2 O 3 C, washing and drying the mixed powder; drying the obtained alpha-Al 2 O 3 Placing the/C mixed powder in a carbon furnace, directly heating to 1700-1750 ℃ by adopting a one-step heating method under the nitrogen atmosphere, and preserving the heat for 10-30min to synthesize pure-phase AlON powder; preserving the temperature of the pure-phase AlON powder in an air environment at 600-680 ℃ for 2-6 h to remove residual C to obtain AlON powder,
wherein the average length of the primary particles of the pure-phase AlON powder is 350-450 nm, and the average width is 200-250 nm.
Preferably, the AlON powder from which the residual C is removed is ball-milled to obtain AlON fine powder with different particle sizes.
Further, the ball milling is carried out on a planetary ball mill, the rotating speed is less than or equal to 200rpm, the ball milling time is less than or equal to 24 hours, and the ball milled AlON powder is nearly spherical.
Specifically, the ball milling time of the AlON powder is 2h, D 50 1.5 to 2.0 μm; the ball milling time is 4h, D 50 0.8-1.0 μm; the ball milling time is 8h, D 50 0.5-0.8 μm; the ball milling time is 18h, D 50 ＝0.3～0.5μm。
Preferably, the raw material is alpha-Al 2 O 3 The powder is commercial alpha-Al 2 O 3 Powder with primary particle size of 0.2 μm or less, D 50 Less than or equal to 5 microns, specific surface area>10m 2 (ii)/g; ball milling is carried out by adopting a planetary ball mill, the rotating speed is 150-170 rpm, the time is 1-24 h, and D of the powder after ball milling is carried out 50 Less than or equal to 0.2 mu m, specific surface area>14m 2 /g。
Preferably, alpha-Al 2 O 3 And the dosage of the deionized water in the mixed slurry of the glucose is alpha-Al 2 O 3 And 60-70 times of the total mass of glucose.
Preferably, the alpha-Al is obtained by hydrothermal synthesis 2 O 3 the/C powder is in a core-shell structure, and the C is coated on the alpha-Al 2 O 3 The surface of the particles, and C is alpha-Al 2 O 3 5-10% of the mass of the powder C.
Preferably, the temperature rise speed of the one-step temperature rise method is 10-50 ℃/min.
The invention has the beneficial effects that: the invention uses commercial alpha-Al 2 O 3 The powder and glucose powder are used as raw materials, the raw materials have stable quality and low price, and alpha-Al is firstly cut off by simple ball milling (the ball milling can be carried out in water or absolute ethyl alcohol) 2 O 3 The connection among the particles ensures that the particles have good dispersibility, and the simple and feasible hydrothermal method is utilized to prepare the alpha-Al with the core-shell structure characteristic 2 O 3 C, mixing the powder. alpha-Al 2 O 3 The pre-ball milling not only effectively increases the specific surface area of the powder and is beneficial to improving the content of C, but also ensures that C has good isolation effect by coating carbon on the surface of dispersed particles, thereby preventing Al before AlON is formed by carbon thermal reduction nitridation 2 O 3 The particle agglomeration and growth can effectively shorten the material transmission distance in the AlON forming process, thereby promoting the AlON to be fastAnd (4) forming. Therefore, pure-phase AlON powder can be obtained by adopting one-step temperature rise and only needing short-time heat preservation of 10-30min under the condition of lower synthesis temperature of 1700-1750 ℃, the size of primary particles of the obtained AlON powder is small, the bonding among the particles is weak, the connection among the particles can be broken through common ball milling to obtain fine particle powder, and the powder obtained after ball milling has good particle shape and is nearly spherical, thereby being beneficial to the forming and densification sintering in the ceramic preparation stage. In addition, the hydrothermal synthesis of alpha-Al of the invention 2 O 3 The requirement on equipment in the process of mixing the powder/C is not high, the process is simple, and the process is environment-friendly; the carbothermic reduction nitridation process is fast in process and high in efficiency, cost is saved, and the energy-saving effect is good on the premise of guaranteeing the quality of the AlON powder.
Drawings
FIG. 1 shows α -Al in example 1 2 O 3 Before and after powder ball milling and alpha-Al obtained by the powder ball milling 2 O 3 SEM image of/C mixed powder;
FIG. 2 shows α -Al obtained in example 1 2 O 3 TEM image of/C mixed powder;
FIG. 3 is an XRD pattern of AlON powder obtained in examples 1, 2, 3, 4 and 5;
FIG. 4 is an SEM photograph of AlON powders obtained in examples 1, 2, 3, 4 and 5;
FIG. 5 is a graph showing the ball milling effect of AlON powder obtained in examples 3, 4 and 5 (the effect of ball milling time on the particle size of the powder);
fig. 6 is an SEM image of AlON powder obtained in examples 3, 4 and 5 after ball milling.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
One of the specific implementation modes is as follows:
a method for rapidly preparing pure-phase AlON fine powder by one-step temperature rise carbon thermal reduction nitridation comprises the following process steps:
①α-Al 2 O 3 pretreatment: commercial alpha-Al 2 O 3 Powder (primary particle size less than or equal to 0.2 mu m, D) 50 Less than or equal to 5 microns, specific surface area>10m 2 /g) is put into a ball milling tank, a planetary ball mill is adopted for ball milling, the rotating speed is 170rpm, the time is 24 hours, and D of the powder after ball milling is finished 50 Less than or equal to 0.2 mu m, specific surface area>14m 2 Drying for later use;
secondly, batching: according to alpha-Al 2 O 3 Weighing raw material powder according to the mass ratio of 1.8: 1-1: 1 to glucose powder, adding deionized water, and preparing alpha-Al 2 O 3 And glucose, wherein the alpha-Al is 2 O 3 Adding deionized water 60-70 times of the total mass of glucose to prepare mixed slurry;
③α-Al 2 O 3 c, preparing mixed powder: placing the slurry obtained in the step II into a reaction kettle, preserving the heat for 24 hours at 180 ℃, and carrying out hydro-thermal synthesis to obtain alpha-Al 2 O 3 Mixing the powder with C, centrifugally washing in deionized water or ethanol solution, drying, and hydrothermally synthesizing to obtain alpha-Al 2 O 3 the/C is in a core-shell structure, and the C is coated on the alpha-Al 2 O 3 The mass content of C on the surface of the particles is 5-10%;
fourthly, carbon thermal reduction nitridation: the alpha-Al obtained in the step III 2 O 3 And placing the/C mixed powder in a carbon furnace, directly heating to 1700-1750 ℃ at a heating rate of 10-50 ℃/min by adopting a one-step heating method, preserving the heat for 10-30min, and quickly synthesizing pure-phase AlON powder with small-size primary particles in a nitrogen environment.
Carbon removal: and (5) preserving the temperature of the AlON powder obtained in the step (IV) in an air environment at 600-680 ℃ for 2-6 h to remove residual C.
Ball milling: ball-milling the AlON powder obtained in the step (v) on a planetary ball mill to obtain AlON fine powder with different particle sizes, wherein the AlON powder is in a nearly spherical shape after ball milling, and the ball milling is carried out for 2h and D 50 1.5-2.0 μm; ball milling for 4h, D 50 0.8-1.0 μm; ball milling for 8h, D 50 0.5-0.8 μm; ball milling time 18h, D 50 ＝0.3～0.5μm。
Example 1
The commercial primary particle diameter is 200nm, and the specific surface area is 11.69m 2 /g、D 50 3.88 μm of alpha-Al 2 O 3 (actually large particles consisting of 200nm powder) was ball-milled for 24 hours at 170rpm in a planetary ball mill, and the specific surface area of the ball-milled powder was 14.27m 2 /g、D 50 0.20 μm, alpha-Al before and after ball milling 2 O 3 The morphology of (A) is shown in FIG. 1.
Then using the alpha-Al after ball milling 2 O 3 alpha-Al with the mass ratio of 1.7:1 2 O 3 Adding 100ml of deionized water into glucose powder, mixing with the total weight of 1.5g for 20min under ultrasonic condition, placing into a reaction kettle, maintaining at 180 deg.C for 24 hr, centrifuging and cleaning the slurry with water for 4 times, and oven drying the obtained powder to obtain the product C coated with alpha-Al 2 O 3 alpha-Al with core-shell structure characteristics on particle surface 2 O 3 Mixed powder of (alpha-Al) 2 O 3 The morphology of the/C mixed powder is shown in FIG. 1 (for comparison, the use of unground alpha-Al is also provided 2 O 3 Hydro-thermal synthesis of alpha-Al 2 O 3 Morphology of/C mixed powder), TEM image is shown in fig. 2).
alpha-Al is reacted with 2 O 3 And putting the/C mixed powder into a carbon furnace, heating to 1750 ℃ at a speed of 50 ℃/min in a nitrogen environment, preserving heat for 10min, cooling, and preserving heat for 4h at 640 ℃ in the air to remove residual carbon, thereby obtaining pure-phase AlON powder with 398nm of average length and 249nm of average width of primary particles. The XRD pattern of the AlON powder is shown in figure 3, the appearance is shown in figure 4, the combination among particles can be observed to be weaker, and the method is favorable for ball milling and refining to obtain small-particle powder.
Example 2
The difference between example 2 and example 1 is that 2 O 3 The mass ratio of the pure phase AlON powder to glucose is 1.25:1, the heating rate is 10 ℃/min, the carbothermic reduction nitridation temperature is 1730 ℃, the XRD pattern of the obtained pure phase AlON powder is shown in figure 3, the appearance is shown in figure 4, the average length of the primary particle size of the obtained powder is 435nm, the average width of the primary particle size of the obtained powder is 233nm, and the bonding between the particles is weaker.
Example 3
Example 3 differs from example 1 in that，α-Al 2 O 3 The mass ratio of the pure phase AlON powder to glucose is 1.25:1, the carbon thermal reduction nitridation temperature is 1730 ℃, the XRD pattern of the obtained pure phase AlON powder is shown in figure 3, the morphology is shown in figure 4, and the primary particle size is 417nm in average length and 223nm in average width. The obtained AlON powder particles are weakly bonded, and are ball-milled for 2h at 170rpm, namely D 50 The particle size of the powder is reduced to 1.54 mu m, the ball milling time is prolonged to 4h, the particle size of the powder is rapidly reduced to 0.88 mu m, the particle size of the powder milled for 8h is further reduced to 0.51 mu m, the particle size of the powder is further reduced in the process that the ball milling time is gradually increased to 24h, the particle size of the powder is 12h @0.44 mu m, 18h @0.39 mu m and 24h @0.33 mu m, the relation between the particle size of the powder and the ball milling time is shown in detail in figure 5, the particle shape of the powder after ball milling is good and nearly spherical, and the shapes of a plurality of typical powders (2h, 8h and 24h) after ball milling are shown in figure 6.
Example 4
Example 4 differs from example 1 in that α -Al 2 O 3 The mass ratio of the pure phase AlON powder to the glucose is 1.25:1, the XRD pattern of the obtained pure phase AlON powder is shown in figure 3, the morphology is shown in figure 4, and the primary particle size is 388nm in average length and 203nm in average width. The obtained AlON powder grains are weakly combined, and are ball-milled for 2h at 170rpm, namely D 50 The particle size of the powder is reduced to 1.97 mu m, the ball milling time is prolonged to 4h, the particle size of the powder is rapidly reduced to 1.00 mu m, the particle size of the powder milled for 8h is further reduced to 0.71 mu m, the particle size of the powder is further reduced in the process that the ball milling time is gradually increased to 24h, the particle size of the powder is 12h @0.57 mu m, 18h @0.48 mu m and 24h @0.46 mu m, the relation between the particle size of the powder and the ball milling time is shown in detail in figure 5, the particle shape of the powder after ball milling is good and nearly spherical, and the shapes of a plurality of typical powders (2h, 8h and 24h) after ball milling are shown in figure 6.
Example 5
The difference between example 5 and example 1 is that α -Al 2 O 3 The mass ratio of the pure phase AlON powder to glucose is 1:1, the carbon thermal reduction nitridation temperature is 1700 ℃, the XRD pattern of the obtained pure phase AlON powder is shown in figure 3, the morphology is shown in figure 4, and the primary particle size is 354nm in average length and 207nm in average width. The obtained AlON powder grains are weakly combined, and are ball-milled for 2h at 170rpm, namely D 50 Reducing the particle size to 1.50 mu m, prolonging the ball milling time to 4h, rapidly reducing the particle size of the powder to 0.90 mu m, and obtaining the ballThe powder particle size after milling for 8h is further reduced to 0.57 μm, and in the process that the ball milling time is gradually increased to 24h, the powder particle size is further reduced, 12h @0.48 μm, 18h @0.37 μm and 24h @0.33 μm, the relation between the powder particle size and the ball milling time is shown in detail in figure 5, the powder particle after ball milling is good in shape and nearly spherical, and the shapes of a plurality of typical powders (2h, 8h and 24h) after ball milling are shown in figure 6.
Claims (8)
1. A method for rapidly preparing pure-phase AlON fine powder by one-step temperature-rise carbon thermal reduction nitridation is characterized by comprising the following steps: the method comprises the following process steps:
firstly, alpha-Al is added 2 O 3 Ball milling the powder, and then carrying out ball milling on the alpha-Al 2 O 3 Adding the powder and glucose powder into water according to the mass ratio of 1.8: 1-1: 1 to obtain alpha-Al 2 O 3 And glucose; the obtained slurry is put into a reaction kettle to be thermally insulated for 24 hours at 180 ℃ for hydro-thermal synthesis of alpha-Al 2 O 3 C, washing and drying the mixed powder; drying the obtained alpha-Al 2 O 3 Placing the/C mixed powder in a carbon furnace, directly heating to 1700-1750 ℃ by adopting a one-step heating method under the nitrogen atmosphere, and preserving the heat for 10-30min to synthesize pure-phase AlON powder; preserving the temperature of the pure-phase AlON powder in an air environment at 600-680 ℃ for 2-6 h to remove residual C to obtain AlON powder,
wherein, the alpha-Al is obtained by hydro-thermal synthesis 2 O 3 the/C powder is in a core-shell structure, and C is coated on alpha-Al 2 O 3 The surface of the particles; the average length of the primary particles of the pure-phase AlON powder is 350-450 nm, and the average width of the primary particles is 200-250 nm.
2. The method of claim 1, wherein: and ball-milling the AlON powder without the residual C to obtain AlON fine powder with different particle sizes.
3. The method of claim 1, wherein: the raw material alpha-Al 2 O 3 The powder is commercial alpha-Al 2 O 3 Powder with primary particle size of 0.2 μm or less, D 50 Less than or equal to 5 mu m, specific surface area>10m 2 /g；Ball milling is carried out by adopting a planetary ball mill, the rotating speed is 150-200 rpm, the time is 1-24 h, and D of the powder after ball milling is carried out 50 Less than or equal to 0.2 mu m, specific surface area>14m 2 /g。
4. The method of claim 1, wherein: alpha-Al 2 O 3 And the dosage of the deionized water in the mixed slurry of the glucose is alpha-Al 2 O 3 And 60-70 times of the total mass of glucose.
5. The method of claim 1, wherein: alpha-Al obtained by hydrothermal synthesis 2 O 3 C in/C powder accounts for alpha-Al 2 O 3 5-10% of the mass of the powder C.
6. The method of claim 1, wherein: the temperature rise speed of the one-step temperature rise method is 10-50 ℃/min.
7. The method of claim 2, wherein: the ball milling is carried out on a planetary ball mill, the rotating speed is less than or equal to 200rpm, the ball milling time is less than or equal to 24h, and AlON powder is nearly spherical after ball milling.
8. The method of claim 7, wherein: the ball milling time of the AlON powder is 2h, D 50 = 1.5-2.0 μm; the ball milling time is 4h, D 50 = 0.8-1.0 μm; the ball milling time is 8h, D 50 = 0.5-0.8 μm; the ball milling time is 18h, D 50 =0.3~0.5μm。
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