CN108585905A - A kind of high-strength carborundum ceramics and preparation method thereof - Google Patents
A kind of high-strength carborundum ceramics and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of ceramic materials.A kind of high-strength carborundum ceramics of the present invention, include the component of following parts by weight:70 ~ 80 parts of sic powder, 10 ~ 20 parts of silicon carbide fibre, 20 ~ 25 parts of binder, 5 ~ 10 parts of pore creating material, 5 ~ 10 parts of sintering aid, 5 ~ 10 parts of dispersant, 2 ~ 3 parts of toughener.The present invention also provides a kind of preparation methods of high-strength carborundum ceramics, are first uniformly mixed raw material, and raw material slurry is made, the raw material slurry is vacuum-treated again, after ceramic slurry after vacuum degassing is injected into mold, the mold is sealed, is heated, natural cooling after heat preservation, after then being dried 12 72 hours in baking oven, biscuit of ceramics is obtained, the biscuit of ceramics is sintered, the time of the sintering processes is 1 5h, and sintering temperature is 1500 ~ 1800 DEG C.The beneficial effects of the present invention are the holes in the present invention uniformly and with high intensity.
Description
Technical field
The present invention relates to a kind of ceramic materials, in particular to a kind of high-strength carborundum ceramics and preparation method thereof.
Background technology
Ceramic material is with natural or synthetic compound by a kind of inorganic non-metallic material made of forming and high temperature sintering
Material.It has many advantages, such as high-melting-point, high rigidity, high-wearing feature, resistance to oxidation.It can be used as structural material, cutter material, due to
Ceramics also have certain special performances, but also as functional material.
Silicon carbide (SiC) (is needed plus is eaten when production green silicon carbide with quartz sand, petroleum coke (or coal tar), sawdust
Salt) etc. raw materials formed by resistance furnace pyrolytic semlting.There is also rare mineral, Mo Sangshi in the Nature for silicon carbide.Silicon carbide
Also known as moissanite.In the non-oxidized substances high-tech refractory raw material such as contemporary C, N, B, silicon carbide is most widely used, most economical
One kind being properly termed as corundum or fire sand.
Porous silicon carbide ceramic is due to low-density, high temperature resistant, corrosion-resistant, high permeability and anti-oxidant, anti-thermal shock
The advantages that performance is good makes it in terms of high-temperature gas filter material, catalyst carrier, gas combustion chamber medium and refractory material
It is with a wide range of applications.Currently, the porous ceramics of more application is mostly oxide ceramics, but its there are high-temperature behaviors
Bad, the shortcomings of corrosion resistance is insufficient, and porous silicon carbide ceramic can just make up these deficiencies;In addition, many special
The advantages of more stringent requirements are proposed for performance of the field to porous ceramic film material, carbofrax material itself become prepare it is porous
One of the ideal material of ceramics, as being used in high temperature gas cooled reactor filter radioactive liquid waste and graphitiferous particle in nuclear energy field
High temperature helium.Preparation accordingly, with respect to porous silicon carbide ceramic becomes one of the hot spot studied at present.
Currently, the method for preparing porous silicon carbide ceramic mainly has:Direct particle is accumulated to form hole, and addition organic matter is made
Hole agent, foaming agent, or porous body, organic foam plastic are formed through Pintsch process using the resin of timber, high carbon sequestration content
As template, or select Polycarbosilane as precursor etc..It is existing to prepare porous silicon carbide ceramic MATERIALS METHODS, some works
Skill is relatively simple, but pore-size and porosity cannot be controlled effectively, it is more difficult to prepare porosity and be higher than 80% and hole
The porous ceramics aligned;Some technique need to exclude organic matter to form pore structure, although porosity in preparation process
And aperture is controllable in a certain range, but be equally difficult to prepare the porous silicon carbide ceramic of high porosity, in addition, the row of organic matter
Except unfriendly to environment;Porous silicon carbide ceramic can be prepared at a lower temperature using Polycarbosilane as precursor, but is made
Standby cost is very high.On the other hand, above-mentioned preparation method is difficult to realize the preparation of the porous silicon carbide ceramic of complicated shape, to system
Standby complex-shaped part needs to carry out larger subsequent mechanical processing, considerably increases production cost.Further, since carbonization
The sintering character of silicon is poor, and the mechanical property of porous silicon carbide ceramic prepared by existing method is relatively low, the gas in manufactured finished product
When porosity reaches 50%, intensity is often below 40MPa, seriously limits the application of porous silicon carbide ceramic.Therefore it needs at present
A kind of hole is uniformly and ceramic with high-strength carborundum.
Invention content
To solve the above-mentioned problems, a kind of high-strength carborundum ceramics and preparation method thereof are provided, the present invention is using following
Technical solution:
A kind of high-strength carborundum ceramics, which is characterized in that include the component of following parts by weight:
70 ~ 80 parts of sic powder, 10 ~ 20 parts of silicon carbide fibre, 20 ~ 25 parts of binder, 5 ~ 10 parts of pore creating material, sintering aid 5 ~
10 parts, 5 ~ 10 parts of dispersant, 2 ~ 3 parts of toughener.
Present invention employs the schemes that silicon carbide powder and silicon carbide fibre are used in conjunction with, by silicon carbide fibre in ceramics
In cementation, strengthen the mechanical strength of silicon carbide ceramics, in addition present invention adds pore creating materials, are realized by pore creating material
The pore-forming of porous silicon carbide ceramic contributes to the quantity of pore-forming in the size for adjusting aperture and ceramics, so as to improve ceramics
Inoxidizability and mechanical strength, and help to prevent the size gap due to aperture excessive, cause the structure of ceramic entirety
The case where intensity declines.
Preferably, a diameter of 0.1 micron~20 microns of the silicon carbide fibre, length is 20 microns~500 micro-
Rice.
The size for the silicon carbide fibre that the present invention uses can make silicon carbide fibre be attached in sic powder, play
The effect being connected and fixed, after sintering
Preferably, the binder includes the component of following parts by weight:3 ~ 5 parts of alumina powder, sodium cellulose glycolate 8 ~
10 parts, 9 ~ 10 parts of silica.
Preferably, the dispersant includes the component of following parts by weight:2 ~ 3 parts of polyvinyl alcohol, 1 ~ 3 part of oleic acid gather
1 ~ 2 part of ethylene glycol.
Present invention employs polyvinyl alcohol, oleic acid, polyethylene glycol helps to improve each component in slurry as dispersant
Dispersion effect so that in ceramic product each component distributing equilibrium, reduce ceramics internal structural defects, improve ceramics
Mechanical strength.
Preferably, further including pore creating material in the component, the pore creating material uses carbon dust, the sintering aid
Using the mixing of aluminium oxide and calcium oxide, the toughener uses yttrium oxide.
Present invention employs carbon dusts as pore creating material, in the solution of the present invention, needs the hole for strictly controlling ceramics big
Small and hole quantity, prevents the hole of ceramics from excessively mechanical performance being caused to decline, therefore, present invention employs carbon dusts to be made
Hole, carbon dust oxidation in sintering leave tiny hole, help to improve the mechanical performance of ceramics.
Preferably, the yttrium oxide uses mesoporous yttrium oxide.
Present invention uses mesoporous yttrium oxides, and present invention utilizes mesoporous Yttrium oxide materials to have bigger serface and three-dimensional
The characteristics of pore passage structure, strengthens yttrium oxide for the function and effect of ceramics, effectively reduces the granularity of component in ceramics, make
Obtaining silicon carbide powder and silicon carbide fibre preferably can bond, and strengthen the mechanical strength of ceramic material.
Preferably, the mesoporous yttrium oxide is prepared using following methods:By six trichloride hydrate yttriums and laruyl alcohol sulphur
Sour sodium is dissolved in absolute ethyl alcohol, and the ammonium hydroxide of 0.1M is added, and casting film-forming under conditions of air humidity is 30%~80% is done
Dry, the temperature of heat treatment, the heat treatment is 550~680 DEG C, and the time is 1.5~4h.
The present invention is used six trichloride hydrate yttriums, is helped to drop using the preparation of the mesoporous yttrium oxide of above method machinery
The production cost of suboxides yttrium improves the ratio of mesoporous yttrium oxide, contributes to the function and effect of oxidation reinforced yttrium, to improve pottery
The mechanical performance of porcelain.
Preferably, the carbon dust is handled using following methods:Coke is subjected to ball milling, is sieved after dry to obtain coke
Powder takes coke powder of the grain size between 15 ~ 20 microns.
The reaction of the present invention be happened on the interface of quartz sand and coke, and be by quartz sand wrap coke occur it is anti-
It answers, therefore the granule size of coke directly determines the granule size of silicon carbide, the granularity of coke is smaller in general, the carbon of production
SiClx granularity is smaller, and the granularity of silicon carbide is small therefore STRENGTH ON COKE carries out processing to improve.And ball milling is carried out for coke to make
The standby compactness for producing required carbon dust and contributing to enhancing ceramic, to reinforce the mechanical strength of ceramics.
A kind of preparation method of high-strength carborundum ceramics, which is characterized in that include the following steps:
(1)Raw material is uniformly mixed, raw material slurry is made;
(2)The raw material slurry is vacuum-treated;
(3)After ceramic slurry after vacuum degassing is injected into mold, the mold is sealed, is then heated, temperature
Degree is 50-80 DEG C, keeps the temperature 3 ~ 4h, and natural cooling obtains biscuit of ceramics after then being dried 12-72 hours in baking oven;
(4)The biscuit of ceramics is sintered, time of the sintering processes is 1-5h, sintering temperature is 1500 ~
1800℃。
Present invention employs vacuum conditions to handle raw material slurry, helps to eliminate using this method tiny present in slurry
Bubble, the hole in ceramic structure to reduce the present invention, avoid causes ceramic internal structure to generate since hole is excessive
Fault of construction, to reduce the mechanical strength of ceramics, in addition the present invention first dries mold, can reduce due to sintering
Liquid evaporation in middle slurry leads to occur stomata on ceramics, leads to mechanical strength the case where declining of ceramics.
Preferably, in step(2)Described in the vacuum degree that is vacuum-treated be 20kPa ~ 40kPa;The vacuum processing
Time is 15 ~ 18min.
Present invention employs the vacuum degree of 20 ~ 40kPa, help to reduce the bubble in slurry,
The beneficial effects of the present invention are:(1)The present invention has good toughness,(2)The present invention has higher mechanical strength,
(3)The advantage that the present invention has step simple, at low cost.
Specific implementation mode
The present invention is further explained with reference to specific implementation case:
Embodiment 1
A kind of high-strength carborundum ceramics, which is characterized in that include the component of following parts by weight:
70 parts of sic powder, 10 parts of silicon carbide fibre, 20 parts of binder, 5 parts of pore creating material, 5 parts of sintering aid, 5 parts of dispersant,
2 parts of toughener.
Wherein, a diameter of 0.1 micron of the silicon carbide fibre, length are 20 microns.
Wherein, the binder includes the component of following parts by weight:3 parts of alumina powder, 8 parts of sodium cellulose glycolate,
9 ~ 10 parts of silica.
Wherein, the dispersant includes the component of following parts by weight:2 parts of polyvinyl alcohol, 1 part of oleic acid, polyethylene glycol 1
Part.
Wherein, further include pore creating material in the component, the pore creating material uses carbon dust, the sintering aid to use
The mixing of aluminium oxide and calcium oxide, the toughener use yttrium oxide.
A kind of high-strength carborundum ceramics according to claim 1, it is characterised in that:The yttrium oxide is using Jie
Hole yttrium oxide.
Wherein, the mesoporous yttrium oxide is prepared using following methods:Six trichloride hydrate yttriums and surfactant are molten
In absolute ethyl alcohol, the ammonium hydroxide of 0.1M is added, casting film-forming under conditions of air humidity is 30% is dry, and heat treatment is described
Heat treatment temperature be 550 DEG C, time 1.5h.
Wherein, the carbon dust is handled using following methods:Coke is subjected to ball milling, is sieved after dry to obtain coke blacking
Coke powder of the grain size at 15 microns is taken at end.
A kind of preparation method of high-strength carborundum ceramics, which is characterized in that include the following steps:
(1)Raw material is uniformly mixed, raw material slurry is made;
(2)The raw material slurry is vacuum-treated;
(3)After ceramic slurry after vacuum degassing is injected into mold, the mold is sealed, is then heated, temperature
Degree is 50 DEG C, keeps the temperature 3h, and natural cooling obtains biscuit of ceramics after then being dried 12 hours in baking oven;
(4)The biscuit of ceramics is sintered, the time of the sintering processes is 1h, and sintering temperature is 1500 DEG C.
Wherein, in step(2)Described in the vacuum degree that is vacuum-treated be 20kPa;The time of the vacuum processing is
15min。
Embodiment 2
A kind of high-strength carborundum ceramics, which is characterized in that include the component of following parts by weight:
80 parts of sic powder, 20 parts of silicon carbide fibre, 25 parts of binder, 10 parts of pore creating material, 10 parts of sintering aid, dispersant 10
Part, 3 parts of toughener.
Wherein, 20 microns of the diameter of the silicon carbide fibre, length are 500 microns.
Wherein, the binder includes the component of following parts by weight:5 parts of alumina powder, 10 parts of sodium cellulose glycolate,
0 part of silica 1.
Wherein, the dispersant includes the component of following parts by weight:3 parts of polyvinyl alcohol, 3 parts of oleic acid, polyethylene glycol 2
Part.
Wherein, further include pore creating material in the component, the pore creating material uses carbon dust, the sintering aid to use
The mixing of aluminium oxide and calcium oxide, the toughener use yttrium oxide.
A kind of high-strength carborundum ceramics according to claim 1, it is characterised in that:The yttrium oxide is using Jie
Hole yttrium oxide.
Wherein, the mesoporous yttrium oxide is prepared using following methods:Six trichloride hydrate yttriums and surfactant are molten
In absolute ethyl alcohol, the ammonium hydroxide of 0.1M is added, casting film-forming under conditions of air humidity is 80% is dry, and heat treatment is described
Heat treatment temperature be 680 DEG C, time 4h.
Wherein, the carbon dust is handled using following methods:Coke is subjected to ball milling, is sieved after dry to obtain coke blacking
Coke powder of the grain size at 20 microns is taken at end.
A kind of preparation method of high-strength carborundum ceramics, which is characterized in that include the following steps:
(1)Raw material is uniformly mixed, raw material slurry is made;
(2)The raw material slurry is vacuum-treated;
(3)After ceramic slurry after vacuum degassing is injected into mold, the mold is sealed, is then heated, temperature
Degree is 80 DEG C, keeps the temperature 4h, and natural cooling obtains biscuit of ceramics after then being dried 72 hours in baking oven;
(4)The biscuit of ceramics is sintered, the time of the sintering processes is 5h, and sintering temperature is 1800 DEG C.
Wherein, in step(2)Described in the vacuum degree that is vacuum-treated be 40kPa;The time of the vacuum processing is
18min。
Embodiment 3
A kind of high-strength carborundum ceramics, which is characterized in that include the component of following parts by weight:
75 parts of sic powder, 15 parts of silicon carbide fibre, 25 parts of binder, 7 parts of pore creating material, 8 parts of sintering aid, 8 parts of dispersant,
2 parts of toughener.
Wherein, a diameter of 10 microns of the silicon carbide fibre, length are 270 microns.
Wherein, the binder includes the component of following parts by weight:4 parts of alumina powder, 9 parts of sodium cellulose glycolate,
9 parts of silica.
Wherein, the dispersant includes the component of following parts by weight:3 parts of polyvinyl alcohol, 2 parts of oleic acid, polyethylene glycol 1 ~ 2
Part.
Wherein, further include pore creating material in the component, the pore creating material uses carbon dust, the sintering aid to use
The mixing of aluminium oxide and calcium oxide, the toughener use yttrium oxide.
A kind of high-strength carborundum ceramics according to claim 1, it is characterised in that:The yttrium oxide is using Jie
Hole yttrium oxide.
Wherein, the mesoporous yttrium oxide is prepared using following methods:Six trichloride hydrate yttriums and surfactant are molten
In absolute ethyl alcohol, the ammonium hydroxide of 0.1M is added, casting film-forming under conditions of air humidity is 80% is dry, and heat treatment is described
Heat treatment temperature be 680 DEG C, time 3h.
Wherein, the carbon dust is handled using following methods:Coke is subjected to ball milling, is sieved after dry to obtain coke blacking
Coke powder of the grain size at 19 microns is taken at end.
A kind of preparation method of high-strength carborundum ceramics, which is characterized in that include the following steps:
(1)Raw material is uniformly mixed, raw material slurry is made;
(2)The raw material slurry is vacuum-treated;
(3)After ceramic slurry after vacuum degassing is injected into mold, the mold is sealed, is then heated, temperature
Degree is 50 ~ 80 DEG C, keeps the temperature 3 ~ 4h, and natural cooling obtains biscuit of ceramics after then being dried 36 hours in baking oven;
(4)The biscuit of ceramics is sintered, the time of the sintering processes is 3h, and sintering temperature is 1800 DEG C.
Wherein, in step(2)Described in the vacuum degree that is vacuum-treated be 30kPa;The time of the vacuum processing is
18min。
Embodiment 4
A kind of high-strength carborundum ceramics, which is characterized in that include the component of following parts by weight:
72 parts of sic powder, 12 parts of silicon carbide fibre, 22 parts of binder, 6 parts of pore creating material, 6 parts of sintering aid, 6 parts of dispersant,
2 parts of toughener.
Wherein, a diameter of 2 microns of the silicon carbide fibre, length are 40 microns.
Wherein, the binder includes the component of following parts by weight:3 parts of alumina powder, 8 parts of sodium cellulose glycolate,
9 parts of silica.
Wherein, the dispersant includes the component of following parts by weight:2 parts of polyvinyl alcohol, 1 part of oleic acid, polyethylene glycol 1
Part.
Wherein, further include pore creating material in the component, the pore creating material uses carbon dust, the sintering aid to use
The mixing of aluminium oxide and calcium oxide, the toughener use yttrium oxide.
A kind of high-strength carborundum ceramics according to claim 1, it is characterised in that:The yttrium oxide is using Jie
Hole yttrium oxide.
Wherein, the mesoporous yttrium oxide is prepared using following methods:Six trichloride hydrate yttriums and surfactant are molten
In absolute ethyl alcohol, the ammonium hydroxide of 0.1M is added, casting film-forming under conditions of air humidity is 50% is dry, and heat treatment is described
Heat treatment temperature be 580 DEG C, time 3h.
Wherein, the carbon dust is handled using following methods:Coke is subjected to ball milling, is sieved after dry to obtain coke blacking
Coke powder of the grain size at 18 microns is taken at end.
A kind of preparation method of high-strength carborundum ceramics, which is characterized in that include the following steps:
(1)Raw material is uniformly mixed, raw material slurry is made;
(2)The raw material slurry is vacuum-treated;
(3)After ceramic slurry after vacuum degassing is injected into mold, the mold is sealed, is then heated, temperature
Degree is 60 DEG C, keeps the temperature 3h, and natural cooling obtains biscuit of ceramics after then being dried 25 hours in baking oven;
(4)The biscuit of ceramics is sintered, the time of the sintering processes is 5h, and sintering temperature is 1600 DEG C.
Wherein, in step(2)Described in the vacuum degree that is vacuum-treated be 240kPa;The time of the vacuum processing is
18min。
Embodiment 5
A kind of high-strength carborundum ceramics, which is characterized in that include the component of following parts by weight:
75 parts of sic powder, 15 parts of silicon carbide fibre, 22 parts of binder, 8 parts of pore creating material, 7 parts of sintering aid, 8 parts of dispersant,
2 parts of toughener.
Wherein, a diameter of 10 microns of the silicon carbide fibre, length are 80 microns.
Wherein, the binder includes the component of following parts by weight:4 parts of alumina powder, 9 parts of sodium cellulose glycolate,
9 parts of silica.
Wherein, the dispersant includes the component of following parts by weight:2 parts of polyvinyl alcohol, 2 parts of oleic acid, polyethylene glycol 1
Part.
Wherein, further include pore creating material in the component, the pore creating material uses carbon dust, the sintering aid to use
The mixing of aluminium oxide and calcium oxide, the toughener use yttrium oxide.
A kind of high-strength carborundum ceramics according to claim 1, it is characterised in that:The yttrium oxide is using Jie
Hole yttrium oxide.
Wherein, the mesoporous yttrium oxide is prepared using following methods:Six trichloride hydrate yttriums and surfactant are molten
In absolute ethyl alcohol, the ammonium hydroxide of 0.1M is added, casting film-forming under conditions of air humidity is 80% is dry, and heat treatment is described
Heat treatment temperature be 680 DEG C, time 3h.
Wherein, the carbon dust is handled using following methods:Coke is subjected to ball milling, is sieved after dry to obtain coke blacking
Coke powder of the grain size at 18 microns is taken at end.
A kind of preparation method of high-strength carborundum ceramics, which is characterized in that include the following steps:
(1)Raw material is uniformly mixed, raw material slurry is made;
(2)The raw material slurry is vacuum-treated;
(3)After ceramic slurry after vacuum degassing is injected into mold, the mold is sealed, is then heated, temperature
Degree is 60 DEG C, keeps the temperature 3h, and natural cooling obtains biscuit of ceramics after then being dried 36 hours in baking oven;
(4)The biscuit of ceramics is sintered, the time of the sintering processes is 5h, and sintering temperature is 1800 DEG C.
Wherein, in step(2)Described in the vacuum degree that is vacuum-treated be 40kPa;The time of the vacuum processing is
18min。
Claims (10)
1. a kind of high-strength carborundum ceramics, which is characterized in that include the component of following parts by weight:
70 ~ 80 parts of sic powder, 10 ~ 20 parts of silicon carbide fibre, 20 ~ 25 parts of binder, 5 ~ 10 parts of pore creating material, sintering aid 5 ~
10 parts, 5 ~ 10 parts of dispersant, 2 ~ 3 parts of toughener.
2. a kind of high-strength carborundum ceramics according to claim 1, it is characterised in that:The silicon carbide fibre it is straight
Diameter is 0.1um~20um, and length is 20um~500um.
3. a kind of high-strength carborundum ceramics according to claim 1, which is characterized in that the binder includes following
The component of parts by weight:3 ~ 5 parts of alumina powder, 8 ~ 10 parts of sodium cellulose glycolate, 9 ~ 10 parts of silica.
4. a kind of high-strength carborundum ceramics according to claim 1, which is characterized in that the dispersant includes following
The component of parts by weight:2 ~ 3 parts of polyvinyl alcohol, 1 ~ 3 part of oleic acid, 1 ~ 2 part of polyethylene glycol.
5. a kind of high-strength carborundum ceramics according to claim 1, it is characterised in that:Further include making in the component
Hole agent, the pore creating material use carbon dust, the sintering aid to use the mixing of aluminium oxide and calcium oxide, the toughener
Using yttrium oxide.
6. a kind of high-strength carborundum ceramics according to claim 1, it is characterised in that:The yttrium oxide is using mesoporous
Yttrium oxide.
7. a kind of preparation method of high-strength carborundum ceramics according to claim 6, which is characterized in that described is mesoporous
Yttrium oxide is prepared using following methods:Six trichloride hydrate yttriums and surfactant are dissolved in absolute ethyl alcohol, are added 0.1M's
Ammonium hydroxide, casting film-forming under conditions of air humidity is 30%~80% is dry, heat treatment, and the temperature of the heat treatment is
550~680 DEG C, the time is 1.5~4h.
8. a kind of preparation method of high-strength carborundum ceramics according to claim 5, which is characterized in that the carbon dust
It is handled using following methods:Coke is subjected to ball milling, is sieved after dry to obtain coke powder, take grain size 15 ~ 20 microns it
Between coke powder.
9. a kind of preparation method of high-strength carborundum ceramics according to one of claim 1-8, which is characterized in that including
Following steps:
(1)Raw material is uniformly mixed, raw material slurry is made;
(2)The raw material slurry is vacuum-treated;
(3)After ceramic slurry after vacuum degassing is injected into mold, the mold is sealed, is then heated, temperature
Degree is 50-80 DEG C, keeps the temperature 3 ~ 4h, and natural cooling obtains biscuit of ceramics after then being dried 12-72 hours in baking oven;
(4)The biscuit of ceramics is sintered, time of the sintering processes is 1-5h, sintering temperature is 1500 ~
1800℃。
10. a kind of preparation method of high-strength carborundum ceramics according to claim 9, it is characterised in that:In step(2)
Described in the vacuum degree that is vacuum-treated be 20kPa ~ 40kPa;The time of the vacuum processing is 15 ~ 18min.
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