CN102875153B - Spray drying granulation method of silicon nitride ceramic powder used for mechanical sealing - Google Patents
Spray drying granulation method of silicon nitride ceramic powder used for mechanical sealing Download PDFInfo
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Abstract
The invention discloses a spray drying granulation method of silicon nitride ceramic powder used for mechanical sealing, which is characterized in that the method comprises the following steps: (1) weighing powder prepared by the following components by weight; (2) proportioning sintering aid slurry; (3) proportioning a binder and an antifoaming agent solution; (4) proportioning silicon nitride slurry; (5) proportioning silicon nitride mixed slurry; (6) obtaining silicon nitride powder with different particle size ranges. The method is high in yield, low in production cost, safe for production, low in environmental pollution, and stable for powder performance.
Description
Technical field
The present invention relates to the drying-granulating method of a kind of powder spraying in technical field of ceramic material, is specifically the powder spray drying granulation method of mechanical seal with silicon nitride ceramics.
Background technology
Nitride ceramics is that the class that 20 century 70s develop rapidly has high strength, high rigidity, high temperature resistant, and has the structural ceramic material of good calorifics, electric property.Silicon nitride ceramics due to it under high temperature and normal temperature condition, has high rigidity, wear-resistant, corrosion-resistant, anti-oxidant and good heat shock resistance and mechanical shock performance, the ideal material that is considered to many high-temperature components in ceramic engine, the turibine rotor parts of silicon nitride ceramics etc. can be used in panzer, in the special cars such as racing car, and the silicon nitride cutting tool, the silicon nitride ceramics bearing is widespread use in modern industry and production, in the use of mechanical seal industry is substantially all reaction sintering silicon nitride, its physical and chemical performance and mechanical property and normal pressure-sintered silicon nitride differ greatly.Silicon nitride is the strong covalent bond compound, and its self-diffusion coefficient is very little, produces densification required volume diffusion and crystal boundary rate of diffusion also very little, and Si
3N
4In temperature more than 1700 ℃, can decompose and evaporation, therefore pure silicon nitride can't reach densification by solid state sintering, must add sintering aid, forms liquid phase and realizes densification with the silicon oxide on alpha-silicon nitride powders surface.
The forming technique of structural ceramics has determined to a great extent the homogeneity of base substrate and has prepared the ability of complicated form part, and directly had influence on the cost of reliability of material and the finished product.Dry-pressing formed and cold isostatic compaction obtains widespread use in laboratory and actual production, although dry-pressing formed, there are density gradient and Density inhomogeneity, because shaping efficiency is high, size is accurate, the first-selected moulding process that becomes general ceramic product with low cost.For reaching steady quality and the requirement of compacting fast in industrial production, the ceramic raw material powder has good mobility in mold filling process be very important, submicron order or micron-sized powder mobility are not fine, usually need to improve its mobility through granulation.
Silicon nitride powder is evenly mixed with various sintering aids, and the powder that obtains good fluidity by spray drying granulation is applicable to dry-pressing formed suitability for industrialized production.For silicon nitride powder, because of the reason of surface hydrophobicity group, water, as medium, prepares low viscous dense suspension slurry very difficult.At present domestic generally with an organic solvent (as dehydrated alcohol etc.) makes slurry and granulation as dispersion medium, for the production of in not only cost is high but also to have a volatilization of certain organic solvent dangerous, namely the steam of volatilization can be rapidly and air mixed, forms explosive mixed gas.
Summary of the invention
The technical problem to be solved in the present invention is, provides that a kind of output is high, production cost is low, production safety, the mechanical seal that low in the pollution of the environment, properties of powder is stable be by the spray drying granulation method of silicon nitride powder.
Technical scheme of the present invention is, a kind of powder spray drying granulation method of the mechanical seal of following steps with silicon nitride ceramics that have is provided, and comprises the following steps: (1) takes powder prepared by each component by following parts by weight:
100 parts of nitrogenize silicon powder ︰,
2.5～11.5 parts of sintering aid Wei Fen ︰,
0.3～3.5 part of Nian Jie Ji ︰,
0.01～2 part of Fen San Ji ︰,
0.2～3 part of Zeng Su Ji ︰,
0.1～2 part of Run Hua Ji ︰,
0.01～0.05 part of Xiao Pao Ji ︰,
Dispersion medium: deionized water is: 50～120 parts;
(2) the sintering aid micro mist that takes the formula rate umber add formula rate umber deionized water 20%～50% in, with 12～24 hours ball millings of ball milling bucket ball milling of urethane protection, mix again, medium ball is agate ball, high purity aluminium oxide ball, silicon nitride ball or silicon carbide ball, thereby forms the sintering aid slurry;
(3) binding agent and the defoamer that take the formula rate umber dissolve in formula rate umber deionized water remaining 50～80%, thereby form binding agent and defoamer solution;
(4) by the formula rate umber, take silicon nitride powder, put into step (3) gained binding agent and defoamer solution, stirred 2～8 hours with stirrer, with dispersion agent, adjust pH value 9.5～12 while stirring; Thereby formation Silicon Nitride;
(5) Silicon Nitride after step (4) is completed adds in the sintering aid slurry of step (2), and adds the softening agent of formula rate umber and lubricant to continue ball milling 12～48 hours, thereby forms the silicon nitride mixed slurry;
(6) after the silicon nitride mixed slurry of step (5) gained is sieved with 200～400 mesh sieve, with the adjustable speed constant flow pump, send in centrifugal Spray Grain-make Drier in the shower nozzle with 5000～8000 rev/mins of rotational speed, spray into small slurry droplet Rotary drying glomeration particle in warm air in the centrifugal spray drying tablets press; Or, after with surge pump, above-mentioned slurry being pressurized to 0.2～1.0MPa, by the pressure nozzle of press spray drying-granulating machine, spraying into the Silicon Nitride mist droplet and be spray dried to spherical particle in the warm air of press spray drying-granulating machine; In drying process, adjusting the hot-air inlets temperature is 200～250 ℃, temperature out is 70～150 ℃, the rapid drying in warm air of small Silicon Nitride droplet becomes solid spherical particle, 10 microns to 150 microns of solid spherical particle diameters, with 80 orders～sub-classification of 250 mesh sieve, sieve, obtain the beta-silicon nitride powder of different-grain diameter scope.
The described silicon nitride powder of step (1), the meta particle diameter D of micro mist
500.30～3.00 microns, α phase content>80wt%, nitrogen content>37wt%, free silica<0.5wt%.
The described sintering aid micro mist of step (1) is that one or more arbitrary proportions in aluminum oxide, yttrium oxide, magnesium oxide, aluminium nitride mix;
Alumina powder wherein, its meta particle diameter D
500.1～3 microns, purity is greater than 99.5wt%,
Yttrium oxide micro mist wherein, its meta particle diameter D
500.3～3 microns, purity is greater than 99.9wt%,
Fine magnesium oxide micro-powder wherein, its meta particle diameter D
500.3～3 microns, purity is greater than 99.9wt%;
Aluminium nitride micro mist wherein, its meta particle diameter D
500.1～3 microns, purity is greater than 99.9wt%.
The described binding agent of step (1) is that one or more arbitrary proportions in polyvinyl alcohol, dextrin, methylcellulose gum, glucose mix.
The described dispersion agent of step (1) is that one or more arbitrary proportions in ammoniacal liquor, Tetramethylammonium hydroxide, sodium cetanesulfonate mix.
The described softening agent of step (1) is polyoxyethylene glycol, and relative molecular weight is in 400 left and right.
The described lubricant of step (1) is whiteruss.
The described defoamer of step (1) is that one or more arbitrary proportions in n-Octanol, propyl carbinol, ethylene glycol mix.
After adopting above method, the present invention has the following advantages: be dispersion medium owing to adopting deionized water, to be mixed in certain sequence slurry by powder and a certain amount of deionized water of certain weight proportion, ball milling homogenizing refinement, the spray-dried silicon nitride mixing granulation powder that is a granulated into, institute's pelletizing shape particulate material has good fluidity, composition is uniformly dispersed, loose density is stablized adjustable, and processability is good, is suitable for normal pressure-sintered silicon nitride continuous batch pressed compact and hot pressed sintering silicon nitride.Present method can produce low viscous dense suspension slurry and cost is low, do not have organic solvent volatilization dangerous, and the silicon nitride powder output of preparation is high simultaneously, production cost is low, production safety, low in the pollution of the environment, properties of powder stable.
Specific embodiment
The invention is further illustrated by the following examples, but the present invention not only is confined to following examples.
Embodiment 1
(1) take powder prepared by each component by following parts by weight:
Nitrogenize silicon powder ︰ 1000 grams,
Sintering aid Wei Fen ︰ 35 grams,
Nian Jie Ji ︰ 3 grams,
Fen San Ji ︰ 0.5 gram,
Zeng Su Ji ︰ 3 grams,
Run Hua Ji ︰ 1 gram,
Xiao Pao Ji ︰ 0.5 gram,
Deionized water is: 700 grams.
Silicon nitride powder (Si wherein
3N
4), the D of micro mist
500.51 micron of diameter, α phase content 91.0wt%, nitrogen content>37wt%, silicon<0.5wt% wanders about as a refugee.
Sintering aid is aluminum oxide and yttrium oxide, and its additional proportion is 6:4,
Alumina powder wherein, its D
50The meta particle diameter is the 0..3 micron, and purity is greater than 99.5wt%,
Yttrium oxide micro mist wherein, its D
503 microns of meta particle diameters, purity is greater than 99.9wt%,
Binding agent is polyvinyl alcohol;
Described dispersion agent is Tetramethylammonium hydroxide;
Described softening agent is polyoxyethylene glycol, and relative molecular weight is in 400 left and right;
Described lubricant is whiteruss;
Described defoamer is n-Octanol.
(2) take aluminum oxide 21 grams, yttrium oxide 14 grams, add in 300 gram deionized waters, mixed in 16 hours at urethane protection ball milling bucket ball milling, and medium ball is the high purity aluminium oxide ball; Thereby form the sintering aid slurry;
(3) take binding agent polyvinyl alcohol 3 grams, defoamer n-Octanol 0.5 gram, add in 400 gram deionized waters and dissolve; Thereby form binding agent and defoamer solution;
(4) take silicon nitride powder 1000 grams, put into the described binding agent of step (3), defoamer solution, stirred 4 hours with stirrer, with dispersion agent, adjust pH value 12 while stirring; Thereby formation Silicon Nitride;
(5) Silicon Nitride of step (4) is added in the sintering aid slurry of step (2), and add softening agent and lubricant to continue ball milling refinement 24 hours, form the silicon nitride mixed slurry;
(6) after the slurry of step (5) gained is sieved with 400 mesh sieve; with the adjustable speed constant flow pump, send in the shower nozzle of centrifugal spray drying tablets press; through 6000 rev/mins of rotating speeds, spray into small slurry droplet and rotate in warm air, adjusting the hot-air inlets temperature is 230 ℃, and temperature out is 90 ℃.The slurry droplet in warm air rapid drying be rotated into spherical particle, 10 microns to 150 microns of the small ball's diameters, sieve respectively with 80 and 250 mesh sieve, meal and fine powder powder mix are removed in acquisition.
The graphite jig of packing into after with 30MPa compression moulding with this powder, under 30MPa pressure, 1850 ℃ of insulations were carried out making sample after hot pressed sintering in one hour, and recording density is 3.188g/cm
3, bending strength 731MPa, fracture toughness property 5.34MPam
1/2.
Embodiment 2
(1) take powder prepared by each component by following parts by weight:
Nitrogenize silicon powder ︰ 1000 grams,
Sintering aid Wei Fen ︰ 100 grams,
Nian Jie Ji ︰ 5 grams,
Fen San Ji ︰ 0.5 gram,
Zeng Su Ji ︰ 6 grams,
Run Hua Ji ︰ 5 grams,
Xiao Pao Ji ︰ 0.2 gram,
Deionized water is: 1000 grams.
Silicon nitride powder (Si wherein
3N
4), the D of micro mist
500.51 micron of diameter, α phase content 91.0wt%, nitrogen content>37wt%, silicon<0.5wt% wanders about as a refugee.
Sintering aid is aluminum oxide, yttrium oxide, and its additional proportion is 6:4,
Alumina powder wherein, its D
50The meta particle diameter is the 0..3 micron, and purity is greater than 99.5wt%,
Yttrium oxide micro mist wherein, its D
503 microns of meta particle diameters, purity is greater than 99.9wt%,
Binding agent is polyvinyl alcohol;
Described dispersion agent is Tetramethylammonium hydroxide;
Described softening agent is polyoxyethylene glycol, and relative molecular weight is in 400 left and right;
Described lubricant is whiteruss;
Described defoamer is n-Octanol.
The concrete technology step is as follows:
(2) take aluminum oxide 60 grams, yttrium oxide 40 grams, put into 400 gram deionized waters, mixed in 24 hours at urethane protection ball milling bucket ball milling, and medium ball is the high purity aluminium oxide ball; Thereby form the sintering aid slurry;
(3) take binding agent polyvinyl alcohol 5 grams, defoamer 0.2 gram, add in other 600 gram deionized waters and dissolve; Thereby form binding agent and defoamer solution;
(4) take silicon nitride powder 1000 grams, put into the described binding agent of step (3) step and defoamer solution, stirred 6 hours with stirrer, with dispersion agent, adjust pH value 11.5 while stirring; Thereby formation Silicon Nitride;
(5) Silicon Nitride of step (4) is added in the sintering aid slurry of step (2), and add softening agent and lubricant to continue ball milling refinement 40 hours, form the silicon nitride mixed slurry;
(6) after the slurry of step (5) gained is sieved with 400 mesh sieve; with the adjustable speed constant flow pump, send in the shower nozzle of centrifugal spray drying tablets press; through 6000 rev/mins of rotating speeds, spraying into small slurry droplet rotates in warm air; adjusting the hot-air inlets temperature is 240 ℃, and temperature out is 100 ℃.The slurry droplet in warm air rapid drying be rotated into spherical particle, 10 microns to 150 microns of the small ball's diameters, sieve respectively with 80-250 mesh sieve, the acquisition be less than 80 orders, be greater than 250 purpose powder mixs.
After 200MPa compression moulding, under-0.02MPa nitrogen atmosphere, insulation, sinter silicon nitride ceramics into and make sample under 1840 ℃, and recording density is 3.226g/cm
3, bending strength 639MPa, fracture toughness property 4.93MPam
1/2.
Embodiment 3
(1) take powder prepared by each component by following parts by weight:
Nitrogenize silicon powder ︰ 1000 grams,
Sintering aid Wei Fen ︰ 50 grams,
Nian Jie Ji ︰ 3 grams,
Fen San Ji ︰ 0.5 gram,
Zeng Su Ji ︰ 3 grams,
Run Hua Ji ︰ 1 gram,
Xiao Pao Ji ︰ 0.5 gram,
Deionized water is: 800 grams.
Silicon nitride powder (Si wherein
3N
4), the D of micro mist
500.51 micron of diameter, α phase content 91.0wt%, nitrogen content>37wt%, silicon<0.5wt% wanders about as a refugee.
Sintering aid is aluminum oxide, yttrium oxide, and its additional proportion is 6:4,
Alumina powder wherein, its D
50The meta particle diameter is the 0..3 micron, and purity is greater than 99.5wt%,
Yttrium oxide micro mist wherein, its D
503 microns of meta particle diameters, purity is greater than 99.9wt%,
Binding agent is polyvinyl alcohol;
Described dispersion agent is Tetramethylammonium hydroxide;
Described softening agent is polyoxyethylene glycol, and relative molecular weight is in 400 left and right;
Described lubricant is whiteruss;
Described defoamer is n-Octanol.
The concrete technology step is as follows:
(2) take aluminum oxide 30 grams, yttrium oxide 20 grams, add in 300 gram deionized waters, mixed in 16 hours at urethane protection ball milling bucket ball milling, and medium ball is the high purity aluminium oxide ball;
(3) take binding agent polyvinyl alcohol 3 grams, defoamer n-Octanol 0.5 gram, add in 500 gram deionized waters and dissolve;
(4) take silicon nitride powder 1000 grams, put into the described binding agent of step (3) step, defoamer solution, stirred 4 hours with stirrer, with dispersion agent, adjust pH value 12 while stirring;
(5) Silicon Nitride of step (4) is added in the sintering aid slurry of step (2), and add softening agent and lubricant to continue ball milling refinement 24 hours, form the silicon nitride mixed slurry;
(6) after the slurry of step (5) gained is sieved with 400 mesh sieve; with the adjustable speed constant flow pump, send in the shower nozzle of centrifugal spray drying tablets press; through 6000 rev/mins of rotating speeds, spraying into small slurry droplet rotates in warm air; adjusting the hot-air inlets temperature is 235 ℃, and temperature out is 100 ℃.The slurry droplet in warm air rapid drying be rotated into spherical particle, 10 microns to 150 microns of the small ball's diameters, sieve respectively with 80 and 250 mesh sieve, meal and fine powder powder mix are removed in acquisition.
The graphite jig of packing into after with 30MPa compression moulding with this powder, under 30MPa pressure, 1850 ℃ of insulations were carried out making sample after hot pressed sintering in one hour, and recording density is 3.208g/cm
3, bending strength 791MPa, fracture toughness property 6.15MPam
1/2.
Claims (1)
1. a mechanical seal by the spray drying granulation method of silicon nitride ceramics powder, is characterized in that: comprise the following steps:
(1) take powder prepared by each component by following parts by weight:
100 parts of nitrogenize silicon powder ︰,
2.5～11.5 parts of sintering aid Wei Fen ︰,
0.3～3.5 part of Nian Jie Ji ︰,
0.01～2 part of Fen San Ji ︰,
0.2～3 part of Zeng Su Ji ︰,
0.1～2 part of Run Hua Ji ︰,
0.01～0.05 part of Xiao Pao Ji ︰,
Dispersion medium: deionized water is: 50～120 parts;
(2) the sintering aid micro mist that takes the formula rate umber add formula rate umber deionized water 20%～50% in, with 12～24 hours ball millings of ball milling bucket ball milling of urethane protection, mix again, medium ball is agate ball, high purity aluminium oxide ball, silicon nitride ball or silicon carbide ball, thereby forms the sintering aid slurry;
(3) binding agent and the defoamer that take the formula rate umber dissolve in formula rate umber deionized water remaining 50～80%, thereby form binding agent and defoamer solution;
(4) by the formula rate umber, take silicon nitride powder, put into step (3) gained binding agent and defoamer solution, stirred 2～8 hours with stirrer, with dispersion agent, adjust pH value 9.5～12 while stirring; Thereby formation Silicon Nitride;
(5) Silicon Nitride after step (4) is completed adds in the sintering aid slurry of step (2), and adds the softening agent of formula rate umber and lubricant to continue ball milling 12～48 hours, thereby forms the silicon nitride mixed slurry;
(6) method 1: after the silicon nitride mixed slurry of step (5) gained is sieved with 200～400 mesh sieve, with the adjustable speed constant flow pump, send in centrifugal Spray Grain-make Drier in the shower nozzle with 5000～8000 rev/mins of rotational speed, spray into Rotary drying glomeration particle in the warm air of small slurry droplet in the centrifugal spray drying tablets press; In drying process, adjusting the hot-air inlets temperature is 200～250 ℃, temperature out is 70～150 ℃, the rapid drying in warm air of small Silicon Nitride droplet becomes solid spherical particle, 10 microns to 150 microns of solid spherical particle diameters, with 80 orders～sub-classification of 250 mesh sieve, sieve, obtain the beta-silicon nitride powder of different-grain diameter scope;
Or method 2: after the silicon nitride mixed slurry of step (5) gained is sieved with 200～400 mesh sieve, after silicon nitride mixed slurry after sieving with surge pump is pressurized to 0.2～1.0MPa, by the pressure nozzle of press spray drying-granulating machine, sprays into the Silicon Nitride mist droplet and be spray dried to spherical particle in the warm air of press spray drying-granulating machine; In drying process, adjusting the hot-air inlets temperature is 200～250 ℃, temperature out is 70～150 ℃, the rapid drying in warm air of small Silicon Nitride droplet becomes solid spherical particle, 10 microns to 150 microns of solid spherical particle diameters, with 80 orders～sub-classification of 250 mesh sieve, sieve, obtain the beta-silicon nitride powder of different-grain diameter scope;
The described silicon nitride powder of step (1), the meta particle diameter D of micro mist
500.30～3.00 microns, α phase content>80wt%, nitrogen content>37wt%, free silica<0.5wt%;
The described sintering aid micro mist of step (1) is that more than one arbitrary proportions in aluminum oxide, yttrium oxide, magnesium oxide, aluminium nitride mix;
Alumina powder wherein, its meta particle diameter D
500.1～3 microns, purity is greater than 99.9wt%,
Yttrium oxide micro mist wherein, its meta particle diameter D
500.3～3 microns, purity is greater than 99.9wt%,
Fine magnesium oxide micro-powder wherein, its meta particle diameter D
500.3～3 microns, purity is greater than 99.9wt%;
Aluminium nitride micro mist wherein, its meta particle diameter D
500.1～3 microns, purity is greater than 99.9wt%;
The described binding agent of step (1) is that more than one arbitrary proportions in polyvinyl alcohol, dextrin, methylcellulose gum, glucose mix;
The described dispersion agent of step (1) is that more than one arbitrary proportions in ammoniacal liquor, Tetramethylammonium hydroxide, sodium cetanesulfonate mix;
The described lubricant of step (1) is whiteruss;
The described defoamer of step (1) is that more than one arbitrary proportions in n-Octanol, propyl carbinol, ethylene glycol mix.
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| CN103102172B (en) * | 2013-01-28 | 2014-06-11 | 西北农林科技大学 | Method for preparing porous silicon nitride ceramic by ammonium bicarbonate foaming method |
| CN103102143B (en) * | 2013-01-31 | 2014-08-06 | 西安理工大学 | Preparation method of ceramic paste slurry molded based on bionics |
| CN104072150B (en) * | 2014-06-12 | 2019-07-02 | 安徽安尔达机电有限公司 | A kind of preparation process of water pump seal silicon nitride ceramic material |
| CN105541342A (en) * | 2016-01-08 | 2016-05-04 | 梁小利 | High-strength silicon nitride composite ceramic material and preparation method thereof |
| CN106270529A (en) * | 2016-08-11 | 2017-01-04 | 合肥毅创钣金科技有限公司 | A kind of high temperature resistant shock resistance ceramic-seal ring and preparation method thereof |
| CN107117971A (en) * | 2017-04-24 | 2017-09-01 | 武汉理工大学 | A kind of method that high-energy ball milling combination spray drying technology prepares superfine boron carbide pelletizing |
| CN107097327B (en) * | 2017-04-28 | 2019-03-01 | 湖北高磁新材料科技有限公司 | Ferrite forming body production line and ferrite forming body production method |
| CN109796211A (en) * | 2019-03-29 | 2019-05-24 | 深圳市宏通新材料有限公司 | For making the binder and ceramic material of thin product |
| CN111825454A (en) * | 2019-08-29 | 2020-10-27 | 宁波伏尔肯科技股份有限公司 | Preparation method of layered structure ceramic ring for mechanical seal |
| CN114085084A (en) * | 2020-08-25 | 2022-02-25 | 西安增材制造国家研究院有限公司 | High-strength silicon nitride ceramic and preparation method thereof |
| CN113999019B (en) * | 2021-11-19 | 2022-09-27 | 中材高新氮化物陶瓷有限公司 | Preparation method of silicon nitride ceramic granulation powder |
| CN116217238A (en) * | 2023-03-10 | 2023-06-06 | 福建镓镒半导体材料有限公司 | Metal-based silicon nitride composite material and preparation method thereof |
| CN116352057B (en) * | 2023-03-27 | 2024-06-18 | 重庆罗曼新材料科技有限公司 | ZTA ceramic particle composite wear-resistant part and preparation method thereof |
| CN117401978A (en) * | 2023-11-22 | 2024-01-16 | 长春设备工艺研究所 | Gradient ceramic material based on bionics and preparation method and application thereof |
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| JP3127225B2 (en) * | 1997-11-18 | 2001-01-22 | 工業技術院長 | Low temperature sintering aid for silicon nitride and sintering method |
| FR2954766B1 (en) * | 2009-12-24 | 2015-04-24 | Saint Gobain Ct Recherches | POWDER OF CERAMIC PELLETS |
| CN102503428A (en) * | 2011-10-17 | 2012-06-20 | 宁波伏尔肯机械密封件制造有限公司 | Spray drying granulation method of boron carbide powder |
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