CN113105246A - 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
- Publication number
- CN113105246A CN113105246A CN202110249505.1A CN202110249505A CN113105246A CN 113105246 A CN113105246 A CN 113105246A CN 202110249505 A CN202110249505 A CN 202110249505A CN 113105246 A CN113105246 A CN 113105246A
- Authority
- CN
- China
- Prior art keywords
- powder
- alpha
- alon
- ball milling
- pure
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/46—Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/95—Products characterised by their size, e.g. microceramics
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
- C04B2235/9653—Translucent or transparent ceramics other than alumina
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
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-Al2O3Ball milling the powder, and then carrying out ball milling on the alpha-Al2O3Adding the powder and glucose powder into water to obtain alpha-Al2O3And glucose; the obtained slurry is hydrothermally synthesized into alpha-Al in a reaction kettle2O3C, washing and drying the mixed powder; drying the alpha-Al2O3the/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, has small primary particle size and is easy to pass through a common ballGrinding to realize grain refinement, thereby obtaining AlON fine powder.
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 Al2O3And 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, densification sintering process based on AlON powder is difficult and the obtained ceramic has good light transmittance, so that the preparation of transparent ceramic by first synthesizing AlON powder and then sintering is favored by researchers in recent years. 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-Al2O3And carbon black as raw materials, and performing two-step heating carbothermal reduction nitridation, namely heating to 1550 ℃ for 1h, then continuing to heat to 1750 ℃ for 2h to obtain pure-phase AlON powder, wherein the particle sizes of the powder are respectively 3.36 mu m and 1.38 mu m (Ceramics International 42(2016) 8290-; yingying Wang at the university of Jinan, with Al2O3And carbon black are taken as raw materials, the mixture is combined by 10 ℃/min and 3 ℃/min, and the D is synthesized by adopting two-stage heat preservation (the temperature at 1550 ℃ is preserved for 1h and the temperature at 1750 ℃ is preserved for 2h)50AlON powder 45.32 μm, ball-milled for 6h by liquid nitrogen, and the particle size was reduced to 3.08 μm (Ceramics International 44 (2018)) 471-; dalian maritime university uses Al2O3And activated carbon as raw materialsThe method comprises the steps of heating to 1550 ℃ at a speed of 10-30 ℃/min for 1 hour through two-step heating, then continuously heating to 1750 ℃ for 1 hour through heating, ball-milling the synthesized AlON powder at 170rpm for 24 hours 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 Al2O3And performing carbothermal reduction and nitridation on the/C core-shell structure precursor to synthesize AlON powder. These studies generally used gamma-Al2O3As a raw material, the carbothermic reduction nitridation process needs two-step heat preservation, and the total heat preservation time is usually more than or equal to 3 h. Xihai Jin et Al use nano gamma-Al2O3Preparing Al2O3UFR core-shell structure precursor, and then obtaining Al by thermal cracking at 800 DEG C2O3Synthesizing 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 Sabaghi2O3Thermal cracking with PAN at 800 ℃ for 2h to obtain Al2O3a/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 technology2O3The 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 structure2O3Harmful 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, it is necessary to search for a more simple and easy method,The technology for preparing the AlON fine powder is energy-saving, environment-friendly, efficient and low-cost, and if the preparation of the AlON fine powder can be realized under the condition of low requirement on equipment, the research and development process of AlON transparent ceramics can be further promoted.
Disclosure of Invention
The invention aims to provide a catalyst based on alpha-Al2O3And 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 milling2O3The 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 Al2O3The 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. 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. The method has the advantages of stable quality of raw materials, low price, low cost and Al2O3The 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 the 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 added2O3Ball milling the powder, and then carrying out ball milling on the alpha-Al2O3Adding the powder and glucose powder into water according to the mass ratio of 1.8: 1-1: 1 to obtain alpha-Al2O3And 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-Al2O3Mixing powder of C andwashing and drying; drying the obtained alpha-Al2O3Placing 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 with residual C 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 24h, and the ball milled AlON powder is nearly spherical.
Specifically, the ball milling time of the AlON powder is 2h, D501.5-2.0 μm; the ball milling time is 4h, D500.8-1.0 μm; the ball milling time is 8h, D500.5-0.8 μm; the ball milling time is 18h, D50＝0.3～0.5μm。
Preferably, the raw material is alpha-Al2O3The powder is commercial alpha-Al2O3Powder with primary particle size not more than 0.2 μm and D50Less than or equal to 5 microns, specific surface area>10m2(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 out50Less than or equal to 0.2 mu m, specific surface area>14m2/g。
Preferably, alpha-Al2O3And the dosage of the deionized water in the mixed slurry of the glucose is alpha-Al2O3And 60-70 times of the total mass of glucose.
Preferably, the alpha-Al is obtained by hydrothermal synthesis2O3the/C powder is in a core-shell structure, and C is coated on alpha-Al2O3The surface of the particles, and C is alpha-Al2O35-10% 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-Al2O3The 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)2O3The 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 characteristic2O3C, mixing the powder. alpha-Al2O3The 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 nitridation2O3The particle agglomeration and growth can effectively shorten the material transmission distance in the AlON forming process, thereby promoting the rapid formation of AlON. 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 invention2O3The 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 example 1. alpha. -Al2O3Before and after powder ball milling and alpha-Al obtained by the powder ball milling2O3SEM image of/C mixed powder;
FIG. 2 shows α -Al obtained in example 12O3TEM 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 photograph 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-Al2O3pretreatment: commercial alpha-Al2O3Powder (primary particle size less than or equal to 0.2 mu m, D)50Less than or equal to 5 microns, specific surface area>10m2/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 finished50Less than or equal to 0.2 mu m, specific surface area>14m2Drying for later use;
secondly, batching: according to alpha-Al2O3Weighing raw material powder according to the mass ratio of 1.8: 1-1: 1 to glucose powder, adding deionized water, and preparing alpha-Al2O3And glucose, wherein the amount of the alpha-Al is in the range of2O3Adding deionized water 60-70 times of the total mass of glucose to prepare mixed slurry;
③α-Al2O3preparation of a/C 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-Al2O3Mixing the powder with C, centrifugally washing in deionized water or ethanol solution, drying, and hydrothermally synthesizing to obtain alpha-Al2O3the/C is in a core-shell structure, and the C is coated on the alpha-Al2O3The 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 III2O3Placing the/C mixed powder in a carbon furnace, adoptingThe one-step heating method is used for directly heating to 1700-1750 ℃ at the heating rate of 10-50 ℃/min, 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 (4) 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 D501.5-2.0 μm; ball milling for 4h, D500.8-1.0 μm; ball milling for 8h, D500.5-0.8 μm; ball milling time 18h, D50＝0.3～0.5μm。
Example 1
The commercial primary particle diameter is 200nm, the specific surface area is 11.69m2/g、D503.88 μm of alpha-Al2O3(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 14.27m2/g、D500.20 μm, alpha-Al before and after ball milling2O3The morphology of (A) is shown in FIG. 1.
Then using the ball-milled alpha-Al2O3alpha-Al with the mass ratio of 1.7:12O3Adding 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-Al2O3alpha-Al with core-shell structure characteristics on particle surface2O3Mixed powder of (alpha-Al)2O3The morphology of the/C mixed powder is shown in FIG. 1 (for comparison, the use of unground alpha-Al is also provided2O3Hydro-thermal synthesis of alpha-Al2O3Morphology of/C mixed powder), TEM image is shown in fig. 2).
alpha-Al is added2O3Putting 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, preserving heat of the obtained powder in air at 640 ℃ for 4h to remove residual carbon, and obtaining the powder IPure-phase AlON powder with the average length of secondary particles of 398nm and the average width of the secondary particles of 249 nm. The XRD spectrum of the AlON powder is shown in figure 3, the appearance is shown in figure 4, the combination among the particles can be observed to be weaker, and the small-particle powder can be obtained by ball milling and refining.
Example 2
The difference between example 2 and example 1 is that α -Al2O3The 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
The difference between example 3 and example 1 is that α -Al2O3The 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 D50The 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 -Al2O3The 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 D50Reducing the particle size of the powder to 1.97 mu m, prolonging the ball milling time to 4h, rapidly reducing the particle size of the powder to 1.00 mu m, further reducing the particle size of the powder milled for 8h to 0.71 mu m, and continuously reducing the particle size of the powder in the process that the ball milling time is gradually increased to 24hThe 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 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 powder (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 -Al2O3The 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 D50The particle size of the powder is reduced to 1.50 mu m, the ball milling time is prolonged to 4h, the particle size of the powder is rapidly reduced to 0.90 mu m, the particle size of the powder milled for 8h is further reduced to 0.57 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 @0.48 mu m, 18h @0.37 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.
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 added2O3Ball milling the powder, and then carrying out ball milling on the alpha-Al2O3Adding the powder and glucose powder into water according to the mass ratio of 1.8: 1-1: 1 to obtain alpha-Al2O3And 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-Al2O3C, washing and drying the mixed powder; drying the obtained alpha-Al2O3Placing 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.
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-Al2O3The powder is commercial alpha-Al2O3Powder with primary particle size not more than 0.2 μm and D50Less than or equal to 5 microns, specific surface area>10m2(ii)/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 out50Less than or equal to 0.2 mu m, specific surface area>14m2/g。
4. The method of claim 1, wherein: alpha-Al2O3And the dosage of the deionized water in the mixed slurry of the glucose is alpha-Al2O3And 60-70 times of the total mass of glucose.
5. The method of claim 1, wherein: alpha-Al obtained by hydrothermal synthesis2O3the/C powder is in a core-shell structure, and C is coated on alpha-Al2O3The surface of the particles, and C is alpha-Al2O35-10% of the mass of the powder C.
6. The method of claim 1, wherein: the temperature rising speed of the one-step temperature rising 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, D50＝1.5～2.0 μm; the ball milling time is 4h, D500.8-1.0 μm; the ball milling time is 8h, D500.5-0.8 μm; the ball milling time is 18h, D50＝0.3～0.5μm。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110249505.1A CN113105246B (en) | 2021-03-08 | 2021-03-08 | Method for rapidly preparing pure-phase AlON fine powder by one-step temperature rise carbon thermal reduction nitridation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110249505.1A CN113105246B (en) | 2021-03-08 | 2021-03-08 | Method for rapidly preparing pure-phase AlON fine powder by one-step temperature rise carbon thermal reduction nitridation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113105246A true CN113105246A (en) | 2021-07-13 |
| CN113105246B CN113105246B (en) | 2022-09-06 |
Family
ID=76710635
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110249505.1A Active CN113105246B (en) | 2021-03-08 | 2021-03-08 | Method for rapidly preparing pure-phase AlON fine powder by one-step temperature rise carbon thermal reduction nitridation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113105246B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113582701A (en) * | 2021-08-02 | 2021-11-02 | 大连海事大学 | Method for preparing high-purity single-phase AlON transparent ceramic powder by one-step rapid heating and carbon thermal reduction nitridation |
| CN115196970A (en) * | 2022-08-08 | 2022-10-18 | 四川大学 | Preparation method of high-fluidity AlON spherical powder |
| CN116062714A (en) * | 2023-01-18 | 2023-05-05 | 大连海事大学 | Pure-phase nanometer AlN powder and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02137711A (en) * | 1988-11-15 | 1990-05-28 | Sumitomo Electric Ind Ltd | Production of aluminum nitride oxide |
| JPH0323206A (en) * | 1989-06-20 | 1991-01-31 | Showa Denko Kk | Aluminum nitride powder and its production |
| CN101928145A (en) * | 2010-06-01 | 2010-12-29 | 上海玻璃钢研究院有限公司 | Preparation method of superfine and high-purity gamma-ALON transparent ceramics powder |
| CN103553093A (en) * | 2013-09-25 | 2014-02-05 | 中国科学院上海光学精密机械研究所 | Gas-flow mixing reaction aluminum oxynitride powder synthesis method and device |
| TW201540655A (en) * | 2014-04-29 | 2015-11-01 | Nat Inst Chung Shan Science & Technology | Manufacturing method for highly purified [gamma]-AlON powders |
-
2021
- 2021-03-08 CN CN202110249505.1A patent/CN113105246B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02137711A (en) * | 1988-11-15 | 1990-05-28 | Sumitomo Electric Ind Ltd | Production of aluminum nitride oxide |
| JPH0323206A (en) * | 1989-06-20 | 1991-01-31 | Showa Denko Kk | Aluminum nitride powder and its production |
| CN101928145A (en) * | 2010-06-01 | 2010-12-29 | 上海玻璃钢研究院有限公司 | Preparation method of superfine and high-purity gamma-ALON transparent ceramics powder |
| CN103553093A (en) * | 2013-09-25 | 2014-02-05 | 中国科学院上海光学精密机械研究所 | Gas-flow mixing reaction aluminum oxynitride powder synthesis method and device |
| TW201540655A (en) * | 2014-04-29 | 2015-11-01 | Nat Inst Chung Shan Science & Technology | Manufacturing method for highly purified [gamma]-AlON powders |
Non-Patent Citations (2)
| Title |
|---|
| 张芳等: "AlON粉体制备及透明陶瓷的烧结", 《稀有金属材料与工程》 * |
| 盛鸿飞等: "碳热还原氮化法制备超细AlON粉体及其烧结性能研究", 《陶瓷学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113582701A (en) * | 2021-08-02 | 2021-11-02 | 大连海事大学 | Method for preparing high-purity single-phase AlON transparent ceramic powder by one-step rapid heating and carbon thermal reduction nitridation |
| CN115196970A (en) * | 2022-08-08 | 2022-10-18 | 四川大学 | Preparation method of high-fluidity AlON spherical powder |
| CN116062714A (en) * | 2023-01-18 | 2023-05-05 | 大连海事大学 | Pure-phase nanometer AlN powder and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113105246B (en) | 2022-09-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113105246B (en) | Method for rapidly preparing pure-phase AlON fine powder by one-step temperature rise carbon thermal reduction nitridation | |
| CN113479918B (en) | Preparation method of nano spherical alpha-alumina powder | |
| CN108383530B (en) | ZrB2Preparation process of-SiC ceramic composite powder by precursor conversion method | |
| KR102210029B1 (en) | Method preparing silicon carbide particle and the silicon carbide particle prepared the same | |
| CN106517114A (en) | Method for preparing superfine aluminum nitride powder through low temperature and low pressure | |
| CN109036753A (en) | A kind of amorphous nano-crystalline composite magnetic powder core and preparation method thereof | |
| CN114044680A (en) | Preparation method of aluminum nitride powder | |
| CN101700977A (en) | Method for rapidly preparing MgAlON transparent ceramic powder | |
| CN114538913B (en) | Pure-phase nano MgAl with high sintering activity 2 O 4 Powder and preparation method and application thereof | |
| CN101456561B (en) | Method for preparing nano mullite powder | |
| CN110451498B (en) | Graphene-boron nitride nanosheet composite structure and preparation method thereof | |
| KR20070040356A (en) | Method for producing aluminum nitride powder | |
| Shan et al. | One-step carbothermal reduction and nitridation (CRN) for fast fabrication of fine and single phase AlON powder by using hydrothermal synthesized α-Al2O3/C mixture | |
| CN113582701A (en) | Method for preparing high-purity single-phase AlON transparent ceramic powder by one-step rapid heating and carbon thermal reduction nitridation | |
| CN114477200A (en) | Method for preparing hafnium boride powder | |
| JPH0292817A (en) | Production of yttrium aluminium garnet | |
| CN113460981B (en) | Aluminum nitride powder and preparation method and application thereof | |
| CN113788466B (en) | θ/α complex phase nano Al 2 O 3 Method for preparing pure-phase gamma-AlON powder by carbothermal reduction nitridation | |
| CN115340093B (en) | Method for preparing nano silicon or amorphous silicon dioxide by silicate | |
| CN115073181B (en) | High-sintering-activity pure-phase MgAlON fine powder and preparation method and application thereof | |
| TWI246997B (en) | Manufacturing method of aluminum nitride | |
| CN106830943B (en) | Method for preparing boron carbide micro powder by dispersing boric acid coated cellulose powder with n-hexane | |
| CN117800737A (en) | High-purity aluminum nitride powder and batch preparation method thereof | |
| CN117024154A (en) | Utilize Y 2 O 3 Method for quickly preparing AlON transparent ceramic at low temperature by using MgO composite sintering aid | |
| CN116062714A (en) | Pure-phase nanometer AlN powder and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |