CN113929472A - Preparation method of composite boron nitride ceramic nozzle - Google Patents

Preparation method of composite boron nitride ceramic nozzle Download PDF

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CN113929472A
CN113929472A CN202111405705.8A CN202111405705A CN113929472A CN 113929472 A CN113929472 A CN 113929472A CN 202111405705 A CN202111405705 A CN 202111405705A CN 113929472 A CN113929472 A CN 113929472A
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powder
pressure
temperature
silicon nitride
boron nitride
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黄向东
王威鹏
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Fuzhou Ceravite New Material Technology Development Co ltd
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Fuzhou Ceravite New Material Technology Development Co ltd
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Abstract

The invention provides a preparation method of a composite boron nitride ceramic nozzle, which increases the strength and corrosion resistance of boron nitride and reduces the heat conductivity by adding silicon nitride granulated powder, so that the composite material disclosed by the invention has the advantages of resisting the corrosion of high-nickel stainless steel, titanium-containing molybdenum cobalt and other high-alloy steel metal liquids and prolonging the service life of the nozzle.

Description

Preparation method of composite boron nitride ceramic nozzle
Technical Field
The invention particularly relates to a preparation method of a composite boron nitride ceramic nozzle.
Background
The nozzle in the preparation of metal powder by the gas atomization process is a key consumable part which determines the performance of the prepared powder. The molten metal with high temperature is made to flow out through nozzle, high speed gas flow (argon gas, etc.) is applied to the outlet to atomize the molten metal, and the atomized liquid drops are cooled into spherical grains. The nozzle material is required to be resistant to high temperature, thermal shock and molten metal corrosion, and has the characteristics of low heat conductivity coefficient and the like. In recent years, metal powder for metal 3D printing is required to have good sphericity and narrow particle size distribution. Because the shape and the dimensional accuracy of the nozzle greatly influence the technological parameters such as air flow distribution, suction effect and the like, the requirements on the processing shape and the dimensional accuracy of the nozzle are higher and higher, the accuracy of the existing ceramics such as zirconia, silicon nitride, silicon carbide and the like is difficult to control due to sintering shrinkage, and the processing cost after sintering is high, so that a novel material which can resist molten metal corrosion, high temperature and thermal shock and has processability after sintering is urgently needed to be found. The products of boron nitride composite silicon oxide, aluminum oxide and zirconium oxide can meet the preparation requirements of some ferrosilicon and other powders, but the corrosion resistance is poor for the preparation of high nickel stainless steel and high alloy steel powder materials containing titanium, molybdenum and cobalt.
Disclosure of Invention
The invention aims to solve the problem of corrosion of high-nickel stainless steel, titanium-containing molybdenum cobalt and other high-alloy steel liquid metal to a nozzle, and provides a preparation method of a nozzle material which has high strength, high liquid metal corrosion resistance and machinability.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a composite boron nitride ceramic nozzle comprises the following steps:
(1) preparing a sintering material: uniformly mixing 60wt% of silicon nitride granulation powder and 40wt% of boron nitride powder by a pulverizer in a dry method;
(2) hot-pressing and sintering: the mixed raw material powder is filled in a rubber bag, the rubber bag is sealed after being vacuumized, then isostatic pressing is carried out at 100 and 200Mpa for pressure maintaining for 60 minutes and compaction is carried out, and then the isostatic pressing blank body is processed into the size of the inner cavity of the hot pressing die by a numerical control diamond wire saw or an end face milling machine (such as L400mm W400mm H300 mm); loading the processed isostatic pressing blank into a hot-pressing die, and sending into a hot-pressing furnace; vacuumizing to about 10Pa, starting heating, keeping the vacuumizing state until the temperature reaches 1000-plus 1200 ℃, then filling nitrogen to one atmosphere, then keeping the flowing nitrogen atmosphere to continue heating, starting pressurizing at 1500 ℃, gradually increasing the pressure, increasing the pressure to 25-30Mpa when the temperature reaches the maximum temperature of 1800-plus 1850 ℃, then keeping the temperature and the pressure for 0.5-3 hours, then stopping heating and naturally cooling, and keeping the pressure constant during the period; when the temperature is reduced to 1200 ℃, the pressure is not maintained any more, the pressure is reduced along with the reduction of the temperature, when the temperature is 800 ℃, the pressure is removed, the furnace temperature is reduced to 80 ℃, then the furnace is opened, the mold is taken out, the mold is continuously cooled to the room temperature, and the sintered blank body is taken out;
(3) processing: and (3) blanking the blank sintered by hot pressing by using a numerical control diamond sand wire cutting machine, and processing the blank into a ceramic nozzle with a certain size and specification by using a numerical control lathe and a processing center.
Further, the boron nitride powder has D50 of 3-5 microns and oxygen content of 0.7-0.9 wt%.
Further, the silicon nitride granulation powder is prepared by grinding 85-92wt% of silicon nitride raw powder, 5-8wt% of yttrium oxide powder, 3-5wt% of alumina powder, 1-2wt% of magnesium oxide powder and 0.5wt% of PVB into slurry through ball milling and then performing spray drying, wherein the sum of the mass percentages of the raw materials is 100%. Wherein D50 of the silicon nitride raw powder is 1-3 microns, and alpha phase is more than 90%; the D50 of the yttrium oxide powder is not more than 1 micron; the alumina powder has a D50 of no greater than 1 micron.
The purpose of adding the silicon nitride granulation powder is that pure silicon nitride is difficult to sinter, a sintering aid needs to be added, if a mode of adding the sintering aid and the silicon nitride respectively is adopted, the added silicon nitride sintering aid is difficult to match with the silicon nitride because the density of boron nitride is minimum and the volume fraction is large, the corresponding volume fraction is about 50% when about 30% of the mass fraction is about, and therefore the silicon nitride granulation powder is utilized, and meanwhile, a dry mixing process is adopted to avoid dispersion of the granulation powder, so that the purpose that the silicon nitride can be sintered smoothly in the composite material is achieved.
Further, the specific way of dry mixing uniformly by using a high-speed blade type rotary pulverizer (the rotating speed of 15000-: starting the grinder for 30 seconds, stopping the grinder for 5-10 minutes to cool the powder, then opening the cover of the grinder, cleaning part of the powder adhered to the cover and the wall of the container by using a brush, then sealing the cover, starting the grinder for 30 seconds, stopping the grinder for 5-10 minutes, and cleaning the powder by using the brush; how to do this repeatedly for 3-5 times.
The invention has the advantages that:
the strength and the corrosion resistance of boron nitride are improved by adding silicon nitride, the thermal conductivity is reduced, the material disclosed by the invention has the advantages of resisting the corrosion of high-nickel stainless steel, titanium-containing molybdenum cobalt and other high-alloy steel metal liquids, and the service life of the nozzle is prolonged.
The addition of silicon nitride granulation powder and the coordination of yttrium oxide, and the effect of reducing the thermal conductivity of a plurality of materials reduce the thermal conductivity of the boron nitride/silicon nitride ceramic with higher thermal conductivity.
The silicon nitride granulation powder is adopted instead of a mode of respectively adding the sintering aid and the silicon nitride, so that the silicon nitride can be smoothly sintered in the composite material, various properties of the composite material are improved, the bending strength is improved from about 100MPa to about 250-300MPa, and the density is improved from about 85% to over 96%.
Drawings
FIG. 1 is an electron micrograph of a composite boron nitride ceramic prepared in example 1;
FIG. 2 is an electron micrograph of the composite boron nitride ceramic prepared in comparative example 1.
Detailed Description
In order to make the aforementioned and other features and advantages of the invention more comprehensible, embodiments accompanied with figures are described in detail below. The method of the present invention is a method which is conventional in the art unless otherwise specified.
The physical properties of the raw materials used in the following examples and comparative examples were as follows: boron nitride powder has a D50 of 4 microns and an oxygen content of 0.8 wt%; d50 of the silicon nitride raw powder is 2 microns, and the alpha phase is more than 90 percent; yttrium oxide powder has a D50 of 1 micron; the alumina powder had a D50 of 1 micron.
Example 1
A preparation method of a composite boron nitride ceramic nozzle comprises the following steps:
(1) preparing a sintering material: uniformly mixing 60wt% of silicon nitride granulation powder and 40wt% of boron nitride powder by a pulverizer in a dry method; the specific way of dry mixing with a high-speed blade type rotary pulverizer (the rotating speed is 20000 rpm) is as follows: starting the grinder for 30 seconds, stopping for 5 minutes to cool the powder, then opening the cover of the grinder, cleaning part of the powder adhered to the cover and the wall of the container by using a brush, then sealing the cover, starting the grinder for 30 seconds, stopping for 5 minutes, and cleaning by using the brush; how to do this 5 times.
(2) Hot-pressing and sintering: filling the mixed raw material powder in a rubber bag, vacuumizing, sealing, performing isostatic pressing at 200Mpa for 60 minutes, compacting, and processing the isostatic pressing blank into the size of the inner cavity of a hot pressing die by using a numerical control diamond wire saw (L400 mm W400mm H300 mm); loading the processed isostatic pressing blank into a hot-pressing die, and sending into a hot-pressing furnace; vacuumizing to 10Pa, heating, keeping the vacuumizing state till 1200 ℃, then filling nitrogen to one atmosphere, keeping the flowing nitrogen atmosphere to continue heating, starting pressurizing to 1500 ℃, gradually increasing the pressure to 25Mpa when the highest temperature is 1820 ℃, then keeping the temperature and the pressure for 0.5 hour, then stopping heating and naturally cooling, and keeping the pressure constant during the period; when the temperature is reduced to 1200 ℃, the pressure is not maintained any more, the pressure is reduced along with the reduction of the temperature, when the temperature is 800 ℃, the pressure is removed, the furnace temperature is reduced to 80 ℃, then the furnace is opened, the mold is taken out, the mold is continuously cooled to the room temperature, and the sintered blank body is taken out; the density of the sintered body is 96 percent, and the breaking strength is 320Mpa +/-30 Mpa.
(3) Processing: and (3) blanking the blank sintered by hot pressing by using a numerical control diamond sand wire cutting machine, and processing the blank into a ceramic nozzle with a certain size and specification by using a numerical control lathe and a processing center.
Wherein, the silicon nitride granulation powder is prepared by grinding 85wt% of silicon nitride raw powder, 8wt% of yttrium oxide powder, 5wt% of alumina powder, 1.5wt% of magnesium oxide powder and 0.5wt% of PVB into slurry through ball milling and then performing spray drying.
Comparative example 1
The composite boron nitride ceramic nozzle is prepared by respectively adding a sintering aid and silicon nitride, and specifically, silicon nitride, boron nitride, yttrium oxide, aluminum oxide and magnesium oxide are put into a high-speed pulverizer to be dry-stirred, mixed and sintered, and a hot-pressed silicon nitride/boron nitride blank body is prepared by adopting the same sintering process as in example 1, wherein the density of the blank body is only 88%, and the bending strength is 95Mpa +/-15 Mpa.
In comparative example 1, no PVB binder was added, and the amount of the other raw materials was the same as in example 1.
The SEM photograph of the sample of comparative example 1 and the SEM photograph of the sample of example 1 show that the sintered density of the sample of comparative example 1 is relatively poorer.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.

Claims (6)

1. The preparation method of the composite boron nitride ceramic nozzle is characterized by comprising the following steps of:
(1) preparing a sintering material: uniformly mixing 60wt% of silicon nitride granulation powder and 40wt% of boron nitride powder by a pulverizer in a dry method;
(2) hot-pressing and sintering: the mixed raw material powder is filled in a rubber bag, the rubber bag is sealed after being vacuumized, then isostatic pressing is carried out at 100 and 200Mpa for pressure maintaining for 60 minutes for compaction, and then the isostatic pressing blank is processed into the size of the inner cavity of the hot pressing die by a numerical control diamond wire saw or an end face milling machine; loading the processed isostatic pressing blank into a hot-pressing die, and sending into a hot-pressing furnace; vacuumizing to 10Pa, starting heating, keeping the vacuumizing state till 1200 ℃ of 1000 plus materials, then filling nitrogen to one atmosphere, then keeping the flowing nitrogen atmosphere for continuously heating, starting pressurizing at 1500 ℃, gradually increasing the pressure until 1850 ℃ of the highest temperature 1800 plus materials, increasing the pressure to 25-30Mpa, then keeping the temperature and the pressure for 0.5-3 hours, then stopping heating and naturally cooling, and keeping the pressure constant during the period; when the temperature is reduced to 1200 ℃, the pressure is not maintained any more, the pressure is reduced along with the reduction of the temperature, when the temperature is 800 ℃, the pressure is removed, the furnace temperature is reduced to 80 ℃, then the furnace is opened, the mold is taken out, the mold is continuously cooled to the room temperature, and the sintered blank body is taken out;
(3) processing: and (3) blanking the blank sintered by hot pressing by using a numerical control diamond sand wire cutting machine, and processing the blank into the ceramic nozzle by using a numerical control lathe and a processing center.
2. The method according to claim 1, wherein the boron nitride powder has a D50 value of 3 to 5 μm and an oxygen content of 0.7 to 0.9 wt%.
3. The method according to claim 1, wherein the silicon nitride granulated powder is prepared by ball-milling 85 to 92wt% of silicon nitride raw powder, 5 to 8wt% of yttrium oxide powder, 3 to 5wt% of aluminum oxide powder, 1 to 2wt% of magnesium oxide powder, and 0.5wt% of PVB into slurry and then spray-drying, and the sum of the mass percentages of the raw materials is 100%.
4. The method according to claim 3, wherein D50 of the silicon nitride raw powder is 1 to 3 μm and the alpha phase is 90% or more.
5. A method of producing a yttrium oxide powder according to claim 3, wherein the yttrium oxide powder has a D50 of not more than 1 μm.
6. The method according to claim 3, wherein the alumina powder has a D50 of not more than 1 μm.
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JPH06100369A (en) * 1992-09-18 1994-04-12 Nippon Cement Co Ltd Method for producing composite product of silicon nitride with boron nitride
JPH06329473A (en) * 1993-05-21 1994-11-29 Ube Ind Ltd Normal-pressure sintering silicon nitride material having abrasion resistance
CN104892005A (en) * 2015-05-04 2015-09-09 齐鲁工业大学 Preparation method of silicon nitride-based self-lubricating ceramic cutter material containing alumina-coated hexagonal boron nitride composite powder
CN106431414A (en) * 2016-09-29 2017-02-22 连云港东渡碳化硅有限公司 Preparation method of pressureless-sintered silicon carbide ceramic
CN106495703A (en) * 2016-10-27 2017-03-15 中国工程物理研究院材料研究所 A kind of preparation method of silicon nitride sealing ring
CN106518088A (en) * 2016-10-27 2017-03-22 中国工程物理研究院材料研究所 Manufacturing method of high-performance silicon nitride sealing ring
CN106915961A (en) * 2017-02-24 2017-07-04 华南理工大学 A kind of Graphene zirconium oxide composite material and preparation method thereof
CN112028637A (en) * 2020-08-24 2020-12-04 中材高新氮化物陶瓷有限公司 Preparation method of high-reliability long-life silicon nitride ceramic ball for aviation bearing
CN112266250A (en) * 2020-10-27 2021-01-26 河南雅利安新材料有限公司 Silicon carbide ceramic sealing ring and preparation method thereof
CN113105252A (en) * 2021-04-20 2021-07-13 中材高新氮化物陶瓷有限公司 Sintering aid for preparing silicon nitride ceramic, application of sintering aid and preparation method of silicon nitride ceramic
CN113443919A (en) * 2021-06-30 2021-09-28 北京双盛永科技发展有限公司 Amorphous alloy nozzle material and preparation method thereof

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* Cited by examiner, † Cited by third party
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CN1030402A (en) * 1987-07-06 1989-01-18 国家建筑材料工业局山东工业陶瓷研究设计院 Silicon nitride/boron nitride composite and manufacture method thereof
EP0439419A1 (en) * 1990-01-23 1991-07-31 Ercros S.A. Composite ceramic materials for applications in engineering at high temperature and under severe conditions of thermal shock and a process for their production
JPH06100369A (en) * 1992-09-18 1994-04-12 Nippon Cement Co Ltd Method for producing composite product of silicon nitride with boron nitride
JPH06329473A (en) * 1993-05-21 1994-11-29 Ube Ind Ltd Normal-pressure sintering silicon nitride material having abrasion resistance
CN104892005A (en) * 2015-05-04 2015-09-09 齐鲁工业大学 Preparation method of silicon nitride-based self-lubricating ceramic cutter material containing alumina-coated hexagonal boron nitride composite powder
CN106431414A (en) * 2016-09-29 2017-02-22 连云港东渡碳化硅有限公司 Preparation method of pressureless-sintered silicon carbide ceramic
CN106495703A (en) * 2016-10-27 2017-03-15 中国工程物理研究院材料研究所 A kind of preparation method of silicon nitride sealing ring
CN106518088A (en) * 2016-10-27 2017-03-22 中国工程物理研究院材料研究所 Manufacturing method of high-performance silicon nitride sealing ring
CN106915961A (en) * 2017-02-24 2017-07-04 华南理工大学 A kind of Graphene zirconium oxide composite material and preparation method thereof
CN112028637A (en) * 2020-08-24 2020-12-04 中材高新氮化物陶瓷有限公司 Preparation method of high-reliability long-life silicon nitride ceramic ball for aviation bearing
CN112266250A (en) * 2020-10-27 2021-01-26 河南雅利安新材料有限公司 Silicon carbide ceramic sealing ring and preparation method thereof
CN113105252A (en) * 2021-04-20 2021-07-13 中材高新氮化物陶瓷有限公司 Sintering aid for preparing silicon nitride ceramic, application of sintering aid and preparation method of silicon nitride ceramic
CN113443919A (en) * 2021-06-30 2021-09-28 北京双盛永科技发展有限公司 Amorphous alloy nozzle material and preparation method thereof

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Application publication date: 20220114