CN109320250A - A kind of porous B based on agarose macromolecules gel casting forming4C ceramics preparative body - Google Patents
A kind of porous B based on agarose macromolecules gel casting forming4C ceramics preparative body Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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
- C04B35/563—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 boron carbide
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- C—CHEMISTRY; METALLURGY
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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Abstract
The present invention relates to a kind of porous B based on agarose macromolecules gel casting forming4The preparation method of C ceramics preparative body, the preparation method are easy to operate, economic and environment-friendly, the special-shaped porous B of near-net-shape of one kind4The preparation method of C ceramics preparative body.The preparation method specifically: addition accounts for B in ceramic slurry4The agarose macromolecules of C powder mass percent 0.5~5%, then cured molding, demoulding, sintering are to get porous B4C ceramics preparative body.Using porous B made from preparation method of the present invention4C ceramics preparative body, intensity is enough, and through-hole aperture can guarantee the complete infiltration of metal；Suitable for preparing B4C/ metallic composite.
Description
Technical field
The invention belongs to porous ceramic film material fields, and in particular to a kind of based on agarose macromolecules gel casting forming
Porous B4C ceramics preparative body.
Background technique
B4C has low-density, ultrahigh hardness, wear-resisting, high temperature resistant, good as a kind of very important ceramic material
Chemical stability and neutron absorption capability and be widely used in bulletproof armour, high-temperature and wear-proof, reactor control and shielding
Material.However, B4C one-component ceramic toughness is insufficient, significantly limits B4The application development of C ceramics.B4C/ metallic composite is
Improve B4The insufficient effective way of C one-component ceramic toughness, wherein with B4The research of C/ aluminium composite material is more, and industrial applications are most
It is mature.
B4The common preparation method of C/ metallic composite has powder metallurgic method, stir-mixing method, method of impregnation etc..Powder smelting
Golden method complex process, at high cost, B4C is unevenly distributed；Stir-mixing method unavoidably has in stirring and casting process to be mingled with
And the problems such as being also easy to produce segregation.In recent years, method of impregnation is to prepare B with complex shape4C/ metallic composite provides
New approaches.Method of impregnation prepares B4C/ metallic composite is first by B4C is prepared into porous preform, then again arrives metal infiltration
Porous B4In C.
Porous B4C moulding process mainly has pore creating material method, foam impregnation method, injection forming etc..Gel-casting method
Simply, the advantages such as easily prepared shaped piece and near-net-shape are a kind of promising methods for preparing porous ceramics.?
B4In terms of C precast body, Chinese patent CN105483487A discloses one kind by porous B4The B of C matrix and zirconium alloy composition4C-
Al alloy composite, the invention prepare porous B using powder sintering method4C matrix, then by the molten infiltration of the zirconium alloy of melting
Into porous B4B is made in C matrix4C- Al alloy composite.Chinese patent CN106830942A discloses a kind of porous B4C pottery
Porcelain body frame and its freezing molding process, using method of impregnation in porous B4Al is penetrated into C ceramic skeleton prepares B4C/Al composite material.
For this method using water as freezing injection molding solvent, B is added in precentagewise4C adds suitable dispersing agent and binder, freezing, liter
B is obtained after China4C ceramic body can obtain the porous B for infiltration after sintering4C ceramic skeleton.Porous B in the invention4C ceramics
Skeleton has higher-strength, good through-hole structure, preparation process simple.Chinese patent CN1044110C is disclosed by that will melt
Molten aluminum or aluminium alloy are percolated to porous B4B is prepared in C precast body4C- constructed of aluminium composite material.In this material preparation process
In, porous B is prepared first4C precast body.The B of preparation4C- constructed of aluminium composite material can be resisted to be exposed to for a long time to be melted higher than aluminium
The temperature of point is without reducing physical property.
Summary of the invention
In order to overcome B4The insufficient defect of C one-component ceramic toughness, it is solidifying based on agarose macromolecules that the present invention provides one kind
The porous B of glue casting4The preparation method of C ceramics preparative body prepares B with complex shape for method of impregnation4C/ metal composite
Material provides new approaches.Using porous B made from preparation method of the present invention4C ceramics preparative body, intensity is enough, and logical
Hole aperture can guarantee the complete infiltration of metal.
The preparation method specifically: addition accounts for B in ceramic slurry4The agarose of C powder mass percent 0.5~5%
Macromolecular, then cured molding, demoulding, sintering are to get porous B4C ceramics preparative body.
The agarose macromolecules system that the present invention uses compared with the prior art, has nontoxic, environmentally friendly, green compact not
Easy to crack, content of organics is not necessarily to the advantages that dumping less.
The present invention is in order to obtain the porous B haveing excellent performance4C ceramics preparative body, the further preferred preparation method
Technique；Wherein, the present invention is different according to solid content in ceramic slurry, carries out ingredient to each raw material, through ball milling, heating plus agar
Sugared macromolecular, the molding of injection molding in-situ solidifying, dry demoulding, high temperature sintering, finally obtain porous B4C ceramics preparative body.
Present invention further propose that, the ceramic slurry takes water as a solvent, the ratio for being 40%~60% in solid content
Add B4C powder；
Preferably, the B4The partial size of C powder is 1~2 μm.
Water of the present invention is the water for being applicable to configuration ceramic slurry, such as deionized water.
Present invention further propose that, it further include dispersing agent in the ceramic slurry；The dispersing agent is the B4C silty
The 0.1~0.3% of amount；
Preferably, the dispersing agent is a kind of in polyacrylic acid, polyvinyl alcohol, ammonium citrate, tetramethylammonium hydroxide
Or it is a variety of, more preferably use polyacrylic acid.
Present invention further propose that, the pH value of the ceramic slurry is 7~8；
Preferably, the pH value is adjusted using ammonium hydroxide.
Present invention further propose that, after the abundant ball milling of the ceramic slurry, 50~70 DEG C are heated to, is then added
Add and accounts for B4The agarose macromolecules of C powder mass percent 0.8~1.5% after mixing evenly, then carry out froth in vacuum processing；
Preferably, the ball milling specifically: with the revolving speed of 150~200r/min, 20~30h of ball milling.Using ball milling operation
On the one hand it can make raw material mixing more uniformly, and it is made to obtain good fluidity, the better ceramic slurry of stable homogeneous.
Present invention further propose that, the demoulding specifically: it is 90 that the ceramic slurry after curing molding, which is placed in humidity,
2~3 days in~95% environment；Again in room temperature environment, spontaneously dry 15~20 days；Then being placed in temperature again is 80~100
DEG C environment in dry 24~48 hours, obtain green compact.
Present invention further propose that, the sintering specifically: the green compact after demoulding are placed in vacuum drying oven and are carried out without pressure
Sintering, the temperature of the sintering are 2000~2500 DEG C, and the time is 0.8~1.5h；
Preferably, the temperature of the sintering is 2300 DEG C, time 1h.
The present invention provides a kind of preferred embodiment, and the preparation method includes the following steps:
1) by B4C powder and account for the B4The polyacrylic acid of C silty amount 0.1~0.3% is added to the water, and adjusting pH value to 7~
8；Then it is placed in revolving speed again as under conditions of 150~200r/min, 20~30h of ball milling obtains ceramic slurry；
Wherein, the B4C powder is added in water in the ratio that solid content is 40%~60%；
2) ceramic slurry is heated to 50~70 DEG C, then addition accounts for B4C powder mass percent 0.8~1.5%
Agarose macromolecules after mixing evenly, then carry out froth in vacuum processing；
3) by step 2) froth in vacuum, treated that ceramic slurry is poured into mold, declines with temperature, the ceramic slurry
Expect in-situ solidifying molding；
4) ceramic slurry after step 3) curing molding is placed in the environment that humidity is 90~95% 2~3 days；Again in room
In warm environment, spontaneously dry 15~20 days；Then it is placed in drying 24~48 hours in the environment that temperature is 80~100 DEG C again, obtains
Obtain green compact；
5) green compact being placed in vacuum drying oven and carries out pressureless sintering, the temperature of the sintering is 2000~2500 DEG C, when
Between be 0.8~1.5h.
The present invention is using porous B made from above-mentioned preparation method4C ceramics preparative body.Overcome B4C one-component ceramic toughness is insufficient
Defect.Porous B obtained4C ceramics preparative body has intensity height, near-net-shape, good through-hole structure, Ke Yibao
Demonstrate,prove the porous B of metal infiltrated completely4C ceramics preparative body.Also, agarose is as environment amenable macromolecular system, system
Content of organics is seldom in standby green compact, without dumping before sintering.
It is a further object of the present invention to provide a kind of B4C/ metallic composite, using above-mentioned porous B4C ceramics preparative
Body is as ceramics preparative body；
Preferably, the B4C/ metallic composite is made by such as under type, using method of impregnation, by metal infiltration to described
Porous B4In C ceramics preparative body.
Detailed description of the invention
Fig. 1 is porous B prepared by the present invention4The process flow chart of C ceramics preparative body；
Fig. 2 is porous B made from embodiment 14The XRD diagram of C ceramics preparative body；
Fig. 3 is porous B made from embodiment 14The fracture SEM picture of C ceramics preparative body；
Fig. 4 is porous B made from embodiment 14The fracture SEM picture of C ceramics preparative body；
Fig. 5 is the porous B that embodiment 7 is dried at room temperature for cracking4C ceramic green picture；
Fig. 6 (a), (b) are respectively porous B made from embodiment 2~34The fracture SEM picture of C ceramics preparative body.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
The present embodiment provides a kind of porous B based on agarose macromolecules gel casting forming4The preparation of C ceramics preparative body
Method, as shown in Figure 1, including the following steps:
1) 0.03g dispersing agent polyacrylic acid is added in 24.4ml deionized water, stirs to being completely dissolved, adds
20gB4C (solid content 45%), being uniformly mixed makes to be formed suspension, then adds ammonium hydroxide and adjusts pH value to 7~8；So
It is placed in revolving speed again afterwards as under conditions of 200r/min, ball milling for 24 hours, obtains the ceramic slurry of good fluidity；
2) ceramic slurry is heated to 60 DEG C, then adds the agarose macromolecules of 0.2g, after mixing evenly, then into
The processing of row froth in vacuum；
3) by the polytetrafluoroethylene (PTFE) mould of step 2) froth in vacuum treated ceramic slurry is poured into inner wall coating lubricant
In tool, decline with temperature, the ceramic slurry in-situ solidifying molding；
4) ceramic slurry after step 3) curing molding is placed in the environment that humidity is 90~95% 2~3 days；Again in room
In warm environment, spontaneously dry 15~20 days；Then it is placed in drying 24~48 hours in environment at a temperature of 90 °C again, is given birth to
Base；
5) green compact are placed in vacuum drying oven and carry out pressureless sintering, the temperature of the sintering is 2300 DEG C, time 1h.
Porous B obtained described in the present embodiment4C ceramics preparative body: Fig. 2 is XRD diagram, the results showed that, prepare ceramic material
Principal crystalline phase be B4C, B4C ceramics fracture SEM photo are as shown in Figure 3 and Figure 4, the results showed that, B4C ceramic micro-structure mesoporous is big
It is small uniform, apparent porosity 61%, B4There is sintering neck to be formed between C ceramic particle.
Embodiment 2~3
The present embodiment provides a kind of porous B based on agarose macromolecules gel casting forming4The preparation of C ceramics preparative body
Method, the difference from embodiment 1 is that:
1, " 24.4ml deionized water " is replaced with into " 30ml deionized water " and " 20ml deionized water " respectively；
The solid content of obtained ceramic slurry is respectively 40% and 50%；
2, step 2) is handled without froth in vacuum, specifically: 2) ceramic slurry is heated to 60 DEG C, then added
The agarose macromolecules of 0.2g, stir evenly；
Porous B obtained described in the present embodiment4C ceramics preparative body: (a) in Fig. 6, (b) are respectively the XRD of embodiment 2-3
Figure, the results showed that, B4C ceramic micro-structure mesopore size is uniform.Precast body apparent porosity is respectively 72%, 55%, B4C ceramics
There is sintering neck to be formed between particle.
Embodiment 4
The present embodiment provides a kind of porous B based on agarose macromolecules gel casting forming4The preparation of C ceramics preparative body
Method, the difference with embodiment 1 are only that:
Agglutinant yttrium oxide and aluminium oxide are added in step 1) (yttrium oxide: alumina weight ratio is 1:1), wherein sintering
Agent total amount is the 5% of solid content, and appropriate ammonium hydroxide adjusts slurry pH value to 8~10；
Specifically: 0.03g dispersing agent polyacrylic acid is added in 24.4ml deionized water, stirring to being completely dissolved, then plus
Enter 20gB4C, being uniformly mixed makes to be formed suspension, and then adding 1g agglutinant, (weight ratio is the yttrium oxide of 1:1: oxidation
Aluminium is), it then adds ammonium hydroxide and adjusts pH value to 8~10；Then be placed in again revolving speed be 150-200r/min under conditions of, ball milling
For 24 hours, the ceramic slurry of good fluidity, the B of preparation are obtained4The apparent porosity of C ceramics preparative body is 50%.
Embodiment 5
The present embodiment provides a kind of porous B based on agarose macromolecules gel casting forming4The preparation of C ceramics preparative body
Method, the difference with embodiment 1 are only that:
5) green compact are placed in vacuum drying oven and carry out pressureless sintering, the temperature of the sintering is 2200 DEG C, time 1h.
Embodiment 6
The present embodiment provides a kind of porous B based on agarose macromolecules gel casting forming4The preparation of C ceramics preparative body
Method, the difference with embodiment 1 are only that:
Step 4) specifically: by the ceramic slurry after step 3) curing molding in room temperature environment, spontaneously dry 15~20
It；Then dry 24~48 hour, acquisition green compact are placed in environment at a temperature of 90 °C again；
As shown in figure 5, green compact cracking occurs in convection drying at room temperature, it is complete to illustrate that rate of drying is unfavorable for very much obtaining fastly
Green compact.
Experimental example 1
By porous B obtained by embodiment 14C ceramics preparative body carries out apparent porosity test, chooses 5 samples, such as the following table 1
And shown in Fig. 3, B in embodiment 14C ceramic micro-structure mesopore size is uniform, apparent porosity 60-62%.
Table 1
| Sample | S1 | S2 | S3 | S4 | S5 |
| Apparent porosity | 60 | 61.5 | 62 | 61 | 62 |
It follows that B obtained by embodiment 14C/ metallic composite has higher through-hole rate, it is ensured that metal is complete
The porous B of infiltration4C ceramics preparative body.
Although above having used general explanation, specific embodiment and test, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (10)
1. a kind of porous B based on agarose macromolecules gel casting forming4The preparation method of C ceramics preparative body, feature exist
In addition accounts for B in ceramic slurry4The agarose macromolecules of C powder mass percent 0.5~5%, then it is cured molding, demoulding,
Sintering is to get porous B4C ceramics preparative body.
2. preparation method according to claim 1, which is characterized in that the ceramic slurry takes water as a solvent, by solid content
B is added for 40%~60% ratio4C powder；
Preferably, the B4The partial size of C powder is 1~2 μm.
3. preparation method according to claim 1 or 2, which is characterized in that further include dispersing agent in the ceramic slurry；Institute
Stating dispersing agent is the B4The 0.1~0.3% of C silty amount；
Preferably, the dispersing agent is a kind of or more in polyacrylic acid, polyvinyl alcohol, ammonium citrate, tetramethylammonium hydroxide
Kind.
4. described in any item preparation methods according to claim 1~3, which is characterized in that the pH value of the ceramic slurry be 7~
8；
Preferably, the pH value is adjusted using ammonium hydroxide.
5. preparation method according to any one of claims 1 to 4, which is characterized in that by the abundant ball milling of the ceramic slurry
After uniformly, 50~70 DEG C are heated to, then addition accounts for B4The agarose macromolecules of C powder mass percent 0.8~1.5%, stirring
After uniformly, then carry out froth in vacuum processing；
Preferably, the ball milling specifically: with the revolving speed of 150~200r/min, 20~30h of ball milling.
6. described in any item preparation methods according to claim 1~5, which is characterized in that the demoulding specifically: will be solidified into
Ceramic slurry after type is placed in the environment that humidity is 90~95% 2~3 days；Again in room temperature environment, 15~20 are spontaneously dried
It；Then it is placed in 24~48 hours dry in the environment that temperature is 80~100 DEG C, acquisition green compact again.
7. described in any item preparation methods according to claim 1~6, which is characterized in that the sintering specifically: after demoulding
Green compact be placed in vacuum drying oven and carry out pressureless sintering, the temperature of the sintering is 2000~2500 DEG C, and the time is 0.8~1.5h；
Preferably, the temperature of the sintering is 2300 DEG C, time 1h.
8. described in any item preparation methods according to claim 1~7, which comprises the steps of:
1) by B4C powder and account for the B4The polyacrylic acid of C silty amount 0.1~0.3% is added to the water, and adjusts pH value to 7~8；So
It is placed in revolving speed again afterwards as under conditions of 150~200r/min, 20~30h of ball milling obtains ceramic slurry；
Wherein, the B4C powder is added in water in the ratio that solid content is 40%~60%；
2) ceramic slurry is heated to 50~70 DEG C, then addition accounts for B4The agarose of C powder mass percent 0.8~1.5%
Macromolecular after mixing evenly, then carries out froth in vacuum processing；
3) by step 2) froth in vacuum, treated that ceramic slurry is poured into mold, declines with temperature, and the ceramic slurry is former
Position curing molding；
4) ceramic slurry after step 3) curing molding is placed in the environment that humidity is 90~95% 2~3 days；Again in room temperature ring
In border, spontaneously dry 15~20 days；Then it is placed in drying 24~48 hours in the environment that temperature is 80~100 DEG C again, is given birth to
Base；
5) green compact are placed in vacuum drying oven and carry out pressureless sintering, the temperature of the sintering is 2000~2500 DEG C, and the time is
0.8~1.5h.
9. porous B made from any one of claim 1~8 preparation method4C ceramics preparative body.
10. a kind of B4C/ metallic composite, which is characterized in that with porous B as claimed in claim 94C ceramics preparative body is pottery
Porcelain precast body；
Preferably, the B4C/ metallic composite is made by such as under type, using method of impregnation, by metal infiltration to described porous
B4In C ceramics preparative body.
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| CN111960850A (en) * | 2020-08-10 | 2020-11-20 | 宁波普莱斯帝金属制品有限公司 | Preparation method and application of boron carbide composite material |
| CN114262236A (en) * | 2021-12-16 | 2022-04-01 | 江苏领瑞新材料科技有限公司 | Ceramic composite material |
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