CN107382322A - A kind of preparation method of silicon carbide woodceramics - Google Patents
A kind of preparation method of silicon carbide woodceramics Download PDFInfo
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/575—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by pressure sintering
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Abstract
The present invention relates to a kind of preparation method of silicon carbide woodceramics, belong to ceramic materials preparation technology field.The present invention freezes after hemp stalk is soaked with sodium hydroxide solution constant temperature, again through thawing, such constant temperature immersion, freezing and thaw cycles are several times, the hemp stalk that last time is thawed is washed with water and dried again, again through crushing and sieving, obtain hemp stalk powder, hemp stalk powder is transferred to tube furnace, and preheat tube furnace, again tetraethyl orthosilicate is heated to seething with excitement, tetraethyl orthosilicate steam is imported in the tube furnace after preheating, hemp stalk powder is fumigated with tetraethyl orthosilicate steam, hemp stalk powder must be pre-processed, will pretreatment hemp stalk powder it is hot-forming after, charing, base substrate must be carbonized, charing base substrate is placed in graphite crucible, and covered with simple substance silicon grain, liquid Si infiltration is carried out again, naturally cool to room temperature, discharging.Silicon carbide woodceramics density prepared by the present invention is high, and mechanical property is improved, and expands its use range.
Description
Technical field
The present invention relates to a kind of preparation method of silicon carbide woodceramics, belong to ceramic materials preparation technology field.
Background technology
Closely during the last ten years, wood materials are also used for reaction sintering technology and prepare silicon carbide ceramics（The wooden potteries of referred to as SiC
Porcelain）, its method be using timber, density board and wood powder/polymer matrix composites etc. as wooden base substrate in nitrogen atmosphere ceiling
Pyrolysis obtains porous charcoal base under part, then carries out siliconising at high temperature and prepares SiC wood ceramics.Can after wood ceramics are processed
Traditional ceramics is substituted, can be used as electrode, heater, motor carbon, brake lining, resistant material, heat-insulating material, filtering material
Deng there is wide development prospect, be the ideal substitute of some non-renewable materials.
But result of study and reaction-sintered theory show, the technology for preparing SiC wood ceramics with wood materials does not have
Standby actual application value, timber is a kind of natural porous material, its aperture is had wide be distributed because of the complexity of microstructure
Feature；Make its pore-size distribution that there is larger variation because of the difference of stem sample site etc. residing for arboreal growth environment, timber again
Property, while the presence of some faults of construction also causes the change of pore-size distribution and pore character, therefore directly prepared using timber
During SiC wood ceramics, because density of wood is low, structural fluctuation is big, and prepared ceramic density is also low, and mechanical property is not very managed
Think；When using fiberboard as raw material, structural homogeneity is improved, but density is still relatively low, and prepared ceramic density is still
It is relatively low；During using wood powder/polymer matrix composites as raw material, highdensity SiC wood ceramics, but material system can be obtained
The middle resin-oatmeal being introduced into makes remaining carbon in ceramics too high, limits the further raising of its mechanical property.
Therefore, the mechanical property and density of silicon carbide woodceramics are improved, is advantageous to expand making for silicon carbide woodceramics
Use scope.
The content of the invention
The technical problems to be solved by the invention：Low for existing wood ceramics density, mechanical property is undesirable, limitation
A kind of the problem of its use range, there is provided the preparation method of silicon carbide woodceramics.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）After hemp stalk is soaked into 20~40min with sodium hydroxide solution constant temperature, 10~20s is freezed with liquid nitrogen spraying, then through micro-
Ripple thaws 2~4min, the immersion of such constant temperature, freezing and thaw cycles 3~5 times, then will the hemp stalk water that thaws of last time
Washing 3~5 times, and it is 10~15% to dry to moisture content, then dried hemp stalk is crushed, sieve, obtain hemp stalk powder；
（2）Above-mentioned gained hemp stalk powder is transferred to tube furnace, is preheated to 150~160 DEG C, then tetraethyl orthosilicate is heated to boiling
Rise, imported tetraethyl orthosilicate steam in the tube furnace after preheating with conduit, with tetraethyl orthosilicate steam to Chinese fiber crops in tube furnace
Bar powder carries out stifling 2~4h, must pre-process hemp stalk powder；
（3）By gained pretreatment hemp stalk powder it is hot-forming after, charing, obtain charing base substrate；
（4）Above-mentioned gained charing base substrate is placed in graphite crucible, and covered with simple substance silicon grain, is then moved into graphite crucible true
Liquid Si infiltration is carried out in empty stove, after naturally cool to room temperature, discharging, produces silicon carbide woodceramics.
Step（1）Described sieving was 100~200 mesh sieves.
Step（3）Described hot-forming condition is：Hot pressing temperature is 180~200 DEG C, and hot pressing pressure is 10~20MPa.
Step（3）Described carbonization condition is：In retort, argon gas is passed through into stove with 60~90mL/min speed,
Under argon gas guard mode, 300~400 DEG C are warming up to 3~5 DEG C/min rate programs, after being incubated 30~40min, is continued with 4
~6 DEG C/min rate programs are warming up to 800~900 DEG C, after being incubated 40~60min, continue with 6~8 DEG C/min rate program liters
Temperature after being incubated 2~4h, cools to room temperature with the furnace to 1400~1500 DEG C.
Step（4）Described elemental silicon mean particle size is 0.6~3.5mm, and purity is 99.1~99.4%；The list
Matter silicon grain cladding thickness is 0.5~0.8 times of charing base substrate thickness.
Step（4）Described liquid Si infiltration condition is：Vacuum is 40~80Pa, and temperature is 1450~1550 DEG C, insulation
Time is 60~90min.
Compared with other method, advantageous effects are the present invention：
（1）The present invention soaks first with sodium hydroxide solution, and hemp stalk fiber occurs, and preliminary solution is fine, and fiber is loose, and fills
Point water suction, then coordinates liquid nitrogen frozen, makes the moisture icing volumetric expansion in the hemp stalk cell after water suction, through repeatedly immersion, cold
Jelly and thaw cycles, expand hemp stalk cell and space between cells, be easy to gas molecule to enter, dried in baking oven, dried
During dry, the moisture in outside and space between cells volatilizees first, and the moisture evaporation of cell interior is slower, by strictly controlling
Moisture content, most of moisture in space between cells is volatilized, only cell interior residual fraction moisture, recycle tetraethyl orthosilicate
Steam steaming, the hemp stalk cell interior for making tetraethyl orthosilicate steam gradually penetrate into after expanding, and remained with cell interior
Contact with moisture, hydrolyze, generate silica after be filled in cell interior, because most of water has been waved in space between cells
Hair, it can effectively avoid tetraethyl orthosilicate from occurring to hydrolyze and block duct in process of osmosis, be advantageous to tetraethyl orthosilicate and fully enter
Enter cell interior, and be filled in cell interior silica can in follow-up carbonization process, under the high temperature conditions with after charing
Organic qualitative response, generate carborundum, the carborundum of generation can realize effective filling to cell interior, improve interiors of products and cause
Density；
（2）The present invention improves product consistency to a certain extent by hot-forming, recycles liquid Si infiltration, melts elemental silicon
Penetrate into afterwards charing base substrate space between cells and surface, and with the organic qualitative response of charing on space between cells and surface, generate carbon
SiClx, filling and covering to space between cells and surface are realized, further improve the consistency in product gap；
（3）The present invention by the way that to plant tissue cell inside, the position such as space between cells and plant tissue surface is realized and is sufficient filling with,
The consistency of product is effectively improved, so that product mechanical property is effectively lifted.
Embodiment
First by hemp stalk with mass fraction be 8~10% sodium hydroxide solutions under the conditions of temperature is 40~50 DEG C, constant temperature
After soaking 20~40min, 10~20s is freezed with liquid nitrogen spraying, then through 2~4min of microwave thawing, such constant temperature immersion, freezing and
Thaw cycles 3~5 times, then the hemp stalk that last time is thawed is washed with deionized 3~5 times, then the Chinese after washing is numb
Bar is moved into baking oven, and it is 10~15% to be dried under the conditions of being 80~100 DEG C in temperature to moisture content, then by dried hemp stalk
Pour into pulverizer, 100~200 mesh sieves are crossed after crushing, obtain hemp stalk powder；Gained hemp stalk powder is transferred to tube furnace, is preheated to
150~160 DEG C, then tetraethyl orthosilicate is heated to seething with excitement, tetraethyl orthosilicate steam will be imported in advance caused by boiling with conduit
In tube furnace after heat, stifling 2~4h is carried out to hemp stalk powder in tube furnace with tetraethyl orthosilicate steam, obtains pretreatment hemp stalk
Powder；It is 180~200 DEG C that gained is pre-processed into hemp stalk powder in temperature again, hot-forming under the conditions of pressure is 10~20MPa, is obtained
Base substrate, then gained base substrate is moved into retort, argon gas is passed through into stove with 60~90mL/min speed, in argon gas guard mode
Under, 300~400 DEG C are warming up to 3~5 DEG C/min rate programs, after being incubated 30~40min, is continued with 4~6 DEG C/min speed
Temperature programming after being incubated 40~60min, continues to be warming up to 1400~1500 with 6~8 DEG C/min rate programs to 800~900 DEG C
DEG C, after being incubated 2~4h, cool to room temperature with the furnace, discharge, obtain charing base substrate；Gained charing base substrate is placed in graphite crucible again, and
Covered with simple substance silicon grain, control cladding thickness then to be moved into graphite crucible true for 0.5~0.8 times of charing base substrate thickness
In empty stove, liquid Si infiltration is carried out, be 40~80Pa in vacuum, under the conditions of temperature is 1450~1550 DEG C, it is incubated 60~
90min, after naturally cool to room temperature, discharging, produce silicon carbide woodceramics.Described elemental silicon mean particle size is 0.6
~3.5mm, purity are 99.1~99.4%.
Example 1
First by hemp stalk with mass fraction be 10% sodium hydroxide solution under the conditions of temperature is 50 DEG C, constant temperature immersion 40min
Afterwards, 20s is freezed with liquid nitrogen spraying, then through microwave thawing 4min, such constant temperature immersion, freezing and thaw cycles 5 times, then will be last
The hemp stalk once thawed is washed with deionized 5 times, then by after washing hemp stalk move into baking oven in, in temperature be 100 DEG C
Under the conditions of to dry to moisture content be 15%, then dried hemp stalk poured into pulverizer, 200 mesh sieves crossed after crushing, obtain Chinese fiber crops
Bar powder；Gained hemp stalk powder is transferred to tube furnace, 160 DEG C is preheated to, then is heated to seething with excitement by tetraethyl orthosilicate, will with conduit
Tetraethyl orthosilicate steam caused by boiling is imported in the tube furnace after preheating, with tetraethyl orthosilicate steam to hemp stalk in tube furnace
Powder carries out stifling 4h, must pre-process hemp stalk powder；It is 200 DEG C that gained is pre-processed into hemp stalk powder in temperature again, pressure 20MPa
Under the conditions of, it is hot-forming, base substrate is obtained, then gained base substrate is moved into retort, argon gas is passed through into stove with 90mL/min speed,
Under argon gas guard mode, 400 DEG C are warming up to 5 DEG C/min rate programs, after being incubated 40min, is continued with 6 DEG C/min rate programs
900 DEG C are warming up to, after being incubated 60min, continues to be warming up to 1500 DEG C with 8 DEG C/min rate programs, after being incubated 4h, cools to the furnace
Room temperature, discharging, obtains charing base substrate；Gained charing base substrate is placed in graphite crucible again, and covered with simple substance silicon grain, control covering
Thickness is 0.8 times of charing base substrate thickness, then moves into graphite crucible in vacuum drying oven, carries out liquid Si infiltration, is in vacuum
80Pa, under the conditions of temperature is 1550 DEG C, 90min is incubated, after naturally cool to room temperature, discharging, produces silicon carbide woodceramics.Institute
The elemental silicon mean particle size stated is 3.5mm, purity 99.4%.
Example 2
First by hemp stalk with mass fraction be 8% sodium hydroxide solution under the conditions of temperature is 40 DEG C, constant temperature immersion 20min after,
Freeze 10s with liquid nitrogen spraying, then through microwave thawing 2min, such constant temperature immersion, freezing and thaw cycles 3 times, then by last
The hemp stalk of secondary defrosting is washed with deionized 3 times, then by after washing hemp stalk move into baking oven in, in temperature be 80 DEG C of conditions
Lower drying to moisture content is 10%, then dried hemp stalk is poured into pulverizer, and 100 mesh sieves are crossed after crushing, obtain hemp stalk
Powder；Gained hemp stalk powder is transferred to tube furnace, 150 DEG C is preheated to, then is heated to seething with excitement by tetraethyl orthosilicate, will be boiled with conduit
Tetraethyl orthosilicate steam is imported in the tube furnace after preheating caused by rising, with tetraethyl orthosilicate steam to hemp stalk powder in tube furnace
Stifling 2h is carried out, hemp stalk powder must be pre-processed；It is 180 DEG C that gained is pre-processed into hemp stalk powder in temperature again, and pressure is 10MPa bars
It is hot-forming under part, base substrate is obtained, then gained base substrate is moved into retort, argon gas is passed through into stove with 60mL/min speed, in argon
Under gas shielded state, 300 DEG C are warming up to 3 DEG C/min rate programs, after being incubated 30min, is continued with 4 DEG C/min rate program liters
Temperature is to 800 DEG C, after being incubated 40min, continues to be warming up to 1400 DEG C with 6 DEG C/min rate programs, after being incubated 2h, cools to room with the furnace
Temperature, discharging, obtains charing base substrate；Gained charing base substrate is placed in graphite crucible again, and covered with simple substance silicon grain, control covering is thick
Spend to carbonize 0.5 times of base substrate thickness, then move into graphite crucible in vacuum drying oven, carry out liquid Si infiltration, be in vacuum
40Pa, under the conditions of temperature is 1450 DEG C, 60min is incubated, after naturally cool to room temperature, discharging, produces silicon carbide woodceramics.Institute
The elemental silicon mean particle size stated is 0.6mm, purity 99.1%.
Example 3
First by hemp stalk with mass fraction be 9% sodium hydroxide solution under the conditions of temperature is 45 DEG C, constant temperature immersion 30min after,
Freeze 15s with liquid nitrogen spraying, then through microwave thawing 3min, such constant temperature immersion, freezing and thaw cycles 4 times, then by last
The hemp stalk of secondary defrosting is washed with deionized 4 times, then by after washing hemp stalk move into baking oven in, in temperature be 90 DEG C of conditions
Lower drying to moisture content is 12%, then dried hemp stalk is poured into pulverizer, and 150 mesh sieves are crossed after crushing, obtain hemp stalk
Powder；Gained hemp stalk powder is transferred to tube furnace, 155 DEG C is preheated to, then is heated to seething with excitement by tetraethyl orthosilicate, will be boiled with conduit
Tetraethyl orthosilicate steam is imported in the tube furnace after preheating caused by rising, with tetraethyl orthosilicate steam to hemp stalk powder in tube furnace
Stifling 3h is carried out, hemp stalk powder must be pre-processed；It is 190 DEG C that gained is pre-processed into hemp stalk powder in temperature again, and pressure is 15MPa bars
It is hot-forming under part, base substrate is obtained, then gained base substrate is moved into retort, argon gas is passed through into stove with 80mL/min speed, in argon
Under gas shielded state, 350 DEG C are warming up to 4 DEG C/min rate programs, after being incubated 35min, is continued with 5 DEG C/min rate program liters
Temperature is to 850 DEG C, after being incubated 50min, continues to be warming up to 1450 DEG C with 7 DEG C/min rate programs, after being incubated 3h, cools to room with the furnace
Temperature, discharging, obtains charing base substrate；Gained charing base substrate is placed in graphite crucible again, and covered with simple substance silicon grain, control covering is thick
Spend to carbonize 0.6 times of base substrate thickness, then move into graphite crucible in vacuum drying oven, carry out liquid Si infiltration, be in vacuum
60Pa, under the conditions of temperature is 1500 DEG C, 70min is incubated, after naturally cool to room temperature, discharging, produces silicon carbide woodceramics.Institute
The elemental silicon mean particle size stated is 2.1mm, purity 99.3%.
Reference examples：The wood ceramics of Fujian Industrial Co., Ltd. production.
The silicon carbide woodceramics of example and reference examples are cut into 45mm × 5mm × 3mm samples, and sample is examined
Survey, specific detection is as follows：
1. density measurement：Using the density of Archimedes's drainage measure sample；
2. bending strength test：The bending strength of sample, controlled loading side are determined with three-point bending method with electronic universal tester
To, span 20mm vertical with stress surface, ram movement speed is 0.5mm/min；
3. modulus of elasticity is tested：According to GB/T 10700-2006 testing standard, test sample modulus of elasticity；
4. fracture toughness：With AG-2000A type Material Testing Machine, using the fracture toughness of Single edge notch beam test sample, otch
Depth is the 1/2 of specimen height, kerf width 0.2mm.
Specific testing result such as table 1.
Table 1
As shown in Table 1, the wood ceramics density that prepared by the present invention is big, the excellent in mechanical performance such as bending strength, modulus of elasticity.
Claims (6)
1. a kind of preparation method of silicon carbide woodceramics, it is characterised in that specifically preparation process is：
（1）After hemp stalk is soaked into 20~40min with sodium hydroxide solution constant temperature, 10~20s is freezed with liquid nitrogen spraying, then through micro-
Ripple thaws 2~4min, the immersion of such constant temperature, freezing and thaw cycles 3~5 times, then will the hemp stalk water that thaws of last time
Washing 3~5 times, and it is 10~15% to dry to moisture content, then dried hemp stalk is crushed, sieve, obtain hemp stalk powder；
（2）Above-mentioned gained hemp stalk powder is transferred to tube furnace, is preheated to 150~160 DEG C, then tetraethyl orthosilicate is heated to boiling
Rise, imported tetraethyl orthosilicate steam in the tube furnace after preheating with conduit, with tetraethyl orthosilicate steam to Chinese fiber crops in tube furnace
Bar powder carries out stifling 2~4h, must pre-process hemp stalk powder；
（3）By gained pretreatment hemp stalk powder it is hot-forming after, charing, obtain charing base substrate；
（4）Above-mentioned gained charing base substrate is placed in graphite crucible, and covered with simple substance silicon grain, is then moved into graphite crucible true
Liquid Si infiltration is carried out in empty stove, after naturally cool to room temperature, discharging, produces silicon carbide woodceramics.
A kind of 2. preparation method of silicon carbide woodceramics according to claim 1, it is characterised in that：Step（1）It is described
Sieving be 100~200 mesh sieves.
A kind of 3. preparation method of silicon carbide woodceramics according to claim 1, it is characterised in that：Step（3）It is described
Hot-forming condition be：Hot pressing temperature is 180~200 DEG C, and hot pressing pressure is 10~20MPa.
A kind of 4. preparation method of silicon carbide woodceramics according to claim 1, it is characterised in that：Step（3）It is described
Carbonization condition be：In retort, argon gas is passed through into stove with 60~90mL/min speed, under argon gas guard mode, with 3
~5 DEG C/min rate programs are warming up to 300~400 DEG C, after being incubated 30~40min, continue with 4~6 DEG C/min rate program liters
Temperature is to 800~900 DEG C, after being incubated 40~60min, continues to be warming up to 1400~1500 DEG C with 6~8 DEG C/min rate programs, protects
After 2~4h of temperature, room temperature is cooled to the furnace.
A kind of 5. preparation method of silicon carbide woodceramics according to claim 1, it is characterised in that：Step（4）It is described
Elemental silicon mean particle size be 0.6~3.5mm, purity is 99.1~99.4%；The simple substance silicon grain cladding thickness is charcoal
Change base substrate thickness 0.5~0.8 times.
A kind of 6. preparation method of silicon carbide woodceramics according to claim 1, it is characterised in that：Step（4）It is described
Liquid Si infiltration condition be：Vacuum is 40~80Pa, and temperature is 1450~1550 DEG C, and soaking time is 60~90min.
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| CN108706979A (en) * | 2018-07-18 | 2018-10-26 | 东北林业大学 | A kind of Silica hydrogel is modified the preparation method of wooden base silicon carbide ceramic material |
| CN110105071A (en) * | 2019-06-06 | 2019-08-09 | 南通通州湾新材料科技有限公司 | A kind of preparation method and its mobile phone backboard of silicified wood surface structure part |
| CN112960906A (en) * | 2021-04-13 | 2021-06-15 | 刘永广 | Lead-free environment-friendly ceramic glaze and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108706979A (en) * | 2018-07-18 | 2018-10-26 | 东北林业大学 | A kind of Silica hydrogel is modified the preparation method of wooden base silicon carbide ceramic material |
| CN108706979B (en) * | 2018-07-18 | 2021-03-23 | 东北林业大学 | Preparation method of silica gel modified wood-based silicon carbide ceramic material |
| CN110105071A (en) * | 2019-06-06 | 2019-08-09 | 南通通州湾新材料科技有限公司 | A kind of preparation method and its mobile phone backboard of silicified wood surface structure part |
| CN112960906A (en) * | 2021-04-13 | 2021-06-15 | 刘永广 | Lead-free environment-friendly ceramic glaze and preparation method thereof |
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Application publication date: 20171124 |