CN109761611A - A kind of fiber reinforced micro porous silicon nitride compound carbonizing silica brick and preparation method thereof - Google Patents
A kind of fiber reinforced micro porous silicon nitride compound carbonizing silica brick and preparation method thereof Download PDFInfo
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- CN109761611A CN109761611A CN201910118469.8A CN201910118469A CN109761611A CN 109761611 A CN109761611 A CN 109761611A CN 201910118469 A CN201910118469 A CN 201910118469A CN 109761611 A CN109761611 A CN 109761611A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 239000011449 brick Substances 0.000 title claims abstract description 74
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 54
- 239000000835 fiber Substances 0.000 title claims abstract description 49
- 238000010000 carbonizing Methods 0.000 title claims abstract description 46
- -1 silicon nitride compound Chemical class 0.000 title claims abstract description 45
- 229910021426 porous silicon Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 78
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 67
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 67
- 239000010703 silicon Substances 0.000 claims abstract description 67
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 64
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 51
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000010304 firing Methods 0.000 claims abstract description 33
- 238000002156 mixing Methods 0.000 claims abstract description 33
- 229920005989 resin Polymers 0.000 claims abstract description 33
- 239000011347 resin Substances 0.000 claims abstract description 33
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000003825 pressing Methods 0.000 claims abstract description 3
- 239000011452 unfired brick Substances 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000000465 moulding Methods 0.000 claims description 10
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 7
- 229910003978 SiClx Inorganic materials 0.000 claims description 7
- 239000005011 phenolic resin Substances 0.000 claims description 7
- 229920001568 phenolic resin Polymers 0.000 claims description 7
- 229920001187 thermosetting polymer Polymers 0.000 claims description 7
- 206010020843 Hyperthermia Diseases 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 230000036031 hyperthermia Effects 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000005096 rolling process Methods 0.000 claims 1
- 239000002699 waste material Substances 0.000 abstract description 14
- 238000011065 in-situ storage Methods 0.000 abstract description 8
- 230000035939 shock Effects 0.000 abstract description 8
- 238000005245 sintering Methods 0.000 abstract description 8
- 239000007767 bonding agent Substances 0.000 abstract description 6
- 239000000919 ceramic Substances 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 5
- 238000005299 abrasion Methods 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract description 3
- 230000001458 anti-acid effect Effects 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 10
- 239000010813 municipal solid waste Substances 0.000 description 8
- 239000011148 porous material Substances 0.000 description 7
- 229920000433 Lyocell Polymers 0.000 description 6
- 230000002708 enhancing effect Effects 0.000 description 6
- 241001504664 Crossocheilus latius Species 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000010348 incorporation Methods 0.000 description 3
- 238000005121 nitriding Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 230000000750 progressive effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000003610 charcoal Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000004056 waste incineration Methods 0.000 description 2
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910021386 carbon form Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000010791 domestic waste Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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- Ceramic Products (AREA)
Abstract
The invention discloses a kind of fiber reinforced micro porous silicon nitride compound carbonizing silica bricks and preparation method thereof.The silicon carbide brick by silicon carbide, silicon nitride, metallic silicon, silicon ash, resin, by the premix of different-grain diameter powder and aggregate, mixing, pressing unfired brick, drying, firing and etc. be prepared.Utilize silicon carbide, silicon nitride, metallic silicon, silicon ash are primary raw material, using resin as bonding agent, it is prepared through high temperature sintering under air atmosphere, since plastic deformation mutually introduces, resin-bonded mode, so that novel silicon carbide brick has silicon carbide fibre-plastic deformation phase-Ceramic Composite integrated structure, in-situ carburization silica fibre is intersected with each other at network, greatly improves the intensity of material, anti-erosion and wear-resisting property；The product has the features such as low stomata, high intensity, high thermal shock resistance, high abrasion and antiacid alkali erosiveness can be excellent, has good application performance in key areas such as waste incinerator side walls.
Description
Technical field
The invention belongs to technical field of refractory materials.More particularly to a kind of fiber reinforced micro porous silicon nitride compound carbonizing silica brick
And preparation method thereof.
Background technique
The solid waste generated in mankind's daily life and industrial production, discharge rate is big, complicated component multiplicity, and has
Pollution, resource and social, cannot such as deal carefully with, just pollute the environment, and influence environmental sanitation, and waste of resource is destroyed
Production and living safety, destroys social harmony.Therefore, it is necessary to innoxious, recycling, minimizing and socialization processing.It uses at present
Incinerator, which is burnt away the refuse, has become the important component of circular economy, by waste resource and waste and scrap recycling and reusing, no
But it solves the problems, such as shortage of resources, while reducing garbage emission.
As a large amount of discharges of rubbish and the strict demand to environmental protection, waste incinerator have obtained pole in garbage disposal
To be widely applied.Tercod is commonly used in domestic waste incineration due to its good performance.This is answered
With being particularity based on this material and anti-erosion and the Thermal properties washed away.The rubbish burned with waste incinerator
Type becomes complicated, when rubbish is the heterogeneity mixture of different compositions, also has in terms of type, quantity and thermal content very big
Difference；And processing quantity of refuse is increasing, proposes requirements at the higher level to the physical and chemical properties adaptability of waste incineration inner lining of furnace.
Currently, the silicon carbide brick that waste incinerator uses is mostly that silicon carbide is cooperated alumina, in conjunction with clay, using paper pulp
For bonding agent, although silicon carbide itself has preferable performance, the silicon carbide brick being prepared using this combination
The porosity is high, and erosion-resisting characteristics and wear-resisting property are poor, partially short in waste incinerator side wall service life.For existing silicon carbide
Defect existing for brick is prepared for silicon nitride combined silicon carbide brick in the prior art, specially combines silicon carbide with metallic silicon,
Then the Nitride firing in nitriding furnace, metallic silicon in-situ preparation silicon nitride forms nitride combined with silicon carbide in turn in sintering process
Silica brick.Should during, in nitrogen furnace, metallic silicon is difficult nitridation sufficiently, and metallic silicon, which nitrogenizes, insufficient can cause products obtained therefrom
Volume stability is poor, will lead to products obtained therefrom firing when serious or occurs cracking phenomena in use, seriously affecting makes
Use effect.It has been greatly reduced the service life of waste incinerator to a certain extent.
Since (erosion of such as gas, rubbish are during high-temperature mobile to furnace body for the working environment of waste incinerator complexity
Internal abrasion and impact) it requires to optimize upgrading to former silicon carbide brick, more good refractory lining is provided, rubbish is met
Rubbish incinerator specific demand.
Summary of the invention
The present invention for the technical issues of be: the silicon carbide brick porosity prepared in the prior art is high, erosion-resisting characteristics and
Wear-resisting property is poor, partially short in waste incinerator side wall service life；The silicon nitride combined silicon carbide brick volume stability of preparation
Difference will lead to products obtained therefrom firing or occur cracking phenomena in use, seriously affects using effect when serious.One
Determine the service life that waste incinerator has been greatly reduced in degree.
In view of the above-mentioned problems, the present invention provides a kind of fiber reinforced micro porous silicon nitride compound carbonizing silica brick and its preparation sides
Method.Novel silicon nitride complex silicon carbide brick uses silicon carbide, silicon nitride, metallic silicon, silicon ash for primary raw material, is to combine with resin
Agent, novel silicon nitride complex silicon carbide brick have silicon carbide fibre-plastic deformation phase-Ceramic Composite integrated structure, ultralow stomata
Rate and stomata are microcellular structure, have the characteristics that high-intensitive, high thermal shock resistance, high abrasion and antiacid alkali erosiveness can be excellent,
It replaces common silicon carbide brick and common silicon nitride combined silicon carbide brick, solves due to common silicon carbide brick wear-resisting property
The disadvantages of difference, volume stability are poor, and anti-erosion is insufficient, improving properties, prolong the service life and reducing is produced into
This.
A kind of the present invention is achieved by the following technical solutions fiber reinforced micro porous silicon nitride compound carbonizing silica brick, by with
The raw material of lower weight percentage is prepared: silicon carbide 70%~85%, silicon nitride 3%~20%, metallic silicon 2%~8%,
Silicon ash 3%~6%；The additional resin for accounting for above-mentioned raw materials total weight 2%~6%.
The fiber reinforced micro porous silicon nitride compound carbonizing silica brick, content >=97% of SiC in the silicon carbide, carbonization
Bulk density > 3.2g/cm of silicon3。
The fiber reinforced micro porous silicon nitride compound carbonizing silica brick, the silicon carbide partial size Mass Distribution is as follows, and 1mm≤
The mass ratio of 0.074mm: the partial size < 0.005mm of partial size < 3mm:0.074mm≤partial size < 1mm: partial size < is 2~4:1~2:1
~4:0.5~1.
The fiber reinforced micro porous silicon nitride compound carbonizing silica brick, the partial size < 0.074mm of the silicon nitride, silicon nitride
In Si3N4Content > 90%.
The fiber reinforced micro porous silicon nitride compound carbonizing silica brick, the partial size < 0.074mm of the metallic silicon, the gold
Belong to Si content > 97% in silicon；
The fiber reinforced micro porous silicon nitride compound carbonizing silica brick, the partial size < 0.01mm of the silicon ash, in silicon ash
SiO2Content > 92%.
The fiber reinforced micro porous silicon nitride compound carbonizing silica brick, the resin are thermosetting phenolic resin；The tree
Rouge viscosity is 16000~19000cp (viscosity under the conditions of 25 DEG C)；The mass percentage of moisture is 2~3% in the resin,
Solid component mass percentage 77~83%, free phenol mass percentage 9.8~12%.
The preparation method of above-mentioned fiber reinforced micro porous silicon nitride compound carbonizing silica brick, comprising the following steps:
(1) mass ratio as requested prepares raw material；
(2) carborundum powder, the granularity < of the partial size < 0.074mm and partial size < 0.005mm that prepare step (1)
0.074mm silicon nitride powder, granularity < 0.074mm metallic silicon power and granularity < 0.01mm silicon ash are pre-mixed, and are uniformly mixed；
It (3) is 1mm≤partial size < 3mm by partial size and partial size is that 0.074mm≤partial size < 1mm carborundum aggregate is dry-mixed,
It is dry-mixed that uniformly resin is then added, carries out mixing, it is uniformly mixed；Then premix described in step (1) is added, continues to mix
Material is uniformly mixed to get pug is arrived；
(4) pug that step (3) obtains is suppressed into adobe, the bulk density for controlling adobe is 2.60g/cm3~
2.75g/cm3；
(5) adobe obtained by step (4) is dried, is burnt into, cooled to room temperature is after firing to get arriving the fibre
Dimension enhancing micropore silicon nitride compound carbonizing silica brick.
The preparation method of the fiber reinforced micro porous silicon nitride compound carbonizing silica brick, step (2) premixing is in ball milling
It is carried out in machine, the premixing time is 0.5~1h；Dry-mixed described in step (3) to carry out in edgd runner, the dry-mixed time is
3min~5min；The mixing time of mixing is carried out after resin is added as 5min~15min；The addition premix continues mixing
Time is 10min~25min；During step (4) described pressing unfired brick, moulding press tonnage used is 630T.
The preparation method of the fiber reinforced micro porous silicon nitride compound carbonizing silica brick, step (5) described drying are as follows: by step
(4) adobe obtained in dry kiln as being dried, and at 45 DEG C~90 DEG C, drying temperature controls the control of dry kiln inlet temperature
At 110 DEG C~180 DEG C, drying time is 20h~50h, the moisture < 0.5% after control is dry in adobe, kiln discharge.
The preparation method of the fiber reinforced micro porous silicon nitride compound carbonizing silica brick, step (5) described firing are as follows: will dry
Adobe afterwards in hyperthermia tunnel Kiln or shuttle kiln using being burnt into, and firing temperature is 1350 DEG C~1450 DEG C, in firing temperature
Lower heat preservation 10h~20h completes firing, cooled to room temperature kiln discharge after firing.
Fiber reinforced micro porous silicon nitride compound carbonizing silica brick prepared by the present invention is with silicon carbide, silicon nitride, metallic silicon, silicon ash
For raw material, using resin as bonding agent.Silicon nitride combined silicon carbide brick in compared with the existing technology, silicon nitride of the invention are straight
It connects and introduces oxidizing atmosphere firing, it is insufficient thoroughly to solve the problems, such as that silicon nitride nitrogenizes, while being burnt into cost and being also greatly lowered；
The silicon nitride, silicon carbide in air atmosphere sintering process can partial oxidation form the cenotypes such as silicon oxynitride, silica, have
Effect filling stomata, reduces the porosity, brick body stomata is promoted to become smaller or formed closed pore.In addition, silicon nitride of the present invention is compound
Silicon carbide brick, resin are bonding agent, and resin forms carbon residue in sintering process, forms reducing atmosphere, promotion division inside brick body
Divide metallic silicon that silicon carbide fibre is formed in situ, and then forms silicon carbide fibre-plastic deformation phase-Ceramic Composite integrated structure, it is former
Position silicon carbide fibre is crossed as network each other, fills stomata, the intensity of material is greatly improved, improves corrosion resistance
Energy and wear-resisting property.Resin-bonded makes product cause certain reducing atmosphere inside brick body in sintering process, and has
A small amount of charcoal is remaining, and reducing atmosphere and charcoal remnants can promote brick body interior metal silicon that SiC fiber is formed in situ, in addition silicon nitride, carbon
SiClx partial oxidation forms the cenotypes such as silicon oxynitride, silica and material is made to form microcellular structure, is effectively improved the anti-gas of material
Phase, anti-liquid phase corrode penetrating power, and then improve antistrip performance.
Compared with prior art, the present invention has following positive beneficial effect
1, tencel enhancing micropore silicon nitride compound carbonizing silica brick using silicon carbide, silicon nitride, metallic silicon, based on silicon ash
Raw material is wanted, using resin as bonding agent, is prepared through high temperature sintering under air atmosphere, since plastic deformation mutually introduces, resin knot
Conjunction mode, so that novel silicon carbide brick has silicon carbide fibre-plastic deformation phase-Ceramic Composite integrated structure, in-situ carbon SiClx
Fiber is intersected with each other at network, greatly improves the intensity, anti-erosion and wear-resisting property of material；
Silicon nitride and silicon carbide are introduced directly into oxidizing atmosphere firing by the present invention, avoid original of the metallic silicon in nitriding furnace
It is more stable thoroughly to solve the problems, such as that silicon nitride nitrogenizes silicon nitride that is insufficient, obtaining for position synthesis, be greatly reduced firing at
This；And during being somebody's turn to do, silicon nitride and the silicon carbide partial oxidation in air atmosphere sintering process form silicon oxynitride, silica
Etc. cenotypes, hence it is evident that reduce the porosity；Simultaneously under conditions of resin is bonding agent, resin will form residual in sintering process
Carbon forms reducing atmosphere inside brick body, promotes part metals silicon that silicon carbide fibre is formed in situ, and then it is fine to form silicon carbide
Dimension-plastic deformation phase-Ceramic Composite integrated structure, in-situ carburization silica fibre are crossed as network each other, fill stomata, substantially
Improve the intensity of material, anti-erosion and wear-resisting property.So the obtained properties of product of the present invention are far superior in the prior art
Product, and its preparation process is simple, at low cost, has a good application prospect.
2, for tencel enhancing micropore silicon nitride compound carbonizing silica brick relative market silicon nitride combined silicon carbide brick,
Preparation process is entirely different, and silicon nitride is to be introduced directly into oxidizing atmosphere to be burnt into, rather than pass through nitriding furnace fabricated in situ by the present invention,
Silicon nitride is more stable, solves metallic silicon and nitrogenizes insufficient and cause volume stability poor, or even the problem of cracking；
3, prepared tencel enhances micropore silicon nitride compound carbonizing silica brick, chemical component are as follows: and SiC70%~
90%, silicon nitride content 5-20%；Silicon nitride thermal shock resistance, high-temerature creep is small, and chemical stability is high, and anti-scour property is excellent
It is good, silicon carbide brick service performance is improved by the introducing of certain proportion silicon nitride, in addition silicon nitride is in firing and use process
The cenotypes such as silicon oxynitride, silica can be formed, effectively filling stomata, reduce the porosity, brick body stomata is promoted to become smaller or formed
Closed pore improves the anti-erosion and antistrip performance of material；
4, the prepared tencel enhancing micropore silicon nitride compound carbonizing silica brick porosity it is very low, less than 14%, volume
Density 2.55g/cm3~2.70g/cm3, compressive resistance is greater than 130MPa, thermal shock resistance > 50 time, indices function admirable；
The product has the features such as low stomata, high intensity, high thermal shock resistance, high abrasion and antiacid alkali erosiveness can be excellent.Therefore, should
Tencel enhancing micropore silicon nitride compound carbonizing silica brick can be applied to the key areas such as waste incinerator side wall.
5, prepared tencel enhancing micro-pore silicon carbide brick major part stomata exists with cellular form, and average pore size is small
In 1 μm；A large amount of uniform micros exist, and can effectively reduce gas phase in the waste incinerator of product, liquid phase corrodes infiltration.And then improve
Product erosion-resisting characteristics, antistrip performance prolong the service life.
Specific embodiment
The present invention is described in more details below by specific embodiment, but and do not have to, in limiting this hair
Bright protection scope.
The present invention provides a kind of fiber reinforced micro porous silicon nitride compound carbonizing silica bricks, by the original of following mass percentage
Material is prepared: silicon carbide 70%~85%, silicon nitride 3%~20%, metallic silicon 2%~8%, silicon ash 3%~6%；It is additional
Account for the resin of above-mentioned raw materials gross mass 2%~6%.
Wherein, in the silicon carbide SiC content >=97%, bulk density > 3.2g/cm of silicon carbide3；
The silicon carbide includes that partial size is 1mm≤partial size < 3mm, 0.074mm≤partial size < 1mm, partial size <
The particle of 0.074mm and partial size < 0.005mm；The mass ratio of different-grain diameter is 1mm≤partial size < in the silicon carbide
The mass ratio of 0.074mm: the partial size < 0.005mm of 3mm:0.074mm≤partial size < 1mm: partial size < is 2~4:1~2:1~4:
0.5~1.
Wherein, the partial size < 0.074mm of the silicon nitride, the Si in silicon nitride3N4Content > 90%.
Wherein, partial size<0.074mm of the metallic silicon, Si content>97% in the metallic silicon.
Wherein, partial size < 0.01mm of the silicon ash, SiO in silicon ash2Content > 92%.
Wherein, the resin is thermosetting phenolic resin；Viscosity of resin under the conditions of 25 DEG C be 16000~
19000cp；The mass percentage of moisture is 2~3% in the resin, and solid component mass percentage 77~83% dissociates
Phenol mass percentage 9.8~12%.
The present invention also provides the preparation method of fiber reinforced micro porous silicon nitride compound carbonizing silica brick, this method includes following
Step:
(1) mass ratio as requested prepares raw material；
(2) carborundum powder, the granularity < of the partial size < 0.074mm and partial size < 0.005mm that prepare step (1)
0.074mm silicon nitride powder, granularity < 0.074mm metallic silicon power and granularity < 0.01mm silicon ash are pre-mixed, and are uniformly mixed；
It (3) is 1mm≤partial size < 3mm by partial size and partial size is that 0.074mm≤partial size < 1mm carborundum aggregate is done
It is mixed, it is dry-mixed uniform；Then resin is added, carries out mixing, is uniformly mixed；Then premix described in step (1) is added, continues
Mixing is uniformly mixed to get pug is arrived；
(4) pug that step (3) obtains is suppressed into adobe using moulding press, moulding press tonnage used is
630T, the bulk density for controlling adobe is 2.60g/cm3~2.75g/cm3；
(5) by adobe obtained by step (4) as being dried in dry kiln, dry kiln inlet temperature is controlled 45 DEG C~90
DEG C, at 110 DEG C~180 DEG C, drying time is 20h~50h for drying temperature control, it is dry to moisture < 0.5% therein, out
Kiln；Using being burnt into hyperthermia tunnel Kiln or shuttle kiln after the completion of dry, firing temperature is 1350 DEG C~1450 DEG C, is being burnt into
At a temperature of keep the temperature 10h~20h, cooled to room temperature kiln discharge is after firing to get multiple to the fiber reinforced micro porous silicon nitride
Close silicon carbide brick.
The present invention also provides another embodiment, premixing described in step (2) is pre-mixed in the ball mill,
The premixing time is 0.5~1.0h.Wherein the typical but non-limiting premixing time be 0.5h, 0.6h, 0.7h, 0.8h,
0.9h or 1.0h.
The present invention also provides another embodiment, time when step (3) described carborundum aggregate carries out dry-mixed is
3min~5min.Wherein the typical but non-limiting dry-mixed time is 3min, 3.5min, 4min, 4.5min or 5min.
The present invention also provides another embodiment, the mixing time of mixing is carried out after step (3) the addition resin
For 5min~15min.Wherein typical but non-limiting mixing time be 5min, 6min, 7min, 8min, 9min, 10min,
11min, 12min, 13min, 14min or 15min.
The present invention also provides another embodiment, continue mixing when mixing after step (3) the addition premix
Time is 10min~25min.Wherein typical but non-limiting mixing time is 10min, 15min, 20min or 25min.
The present invention also provides another embodiment, drying temperature when step (5) is described dry is 110 DEG C~180
DEG C, typical but non-limiting temperature is 120 DEG C, 130 DEG C, 140 DEG C, 150 DEG C, 160 DEG C, 170 DEG C or 180 DEG C.It is therein dry
The dry time is 20h~50h, and the typical but non-limiting time is 20h, 30h, 40h or 50h；
It is 45 DEG C~90 DEG C that inlet temperature control is wanted in the drying, and typical but non-limiting temperature is 45 DEG C, 50 DEG C, 55
℃、60℃、65℃、70℃、75℃、80℃、85℃、90℃。
The present invention also provides another embodiment, firing temperature when step (5) described firing is 1350 DEG C~
1450 DEG C, typical but non-limiting temperature is 1350 DEG C, 1400 DEG C or 1450 DEG C；Firing time therein can for 10~
20h, typical but non-limiting time are 10h, 11h, 12h, 13h, 14h, 15h, 16h, 17h, 18h, 19h or 20h.
Below by specific embodiment to fiber reinforced micro porous silicon nitride compound carbonizing silica brick of the present invention and its system
Preparation Method is described in detail, in following embodiment:
Content >=97% of SiC in the silicon carbide, bulk density > 3.2g/cm of silicon carbide3；
The partial size < 0.074mm of the silicon nitride, the Si in silicon nitride3N4Content > 90%；
Partial size<0.074mm of the metallic silicon, Si content>97% in the metallic silicon；
Partial size < 0.01mm of the silicon ash, SiO in silicon ash2Content > 92%；
The resin is thermosetting phenolic resin；The resin viscosity is 16000~19000cp (under the conditions of 25 DEG C
Viscosity)；The mass percentage of moisture is 2~3% in the resin, solid component mass percentage 77~83%, free phenol
Mass percentage 9.8~12%.
Embodiment 1
A kind of fiber reinforced micro porous silicon nitride compound carbonizing silica brick, is prepared by the raw material of following mass percentage:
Silicon carbide 85%, silicon nitride 5%, metallic silicon 5%, silicon ash 5%；
The additional thermosetting phenolic resin for accounting for above-mentioned raw materials gross mass 4%.
Wherein, the silicon carbide partial size Mass Distribution is as follows, 1mm≤partial size < 3mm:0.074mm≤partial size < 1mm: grain
The quality of diameter < 0.074mm: partial size < 0.005mm is respectively 40%, 20%, 20%, 5%；
The preparation method of the product the following steps are included:
(1) mass ratio as requested prepares raw material；
(2) carborundum powder, the granularity < of the partial size < 0.074mm and partial size < 0.005mm that prepare step (1)
0.074mm silicon nitride powder, granularity < 0.074mm metallic silicon power and granularity < 0.01mm silicon ash are pre-mixed in the ball mill, in advance
Incorporation time is 0.5~1h, is uniformly mixed；
It (3) is 1mm≤partial size < 3mm by partial size and partial size is that 0.074mm≤partial size < 1mm carborundum aggregate is placed in wheel
Dry-mixed in stone roller formula batch mixer, the dry-mixed time is 5min, dry-mixed uniform；Then resin is added, carries out mixing, mixing time is
15min is uniformly mixed；Then premix described in step (1) is added, continues mixing, mixing time 20min, mixing is
It is even to get arrive pug；
(4) pug that step (3) obtains is suppressed into adobe using moulding press, the bulk density for controlling adobe is
2.75g/cm3, moulding press tonnage used is 630T；
(5) by adobe obtained by step (4) as being dried in dry kiln, dry kiln inlet temperature is controlled at 60 DEG C, is done
Dry temperature control is dry to moisture < 0.5% therein, kiln discharge at 130 DEG C, drying time 30h；
By the adobe after the completion of drying using being burnt into hyperthermia tunnel Kiln or shuttle kiln, firing temperature is 1350~
1450 DEG C, 10h is kept the temperature under firing temperature, cooled to room temperature kiln discharge is to obtain the fiber reinforced micro porous nitrogen after firing
SiClx compound carbonizing silica brick.
The fiber reinforced micro porous silicon nitride compound carbonizing silica brick progressive of embodiment preparation can be detected, as a result as follows:
Apparent porosity 13.5%, bulk density 2.65g/cm3, cold crushing strength 137MPa, thermal shock resistance (1100
DEG C, water cooling) it is greater than 50 times, wear-resisting 4.75cm3, average pore size is less than 0.80 μm.
Embodiment 2
A kind of fiber reinforced micro porous silicon nitride compound carbonizing silica brick, is prepared by the raw material of following mass percentage:
Silicon carbide 78%, silicon nitride 14%, metallic silicon 2%, silicon ash 6%；
The additional thermosetting phenolic resin for accounting for above-mentioned raw materials gross mass 3%.
Wherein, the silicon carbide partial size Mass Distribution is as follows, 1mm≤partial size < 3mm:0.074mm≤partial size < 1mm: grain
The mass ratio of diameter < 0.074mm: partial size < 0.005mm is respectively 40%, 15%, 17%, 6%；
The preparation method of the product the following steps are included:
(1) mass ratio as requested prepares raw material；
(2) carborundum powder, the granularity < of the partial size < 0.074mm and partial size < 0.005mm that prepare step (1)
0.074mm silicon nitride powder, granularity < 0.074mm metallic silicon power and granularity < 0.01mm silicon ash are pre-mixed in the ball mill, in advance
Incorporation time is 0.5~1h, is uniformly mixed；
It (3) is 1mm≤partial size < 3mm by partial size and partial size is that 0.074mm≤partial size < 1mm carborundum aggregate is placed in wheel
Dry-mixed in stone roller formula batch mixer, the dry-mixed time is 3min, dry-mixed uniform；Then resin is added, carries out mixing, mixing time is
15min is uniformly mixed；Then premix described in step (1) is added, continues mixing, mixing time 20min, mixing is
It is even to get arrive pug；
(4) pug that step (3) obtains is suppressed into adobe using moulding press, the bulk density for controlling adobe is
2.75g/cm3, moulding press tonnage used is 630T；
(5) by adobe obtained by step (4) as being dried in dry kiln, dry kiln inlet temperature is controlled at 80 DEG C, is done
Dry temperature control is dry to moisture < 0.5% therein, kiln discharge at 160 DEG C, drying time 36h；
By the adobe after the completion of drying using being burnt into hyperthermia tunnel Kiln or shuttle kiln, firing temperature is 1350~
1450 DEG C, 12h is kept the temperature under firing temperature, cooled to room temperature kiln discharge is to obtain the fiber reinforced micro porous nitrogen after firing
SiClx compound carbonizing silica brick.
The fiber reinforced micro porous silicon nitride compound carbonizing silica brick progressive of embodiment preparation can be detected, as a result as follows:
Apparent porosity 13.2%, bulk density 2.68g/cm3, cold crushing strength 142MPa, thermal shock resistance (1100
DEG C, water cooling) it is greater than 50 times, wear-resisting 4.55cm3, average pore size is less than 0.07 μm.
Embodiment 3
A kind of fiber reinforced micro porous silicon nitride compound carbonizing silica brick, is prepared by the raw material of following mass percentage:
Silicon carbide 70%, silicon nitride 20%, metallic silicon 4%, silicon ash 6%；
The additional thermosetting phenolic resin for accounting for above-mentioned raw materials gross mass 5%.
Wherein, the silicon carbide partial size Mass Distribution is as follows, 1mm≤partial size < 3mm:0.074mm≤partial size < 1mm: grain
The mass ratio of diameter < 0.074mm: partial size < 0.005mm is 35%, 20%, 10%, 5%；
The preparation method of the product the following steps are included:
(1) mass ratio as requested prepares raw material；
(2) carborundum powder, the granularity < of the partial size < 0.074mm and partial size < 0.005mm that prepare step (1)
0.074mm silicon nitride powder, granularity < 0.074mm metallic silicon power and granularity < 0.01mm silicon ash are pre-mixed in the ball mill, in advance
Incorporation time is 0.5~1h, is uniformly mixed；
It (3) is 1mm≤partial size < 3mm by partial size and partial size is that 0.074mm≤partial size < 1mm carborundum aggregate is placed in wheel
Dry-mixed in stone roller formula batch mixer, the dry-mixed time is 5min, dry-mixed uniform；Then resin is added, carries out mixing, mixing time is
10min is uniformly mixed；Then premix described in step (1) is added, continues mixing, mixing time 25min, mixing is
It is even to get arrive pug；
(4) pug that step (3) obtains is suppressed into adobe using moulding press, the bulk density for controlling adobe is
2.70g/cm3, moulding press tonnage used is 630T；
(5) by adobe obtained by step (4) as being dried in dry kiln, dry kiln inlet temperature is controlled at 50 DEG C, is done
Dry temperature control is dry to moisture < 0.5% therein, kiln discharge at 120 DEG C, drying time 22h；
By the adobe after the completion of drying using being burnt into hyperthermia tunnel Kiln or shuttle kiln, firing temperature is 1350~
1450 DEG C, 12h is kept the temperature under firing temperature, cooled to room temperature kiln discharge is to obtain the fiber reinforced micro porous nitrogen after firing
SiClx compound carbonizing silica brick.
The fiber reinforced micro porous silicon nitride compound carbonizing silica brick progressive of embodiment preparation can be detected, as a result as follows:
Apparent porosity 13.1%, bulk density 2.68g/cm3, cold crushing strength 155MPa, thermal shock resistance (1100
DEG C, water cooling) it is greater than 50 times, wear-resisting 4.30cm3, average pore size is less than 0.76 μm.
Claims (10)
1. a kind of fiber reinforced micro porous silicon nitride compound carbonizing silica brick, which is characterized in that by the raw material of following weight percentage
It is prepared: silicon carbide 70%~85%, silicon nitride 3%~20%, metallic silicon 2%~8%, silicon ash 3%~6%；
The additional resin for accounting for above-mentioned raw materials total weight 2%~6%.
2. fiber reinforced micro porous silicon nitride compound carbonizing silica brick according to claim 1, which is characterized in that the silicon carbide
Content >=97% of middle SiC, bulk density > 3.2g/cm of silicon carbide3。
3. fiber reinforced micro porous silicon nitride compound carbonizing silica brick according to claim 1 or 2, which is characterized in that the carbon
SiClx partial size Mass Distribution is as follows, 1mm≤partial size < 3mm:0.074mm≤partial size < 1mm: partial size < 0.074mm: partial size <
The mass ratio of 0.005mm is 2~4:1~2:1~4:0.5~1.
4. fiber reinforced micro porous silicon nitride compound carbonizing silica brick according to claim 1, which is characterized in that the silicon nitride
Partial size < 0.074mm, the Si in silicon nitride3N4Content > 90%.
5. fiber reinforced micro porous silicon nitride compound carbonizing silica brick according to claim 1, which is characterized in that the metallic silicon
Partial size<0.074mm, Si content>97% in the metallic silicon；Partial size < 0.01mm of the silicon ash, SiO in silicon ash2Content >
92%.
6. fiber reinforced micro porous silicon nitride compound carbonizing silica brick according to claim 1, which is characterized in that the resin
For thermosetting phenolic resin；The resin viscosity is 16000~19000cp；In the resin mass percentage of moisture be 2~
3%, solid component mass percentage 77~83%, free phenol mass percentage 9.8~12%.
7. the preparation method of fiber reinforced micro porous silicon nitride compound carbonizing silica brick described in a kind of claim 1, which is characterized in that packet
Include following steps:
(1) mass ratio as requested prepares raw material；
(2) carborundum powder, the granularity < 0.074mm nitrogen of the partial size < 0.074mm and partial size < 0.005mm that prepare step (1)
SiClx powder, granularity < 0.074mm metallic silicon power and granularity < 0.01mm silicon ash are pre-mixed, and are uniformly mixed；
It (3) is 1mm≤partial size < 3mm by partial size and partial size is that 0.074mm≤partial size < 1mm carborundum aggregate is dry-mixed, it is dry-mixed
Uniformly, resin is then added, carries out mixing, is uniformly mixed；Then premix described in step (1) is added, continues mixing, mixes
Close uniformly to get arrive pug；
(4) pug that step (3) obtains is suppressed into adobe, the bulk density for controlling adobe is 2.60g/cm3~2.75g/
cm3；
(5) adobe obtained by step (4) is dried, is burnt into, cooled to room temperature increases after firing to get to the fiber
Strong micropore silicon nitride compound carbonizing silica brick.
8. the preparation method of fiber reinforced micro porous silicon nitride compound carbonizing silica brick according to claim 7, which is characterized in that step
Suddenly (2) described premixing carries out in the ball mill, and the premixing time is 0.5~1h；It is dry-mixed mixed in rolling wheel described in step (3)
It is carried out in material machine, the dry-mixed time is 3min~5min；The mixing time of mixing is carried out after resin is added as 5min~15min；Institute
It states addition premix and continues the time of mixing as 10min~25min；During step (4) described pressing unfired brick, molding pressure used
Machine tonnage is 630T.
9. the preparation method of fiber reinforced micro porous silicon nitride compound carbonizing silica brick according to claim 7, which is characterized in that step
Suddenly (5) drying are as follows: by adobe that step (4) obtains as being dried in dry kiln, the control of dry kiln inlet temperature exists
45 DEG C~90 DEG C, at 110 DEG C~180 DEG C, drying time is 20h~50h for drying temperature control, dry to moisture < therein
0.5%, kiln discharge.
10. the preparation method of fiber reinforced micro porous silicon nitride compound carbonizing silica brick according to claim 7, which is characterized in that
Step (5) described firing are as follows: by the adobe after drying using being burnt into hyperthermia tunnel Kiln or shuttle kiln, firing temperature is
1350 DEG C~1450 DEG C, 10h~20h, cooled to room temperature kiln discharge after firing are kept the temperature under firing temperature.
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| CN110483023A (en) * | 2019-08-21 | 2019-11-22 | 通达耐火技术股份有限公司 | A kind of microporous corundum brick and preparation method thereof |
| CN110981510A (en) * | 2019-12-18 | 2020-04-10 | 宜兴市丁山耐火器材有限公司 | Silicon oxynitride and silicon carbide combined refractory brick and preparation method thereof |
| CN111925219A (en) * | 2020-05-29 | 2020-11-13 | 朝阳燕山湖发电有限公司 | Preparation method of inorganic fiber reinforced silicon nitride ceramic for cyclone burner |
| CN111559917B (en) * | 2020-06-05 | 2021-09-21 | 中钢集团洛阳耐火材料研究院有限公司 | Silicon carbide refractory wear-resistant material with microporous structure |
| CN115180956A (en) * | 2022-07-26 | 2022-10-14 | 重庆鸽牌电瓷有限公司 | Formula of low-cost high-performance siliceous porcelain blank |
| CN115448725A (en) * | 2022-09-30 | 2022-12-09 | 安徽瑞泰新材料科技有限公司 | Refractory brick and preparation method thereof |
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| CN110483023A (en) * | 2019-08-21 | 2019-11-22 | 通达耐火技术股份有限公司 | A kind of microporous corundum brick and preparation method thereof |
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| CN111925219A (en) * | 2020-05-29 | 2020-11-13 | 朝阳燕山湖发电有限公司 | Preparation method of inorganic fiber reinforced silicon nitride ceramic for cyclone burner |
| CN111559917B (en) * | 2020-06-05 | 2021-09-21 | 中钢集团洛阳耐火材料研究院有限公司 | Silicon carbide refractory wear-resistant material with microporous structure |
| CN115180956A (en) * | 2022-07-26 | 2022-10-14 | 重庆鸽牌电瓷有限公司 | Formula of low-cost high-performance siliceous porcelain blank |
| CN115448725A (en) * | 2022-09-30 | 2022-12-09 | 安徽瑞泰新材料科技有限公司 | Refractory brick and preparation method thereof |
| CN115448725B (en) * | 2022-09-30 | 2023-10-03 | 安徽瑞泰新材料科技有限公司 | Refractory brick and preparation method thereof |
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