CN115504808B - Preparation method of BN nozzle for gas atomization - Google Patents

Preparation method of BN nozzle for gas atomization Download PDF

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CN115504808B
CN115504808B CN202211353114.5A CN202211353114A CN115504808B CN 115504808 B CN115504808 B CN 115504808B CN 202211353114 A CN202211353114 A CN 202211353114A CN 115504808 B CN115504808 B CN 115504808B
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nozzle
temperature
siliconizing
green body
stirring
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CN115504808A (en
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于建宾
钱凡
李红霞
刘国齐
杨文刚
马渭奎
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Abstract

The invention belongs to the technical field of high-temperature ceramics, and particularly relates to a preparation method of a BN nozzle for gas atomization. The preparation method of the BN nozzle for gas atomization adopts hot die casting molding, and is assisted with the process of siliconizing and nitriding sintering to prepare the BN ceramic nozzle; firstly, preparing a BN nozzle green body, placing the formed nozzle in a sagger with good air permeability, burying alumina fine powder, and carrying out wax removal in a degreasing furnace from room temperature to 280 ℃; and placing the BN nozzle green body after wax removal in a high-temperature furnace for siliconizing, wherein the temperature in the furnace is 1600-1700 ℃. The invention adopts a hot die casting molding process, realizes the near net size molding of the BN nozzle, avoids subsequent processing, combines a siliconizing and nitriding sintering process, and realizes the densification sintering of the BN nozzle.

Description

Preparation method of BN nozzle for gas atomization
Technical Field
The invention belongs to the technical field of high-temperature ceramics, and particularly relates to a preparation method of a BN nozzle for gas atomization.
Background
In many methods for pulverizing materials, the proportion of powder produced by gas atomization pulverizing is 80% of the whole; the powder prepared by the gas atomization technology has small granularity, high sphericity, low oxygen content, mass production capacity and low cost, and is a main method for producing high-performance spherical metal and alloy powder at present, so that the gas atomization technology is widely applied to industry; the process of gas atomization is generally described as the process of molten metal flowing out through ceramic holes in the bottom of a crucible to form droplets of metal, which in free-fall processes, through the action of gas shearing and extrusion, thin the metal stream and cause laminar flow fiberization. When the liquid drops leave the effective atomization area, the external pressure of the liquid drops is reduced, and the self-excitation crushing is caused by the imbalance of the internal pressure and the external pressure of the liquid drops.
Ceramic nozzle materials mainly made of BN material and ZrO for current mainstream application 2 Mass is the main, but ZrO 2 The thermal shock resistance is inferior to that of BN, the crystal form is transformed in the sintering and application processes, the crystal is easy to crack, and the stability is poorer than that of BN as a whole; the BN-based ceramic is prepared by hot press molding, the sintering cost is high, and the ceramic nozzle is obtained by precision machining, so that the problem of low raw material yield is caused; BN has strong covalent bond characteristics, is difficult to sinter under normal pressure, and is difficult to compact at normal temperature in a card-type structure.
Disclosure of Invention
The invention aims to solve the difficult problems of complex forming and densification of a BN ceramic nozzle, and provides a BN nozzle for gas atomization and a preparation method thereof.
The invention adopts the following technical scheme for accomplishing the purposes:
a preparation method of BN nozzle for gas atomization adopts hot die casting molding, and a process of siliconizing and nitriding sintering is adopted to prepare BN ceramic nozzle; firstly, preparing a BN nozzle green body, wherein the raw body comprises the following materials in percentage: paraffin wax: 15-24%; beeswax: 1% -4%; oleic acid: 0.5 to 1 percent; BN powder: 75-82%, wherein BN powder has three particle sizes of 800 mu m, 2000 mu m and 5000 mu m respectively, the purity of BN is more than or equal to 99%, and the adding amount ratio of the three BN powders is 2:1:2; adding paraffin, beeswax and oleic acid into an oil bath, controlling the temperature of the oil bath, stirring, adding oleic acid, stirring, sequentially adding BN powder with different particle sizes, stirring for 0.5h, pouring into a hot die casting machine slurry barrel, setting the temperature to 60-70 ℃, vacuumizing while stirring, and carrying out molding after 10-30 min; placing the molded nozzle into a sagger with good air permeability, burying with alumina fine powder,the degreasing furnace is used for removing wax, and the temperature of the wax is from room temperature to 280 ℃, and the BN nozzle green body after the wax removal still has certain residual carbon, so the BN nozzle green body has certain strength to meet the requirement of the subsequent preparation process, and the apparent porosity is 15-20%; the BN nozzle green body after wax removal is placed in a high temperature furnace for siliconizing, the temperature in the furnace is 1600-1700 ℃, because the wall thickness of the nozzle is thinner, liquid phase silicon is very easy to infiltrate into the interior of a material nozzle, meanwhile, the infiltrated liquid phase silicon reacts with residual carbon of the nozzle to form SiC, after the siliconizing is finished, the apparent porosity of the nozzle is less than 5%, then nitriding sintering is carried out, the nitriding temperature is 1450-1550 ℃, and after the nitriding is finished, the apparent porosity is less than 1%, thus obtaining SiC and Si 3 N 4 And (3) bonded dense BN ceramic.
According to the preparation method of the BN nozzle for gas atomization, disclosed by the invention, a hot die casting forming process is adopted, so that the near net size forming of the BN nozzle is realized, the subsequent processing is avoided, and the densification sintering of the BN nozzle is realized by combining a siliconizing and nitriding sintering process; siC and Si in a material system 3 N 4 The BN nozzle prepared by the process route has better thermal shock resistance and scouring resistance, and has obvious innovation and economic benefit.
Detailed Description
The invention will be described in detail with reference to specific examples:
example 1:
firstly, preparing a BN nozzle green body, wherein the material scheme is paraffin: 15%; beeswax: 4%; oleic acid: 1%; the addition amounts of BN powder are respectively 32%, 16% and 32% at 800 μm, 2000 μm and 5000 μm. Adding paraffin, beeswax and oleic acid into an oil bath according to the proportion, controlling the temperature of the oil bath, stirring, adding oleic acid, stirring, sequentially adding BN powder with different particle sizes, stirring for 0.5h, pouring into a hot die casting machine slurry barrel, setting the temperature to 65 ℃, vacuumizing while stirring, and carrying out molding after 30 min. Placing the molded nozzle into a sagger with good air permeability, embedding the molded nozzle with alumina fine powder, and carrying out wax removal in a degreasing furnace from room temperature to 280 ℃. The BN nozzle green body after wax removal is placed in a high temperature furnace for siliconizing, the temperature in the furnace is 1650 ℃ and the siliconizing is carried outAfter silicon is nitrided and sintered, the nitriding temperature is 1550 ℃, and SiC and Si are obtained 3 N 4 The combined dense BN ceramic has a apparent porosity of 0.4%.
Example 2:
firstly, preparing a BN nozzle green body, wherein the material scheme is paraffin: 24%; beeswax: 0.5%; oleic acid: 0.5%; the addition amounts of BN powder are respectively 30%, 15% and 30% at 800 μm, 2000 μm and 5000 μm. Adding paraffin, beeswax and oleic acid into an oil bath according to the proportion, controlling the temperature of the oil bath, stirring, adding oleic acid, stirring, sequentially adding BN powder with different particle sizes, stirring for 0.5h, pouring into a hot die casting machine slurry barrel, setting the temperature to 60 ℃, vacuumizing while stirring, and carrying out molding after 10 min. Placing the molded nozzle into a sagger with good air permeability, embedding the molded nozzle with alumina fine powder, and carrying out wax removal in a degreasing furnace from room temperature to 280 ℃. The BN nozzle green body after wax removal is placed in a high temperature furnace for siliconizing at 1600 ℃, and then is subjected to nitriding sintering at 1450 ℃ after siliconizing, thus obtaining SiC and Si 3 N 4 The combined dense BN ceramic has a apparent porosity of 0.7%.
Example 3:
firstly, preparing a BN nozzle green body, wherein the material scheme is paraffin: 16.2%; beeswax: 1%; oleic acid: 0.8%; the addition amounts of BN powder were 32.8%, 16.4% and 32.8% respectively at 800. Mu.m, 2000. Mu.m, 5000. Mu.m. Adding paraffin, beeswax and oleic acid into an oil bath according to the proportion, controlling the temperature of the oil bath, stirring, adding oleic acid, stirring, sequentially adding BN powder with different particle sizes, stirring for 0.5h, pouring into a hot die casting machine slurry barrel, setting the temperature to 70 ℃, vacuumizing while stirring, and carrying out molding after 20 min. Placing the molded nozzle into a sagger with good air permeability, embedding the molded nozzle with alumina fine powder, and carrying out wax removal in a degreasing furnace from room temperature to 280 ℃. The BN nozzle green body after wax removal is placed in a high temperature furnace for siliconizing at 1700 ℃ in the furnace, and then is subjected to nitriding sintering at 1550 ℃ after siliconizing, thus obtaining SiC and Si 3 N 4 The combined dense BN ceramic has a apparent porosity of 0.2%.

Claims (1)

1.A preparation method of a BN nozzle for gas atomization is characterized by comprising the following steps: adopting hot die casting molding, and preparing the BN ceramic nozzle by aided with the process of siliconizing and nitriding sintering; firstly, preparing a BN nozzle green body, wherein the raw body comprises the following materials in percentage: paraffin wax: 15-24%; beeswax: 1% -4%; oleic acid: 0.5 to 1 percent; BN powder: 75-82%, total 100%, wherein BN powder has three particle sizes of 800 mu m, 2000 mu m and 5000 mu m, the purity of BN is more than or equal to 99%, and the adding amount ratio of the three BN powders is 2:1:2; adding paraffin, beeswax and oleic acid into an oil bath, controlling the temperature of the oil bath, stirring, adding oleic acid, stirring, sequentially adding BN powder with different particle sizes, stirring for 0.5h, pouring into a hot die casting machine slurry barrel, setting the temperature to 60-70 ℃, vacuumizing while stirring, and carrying out molding after 10-30 min; placing the molded nozzle in a sagger with good air permeability, burying with alumina fine powder, performing paraffin removal in a degreasing furnace, wherein the paraffin removal is performed from room temperature to 280 ℃, and the BN nozzle green body after the paraffin removal has certain residual carbon, so that the BN nozzle green body has certain strength to meet the requirement of the subsequent preparation process, and the apparent porosity is 15-20%; the BN nozzle green body after wax removal is placed in a high temperature furnace for siliconizing, the temperature in the furnace is 1600-1700 ℃, because the wall thickness of the nozzle is thinner, liquid phase silicon is very easy to infiltrate into the interior of a material nozzle, meanwhile, the infiltrated liquid phase silicon reacts with residual carbon of the nozzle to form SiC, after the siliconizing is finished, the apparent porosity of the nozzle is less than 5%, then nitriding sintering is carried out, the nitriding temperature is 1450-1550 ℃, and the apparent porosity after the nitriding is finished is less than 1%, thus obtaining SiC and Si 3 N 4 And (3) bonded dense BN ceramic.
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JPH03281709A (en) * 1990-03-29 1991-12-12 Daido Steel Co Ltd Apparatus for manufacturing metal powder and gas atomizing nozzle
CN101407421A (en) * 2008-11-04 2009-04-15 西安交通大学 Method for preparing non-grain boundary phase porous silicon nitride ceramic based on siliconizing nitridation
CN103626498A (en) * 2013-12-13 2014-03-12 山东鹏程特种陶瓷有限公司 Boron nitride based ceramic nozzle and preparation method thereof
CN105418070A (en) * 2015-11-20 2016-03-23 李安成 Electronic cigarette atomization core for implanting heating wire into green body and preparation method thereof
CN110218094A (en) * 2019-07-11 2019-09-10 沈阳西卡精细陶瓷有限公司 A kind of nitrate nitroge injection moulding oven holds the preparation method of burning beryllium

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