CN108947536A - A kind of high-densit B-Ti-C system ceramics of strong ultrasonic wave added method preparation even tissue - Google Patents

A kind of high-densit B-Ti-C system ceramics of strong ultrasonic wave added method preparation even tissue Download PDF

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Publication number
CN108947536A
CN108947536A CN201810741507.0A CN201810741507A CN108947536A CN 108947536 A CN108947536 A CN 108947536A CN 201810741507 A CN201810741507 A CN 201810741507A CN 108947536 A CN108947536 A CN 108947536A
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ceramics
densit
ultrasonic wave
even tissue
wave added
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CN201810741507.0A
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黎军军
刘碧桃
阮海波
关有为
闫恒庆
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Chongqing University of Arts and Sciences
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Chongqing University of Arts and Sciences
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped 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
    • C04B35/56Shaped 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
    • C04B35/563Shaped 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40Metallic constituents or additives not added as binding phase
    • C04B2235/404Refractory metals
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/608Green bodies or pre-forms with well-defined density

Abstract

The invention discloses a kind of high-densit B-Ti-C system ceramics of strong ultrasonic wave added method preparation even tissue, consistency is 91.3 ± 0.3%, the ceramics main preparation methods be 50nm by partial size, it is 50nm, the B of purity >=99.7% that partial size, which is added, in the Ti powder of purity >=99.99%4(B in C powder4C:Ti=95:5, wt%) pass through dry granulating machine, the fluffy particle of 15-20um or so size is made.The fluffy ITO particle by granulation is loaded in a mold again and is placed in calm pressure, the pressure of hydraulic press is adjusted, mould inside pressure is respectively set to 400MPa, 600MPa, 800MPa, 1000MPa, 1200MPa and 1500MPa.Introduce the biscuit sample that molding consistency under power P=3Kw ultrasonic vibration is up to 53.4 ± 0.2%.Finally, 2100 DEG C at a temperature of be sintered 2.5h, that is, prepare the ceramics.The B-Ti-C system ceramics that this method is prepared, microstructure is uniform, crystal grain is tiny, improves the use value of ceramics.

Description

A kind of high-densit B-Ti-C system ceramics of strong ultrasonic wave added method preparation even tissue
Technical field
The present invention designs a kind of preparation method of ceramics, and in particular to the high-densit B-Ti-C system ceramics of even tissue Preparation method.
Background technique
Special ceramic material is due to having high intensity, high hardness and corrosion resistance, wear-resistant, chemical stability and bio-compatible Property well equal excellent properties, obtain more and more answer in fields such as the energy, aviation, machinery, chemical industry, electronics, semiconductor, medicine With.When due to being equipped with complexity, production there are technique with traditional complex-shaped accurate special cermacis of ceramic process manufacture Between it is long, cost of manufacture is high the problems such as, preparing special cermacis by traditional ceramic process can not keep up with now to special type Ceramic product growing research and development and use demand.Especially for high-densit ceramics, the high, chemical stability with hardness Well, the advantages that high-temperature behavior is excellent, but these advantages give the molding of high-densit ceramic member and processing to bring very big be stranded simultaneously It disturbs, especially complex-shaped high-densit ceramic shaped piece, it usually needs it is formed using complicated mold, and complicated mold Production cost and period is increased, the small lot production or experimental production of high-densit ceramic member are unsuitable for.Although international at present On developed various new shaping method of ceramics, such as injection, curtain coating, gel injection-moulding, Direct Coagulation Casting etc., but nothing By being these novel methods or the methods of traditional slip casting, dry-pressing formed, mold can not be all got rid of to the system of ceramics manufacture About.In addition, for high-densit ceramic member, in addition to the blank forming the problem of other than, the drying process in traditional ceramic preparation process Green body can be made to generate biggish deformation quantity, the ceramic shaped piece of complex-shaped precision can not be produced, binder removal is also unable to satisfy Fire the requirement of high-densit ceramics.
On the other hand it is to improve boron carbide that boron carbide is made to complex phase ceramic together with transition metal boride such as titanium boride One important method of performance.Boron carbide and titanium carbide powder generally use hot-pressing sintering method can get relative density 95% with On ceramic material, the purer boron carbide of hardness toughness of composite diphase material is improved to some extent.Japan Patent JP60/235764 B is obtained by pressureless sintering at 2200 DEG C4C-TiB2Ceramics, density reach 95%, but since sintering temperature is higher, material Crystal grain is grown up obviously, and performance is by a degree of influence.
United States Patent (USP) US5,720,910 proposes to use boron carbide powder and TiO2Powder is raw material, can be at a lower temperature Prepare B4C-TiB2Ceramics.However when using this ingredient, TiB2It is all converted into, is had during the sintering process a large amount of by TiO2 Gas is released, and greatly, sample is easy to that cracking and deformation occurs the weightless big, contraction of biscuit.
In addition application No. is 201210267777.5 Chinese invention patents to disclose one kind using chromium carbide as sintering aid Using its generate liquid phase chromium boride when boron carbide sintering densification, although oxygen can also be increased by also broadly mentioning in system Change titanium, chromium oxide as sintering aid does not provide substantive embodiment, titanium oxide therein, chromium oxide act on not It is clear.
In view of above-mentioned situation, the quick mould-free forming technology of research and extension carrys out the ceramic industry that China is more backward as early as possible It is imperative to say.Strong ultrasonic wave added the preparation method used in the present invention, preparation condition do not need more complex equipment simply, while It is higher to joined the ceramic dense degree that Ti is prepared in B-C system, the fields such as aviation, chemical machinery can be widely used in.
Summary of the invention
The purpose of the present invention is to provide a kind of high-densit B-Ti-C system potteries of strong ultrasonic wave added method preparation even tissue Porcelain, to solve the ceramic shaped piece that can not produce complex-shaped precision currently on the market that above-mentioned background technique proposes, dumping work Skill is also unable to satisfy the problem for firing high-densit ceramics.
To achieve the above object, the invention provides the following technical scheme: a kind of strong ultrasonic wave added method prepares even tissue The high-densit ceramics of B-Ti-C system, it is characterised in that preparation step is as follows:
(1) B is added in Ti powder4Pass through dry granulating machine in C powder, particle is made;(2) it will make pellet and be filled in mold And it is placed in calm pressure, the pressure of hydraulic press is adjusted, setting mould inside pressure is prepared into particle under ultrasonic vibration Biscuit sample;(3) ceramics are made in sintering biscuit sample.
A kind of high-densit ceramics of B-Ti-C system of the preferably described strong ultrasonic wave added method preparation even tissue, feature Be: the ceramic dense degree is 99.7 ± 0.2%.
A kind of high-densit ceramics of B-Ti-C system of the preferably described strong ultrasonic wave added method preparation even tissue, feature Be: Ti powder, B4C powder diameter in the preparation step (1) are 50nm, purity >=99.99%, ratio B4C:Ti= 95:5, wt%.
A kind of high-densit ceramics of B-Ti-C system of the preferably described strong ultrasonic wave added method preparation even tissue, feature Be: particle diameter described in the preparation step (2) is 15-20um.
A kind of high-densit ceramics of B-Ti-C system of the preferably described strong ultrasonic wave added method preparation even tissue, feature Be: in the preparation step (2) mould inside pressure be respectively set to 150MPa, 300MPa, 450MPa, 600MPa, 750MPa and 900MPa, ultrasonic power 3Kw.
A kind of high-densit ceramic device of the preferably described strong ultrasonic wave added preparation even tissue, it is characterised in that: institute Stating the consistency of biscuit sample described in preparation step is 53.4 ± 0.2%, and the temperature of sintering biscuit sample is the sintering at 2100 DEG C Time is 2.5h.
Compared with prior art, the beneficial effects of the present invention are: the high-densit pottery of the strong ultrasonic wave added preparation even tissue Porcelain will not generate biggish deformation, and consistency is preferable.
Detailed description of the invention
Fig. 1: the calm pressure of difference introduces strong ultrasonic vibration to the molding influence of B-Ti-C system biscuit of ceramics.
Fig. 2: the B-Ti-C system ceramic dense of different time sintering is write music line.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
A kind of preparation method of B-Ti-C system ceramic material, it is characterised in that: by partial size ≈ 50nm, purity >= Partial size ≈ 50nm is added in 99.99% Ti powder, and (B4C:Ti=95:5, wt%) passes through dry method in the B4C powder of purity >=99.7% The fluffy particle of 15-20um or so size is made in granulator.The fluffy ITO particle by granulation is loaded in a mold simultaneously again It is placed in calm pressure.Adjust hydraulic press pressure, by mould inside pressure be respectively set to 400MPa, 600MPa, 800MPa, 1000MPa, 1200MPa and 1500MPa.It introduces molding consistency under power P=3Kw ultrasonic vibration and is up to 53.4 ± 0.2% Biscuit sample.Finally, 2100 DEG C at a temperature of be sintered 2.5h.The preparation method of the present invention consistency obtained that obtains is 91.3 ± 0.3%, the B-Ti-C system ceramics that microstructure is uniform, crystal grain is tiny.Fig. 1 introduces the calm pressure of ultrasonic vibration difference, right The molding effect curves of B-Ti-C system biscuit of ceramics, as shown in Figure 1, as the consistency of the raising biscuit of pressure also gradually mentions Height, but increase trend and gradually weaken.It introduces after strong ultrasonic vibration under identical pressure, the consistency of biscuit significantly improves, and works as pressure When reaching 1000MPa by force, consistency is 53.4 ± 0.2%, continues to increase with pressure, the consistency rate of biscuit is very slow Slowly, thus pressure be 1000MPa be this method optimal pressure conditions.
Influence of the different time to B-Ti-C system ceramic post sintering: to the calm pressure of P=1000MPa, if introduce P= The B-Ti-C system biscuit of ceramics of 3Kw ultrasonic vibration production is sintered B-Ti-C after 1h, 1.5h, 2h and 2.5h respectively at 2100 DEG C As shown in Fig. 2, being introduced into ultrasonic wave added molding biscuit sample in 2100 DEG C of high temperature, sintering 2.5h is obtained the consistency of system ceramics Highest consistency is obtained, reaches 91.3 ± 0.3%.

Claims (6)

1. a kind of high-densit ceramics of B-Ti-C system of strong ultrasonic wave added method preparation even tissue, it is characterised in that preparation step is such as Under:
(1) B is added in Ti powder4Pass through dry granulating machine in C powder, particle is made;(2) it will make pellet and be filled in mold and put It is placed in calm pressure, adjusts the pressure of hydraulic press, setting mould inside pressure makes particle be prepared into biscuit under ultrasonic vibration Sample;(3) ceramics are made in sintering biscuit sample.
2. a kind of high-densit ceramics of B-Ti-C system of strong ultrasonic wave added method preparation even tissue according to claim 1, It is characterized by: the ceramic dense degree is 99.7 ± 0.2%.
3. a kind of high-densit ceramics of B-Ti-C system of strong ultrasonic wave added method preparation even tissue according to claim 1, It is characterized by: Ti powder, B in the preparation step (1)4C powder diameter is 50nm, purity >=99.99%, ratio B4C: Ti=95:5, wt%.
4. a kind of high-densit ceramics of B-Ti-C system of strong ultrasonic wave added method preparation even tissue according to claim 1, It is characterized by: particle diameter described in the preparation step (2) is 15-20um.
5. a kind of high-densit ceramics of B-Ti-C system of strong ultrasonic wave added method preparation even tissue according to claim 1, It is characterized by: in the preparation step (2) mould inside pressure be respectively set to 150MPa, 300MPa, 450MPa, 600MPa, 750MPa and 900MPa, ultrasonic power 3Kw.
6. a kind of high-densit ceramic device of strong ultrasonic wave added preparation even tissue according to claim 1, feature exist In: biscuit sample consistency described in the preparation step is 53.4 ± 0.2%, and the temperature of sintering biscuit sample is 2100 DEG C, sintering time 2.5h.
CN201810741507.0A 2018-07-05 2018-07-05 A kind of high-densit B-Ti-C system ceramics of strong ultrasonic wave added method preparation even tissue Pending CN108947536A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112301252A (en) * 2020-09-16 2021-02-02 河南科技大学 Preparation method of nano copper-based composite material

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Application publication date: 20181207