CN105315006A - Method for preparing gradient porous silicon nitride ceramic - Google Patents
Method for preparing gradient porous silicon nitride ceramic Download PDFInfo
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- CN105315006A CN105315006A CN201510875817.8A CN201510875817A CN105315006A CN 105315006 A CN105315006 A CN 105315006A CN 201510875817 A CN201510875817 A CN 201510875817A CN 105315006 A CN105315006 A CN 105315006A
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Abstract
The invention discloses a method for preparing gradient porous silicon nitride ceramic. The method comprises the following steps: 1) pretreating biomass, carbonizing, grinding so as to obtain a carbon-silicon precursor, mixing the carbon-silicon precursor with silicon nitride and an additive, grinding and pelleting, so as to obtain mixtures containing carbon and silicon; 2) sequentially feeding two or more than two mixtures containing carbon and silicon obtained in the step 1) into a mold, feeding each layer in turn, performing jump vibration, and molding under the pressure of 3-20MPa, so as to obtain a blank; and 3) sintering the blank in nitrogen atmosphere at normal pressure, and cooling, thereby obtaining the gradient porous silicon nitride ceramic. The gradient porous silicon nitride ceramic can be prepared by using a one-step carbon thermal recovery-normal pressure sintering method which is simple in process and low in cost.
Description
Technical field
The invention belongs to field of ceramic preparation, relate to a kind of preparation method of gradient porous silicon nitride ceramics.
Background technology
Gradient porous ceramics refers to that void content or aperture or pore structure make the pottery of regular change with sample size.Owing to having asymmetrical pore structure, easily realize small-bore ventilative greatly, have the advantages that high filtering precision, large air transmission coefficient, backwash are effective, be used in filtering separation field and can greatly improve filtering accuracy and filtration efficiency, reduce pressure drop, thus reduce production cost, be specially adapted to that temperature is high, the separation with the mixed stream containing minuteness particle such as corrodibility, high temperature fume dust removal and fine filtering etc.At present, gradient porous ceramics is for solid-liquid separation membrane, support of the catalyst, sensor stand etc.Meanwhile, due to the high-temperature behavior that it is good, be also used as alloy casting core pipe, thermal barrier coating, engine chamber etc.
At present, the preparation method of gradient porous ceramics mainly contains pore former gradient array method, organic precursor pickling process and precipitation method of formation etc.1) advantage of pore former gradient array method is that technique is simple, easy to operate, and equipment is simple, and shortcoming is the out-of-shape in hole and the consecutive variations in aperture is poor.The method is applicable to the preparation of simple shape goods in addition, and is difficult to the goods for preparing complicated shape.2) advantage of organic precursor pickling process is that technique is simple, easy to operate, and without the need to complex apparatus, the pore size of goods and change are determined by selecting organic precursor.But the shortcoming of the method is that the performance of goods is comparatively large by the impact of organic precursor, and the polyurethane foam of especially China's production is in elasticity and tensile strength, and all more abroad there is a big difference.In addition, the preparation of slurry and the adjustment of performance thereof are also a more difficult job, have impact on the raising of the drilling plan performance that precursor process is produced to a certain extent.3) technology key precipitating method of formation is: should ensure ceramic particle and voiding-agent particle sedimentation simultaneously, make pore former be distributed in settled layer equably again.The advantage of this method is that the performance of green compact is more stable, and the shape in hole is more regular, and shortcoming is that technological process and equipment are complicated, and this method needs further research.
Summary of the invention
Goal of the invention: the object of the present invention is to provide a kind of simple to operate and be easy to the preparation method of a kind of gradient porous silicon nitride ceramics of technology controlling and process.Preparation method of the present invention prepares on the basis of porous ceramics original, and the structure based on biological material (rice husk, stalk etc.) there are differences, and prepares the porous ceramics of a kind of different pore structures distribution.
Technical scheme: the preparation method that the invention provides a kind of gradient porous silicon nitride ceramics, concrete, comprise the following steps:
Step 1) by after biomass pre-treatment, carry out carbonization, grinding, obtain the siliceous presoma of carbon, then it mixed with silicon nitride, additive, grinding granulation, obtains the mixture that carbon containing is siliceous;
Step 2) mixture siliceous for two or more the carbon containing obtained in step 1 is loaded in mould successively, each layer loads successively; Bounce after filling; Compression molding under 3 ~ 20MPa, obtains base substrate;
Step 3) base substrate is sintered under nitrogen atmosphere and normal pressure, after cooling, obtain gradient porous silicon nitride ceramics.
In above-mentioned preparation method, described biomass are cotton stalk, rice husk, corn stalk, rice straw or straw.Described pre-treatment is: adopt volume fraction be 10% hydrochloric acid soln be dipped to and soak into completely, then boil and boil 1h, finally with distilled water cleaning, dry.
Described carbonization is carbonization at 540 DEG C, time 40 ~ 150min.C and SiO in the siliceous presoma of described carbon obtained after carbonization
2weight ratio be 0.5 ~ 1.5, preferably 0.7 ~ 1.3.
The mass ratio of the siliceous presoma of described carbon and silicon nitride, additive is (46 ~ 86): (5 ~ 45): (9 ~ 15), preferably (49 ~ 61): (30 ~ 40): (9 ~ 11).
Described additive elects Fe as
2o
3, NaF, Y
2o
3, Al
2o
3, MgO, CeO
2, Yb
2o
3, SiO
2, La
2o
3, Lu
2o
3, Sm
2o
3, Nd
2o
3, Eu
2o
3in one or more.
Described is mixed into ball milling mixing, and grinding medium is dehydrated alcohol; To mix and after drying, then carry out grinding granulation.
Described grinding granulation, with polyvinyl alcohol solution (PVA) for binding agent, the concentration of described polyvinyl alcohol solution is 5% (weight ratio), crosses 120 sieves, obtain the mixture that carbon containing is siliceous after grinding granulation.The described siliceous mixture of two or more carbon containing, the quality fillings such as the amount in loading mould is preferred.Namely 1:1 or 1:1:1 by that analogy.
Bounce after filling in the present invention, very important, during filling Multi-layer material, can utilize bounce that each layered material is interpenetrated, not easy fracture layering during sintering.
Described is sintered to: the graphite tank putting into painting boron nitride after being dried by base substrate, and graphite tank is placed in High Temperature Furnaces Heating Apparatus, then sinters under nitrogen atmosphere and normal pressure.
Beneficial effect:
(1) the present invention develops the open pore structure that interpenetrates that every layer all has graded, and forms the gradient porous silicon nitride ceramics of transition gradient layer between adjacent two layers.
(2) the present invention is raw materials used is mainly agricultural wastes waste material, low production cost.
(3) the present invention is by one-step moulding carbothermic reduction-normal pressure-sintered method, and technique is simple, and method with low cost prepares gradient porous silicon nitride ceramics.
Embodiment:
Referring to specific embodiment, the present invention is described.It will be appreciated by those skilled in the art that these embodiments are only for illustration of the present invention, its scope do not limited the present invention in any way.
Raw material used in following embodiment, reagent material etc., if no special instructions, be commercially available purchase product.
Embodiment 1
Prepared by raw material: rice husk adopt volume fraction be 10% hydrochloric acid soln be dipped to that soaking into boils completely again boils 1h, finally clean 5 times with distilled water, to load in saggar carbonization 80min at 540 DEG C after drying and become C/SiO
2be 0.7, grinding 10h, the siliceous precursor A of carbon that median is less than 2.0 μm; The siliceous precursor B of carbon is obtained, its C/SiO as stated above with rice husk carbonizing 70min
2be 0.9;
Batch mixing: raw material A (comprising the siliceous precursor A of 49% carbon, 40% α-siliconnitride powder, 6% aluminum oxide and 5% magnesium oxide) is placed in ball grinder, adding weight is that the ethanol of above-mentioned raw materials gross weight 1.5 times carries out ball milling mixing, 5% (weight ratio) polyvinyl alcohol solution is added after oven dry, grinding granulation, cross 120 mesh sieves, obtain mixing blank A; Mixing blank B is obtained by identical proportioning by the siliceous precursor B of carbon;
Shaping: to weigh blank A and B mass ratio 1:1, load successively, bounce on plain bumper; Again by compound compression molding under 5MPa, obtain base substrate;
Burn till: the plumbago crucible putting into painting boron nitride after being dried by base substrate, and plumbago crucible is placed in High Temperature Furnaces Heating Apparatus, 800 DEG C are warming up to 10 DEG C/min, then under nitrogen atmosphere and normal pressure with the intensification of 8 DEG C/min, respectively at 1400 DEG C of insulation 2h, 1550 DEG C of insulation 2h, obtain gradient porous silicon nitride ceramics.
Performance test: adopting three-point bending method to record its bending strength is 92.20MPa, and the void content adopting Archimedes's drainage to record the silicon nitride ceramics with gradient porous structure is 40.86%, and pore diameter range is 0.03 ~ 5 μm.
Embodiment 2
Prepared by raw material: rice husk adopt volume fraction be 10% hydrochloric acid soln be dipped to that soaking into boils completely again boils 1h, finally clean 5 times with distilled water, to load in saggar carbonization 50min at 540 DEG C after drying and become C/SiO
2be 1.2, grinding 10h, the siliceous precursor A of carbon that median is less than 2.0 μm; The siliceous precursor B of carbon is obtained, its C/SiO as stated above with rice husk carbonizing 40min
2be 1.5;
Batch mixing: raw material A (comprising the siliceous precursor A of 86% carbon, 5% α-siliconnitride powder, 5% Sodium Fluoride, 2% aluminum oxide and 2% magnesium oxide) is placed in ball grinder, adding weight is that the ethanol of above-mentioned raw materials gross weight 1.5 times carries out ball milling mixing, 5% (weight ratio) polyvinyl alcohol solution is added after oven dry, grinding granulation, cross 120 mesh sieves, obtain mixing blank A; Mixing blank B is obtained by identical proportioning by the siliceous precursor B of carbon;
Shaping: to weigh blank A and B mass ratio 2:1, load successively, bounce on plain bumper; Again by compound compression molding under 20MPa, obtain base substrate;
Burn till: the plumbago crucible putting into painting boron nitride after being dried by base substrate, and plumbago crucible is placed in High Temperature Furnaces Heating Apparatus, 800 DEG C are warming up to 10 DEG C/min, then under nitrogen atmosphere and normal pressure with the intensification of 8 DEG C/min, respectively at 1400 DEG C of insulation 2h, 1550 DEG C of insulation 2h, obtain gradient porous silicon nitride ceramics.
Performance test: adopting three-point bending method to record its bending strength is 91.30MPa, and the void content adopting Archimedes's drainage to record the silicon nitride ceramics with gradient porous structure is 41.92%, and pore diameter range is 0.05 ~ 8 μm.
Embodiment 3
Prepared by raw material: cotton stalk adopt volume fraction be 10% hydrochloric acid soln be dipped to that soaking into boils completely again boils 1h, finally clean 5 times with distilled water, to load in saggar carbonization 150min at 540 DEG C after drying and become C/SiO
2be 0.5, grinding 10h, the siliceous precursor A of carbon that median is less than 2.0 μm; The siliceous precursor B of carbon is obtained, its C/SiO as stated above with rice husk carbonizing 90min
2be 0.5;
Batch mixing: raw material A (comprising the siliceous precursor A of 46% carbon, 45% α-siliconnitride powder, 5% Sodium Fluoride, 2% aluminum oxide and 2% magnesium oxide) is placed in ball grinder, adding weight is that the ethanol of above-mentioned raw materials gross weight 1.5 times carries out ball milling mixing, 5% (weight ratio) polyvinyl alcohol solution is added after oven dry, grinding granulation, cross 120 mesh sieves, obtain mixing blank A; Mixing blank B is obtained by identical proportioning by the siliceous precursor B of carbon;
Shaping: to weigh blank A and B mass ratio 1:2, load successively, bounce on plain bumper; Again by compound compression molding under 3MPa, obtain base substrate;
Burn till: the plumbago crucible putting into painting boron nitride after being dried by base substrate, and plumbago crucible is placed in High Temperature Furnaces Heating Apparatus, 800 DEG C are warming up to 10 DEG C/min, then under nitrogen atmosphere and normal pressure with the intensification of 8 DEG C/min, respectively at 1400 DEG C of insulation 2h, 1550 DEG C of insulation 2h, obtain gradient porous silicon nitride ceramics.
Performance test: adopting three-point bending method to record its bending strength is 88.81MPa, and the void content adopting Archimedes's drainage to record the silicon nitride ceramics with gradient porous structure is 41.51%, pore diameter range 0.02 ~ 10 μm.
Embodiment 4
Prepared by raw material: rice husk adopt volume fraction be 10% hydrochloric acid soln be dipped to that soaking into boils completely again boils 1h, finally clean 5 times with distilled water, to load in saggar carbonization at 540 DEG C after drying and become C/SiO
2be 1.3, grinding 10h, the siliceous precursor A of carbon that median is less than 2.0 μm; Change carbonization time by rice straw as stated above and obtain the siliceous precursor B of carbon, its C/SiO
2be 1.3;
Batch mixing: raw material A (comprising the siliceous precursor A of 49% carbon, 40% α-siliconnitride powder, 6% aluminum oxide and 5% magnesium oxide) is placed in ball grinder, adding weight is that the ethanol of above-mentioned raw materials gross weight 1.5 times carries out ball milling mixing, 5% (weight ratio) polyvinyl alcohol solution is added after oven dry, grinding granulation, cross 120 mesh sieves, obtain mixing blank A; Blank B is obtained by different proportionings (the siliceous precursor A of 51% carbon, 40% α-siliconnitride powder, 5% Sodium Fluoride, 2% aluminum oxide and 2% magnesium oxide) by the siliceous precursor B of carbon;
Shaping: the blank A of weighing and B mass ratio 1:1, first blank A is inserted mould, then fill out blank B, bounce on plain bumper; Again by compound compression molding under 10MPa, obtain base substrate;
Burn till: the plumbago crucible putting into painting boron nitride after being dried by base substrate, and plumbago crucible is placed in High Temperature Furnaces Heating Apparatus, 800 DEG C are warming up to 10 DEG C/min, then under nitrogen atmosphere and normal pressure with the intensification of 8 DEG C/min, respectively at 1400 DEG C of insulation 2h, 1550 DEG C of insulation 2h, obtain gradient porous silicon nitride ceramics.
Performance test: adopting three-point bending method to record its bending strength is 90.38MPa, and the void content adopting Archimedes's drainage to record the silicon nitride ceramics with gradient porous structure is 43.36%, and pore diameter range is 0.05 ~ 20 μm.
Embodiment 5
Prepared by raw material: rice husk adopt volume fraction be 10% hydrochloric acid soln be dipped to that soaking into boils completely again boils 1h, finally clean 5 times with distilled water, load carbonization at 540 DEG C in saggar after drying, grinding 10h, makes C/SiO
2be 1.0, the median siliceous precursor A of carbon that is less than 2.0 μm; Change carbonization time rice straw as stated above by the siliceous precursor B of carbon and obtain the siliceous precursor B of carbon, its C/SiO
2be 1.0; Change carbonization time straw as stated above with carbon siliceous presoma C and obtain the siliceous presoma C of carbon, its C/SiO
2be 1.0;
Batch mixing: raw material A (comprising the siliceous precursor A of 49% carbon, 40% α-siliconnitride powder, 5% Sodium Fluoride, 2% aluminum oxide and 2% magnesium oxide) is placed in ball grinder, adding weight is that the ethanol of above-mentioned raw materials gross weight 1.5 times carries out ball milling mixing, 5% (weight ratio) polyvinyl alcohol solution is added after oven dry, grinding granulation, cross 120 mesh sieves, obtain mixing blank A; Mixing blank B is obtained by identical proportioning by the siliceous precursor B of carbon; Mixing blank C is obtained by identical proportioning with carbon siliceous presoma C;
Shaping: blank A, B, C mass ratio 1:1:1 of weighing, load successively, bounce on plain bumper; Again by compound compression molding under 15MPa, obtain base substrate;
Burn till: the plumbago crucible putting into painting boron nitride after being dried by base substrate, and plumbago crucible is placed in High Temperature Furnaces Heating Apparatus, 800 DEG C are warming up to 10 DEG C/min, then under nitrogen atmosphere and normal pressure with the intensification of 8 DEG C/min, respectively at 1400 DEG C of insulation 2h, 1550 DEG C of insulation 2h, obtain gradient porous silicon nitride ceramics.
Performance test: adopting three-point bending method to record its bending strength is 89.30MPa, and the void content adopting Archimedes's drainage to record the silicon nitride ceramics with gradient porous structure is 45.92%, and pore diameter range is 0.1 ~ 25 μm.
Embodiment 6
Prepared by raw material: rice husk adopt volume fraction be 10% hydrochloric acid soln be dipped to that soaking into boils completely again boils 1h, finally clean 5 times with distilled water, load carbonization at 540 DEG C in saggar after drying, grinding 10h, makes C/SiO
2be 0.7, the median siliceous precursor A of carbon that is less than 2.0 μm; Change carbonization time as stated above by the siliceous precursor B of carbon and obtain the siliceous precursor B of carbon, its C/SiO
2be 1.0; Change carbonization time as stated above with carbon siliceous presoma C and obtain the siliceous presoma C of carbon, its C/SiO
2be 1.3;
Batch mixing: by raw material A (comprising the siliceous precursor A of 61% carbon, 30% α-siliconnitride powder, 5% Sodium Fluoride, 2% aluminum oxide and 2% magnesium oxide)) be placed in ball grinder, adding weight is that the ethanol of above-mentioned raw materials gross weight 1.5 times carries out ball milling mixing, 5% (weight ratio) polyvinyl alcohol solution is added after oven dry, grinding granulation, cross 120 mesh sieves, obtain mixing blank A; Mixing blank B is obtained by identical proportioning by the siliceous precursor B of carbon; Mixing blank C is obtained by identical proportioning with carbon siliceous presoma C;
Shaping: blank A, B, C mass ratio 1:1:1 of weighing, load successively, bounce on plain bumper; Again by compound compression molding under 5MPa, obtain base substrate;
Burn till: the plumbago crucible putting into painting boron nitride after being dried by base substrate, and plumbago crucible is placed in High Temperature Furnaces Heating Apparatus, 800 DEG C are warming up to 10 DEG C/min, then under nitrogen atmosphere and normal pressure with the intensification of 8 DEG C/min, respectively at 1400 DEG C of insulation 2h, 1550 DEG C of insulation 2h, obtain gradient porous silicon nitride ceramics.
Performance test: adopting three-point bending method to record its bending strength is 80.64MPa, and the void content adopting Archimedes's drainage to record the silicon nitride ceramics with gradient porous structure is 39.19%, and pore diameter range is 0.02 ~ 10 μm.
Claims (10)
1. a preparation method for gradient porous silicon nitride ceramics, is characterized in that comprising the following steps:
Step 1) by after biomass pre-treatment, carry out carbonization, grinding, obtain the siliceous presoma of carbon, then it mixed with silicon nitride, additive, grinding granulation, obtains the mixture that carbon containing is siliceous;
Step 2) mixture siliceous for two or more the carbon containing obtained in step 1 is loaded in mould successively, each layer loads successively; Bounce after filling; Compression molding under 3 ~ 20MPa, obtains base substrate;
Step 3) base substrate is sintered under nitrogen atmosphere and normal pressure, after cooling, obtain gradient porous silicon nitride ceramics.
2. preparation method as claimed in claim 1, is characterized in that described biomass are cotton stalk, rice husk, corn stalk, rice straw or straw.
3. preparation method as claimed in claim 1, is characterized in that described pre-treatment is: adopt volume fraction be 10% hydrochloric acid soln be dipped to and soak into completely, then boil and boil 1h, finally with distilled water cleaning, dry.
4. preparation method as claimed in claim 1, is characterized in that described carbonization is carbonization at 540 DEG C, time 40 ~ 150min.
5. preparation method as claimed in claim 1, is characterized in that C and SiO in the siliceous presoma of described carbon
2weight ratio be 0.5 ~ 1.5.
6. preparation method as claimed in claim 1, is characterized in that the siliceous presoma of described carbon is (46 ~ 86) with the mass ratio of silicon nitride, additive: (5 ~ 45): (9 ~ 15).
7. preparation method as claimed in claim 1, is characterized in that described additive elects Fe as
2o
3, NaF, Y
2o
3, Al
2o
3, MgO, CeO
2, Yb
2o
3, SiO
2, La
2o
3, Lu
2o
3, Sm
2o
3, Nd
2o
3, Eu
2o
3in one or more.
8. preparation method as claimed in claim 1, it is characterized in that the described ball milling that is mixed into mixes, grinding medium is dehydrated alcohol; To mix and after drying, then carry out grinding granulation.
9. preparation method as claimed in claim 1, it is characterized in that described grinding granulation, take polyvinyl alcohol solution as binding agent, and the concentration of described polyvinyl alcohol solution is 5% (weight ratio), cross 120 sieves after grinding granulation, obtain the mixture that carbon containing is siliceous.
10. preparation method as claimed in claim 1, is characterized in that described being sintered to: the graphite tank putting into painting boron nitride after being dried by base substrate, and graphite tank is placed in High Temperature Furnaces Heating Apparatus, then sinters under nitrogen atmosphere and normal pressure.
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| CN105777187A (en) * | 2016-03-24 | 2016-07-20 | 西安建筑科技大学 | Magnesium light-weight refractory material and preparation method thereof |
| CN105859301A (en) * | 2016-04-05 | 2016-08-17 | 盐城工学院 | Silicon nitride ceramic and preparation method thereof |
| CN108002843A (en) * | 2017-11-17 | 2018-05-08 | 华中科技大学 | A kind of preparation method of the high-precision porous silicon nitride complicated shape part based on lotion |
| CN109095931A (en) * | 2018-09-22 | 2018-12-28 | 新疆大学科学技术学院 | A method of it is prepared using rice straw from isolated superfine silicon nitride fiber |
| CN109465951A (en) * | 2018-11-26 | 2019-03-15 | 华中科技大学 | A kind of graded ceramics forming device |
| CN111943716A (en) * | 2020-08-20 | 2020-11-17 | 安徽工业大学 | Preparation method of novel red mud-fly ash based gradient structure porous ceramic |
| CN113398686A (en) * | 2021-07-29 | 2021-09-17 | 瑞燃(上海)环境工程技术有限公司 | Electronic component and electronic special material production waste gas filtering and adsorbing material |
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| CN105777187A (en) * | 2016-03-24 | 2016-07-20 | 西安建筑科技大学 | Magnesium light-weight refractory material and preparation method thereof |
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| CN109465951A (en) * | 2018-11-26 | 2019-03-15 | 华中科技大学 | A kind of graded ceramics forming device |
| CN109465951B (en) * | 2018-11-26 | 2020-05-19 | 华中科技大学 | Gradient ceramic forming device |
| CN111943716A (en) * | 2020-08-20 | 2020-11-17 | 安徽工业大学 | Preparation method of novel red mud-fly ash based gradient structure porous ceramic |
| CN113398686A (en) * | 2021-07-29 | 2021-09-17 | 瑞燃(上海)环境工程技术有限公司 | Electronic component and electronic special material production waste gas filtering and adsorbing material |
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