CN107445177A - A kind of ZrB2The preparation method of fiber - Google Patents

A kind of ZrB2The preparation method of fiber Download PDF

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Publication number
CN107445177A
CN107445177A CN201710631678.3A CN201710631678A CN107445177A CN 107445177 A CN107445177 A CN 107445177A CN 201710631678 A CN201710631678 A CN 201710631678A CN 107445177 A CN107445177 A CN 107445177A
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CN
China
Prior art keywords
fiber
zrb
raw material
preparation
zro
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Pending
Application number
CN201710631678.3A
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Chinese (zh)
Inventor
任耘
周盼
肖国庆
丁冬海
种小川
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Xian University of Architecture and Technology
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Xian University of Architecture and Technology
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Priority to CN201710631678.3A priority Critical patent/CN107445177A/en
Publication of CN107445177A publication Critical patent/CN107445177A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00—Boron; Compounds thereof
    • C01B35/02—Boron; Borides
    • C01B35/04—Metal borides
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
    • C04B35/62272—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on non-oxide ceramics
    • C04B35/62277—Fibres based on carbides
    • C04B35/806—
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
    • C04B2235/3246—Stabilised zirconias, e.g. YSZ or cerium stabilised zirconia
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax

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

Abstract

The invention discloses a kind of ZrB2The preparation method of fiber, involved raw material include Mg, ZrO2Fiber, B2O3, fused salt auxiliary agent (including MgCl2、Na2B4O7Deng), dispensing on request first, uniformly being placed in powder compressing machine after mixing is pressed into cylindrical sample, and sample is placed in sample bench, vacuumizes logical argon gas, and pressurization igniting takes out sample after the completion of reaction, and required product is produced after pickling filters drying.The invention has the advantages of reaction time is short, energy consumption is low, yield is high, is expected to obtain pure ZrB through pickling2Fiber, can be as the lay-by material of hypersonic flight, Step atmospheric layers vehicle and rocket propulsion system.

Description

A kind of ZrB2The preparation method of fiber
Technical field
The invention belongs to field of inorganic nonmetallic material, more particularly to a kind of ZrB2The preparation method of fiber.
Technical background
Near space hypersonic aircraft flies near space particular surroundings, and the technical problem of involved most critical is suitable Close the material technology of this environment hypersonic flight.ZrB2Ceramics not only can superhigh temperature resistant, and in the mistake being rapidly heated In journey also can retention property stability, and there is high rigidity, relatively low density, the advantages that high thermal conductivity, turn into superb The candidate materials of velocity of sound aircraft.But ZrB2The fracture toughness of ceramics is poor, on 2 1st, 2003, U.S. space shuttle " brother Rival Asia " number, because the object near external tank attachment point comes off, is fired upon space flight and flown during reentry The bottom of wing, causes the heat resistant material (brittle ceramic materials) on wing to crack, ultimately results in space shuttle on the left of machine Blast is disintegrated.So solves ZrB2This problem of ceramic fracture toughness difference is most important.In order to solve this problem, there is scholar to add Enter second its relative modification, but because enhancing does not mutually possess ZrB2The special resistance to elevated temperatures of matrix, can cause globality on the contrary It can decline, and the compatibility of two kinds of materials uses ZrB there is also problem2Fiber reinforcement ZrB2Ceramics can solve to add the second phase institute Existing matching sex chromosome mosaicism.Synthesis ZrB at present2There is the problems such as yielding poorly, complex process more in fiber, the present invention is auxiliary using template Help conbustion synthesis ZrB2Fiber, with the ZrO in raw material2Fiber is template, and technical process is simple, energy-conservation, can be by changing releasing for heat Put the composition and its structure for coming the speed of control process, temperature, conversion ratio and product with transmission speed.
The content of the invention
For in the prior art the defects of and deficiency, it is an object of the invention to provide a kind of ZrB2The preparation side of fiber Method, this method preparation technology is simple, and its reaction time is short, energy consumption is low, yield is high, and in order to realize above-mentioned task, the present invention takes Following technical solution：
A kind of ZrB2The preparation method of fiber, including with Mg, ZrO2Fiber and B2O3For raw material, pass through conbustion synthesis legal system Standby ZrB2Fiber.
Specifically, by mass percentage, ZrO in raw material2Fiber is that 30%~39%, Mg is 37%~48%, B2O3For 20%~25%, mass percent sum is 100%.
Preferably, ZrO in raw material2Fiber is 36%, and Mg powder is 42% in raw material, B in raw material2O3For 22%.
More specifically, in addition to fused salt auxiliary agent, the fused salt include MgCl2And Na2B4O7One or both of.
Preferably, by mass percentage, MgCl2Account for 0%~40%, Na of raw material total amount2B4O7Account for raw material total amount 0%~60%, not comprising 0% endpoint value.
It is furthermore preferred that by mass percentage, MgCl2Account for 3%, Na of raw material total amount2B4O7Account for the 12% of raw material total amount.
Detailed, raw material is subjected to dispensing on request, is molded after well mixed on powder compressing machine, briquetting pressure is 1MPa, the igniting of being powered is placed on sample bench after shaping, reaction atmosphere is argon gas, reaction pressure 1.5MPa.
Advantages of the present invention is：
(1) the invention provides one kind to prepare ZrB2The method of fiber, this method is with Mg, ZrO2Fiber, B2O3Adopted for raw material ZrB is carried out with the synthesis of template auxiliary combustion2The preparation of fiber, the environmental protection of preparation process simple economy, and be easy to largely produce.
(2) ZrB that the present invention prepares2Fiber, for toughness reinforcing ZrB2Ceramics, can solve ZrB2Ceramic fracture toughness is poor The problem of, be not in add the matching sex chromosome mosaicism caused by different phases.
(3) ZrB is prepared using the present invention2Fiber is, it is necessary to obtain the ZrB of different draw ratios, grain size2Fiber, only need root Change template ZrO according to demand2The property of fiber.
Brief description of the drawings
Fig. 1 is ZrO prepared by the embodiment of the present invention 12The XRD of fiber；
Fig. 2 is ZrO prepared by the embodiment of the present invention 12The SEM figures of fiber；
Fig. 3 is ZrO prepared by the embodiment of the present invention 22The XRD of fiber；
Fig. 4 is ZrO prepared by the embodiment of the present invention 22The SEM figures of fiber；
Fig. 5 is ZrO prepared by the embodiment of the present invention 32The XRD of fiber；
Fig. 6 is ZrO prepared by the embodiment of the present invention 32The SEM figures of fiber；
The present invention is illustrated below in conjunction with specification drawings and specific embodiments.
Embodiment
ZrB is prepared using conbustion synthesis synthetic technology2Fiber, technique is simple, efficiency high, energy-conserving and environment-protective, and speed, temperature It is controllable.
The present invention is described in detail with reference to the accompanying drawings and detailed description, it is impossible to assert the specific reality of the present invention Apply and be confined to these explanations.For general technical staff of the technical field of the invention, structure of the present invention is not being departed from On the premise of think of, some simple deduction or replace can also be made, should all be considered as belonging to protection scope of the present invention.In this hair Bright Mg, ZrO provided2Fiber, B2O3, fused salt auxiliary agent (including MgCl2、Na2B4O7Deng) it is that raw material is matched somebody with somebody by mass percentage Material, ZrB can be prepared by conbustion synthesis2Fiber, ZrO2Fiber is as preparation ZrB2The template of fiber.
Embodiment 1：
The present embodiment uses ZrO2Fiber content >=99.7%, purity >=99.9% of described Mg powder, described B2O3's Purity >=98.8%, by mass percentage, ZrO in raw material2Fiber is 36%, and Mg powder is 42% in raw material, B in raw material2O3For 22%, mass percent sum is 100%.
Load weighted raw material is poured into mortar, stirring makes the full and uniform mixing of various raw materials, and mixed material is weighed and put In in powder compressing machine grinding tool, it is molded using powder compressing machine, briquetting pressure 1MPa, then release is stripped, final to be made straight Footpath is 20mm cylindrical sample.Sample is placed in sample bench during conbustion synthesis, logical argon gas is vacuumized, is forced into 1.5Mpa, Then light a fire, react and completed in 1~2s.Reacted sample is placed in the hydrochloric acid that concentration is 10% pickling to remove product In MgO and remaining Mg.
X-ray diffraction analysis are carried out to the sample after pickling, obtain XRD spectrum, referring to Fig. 1, it was found from XRD results, acid The thing phase composition for washing rear product is ZrB2、ZrO2。ZrB2Peak intensity relative to ZrO2Peak intensity will height, illustrate that product is mainly ZrB2, also a small amount of ZrO2.Sem analysis is carried out to product, participates in Fig. 2, it can be seen that existing powder in the product of synthesis, again There is fiber, main cause is that Synthesized temperature is higher, fiber sheath occurred to peel off, melted.
Embodiment 2：
The present embodiment is by mass percentage, on the basis of embodiment 1, to mix account for raw material gross mass 3% outside MgCl2。
X-ray diffraction analysis are carried out to the sample after pickling, XRD spectrum is obtained, referring to Fig. 3, it was found from XRD results, adds Enter MgCl2The thing phase composition of product is ZrB afterwards2、ZrO2、Mg3B2O6.Sem analysis is carried out to product, participates in Fig. 4, it can be seen that The pattern of fiber is changed in the product of synthesis.
Embodiment 3：
The present embodiment is by mass percentage, on the basis of embodiment 1, to mix Na2B4O7For raw material gross mass 12%, mix MgCl2For the 6% of raw material gross mass.
X-ray diffraction analysis are carried out to the sample after pickling, XRD spectrum is obtained, referring to Fig. 5, it was found from XRD results, adds Enter Na2B4O7、MgCl2The thing phase composition of product is ZrB afterwards2、ZrO2、Mg3B2O6.Sem analysis is carried out to product, participates in Fig. 6, can To find out, fiber is dense in the product of generation, and mainly fused salt reduces the volatilization of material in course of reaction.

Claims (7)

  1. A kind of 1. ZrB2The preparation method of fiber, it is characterised in that including with Mg, ZrO2Fiber and B2O3For raw material, pass through burning Synthetic method prepares ZrB2Fiber.
  2. 2. ZrB as claimed in claim 12The preparation method of fiber, it is characterised in that by mass percentage, ZrO in raw material2 Fiber is that 30%~39%, Mg is 37%~48%, B2O3For 20%~25%, mass percent sum is 100%.
  3. 3. ZrB as claimed in claim 12The preparation method of fiber, it is characterised in that by mass percentage, ZrO in raw material2 Fiber is 36%, and Mg powder is 42% in raw material, B in raw material2O3For 22%.
  4. 4. the ZrB as described in claim 1,2 or 32The preparation method of fiber, it is characterised in that described also including lava auxiliary agent Fused salt includes MgCl2And Na2B4O7One or both of.
  5. 5. ZrB as claimed in claim 42The preparation method of fiber, it is characterised in that by mass percentage, MgCl2Account for original Expect 0%~40%, Na of total amount2B4O7The 0%~60% of raw material total amount is accounted for, not comprising 0% endpoint value.
  6. 6. ZrB as claimed in claim 42The preparation method of fiber, it is characterised in that by mass percentage, MgCl2Account for original Expect 3%, Na of total amount2B4O7Account for the 12% of raw material total amount.
  7. 7. the ZrB as described in claim 1,2 or 32The preparation method of fiber, it is characterised in that matched somebody with somebody raw material on request Material, it is molded after well mixed on powder compressing machine, briquetting pressure 1MPa, the igniting that is powered is placed on sample bench after shaping, instead It is argon gas to answer atmosphere, reaction pressure 1.5MPa.
CN201710631678.3A 2017-07-28 2017-07-28 A kind of ZrB2The preparation method of fiber Pending CN107445177A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1587188A (en) * 2004-07-08 2005-03-02 复旦大学 Process for synthesizing high purity zirconium diboride-aluminium oxide Al2O3 ceramic composite powder in one step
CN103466649A (en) * 2013-08-28 2013-12-25 东北大学 Cleaner production method for preparing superfine boride powder through self-propagating metallurgy method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1587188A (en) * 2004-07-08 2005-03-02 复旦大学 Process for synthesizing high purity zirconium diboride-aluminium oxide Al2O3 ceramic composite powder in one step
CN103466649A (en) * 2013-08-28 2013-12-25 东北大学 Cleaner production method for preparing superfine boride powder through self-propagating metallurgy method

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
M. JALALY,ET AL.: "Mechanosynthesis of nanocrystalline ZrB2-based powders by mechanically induced self-sustaining reaction method", 《ADVANCES IN APPLIED CERAMICS》 *
SHAOWEI ZHANG,ET AL.: "Novel Synthesis of ZrB2 Powder Via Molten-Salt-Mediated Magnesiothermic Reduction", 《J. AM. CERAM. SOC.》 *
李权等: "ZrO2纤维模板自蔓延高温合成ZrB2/Al2O3", 《硅酸盐通报》 *

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Application publication date: 20171208