CN106007687A - Method for preparing nano-polycrystalline coesite through high-pressure phase transition method - Google Patents

Method for preparing nano-polycrystalline coesite through high-pressure phase transition method Download PDF

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CN106007687A
CN106007687A CN201610309735.1A CN201610309735A CN106007687A CN 106007687 A CN106007687 A CN 106007687A CN 201610309735 A CN201610309735 A CN 201610309735A CN 106007687 A CN106007687 A CN 106007687A
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coesite
polycrystalline
sio
high pressure
pressure
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CN106007687B (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 invention relates to a preparation method for nano-polycrystalline coesite. Microcrystalline alpha-SiO2 and nanocrystalline alpha-SiO2 serve as initial materials, after purification decontamination, no binder except deionized water is added, a sintering unit is assembled, and the nano-polycrystalline coesite material is prepared directly through high-temperature ultrahigh pressure sintering. The nano-polycrystalline coesite is single in phase and uniform in grain size, and the situations that the nano-polycrystalline coesite is reunited and grains abnormally grow at the high temperature cannot occur. In this way, the method successfully solves the problems that nanometer raw materials are reunited and grains abnormally grow.

Description

A kind of method using phase transition under high pressure method to prepare nano-multicrystal coesite
Technical field
The present invention relates to a kind of with crystallite α-SiO2For raw material, by pre-molding, utilize press to produce the method that superhigh-pressure high-temp prepares nano-multicrystal coesite, belong to field of inorganic materials.
Background technology
Ceramic material belongs to covalent bond compound more, under the conditions of high pressure-temperature or constant-pressure and high-temperature, generally there are multiple phase transformation, and the high pressure-temperature of part ceramic material can be intercepted and captured mutually in atmospheric conditions；Phase transformation great majority under ceramic material constant-pressure and high-temperature also can occur under high pressure-temperature, and can be intercepted and captured by normal temperature and pressure.Therefore, phase transition under high pressure is utilized can to prepare multiple nano ceramics polycrystalline with bulky grain pottery powder crystal for original material.Existing nano-multicrystal pottery prepare many with nanometer powder as original material, nanometer powder exist reunites, adsorb, be difficult to scattered problem constrain sinter gained polycrystalline material mechanical property.How to suppress nanocrystal growing up in high-temperature sintering process so that it is keep nano-meter characteristic and sintered body high-compactness, be that the technical barrier faced prepared by nano-multicrystal material.
This project will use crystallite, nanocrystalline α-SiO2Solve the reunion of nanometer initial powder existence for initial phase, adsorb and be difficult to scattered problem；Utilize high pressure can suppress the long-range diffusion of atom from so that the crystal grain solved constant-pressure and high-temperature sintering nano-multicrystal materials process of growing up of suppression crystal grain grow up problem.
Quartz is a kind of mineral being widely present in nature, the highest at the surface concentrations of the earth, is the important component part of various silicate mineral, for quartz race mineral.Quartz quartz has multiple homogeneity variant, has seven kinds of crystal formations: alpha-quartz, β-quartz, α-tridymite, β under normal pressure1-tridymite, β-tridymite, α-cristobalite and β-cristobalite.Under high pressure quartz also has multiple variant, and coesite is first high pressure variants of quartz, belongs to monoclinic system, and density is 3.01g/cm3.Under high pressure, quartz coesite stishovite CaCl can occur2Structure surpasses stishovite α-PbO2Structure surpasses the phase transformation of stishovite.α-SiO2Undergoing phase transition can form coesite at ~ about 3GPa, the present invention will be with crystallite, nanocrystalline α-SiO2Phase transition under high pressure is utilized to prepare nanometer coesite polycrystalline for original material, by comparing the nanocrystalline α-SiO of employing2, crystallite α-SiO2For original material under high pressure by phase transformation synthesis coesite polycrystalline mechanical property difference, optimization high rigidity, high tenacity nano coesite polycrystalline prepare approach.
Directly utilize crystallite, nanocrystalline α-SiO2Raw material, under superhigh-pressure high-temp prepare high-performance coesite polycrystalline bulk material report not yet occur.
Summary of the invention
The invention aims to overcome the reunion of nanometer initial powder existence when using nanometer initial powder to utilize phase transition under high pressure to prepare nano-multicrystal, adsorb and be difficult to scattered problem.Disclose a kind of with crystallite, manocrystalline powders as raw material, by pre-molding, the method preparing high-performance nano polycrystalline coesite material under the conditions of superhigh-pressure high-temp.
The method preparing high-performance nano polycrystalline coesite of the present invention is carried out in accordance with the following steps:
One, Feedstock treating, by crystallite, nanocrystalline α-SiO2Raw material washes of absolute alcohol, 120 DEG C of drying, add appropriate amount of deionized water as binding agent, pre-molding, molded samples is put in baking oven and is dried,.
Two, assembling sintering unit: the metal material of grinding and buffing parcel, carries out deoiling, ultrasonic waves for cleaning, infrared drying.The crystallite of pre-molding, nanocrystalline α-SiO2Raw material is put in metal cup, again pre-molding, is then charged into the sample cavity of high-pressure synthesizer.
Three, High Temperature High Pressure sintering: sintering pressure is 3-16GPa, heats while pressurize, and sintering temperature is 700-2000 DEG C, is incubated 1-50 minute.Lower the temperature rapidly after insulation, then start blood pressure lowering.
Four, take out the sample in synthetic cavity, carry out polishing, polishing.To obtain coesite polycrystal.
It is an advantage of the current invention that:
The nano-multicrystal coesite material of the present invention, uses the crystallite of pure phase, nanocrystalline α-SiO2Micropowder is raw material, uses High Temperature High Pressure phase transition method sintering to form.And without other impurity in sample, utilizing high pressure to make raw material be broken into uniform crystal grain, high temperature makes multicrystal crystal grain constantly grow up, and constantly growing up of this crystal grain has been suppressed by condition of high voltage simultaneously.Thus obtain the coesite polycrystal that purity is higher, thing is mutually homogeneous.
The present invention is preparation nanometer coesite polycrystalline material under the phase change conditions utilizing superhigh-pressure high-temp.Having phase velocity fast, pressure and temperature condition such as is easily controlled at the advantage.
Below by the drawings and specific embodiments, the present invention will be further described, but is not meant to limiting the scope of the invention.
Accompanying drawing explanation
Accompanying drawing 1 sinters unit installation diagram.
Detailed description of the invention
Below by embodiment, the present invention is specifically described; be necessary it is pointed out here that be that the present embodiment is further described only for the present invention; it is not intended that limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment 1: the crystallite α-SiO selecting mean diameter to be 10 μm2Micropowder, prepares nano-multicrystal coesite material according to technological process shown in the present invention.Feedstock treating: by crystallite α-SiO2Raw material absolute ethyl alcohol and stirring is cleaned, and treats that it settles, removes upper liquid, α-SiO2120 DEG C of drying in baking oven put into by micropowder.Add appropriate deionized water as binding agent, make α-SiO2Micropowder has certain humidity, pre-molding, molded samples is put in baking oven and is dried, and goes out the deionized water of binding agent the most.
Sample after being completely dried loads in metal cup, and pre-molding again puts into synthetic cavity, as shown in Figure 1.Wherein assembly mainly has insulation material, heating plate, adds heat pipe, parcel pipe, wrap sheet, insulation material, conductive electrode.Domestic hinge type cubic hinge press is utilized to produce High Temperature High Pressure.During High Temperature High Pressure sintering, sintering pressure is 12GPa, and sintering temperature is 1200 DEG C.
The nano-multicrystal coesite material thing using this technique to prepare is mutually single, even structure, has higher hardness and consistency, and does not use the produced reunion of nanocrystalline raw material and abnormal grain growth.

Claims (5)

1. use high pressure phase political reform for the method for nano-multicrystal coesite, its feature with: utilize high-temperature and high-pressure conditions, use crystallite, nanocrystalline α-SiO2As original material, synthesize nano-multicrystal coesite；Comprise the technical steps that: one, use the crystallite that purity is higher, nanocrystalline α-SiO2As original material；Two, original material being carried out precompressed becomes block to process；Three, under high-temperature and high-pressure conditions, α-SiO is made2It is changed into coesite polycrystal block materials.
The method that employing phase transition under high pressure method the most according to claim 1 prepares polycrystalline coesite, it is characterised in that: raw material uses crystallite, nanocrystalline α-SiO2For original material, raw-material grain size is 4 nm-500 um.
The method that employing phase transition under high pressure method the most according to claim 1 prepares polycrystalline coesite, it is characterised in that: raw material uses crystallite, nanocrystalline α-SiO2Single-phase for original material, without any sintering aid, mineralizer.
The method that employing phase transition under high pressure method the most according to claim 1 prepares polycrystalline coesite, it is characterised in that: utilize press to produce superhigh-pressure high-temp condition, make six square α-SiO in raw material2The monocline type coesite polycrystalline bulk become nanostructured upon mutually, and crystal grain is evenly distributed in coesite poly grains, large area formed be tightly combined, the nanometer coesite polycrystalline of high intensity, finally sinter coesite polycrystalline bulk into.
The method that employing phase transition under high pressure method the most according to claim 1 prepares polycrystalline coesite, it is characterised in that: the rear α-SiO of pre-molding2Block sinters through High Temperature High Pressure, and the pressure of High Temperature High Pressure sintering is 1.0 30 Gpa, and temperature is 400 2500 DEG C.
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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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN106829968A (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 nano-multicrystal stishovite
CN110424053A (en) * 2019-07-22 2019-11-08 四川大学 A method of preparing nanostructure block materials
CN110550942A (en) * 2019-09-16 2019-12-10 陕西理工大学 Preparation method of nano twin crystal silicon dioxide piezoelectric material
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

Citations (1)

* Cited by examiner, † Cited by third party
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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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

Non-Patent Citations (2)

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刘曙娥等: "地表柯石英的实验室模拟合成及其形成机制的研", 《高压物理学报》 *
张广强等: "纳米SiO2在高压高温下的结构转化", 《吉林大学学报（理学版）》 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN106829968A (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 nano-multicrystal stishovite
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
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
CN110424053A (en) * 2019-07-22 2019-11-08 四川大学 A method of preparing nanostructure block materials
CN110424053B (en) * 2019-07-22 2021-01-15 四川大学 Method for preparing nano-structure block material
CN110550942A (en) * 2019-09-16 2019-12-10 陕西理工大学 Preparation method of nano twin crystal silicon dioxide piezoelectric 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

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