CN106007687B - A method of nano-multicrystal coesite is prepared using phase transition under high pressure method - Google Patents

A method of nano-multicrystal coesite is prepared using phase transition under high pressure method Download PDF

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CN106007687B
CN106007687B CN201610309735.1A CN201610309735A CN106007687B CN 106007687 B CN106007687 B CN 106007687B CN 201610309735 A CN201610309735 A CN 201610309735A CN 106007687 B CN106007687 B CN 106007687B
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coesite
sio
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multicrystal
pressure
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CN106007687A (en
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王海阔
刘俊龙
李颖
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Henan University of Technology
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Abstract

The present invention relates to a kind of technologies of preparing of nano-multicrystal coesite.Using crystallite, nanocrystalline α-SiO2As original material, after purified removal of impurities, any binder in addition to deionized water is not added, assembly sintering unit directly prepares nano-multicrystal coesite material through superhigh-pressure high-temp sintering.This nano-multicrystal coesite material object is mutually single, homogeneous grain size, and agglomeration and crystal grain abnormal growth at high temperature will not occur.This solves the problems, such as the present invention successfully using generation reunion and abnormal grain growth when nano raw material.

Description

A method of nano-multicrystal coesite is prepared using phase transition under high pressure method
Technical field
The present invention relates to one kind with crystallite α-SiO2Superhigh-pressure high-temp is generated using press by pre-molding for raw material The method for preparing nano-multicrystal coesite, belongs to field of inorganic materials.
Background technique
Ceramic material belongs to covalent key compound more, and under the conditions of high pressure-temperature or constant-pressure and high-temperature, generally there are a variety of phases Become, the high pressure-temperature of part ceramic material can mutually be intercepted and captured in atmospheric conditions；Phase transformation under ceramic material constant-pressure and high-temperature is most Number can also occur under high pressure-temperature, and can be intercepted and captured by normal temperature and pressure.Therefore, it is utilized by original material of bulky grain ceramics powder crystal Phase transition under high pressure can prepare a variety of nano ceramics polycrystalline.The preparation of existing nano-multicrystal ceramics mostly using nanometer powder as original material, Nanometer powder there are problems that reuniting, adsorb, be difficult to disperse to constrain the mechanical property of sintering gained polycrystalline material.How to inhibit Nanocrystal growing up in high-temperature sintering process makes it keep nano-meter characteristic and sintered body high-compactness, is nano-multicrystal material The technical problem that material preparation faces.
This project will use crystallite, nanocrystalline α-SiO2It solves existing for nanometer initial powder reunion for initial phase, inhale It is accompanied by and is difficult to the problem of dispersing；The long-range of atom can be inhibited to spread from using high pressure and then growing up for crystal grain is inhibited to solve Crystal grain in constant-pressure and high-temperature sintering nano-multicrystal materials process is grown up problem.
Quartz is a kind of mineral being widely present in nature, very high in the surface concentrations of the earth, is various silicic acid The important component of salt mineral, for quartzy race mineral.Quartzy quartz has seven kinds of crystal forms: α-under normal pressure there are many homogeneity variant Quartz, β-quartz, α-tridymite, β1Tridymite, β-tridymite, α-cristobalite and β-cristobalite.Quartz also has more under high pressure Kind variant, coesite are first high pressure variants of quartz, belong to monoclinic system, density 3.01g/cm3.Under high pressure, it can occur Quartz-coesite-stishovite-CaCl2Super stishovite-α-the PbO of structure2The phase transformation of the super stishovite of structure.α-SiO2In ~ 3GPa Left and right, which is undergone phase transition, can form coesite, and the present invention will be with crystallite, nanocrystalline α-SiO2Phase transition under high pressure system is utilized for original material Standby nanometer coesite polycrystalline, by comparing using nanocrystalline α-SiO2, crystallite α-SiO2Pass through phase transformation under high pressure for original material Synthesize the difference of coesite polycrystalline mechanical property, optimization high rigidity, high tenacity nano coesite polycrystalline preparation approach.
Directly utilize crystallite, nanocrystalline α-SiO2Raw material prepares high-performance coesite polycrystalline bulk under superhigh-pressure high-temp The report of material not yet occurs.
Summary of the invention
Nanometer when using nanometer initial powder to prepare nano-multicrystal using phase transition under high pressure the purpose of the invention is to overcome Initial powder is existing to reunite, adsorbs and be difficult to the problem of dispersing.Disclose one kind using crystallite, manocrystalline powders as raw material, By pre-molding, the method for high-performance nano polycrystalline coesite material is prepared under the conditions of superhigh-pressure high-temp.
The method of the present invention for preparing high-performance nano polycrystalline coesite carries out in accordance with the following steps:
One, feedstock processing, by crystallite, nanocrystalline α-SiO2Raw material washes of absolute alcohol, 120 DEG C of drying, adds and goes in right amount Ionized water is placed in oven and dried molded samples as binder, pre-molding,.
Two, assembly sintering unit: the metal material of grinding and buffing package is deoiled, ultrasonic cleaning, infrared baking It is dry.Crystallite, nanocrystalline α-SiO pre-molding2Raw material is put into metal cup, again pre-molding, is then charged into high pressing At the sample cavity of device.
Three, high temperature and pressure is sintered: sintering pressure 3-16GPa, pressure maintaining while, are heated, sintering temperature 700- 2000 DEG C, keep the temperature 1-50 minutes.Cool down rapidly after heat preservation, then starts to be depressured.
Four, the sample in synthetic cavity is taken out, polished, polished.To obtain coesite polycrystal.
The present invention has the advantages that
Nano-multicrystal coesite material of the invention, using the crystallite of pure phase, nanocrystalline α-SiO2Micro mist is raw material, is used High temperature and pressure phase transition method is sintered.And other impurity are free of in sample, and so that raw material is broken into uniform crystal grain using high pressure, it is high Temperature makes the crystal grain of polycrystal constantly grow up, and condition of high voltage inhibits constantly growing up for this crystal grain simultaneously.To The coesite polycrystal higher to purity, object is mutually uniform.
The present invention is that nanometer coesite polycrystalline material is prepared under the phase change conditions using superhigh-pressure high-temp.With phase velocity Fastly, the advantages that pressure and temperature condition is easy to control.
Below by the drawings and specific embodiments, the present invention will be further described, but is not meant to protect the present invention Protect the limitation of range.
Detailed description of the invention
Attached drawing 1 is sintered unit installation diagram.
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to it is indicated herein be the present embodiment only for The present invention is further described, and should not be understood as limiting the scope of the invention, and the person skilled in the art in the field can Some nonessential modifications and adaptations are made with the content according to aforementioned present invention.
Embodiment 1: selecting average grain diameter is 10 μm of crystallite α-SiO2Micro mist is prepared according to process flow shown in the present invention Nano-multicrystal coesite material.Feedstock processing: by crystallite α-SiO2Raw material is cleaned with absolute ethyl alcohol and stirring, to its sedimentation, is gone Upper liquid, α-SiO2Micro mist is put into 120 DEG C of drying in baking oven.Add suitable deionized water as binder, makes α-SiO2It is micro- Powder has certain humidity, and pre-molding is placed in oven and dried molded samples, the deionized water for the binder the most of going out.
Sample after being completely dried is fitted into metal cup, again pre-molding, is put into synthetic cavity, as shown in Figure 1. Wherein component mainly has thermal insulation material, heating sheet, heating tube, package pipe, wrap sheet, thermal insulation material, conductive electrode.Using domestic Hinge type cubic hinge press generates high temperature and pressure.When high temperature and pressure is sintered, sintering pressure 12GPa, sintering temperature is 1200 DEG C.
The nano-multicrystal coesite material object prepared using this technique is mutually single, and structure is uniform, has higher hardness and cause Density, and there is no using reunion and abnormal grain growth caused by nanocrystalline raw material.

Claims (2)

1. the method for preparing nano-multicrystal coesite using phase transition under high pressure method, it is characterised in that: use six square α-SiO2Crystallite, Nanocrystalline to be used as raw material, the particle sizes of raw material is 4 nm-500 μm, generates high-temperature and high-pressure conditions using press, makes former material Six square α-SiO in material2The monocline type coesite polycrystalline bulk mutually become nanostructured upon, and crystal grain is evenly distributed on coesite In polycrystalline, large area formed be tightly combined, high-intensitive nanometer coesite polycrystalline, finally sinter coesite polycrystalline bulk into；Packet Include following processing step: one, using the higher six squares α-SiO of purity2Crystallite, it is nanocrystalline be used as original material；Two, to initial Material carries out precompressed and handles at block；Three, the block after pre-molding is pressure is 1.0-30 Gpa, temperature is 400-2500 High temperature and pressure sintering is carried out under conditions of DEG C, makes six square α-SiO2It is changed into coesite polycrystal block materials.
2. according to the method described in claim 1, it is characterized by: using six square α-SiO2Crystallite, it is nanocrystalline it is single-phase be initial Material does not add any sintering aid, mineralizer.
CN201610309735.1A 2016-05-11 2016-05-11 A method of nano-multicrystal coesite is prepared using phase transition under high pressure method Expired - Fee Related CN106007687B (en)

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CN106829968B (en) * 2017-03-06 2019-03-22 河南工业大学 A method of nano-multicrystal stishovite is prepared using phase transition under high pressure method
CN106830902A (en) * 2017-03-06 2017-06-13 河南工业大学 A kind of method that use phase transition under high pressure method prepares polycrystalline alpha-aluminium oxide
CN111718197A (en) * 2019-03-20 2020-09-29 山东工业陶瓷研究设计院有限公司 Thin quartz ceramic component and efficient preparation method thereof
CN110424053B (en) * 2019-07-22 2021-01-15 四川大学 Method for preparing nano-structure block material
CN110550942B (en) * 2019-09-16 2022-03-08 陕西理工大学 Preparation method of nano twin crystal silicon dioxide piezoelectric material

Citations (1)

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CN1864841A (en) * 2006-04-26 2006-11-22 东北电力大学 A coesite preparation method

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Publication number Priority date Publication date Assignee Title
CN1864841A (en) * 2006-04-26 2006-11-22 东北电力大学 A coesite preparation method

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