CN105523764A - Boron carbide composite material preparation method - Google Patents

Boron carbide composite material preparation method Download PDF

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Publication number
CN105523764A
CN105523764A CN201510992079.5A CN201510992079A CN105523764A CN 105523764 A CN105523764 A CN 105523764A CN 201510992079 A CN201510992079 A CN 201510992079A CN 105523764 A CN105523764 A CN 105523764A
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China
Prior art keywords
boron carbide
composite material
carbide composite
skeleton
norbide
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Pending
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CN201510992079.5A
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Chinese (zh)
Inventor
黄宗波
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Chongqing Lehu Technology Co Ltd
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Chongqing Lehu Technology Co Ltd
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Priority to CN201510992079.5A priority Critical patent/CN105523764A/en
Publication of CN105523764A publication Critical patent/CN105523764A/en
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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
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B2235/402Aluminium
    • 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
    • C04B2235/602Making the green bodies or pre-forms by moulding

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Products (AREA)

Abstract

The invention relates to a boron carbide composite material preparation method. The method comprises the following steps: preprocessing boron carbide powder; carrying out compression molding on the preprocessed boron carbide powder; pre-burning a boron carbide skeleton; carrying out pressureless infiltration treatment on the pre-burnt boron carbide skeleton and an infiltration metal; and carrying out heat treatment on a pressureless infiltered boron carbide composite material initial blank to obtain a highly pure boron carbide composite material. The method has the advantages of simplicity, low cost and low energy consumption, and the boron carbide composite material prepared in the invention has the advantages of large size, near net shape and large hardness.

Description

A kind of boron carbide composite material preparation method
Technical field
The present invention relates to a kind of composite material and preparation method thereof, particularly relate to a kind of boron carbide composite material preparation method.
Background technology
Norbide (B4C) has excellent over-all properties: high rigidity (being only second to diamond and cubic boron nitride), high-melting-point (24506 DEG C), low density (2.52g/cm3) and efficiently neutron absorption capability, these performances become the control material in the most rising high-temperature and wear-proof and nuclear reaction engineering.In addition, compared with traditional bulletproof ceramic Al2O3, SiC etc., the density of norbide is minimum, and protecting factor is the highest, therefore, also has great development space in military armor field.Preparing the more ripe technique of high-compactness norbide is hot pressing sintering method.Sintering temperature is generally more than 2000 DEG C, and need add extra pressure while sintering, production efficiency is lower, and cost is very high, is not suitable for scale operation.In addition, the fragility that single norbide is intrinsic also seriously restricts its application model week.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of method is simple, low cost, energy consumption are low, and prepared boron carbide composite material has maximizations, closely end form, boron carbide composite material preparation method that hardness is large.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of boron carbide composite material preparation method, is characterized in that, comprise the steps:
The pre-treatment of boron carbide powder;
By pretreated boron carbide powder compression molding;
The pre-burning of norbide skeleton;
Norbide skeleton after pre-burning and infiltration metal are carried out pressure-free impregnation process;
The first base of boron carbide composite material through pressure-free impregnation is heat-treated, obtains highly purified boron carbide composite material.
On the basis of technique scheme, the present invention can also do following improvement.
Further, being implemented as follows of pre-treatment step of described boron carbide powder:
Select the boron carbide powder Homogeneous phase mixing of different-grain diameter size; Hydrochloric acid with 30% carries out pickling to boron carbide powder under the condition of heated and boiled; Boron carbide powder is sintered in 1500 ~ 1600 DEG C at vacuum state; Boron carbide powder is carried out the process of good wettability metal coating.
Further, being implemented as follows of burn in step of described norbide skeleton:
Sinter under nitrogen atmosphere, 1400 ~ 1800 DEG C of conditions, and be incubated 1 ~ 3h.
Further, described by the norbide skeleton after pre-burning with infiltration metal carry out being implemented as follows of pressure-free impregnation treatment step:
First resistance furnace will vacuumize, then applying argon gas protection; The alumina crucible that norbide skeleton and infiltration metal are housed is placed in atmospheric resistance furnace, is rapidly heated to 800 ~ 1200 DEG C and is incubated 10 ~ 30min.And in aluminium powder, add a small amount of Calcium Fluoride (Fluorspan).
Further, described by the boron carbide composite material through pressure-free impregnation just base heat-treat, obtain being implemented as follows of highly purified boron carbide composite material step:
By the boron carbide composite material after infiltration just base in air furnace, be heated to 800 ~ 950 DEG C, and be incubated 10 ~ 75h and obtain highly purified boron carbide composite material.
The invention has the beneficial effects as follows: method is simple, low cost, energy consumption are low, prepared boron carbide composite material has maximization, closely end form, hardness is large.
Accompanying drawing explanation
Fig. 1 is a kind of boron carbide composite material preparation method of the present invention schematic flow sheet.
Embodiment
Be described principle of the present invention and feature below in conjunction with accompanying drawing, example, only for explaining the present invention, is not intended to limit scope of the present invention.
As shown in Figure 1, a kind of boron carbide composite material preparation method, is characterized in that, comprise the steps:
The pre-treatment of boron carbide powder;
By pretreated boron carbide powder compression molding;
The pre-burning of norbide skeleton;
Norbide skeleton after pre-burning and infiltration metal are carried out pressure-free impregnation process;
The first base of boron carbide composite material through pressure-free impregnation is heat-treated, obtains highly purified boron carbide composite material.
Embodiment 1:
Select the boron carbide powder Homogeneous phase mixing of different-grain diameter size; Hydrochloric acid with 30% carries out pickling to boron carbide powder under the condition of heated and boiled; Boron carbide powder is sintered in 1500 DEG C at vacuum state; Boron carbide powder is carried out the process of good wettability metal coating; By pretreated boron carbide powder compression molding; Sinter under nitrogen atmosphere, 1400 DEG C of conditions, and be incubated 1h; First resistance furnace will vacuumize, then applying argon gas protection; The alumina crucible that norbide skeleton and infiltration metal are housed is placed in atmospheric resistance furnace, is rapidly heated to 800 DEG C and is incubated 10min.And in aluminium powder, add a small amount of Calcium Fluoride (Fluorspan); By the boron carbide composite material after infiltration just base in air furnace, be heated to 800 DEG C, and be incubated 10h and obtain highly purified boron carbide composite material.
Embodiment 2:
Select the boron carbide powder Homogeneous phase mixing of different-grain diameter size; Hydrochloric acid with 30% carries out pickling to boron carbide powder under the condition of heated and boiled; Boron carbide powder is sintered in 1550 DEG C at vacuum state; Boron carbide powder is carried out the process of good wettability metal coating; By pretreated boron carbide powder compression molding; Sinter under nitrogen atmosphere, 1500 DEG C of conditions, and be incubated 2h; First resistance furnace will vacuumize, then applying argon gas protection; The alumina crucible that norbide skeleton and infiltration metal are housed is placed in atmospheric resistance furnace, is rapidly heated to 1000 DEG C and is incubated 20min.And in aluminium powder, add a small amount of Calcium Fluoride (Fluorspan); By the boron carbide composite material after infiltration just base in air furnace, be heated to 850 DEG C, and be incubated 50h and obtain highly purified boron carbide composite material.
Embodiment 3:
Select the boron carbide powder Homogeneous phase mixing of different-grain diameter size; Hydrochloric acid with 30% carries out pickling to boron carbide powder under the condition of heated and boiled; Boron carbide powder is sintered in 1600 DEG C at vacuum state; Boron carbide powder is carried out the process of good wettability metal coating; By pretreated boron carbide powder compression molding; Sinter under nitrogen atmosphere, 1800 DEG C of conditions, and be incubated 3h; First resistance furnace will vacuumize, then applying argon gas protection; The alumina crucible that norbide skeleton and infiltration metal are housed is placed in atmospheric resistance furnace, is rapidly heated to 1200 DEG C and is incubated 30min.And in aluminium powder, add a small amount of Calcium Fluoride (Fluorspan); By the boron carbide composite material after infiltration just base in air furnace, be heated to 950 DEG C, and be incubated 75h and obtain highly purified boron carbide composite material.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (5)

1. a boron carbide composite material preparation method, is characterized in that, comprises the steps:
The pre-treatment of boron carbide powder;
By pretreated boron carbide powder compression molding;
The pre-burning of norbide skeleton;
Norbide skeleton after pre-burning and infiltration metal are carried out pressure-free impregnation process;
The first base of boron carbide composite material through pressure-free impregnation is heat-treated, obtains highly purified boron carbide composite material.
2. a kind of boron carbide composite material preparation method according to claim 1, is characterized in that, being implemented as follows of the pre-treatment step of described boron carbide powder:
Select the boron carbide powder Homogeneous phase mixing of different-grain diameter size; Hydrochloric acid with 30% carries out pickling to boron carbide powder under the condition of heated and boiled; Boron carbide powder is sintered in 1500 ~ 1600 DEG C at vacuum state; Boron carbide powder is carried out the process of good wettability metal coating.
3. a kind of boron carbide composite material preparation method according to claim 1, is characterized in that, being implemented as follows of the burn in step of described norbide skeleton:
Sinter under nitrogen atmosphere, 1400 ~ 1800 DEG C of conditions, and be incubated 1 ~ 3h.
4. a kind of boron carbide composite material preparation method according to claim 1, is characterized in that, described norbide skeleton after pre-burning and infiltration metal is carried out being implemented as follows of pressure-free impregnation treatment step:
First resistance furnace will vacuumize, then applying argon gas protection; The alumina crucible that norbide skeleton and infiltration metal are housed is placed in atmospheric resistance furnace, is rapidly heated to 800 ~ 1200 DEG C and is incubated 10 ~ 30min.And in aluminium powder, add a small amount of Calcium Fluoride (Fluorspan).
5. a kind of boron carbide composite material preparation method according to claim 1, is characterized in that, described by the boron carbide composite material through pressure-free impregnation just base heat-treat, obtain being implemented as follows of highly purified boron carbide composite material step:
By the boron carbide composite material after infiltration just base in air furnace, be heated to 800 ~ 950 DEG C, and be incubated 10 ~ 75h and obtain highly purified boron carbide composite material.
CN201510992079.5A 2015-12-25 2015-12-25 Boron carbide composite material preparation method Pending CN105523764A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106050279A (en) * 2016-07-31 2016-10-26 常州天泰矿山设备制造有限公司 Maintenance-free neutral water medium single prop
CN108658602A (en) * 2017-12-25 2018-10-16 成都晋阳科技有限公司 A kind of preparation method of diamond boron carbide composite material
CN109055798A (en) * 2018-08-03 2018-12-21 北京汽车股份有限公司 Preparation method, brake disc and the vehicle of brake disc for vehicle

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106050279A (en) * 2016-07-31 2016-10-26 常州天泰矿山设备制造有限公司 Maintenance-free neutral water medium single prop
CN108658602A (en) * 2017-12-25 2018-10-16 成都晋阳科技有限公司 A kind of preparation method of diamond boron carbide composite material
CN109055798A (en) * 2018-08-03 2018-12-21 北京汽车股份有限公司 Preparation method, brake disc and the vehicle of brake disc for vehicle
CN109055798B (en) * 2018-08-03 2020-08-21 北京汽车股份有限公司 Preparation method of brake disc for vehicle, brake disc and vehicle

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