CN102746013A - Light high-strength silicon nitride bonded silicon carbide refractory and preparation method thereof - Google Patents
Light high-strength silicon nitride bonded silicon carbide refractory and preparation method thereof Download PDFInfo
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- CN102746013A CN102746013A CN2012102878280A CN201210287828A CN102746013A CN 102746013 A CN102746013 A CN 102746013A CN 2012102878280 A CN2012102878280 A CN 2012102878280A CN 201210287828 A CN201210287828 A CN 201210287828A CN 102746013 A CN102746013 A CN 102746013A
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- silicon carbide
- silicon nitride
- silit
- carbide refractory
- particle diameter
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 43
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 31
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical group N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 20
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 239000011230 binding agent Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 11
- 238000005469 granulation Methods 0.000 claims abstract description 7
- 230000003179 granulation Effects 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 239000011819 refractory material Substances 0.000 claims description 31
- 238000010792 warming Methods 0.000 claims description 14
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 10
- 235000013312 flour Nutrition 0.000 claims description 8
- 238000005452 bending Methods 0.000 abstract description 9
- 239000000843 powder Substances 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 abstract 2
- 229920002451 polyvinyl alcohol Polymers 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000009413 insulation Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000000465 moulding Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910006360 Si—O—N Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
Abstract
The invention discloses a light high-strength silicon nitride bonded silicon carbide refractory and a preparation method thereof. The refractory is mainly made of silicon carbide and silica powder, and the weight ratio of the silicon carbide and the silica powder is (65-85): (15-30), wherein the particle size D50 of the silicon carbide is 0.1-150 microns and the particle size D50 of the silica powder is 0.1-1 micron. The preparation method includes subjecting all the raw materials to ball milling for 8-12 hours after mixing, and drying the materials after the ball milling, adding polyvinyl alcohol (PVA) which accounts for 8-12% of the raw materials by weight for granulation, subjecting the mixture to a sieve with 40-80 meshes, standing at a room temperature for more than 24 hours, performing dry pressing with 40-80MPa of the pressing pressure, binder removing, and nitridation sintering. The silicon nitride bonded silicon carbide refractory prepared through the formula and the method has the advantages of being low in production cost, easy to achieve industrial production, low in volume density and high in bending strength of products, and capable of reducing the production energy consumption and improving the utilization rate of equipment.
Description
Technical field
The present invention relates to technical field of refractory materials, be specifically related to a kind of silicon nitride combined with silicon carbide refractory material and preparation method thereof.
Background technology
Existing silicon nitride combined with silicon carbide refractory material has that stable chemical performance, normal temperature bending strength are high, thermal conductivity reaches premium propertiess such as thermal expansivity is little greatly.The silicon nitride combined with silicon carbide refractory material high-temperature bending strength can be higher than normal temperature bending strength, therefore often is applied to kiln, metallurgy and steel industry etc.The sintering method of silicon nitride combined silicon carbide material has a lot, if any normal pressure-sintered, HIP sintering, gas pressure sintering, hot pressed sintering and reaction sintering etc.Utilize reaction sintering to prepare silicon nitride combined with silicon carbide refractory material and obtain using very widely, this is because reaction sintering has a lot of advantages with respect to other method, and is lower such as production cost, is more suitable for large-scale production etc.; Reaction sintering forms the variation that does not almost have shape and size in the silicon nitride combined silicon carbide material process; Help preparing the ceramic component of complicated shape; But the mechanical property of reaction sintering silicon nitride carborundum refractory material is relatively poor; Especially bending strength is very low, and this has just limited its application in a lot of fields.
In industrial production, for the silicon nitride combined with silicon carbide refractory material of reaction sintering preparation, can improve the volume density of material than high-flexural strength as far as possible, the volume density of material is generally at 2.65g/cm
3More than, and bending strength also only has only 40-50MPa, calculates and finds that specific tenacity only reaches 1.89 * 10
4Nm/kg.Shortcomings such as the specific tenacity of refractory materials lower (volume density high) can cause the material thermal capacitance higher and cause the energy consumption aggravation, and the supporting power of equipment is big, the life-span that also can reduce material.
Summary of the invention
The objective of the invention is to overcome above-mentioned weak point a kind of high-strength light silicon nitride combined with silicon carbide refractory material is provided.
Another object of the present invention provides the preparation method of above-mentioned silicon nitride combined with silicon carbide refractory material.
The present invention seeks to realize in the following manner:
A kind of high-strength light silicon nitride combined with silicon carbide refractory material, this material are that raw material is processed with silit and silica flour mainly, and the weight ratio of silit and silica flour is 65~85:15~30; Wherein, silit particle diameter D
50=0.1 μ m~150 μ m, silica flour particle diameter D
50=0.1 μ m~1 μ m.
This material feedstock also can contain aluminum oxide, and the consumption of aluminum oxide is not more than 10% of raw material gross weight, and the consumption of preferred aluminum oxide is 4~10% of a raw material gross weight, aluminum oxide particle diameter 0.1 μ m≤D
50<1 μ m.
In the said silit, particle diameter is D
50The silit of=0.1 μ m~1 μ m and particle diameter are 1 μ m<D
50The silit weight ratio of≤150 μ m is 40 ~ 60:40 ~ 60.
Most preferably in the silit, particle diameter is D
50The silit of=0.1 μ m~1 μ m, particle diameter are 1 μ m<D
50The silit of≤80 μ m and particle diameter are 80 μ m<D
50The weight ratio of the silit of≤150 μ m is 35 ~ 50:15 ~ 30:5 ~ 25.
Silit and silica flour preferably account for more than 85% of raw material gross weight.
The preparation method of above-mentioned high-strength light silicon nitride combined with silicon carbide refractory material may further comprise the steps:
With carrying out ball milling after whole raw materials mix, the ball milling time is 8~12 hours, dries behind the ball milling, adds raw material and weighs 8~12% PVA (Z 150PH) granulation; Cross 40~80 mesh sieves, room temperature was placed more than 24 hours, and is dry-pressing formed; Forming pressure is 40~80MPa, and binder removal is nitridation sintered.Described bake out temperature is preferably 60~80 ℃.The condition that ball milling adopts can be absolute ethyl alcohol: Si
3N
4Ball: raw material=1~2:1~2:1~2.
Described binder removal condition is: the binder removal time is 2 hours under 300~500 ℃ of conditions, and heat-up rate is 1 ~ 3 ℃/min.
Described sintering condition is to be incubated 1~3h under 1300~1350 ℃ of conditions; Under 1400~1450 ℃ of conditions, be incubated 1 ~ 3h again.Sintering intensification condition is for earlier being warming up to 1000 ℃ with the speed of 10 ~ 40 ℃/min, be warming up to 1300-1350 ℃ of insulation 1~3h with the speed of 1 ~ 5 ℃/min again after, the speed with 1 ~ 5 ℃/min is warming up to 1400~1450 ℃ of insulation 1~3h at last.
The strip volume density scope 1.9 ~ 2.2g/cm that burns till
3
The present invention is the requirement of satisfying high-strength light, and the SiC that utilizes specified particle diameter through control particulate grating, can not only increase intergranular effective connection in the material as aggregate, improves the bending strength of material, can also reduce the volume density of material.Al
2O
3Also can be used as sintering aid, when nitridation sintered and the SiO of Si surface oxidation
2Form the Y-Al-Si-O-N liquid phase, can better promote the densification of material, promote the carrying out of reaction sintering, reduce the temperature of reaction sintering, improve the bending strength of refractory materials.Raw material used in the present invention is technical grade and gets final product, all commercially available getting.
In addition, the control forming pressure can further be regulated the volume density of sintered specimen in the inventive method, thereby improves the performance of material; Select rational sintering temperature and soaking time, help to obtain best reaction sintering product, thereby improve the performance of material.
With prior art beneficial effect more of the present invention: the silicon nitride combined with silicon carbide refractory material that the present invention prepares can be realized low volume density and high-intensity requirement; Thereby improve the specific tenacity of silicon nitride combined with silicon carbide refractory material; Improve the rate of utilization of silicon nitride combined with silicon carbide refractory material, in industrial application, can reduce the thermal capacitance of refractory materials, the life-span that the raising refractory materials uses; This method adopts reaction sintering under low-temperature atmosphere-pressure, and step is simple, cost is low, is suitable for producing in batches, can make large size, complex-shaped parts, and product at high temperature can keep high-flexural strength.
Embodiment
Below through embodiment the present invention is done further elaboration, should not be construed as qualification to the total technical scheme of the present invention.Embodiment 1-10 prescription is seen table 1.
The preparation method of embodiment 1,2,4,5,8,9,10:
With carrying out ball milling after whole raw materials mix, be ball-milling medium with the absolute ethyl alcohol, in planetary mills, use Si
3N
4Ball ball milling 24h (mass ratio of raw material, ball and absolute ethyl alcohol is 1:1.5:1), the ball milling time is 10 hours, the slurry behind the ball milling is dried under 60 ℃ of conditions; Add raw material and weigh 10% PVA granulation, cross 40 mesh sieves, room temperature was placed 24 hours; Get powder after an amount of granulation in mould, dry-pressing formed, forming pressure is 40~45MPa; The long 80mm of strip after the moulding, wide 7.5mm, high about 5.7mm, binder removal, behind the binder removal in the high-temperature vacuum atmosphere sintering furnace at mobile high pure nitrogen (Chun Du>99.99%) (nitrogen flow rate: the nitridation sintered high-strength light silicon nitride combined with silicon carbide refractory material that makes under 1~3L/min) condition.The binder removal condition: the speed with 1 ~ 3 ℃/min is warming up to 400 ℃, at 400 ℃ of insulation 2h.The high temperature sintering condition: the speed with 20 ℃/min is warming up to 1000 ℃ earlier, and the speed with 5 ℃/min is warming up to 1300 ℃ again, and at 1300 ℃ of insulation 2h, the speed with 5 ℃/min is warming up to 1400 ℃ at last, sintered heat insulating 2h under 1400 ℃ of conditions of temperature.Burn till the back strip and do not have dimensional change basically.
The preparation method of embodiment 3,6,7:
With carrying out ball milling after whole raw materials mix, be ball-milling medium with the absolute ethyl alcohol, in planetary mills, use Si
3N
4Ball ball milling 24h (mass ratio of raw material, ball and absolute ethyl alcohol is 1:1.5:1.5), the ball milling time is 8 hours, the slurry behind the ball milling is dried under 80 ℃ of conditions; Add raw material and weigh 12% PVA granulation, cross 60 mesh sieves, room temperature was placed 24 hours; Get powder after an amount of granulation in mould, dry-pressing formed, forming pressure is 50~55MPa; The long 80mm of strip after the moulding, wide 7.5mm, high about 5.5mm, binder removal, behind the binder removal in the high-temperature vacuum atmosphere sintering furnace at mobile high pure nitrogen (Chun Du>99.99%) (nitrogen flow rate: the nitridation sintered high-strength light silicon nitride combined with silicon carbide refractory material that makes under 1~3L/min) condition.The binder removal condition: the speed with 1 ~ 3 ℃/min is warming up to 500 ℃, at 500 ℃ of insulation 2h.The high temperature sintering condition: the speed with 20 ℃/min is warming up to 1000 ℃ earlier, and the speed with 5 ℃/min is warming up to 1350 ℃ again, and at 1350 ℃ of insulation 2h, the speed with 5 ℃/min is warming up to 1450 ℃ at last, sintered heat insulating 2h under 1450 ℃ of conditions of temperature.Burn till the back strip and do not have dimensional change basically.
To carry out character according to the material that the embodiment method prepares and detect, and utilize three-point bending method test strip bending strength, concrete experimental result is seen table 1.
The material property that table 1 embodiment 1~10 prepares is table as a result
Wherein, the SiC that mentions among the embodiment 1,2,4,5,8,9,10
1(D
50=0.7 μ m, Chun Du>98%) SiC,
2(D
50=65 μ m, Chun Du>99%) SiC,
3(D
50=120 μ m, Chun Du>99%) SiC,
4(D
50=150 μ m, Chun Du>99%) Si powder (0.1 μ m≤D,
50<1 μ m, Chun Du>99%) technical grade Al,
2O
3(0.1 μ m≤D
50<1 μ m).
The SiC that mentions among the embodiment 3,6,7
1(D
50=0.3 μ m, Chun Du>98%) SiC,
2(D
50=80 μ m, Chun Du>99%) SiC,
3(D
50=100 μ m, Chun Du>99%) SiC,
4(D
50=150 μ m, Chun Du>99%) Si powder (0.1 μ m≤D,
50<1 μ m, Chun Du>99%) technical grade Al,
2O
3(0.1 μ m≤D
50<1 μ m).
Claims (10)
1. a high-strength light silicon nitride combined with silicon carbide refractory material is characterized in that this material is that raw material is processed with silit and silica flour mainly, and the weight ratio of silit and silica flour is 65~85:15~30; Wherein, silit particle diameter D
50=0.1 μ m~150 μ m, silica flour particle diameter D
50=0.1 μ m~1 μ m.
2. high-strength light silicon nitride combined with silicon carbide refractory material according to claim 1 is characterized in that this material feedstock also contains aluminum oxide, and the consumption of aluminum oxide is not more than 10% of raw material gross weight, aluminum oxide particle diameter 0.1 μ m≤D
50<1 μ m.
3. high-strength light silicon nitride combined with silicon carbide refractory material according to claim 2 is characterized in that this material feedstock also contains aluminum oxide, and the consumption of aluminum oxide is 4~10% of a raw material gross weight, aluminum oxide particle diameter 0.1 μ m≤D
50<1 μ m.
4. high-strength light silicon nitride combined with silicon carbide refractory material according to claim 1 is characterized in that in the said silit that particle diameter is D
50The silit of=0.1 μ m~1 μ m and particle diameter are 1 μ m<D
50The silit weight ratio of≤150 μ m is 40 ~ 60:40 ~ 60.
5. high-strength light silicon nitride combined with silicon carbide refractory material according to claim 1 is characterized in that in the said silit that particle diameter is D
50The silit of=0.1 μ m~1 μ m, particle diameter are 1 μ m<D
50The silit of≤80 μ m and particle diameter are 80 μ m<D
50The weight ratio of the silit of≤150 μ m is 35 ~ 50:15 ~ 30:5 ~ 25.
6. high-strength light silicon nitride combined with silicon carbide refractory material according to claim 1 is characterized in that silit and silica flour account for more than 85% of raw material gross weight.
7. the preparation method of the described high-strength light silicon nitride combined with silicon carbide refractory material of claim 1 is characterized in that this method may further comprise the steps:
With carrying out ball milling after whole raw materials mix, the ball milling time is 8~12 hours, dries behind the ball milling, adds 8~12% heavy PVA granulation of raw material, crosses 40~80 mesh sieves, and room temperature was placed more than 24 hours, and dry-pressing formed, forming pressure is 40~80MPa, and binder removal is nitridation sintered.
8. the preparation method of high-strength light silicon nitride combined with silicon carbide refractory material according to claim 7, it is characterized in that the described binder removal condition of this method is: binder removal is 2 hours under 300~500 ℃ of conditions.
9. the preparation method of high-strength light silicon nitride combined with silicon carbide refractory material according to claim 7 is characterized in that the described sintering condition of this method is to be incubated 1~3h under 1300~1350 ℃ of conditions, is incubated 1~3h again under 1400~1450 ℃ of conditions.
10. the preparation method of high-strength light silicon nitride combined with silicon carbide refractory material according to claim 9; It is characterized in that described sintering intensification condition is warming up to 1000 ℃ for first speed with 10 ~ 40 ℃/min; Speed with 1 ~ 5 ℃/min is warming up to 1300~1350 ℃ again, and the speed with 1 ~ 5 ℃/min is warming up to 1400~1450 ℃ at last.
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Cited By (14)
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CN103553647A (en) * | 2013-10-08 | 2014-02-05 | 常州工程职业技术学院 | Method for preparation of silicon nitride bonded silicon carbide refractory material by using silicon cutting waste mortar |
CN104003733A (en) * | 2014-05-19 | 2014-08-27 | 上海大学 | Preparation method of silicon nitride-combined silicon carbide fireproof material |
CN104045358A (en) * | 2014-03-06 | 2014-09-17 | 新疆众和股份有限公司 | Composite refractory material and preparation method thereof |
CN104045357A (en) * | 2014-03-06 | 2014-09-17 | 新疆众和股份有限公司 | Low-cost composite refractory material and preparation method thereof |
CN107311634A (en) * | 2017-07-19 | 2017-11-03 | 宜兴市锦泰耐火材料有限公司 | A kind of nitride bonded sandwich setter plate and preparation method thereof |
CN107540392A (en) * | 2017-08-23 | 2018-01-05 | 中国人民解放军海军工程大学 | The vacuum vibration casting forming method of silicon nitride combined silicon carbide refractory |
CN107540383A (en) * | 2017-08-23 | 2018-01-05 | 中国人民解放军海军工程大学 | The preparation method of silicon nitride combined silicon carbide refractory with double dispersing characteristics |
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