CN106702489B - A kind of preparation method of iron coated magnesium oxide fixed whisker - Google Patents
A kind of preparation method of iron coated magnesium oxide fixed whisker Download PDFInfo
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- CN106702489B CN106702489B CN201610990418.0A CN201610990418A CN106702489B CN 106702489 B CN106702489 B CN 106702489B CN 201610990418 A CN201610990418 A CN 201610990418A CN 106702489 B CN106702489 B CN 106702489B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
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- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of preparation methods that type magnesia crystal whisker is coated and fixed, and belong to magnesia crystal whisker preparation technical field.The present invention will be after the honed sieve of magnesite cracker, it is preheated in Muffle furnace, calcining, it collects Adlerika and collects magnesium carbonate with ammonium carbonate composite precipitation, by by magnesium carbonate iron pentacarbonyl is compound and dry pre-coated, then heating calcining, coat iron to whisker surface, guarantee that whisker fibre does not change in calcination process, so as to improve dispersed between whisker, prepare magnesia crystal whisker not easy to reunite, preparation step of the present invention is simple, it is at low cost, hard aggregation-free phenomenon occurs in preparation process, controllability is strong, and the magnesia crystal whisker of preparation has preferable dispersion performance, particle diameter distribution is uniform, good crystalline, surface is smooth.
Description
Technical field
The present invention relates to a kind of preparation methods of iron coated magnesium oxide fixed whisker, belong to magnesia crystal whisker technology of preparing
Field.
Background technique
Whisker is a kind of whiskers body material, a diameter of several to several microns of zero point, and length is several microns to hundreds of
Micron.Since crystal structure is very complete, with surprising mechanical strength, as changing for the substances such as plastics, metal and ceramics
Property additive, shows splendid physicochemical properties and excellent mechanical performance.Magnesia crystal whisker have good heat resistance,
Insulating properties, heat conductivity, alkali resistance, stability and reinforcing character, the modifying agent as advanced composite material is increasingly noticeable,
It is a kind of multi-functional, H.D inorganic material.
The preparation method of magnesia crystal whisker has very much, mainly there is vapor phase method, liquid phase method and solid phase method.Vapor phase method, which refers to, to be passed through
Various methods generate magnesium vapor, and magnesium vapor is then transported to reaction chamber with inert gas and is reacted with oxygen (or vapor)
Obtain magnesia crystal whisker.The whisker draw ratio that the advantages of method is is big, diameter is evenly distributed, high-quality.But its entire work
Skill reaction process, reaction condition and consersion unit are all complex, poor controllability, and low yield.Liquid phase method is exactly to pass through raw material
Whisker presoma is made in liquid, and presoma whisker is then sintered into magnesia crystal whisker by certain calcine technology.Presoma mainly has
Alkali magnesium sulfate, basic magnesium chloride, magnesium carbonate.Due to its sintering temperature height, destroy precursor fibre shape shape, cause whisker it
Between easy-sintering and generate hard aggregation, dispersion is uneven.Solid phase method refers to that magnesium salts under the action of cosolvent, reacts in high temperature
Generate magnesia crystal whisker.Its simple process is easy to industrialize, but magnesia crystal whisker impurity obtained is more, and purity is low, needs essence
System.
Summary of the invention
The technical problems to be solved by the invention: preparing magnesia crystal whisker for liquid phase method, due to its sintering temperature height, breaks
Bad precursor fibre shape shape leads to easy-sintering between whisker and generates hard aggregation, disperses non-uniform drawback, provide one kind
It after the honed sieve of magnesite cracker, preheats, calcine in Muffle furnace, collect Adlerika and received with ammonium carbonate composite precipitation
Collect magnesium carbonate, by the way that magnesium carbonate iron pentacarbonyl is compound and drying pre-coated, subsequent heating calcining make iron packet in temperature-rise period
It covers to whisker surface, guarantees that whisker fibre does not change in calcination process, be not easy so as to improve dispersibility, preparation between whisker
The method of the magnesia crystal whisker of reunion efficiently solves liquid phase method sintering temperature height, destroys precursor fibre shape shape, lead to crystalline substance
Easy-sintering between palpus and lead to the problem of hard aggregation.Preparation step of the present invention is simple, and preparation cost is low, without hard group in preparation process
Poly- phenomenon occurs, and gained magnesia crystal whisker has preferable dispersion performance.
In order to solve the above technical problems, the present invention is using technical solution as described below:
(1) magnesite is chosen, placing it in hydraulic breaker and being crushed to partial size is 1cm ore particles, then by ore
Particle is placed in ball grinder, 3~5h of ball milling at 350~400r/min, is crossed 90~100 meshes, is collected to obtain giobertite powder；
(2) the giobertite powder of above-mentioned preparation is placed in Muffle furnace, 10~15min is preheated at 150~200 DEG C,
850~1000 DEG C then are warming up to 10 DEG C/min rate, after 1~2h is calcined in heat preservation, standing is cooled to room temperature, and is milled and is prepared into
Calcined magnesite stone powder and 40% sulfuric acid of mass fraction are stirred juxtaposition by calcined magnesite stone powder, in mass ratio 1:8
25~30min of heating water bath at 45~50 DEG C then stands and is cooled to room temperature, filters and collect filtrate and obtain Adlerika；
(3) ammonium carbonate is added in the Adlerika of above-mentioned preparation by 1:8 in mass ratio, is stirred at 55~60 DEG C
45~60min is mixed, filters and collects filter cake, in mass ratio 1:1, filter cake and iron pentacarbonyl are stirred, then 95~100
Rotary evaporated to dryness at DEG C is prepared into preimpregnation magnesium carbonate whisker；
(4) the preimpregnation magnesium carbonate whisker of above-mentioned preparation is placed in crucible, crucible is placed in tube-type atmosphere furnace, lead to nitrogen
Air is excluded, in a nitrogen atmosphere, by iron pentacarbonyl and preimpregnation magnesium carbonate whisker mass ratio 5:1, iron pentacarbonyl is added to earthenware
In crucible, it is warming up to 250~300 DEG C, after 2~3h of insulation reaction, stopping is passed through nitrogen and opens atmospheric communicating pipe, with 10 DEG C/min
Rate is warming up to 950~1000 DEG C, and heat preservation 1~2h of calcining then stops heating and standing being cooled to room temperature, can be prepared into one
Kind iron coated magnesium oxide fixed whisker.
Application method of the invention: 3:2 in mass ratio mixes portland cement, with tap water with 120~160r/min
1~2h is stirred, stirring thing is obtained, then to iron coated magnesium oxide fixed whisker produced by the present invention is added in stirring thing, is controlled
Additive amount is 5~7%, and addition, which finishes, to be uniformly mixed, and mixture is put into mold, the compression moulding at 20~30 DEG C,
8~10h is steamed at 180~200 DEG C again, can be prepared by test block.Magnesia crystal whisker of the present invention is uniformly dispersed in the base, can have
The bending strength and impact strength of effect enhancing test block, the bending strength of test block is up to 260~300kg/m2, impact strength up to 20.5~
42.3kg/m2, it is worthy to be popularized and uses.
The present invention is compared with other methods, and advantageous effects are:
(1) preparation step of the present invention is simple, at low cost, and hard aggregation-free phenomenon occurs in preparation process, and controllability is strong；
(2) magnesia crystal whisker of the present invention has preferable dispersion performance, and particle diameter distribution is uniform, good crystalline, and surface is smooth.
Specific embodiment
Magnesite is chosen first, and placing it in hydraulic breaker and being crushed to partial size is 1cm ore particles, then by ore
Particle is placed in ball grinder, 3~5h of ball milling at 350~400r/min, is crossed 90~100 meshes, is collected to obtain giobertite powder；
The giobertite powder of above-mentioned preparation is placed in Muffle furnace, at 150~200 DEG C preheat 10~15min, then with 10 DEG C/
Min rate is warming up to 850~1000 DEG C, and after 1~2h is calcined in heat preservation, standing is cooled to room temperature, and is milled and is prepared into calcined magnesite
Calcined magnesite stone powder and 40% sulfuric acid of mass fraction are stirred and are placed in 45~50 DEG C by stone powder, in mass ratio 1:8
25~30min of lower heating water bath then stands and is cooled to room temperature, filters and collect filtrate and obtain Adlerika；In mass ratio 1:
8, ammonium carbonate is added in the Adlerika of above-mentioned preparation, is stirred 45~60min at 55~60 DEG C, filtered and receive
Collect filter cake, filter cake and iron pentacarbonyl are stirred by 1:1 in mass ratio, then the rotary evaporated to dryness at 95~100 DEG C, preparation
Magnesium carbonate whisker must be presoaked；The preimpregnation magnesium carbonate whisker of above-mentioned preparation is placed in crucible, crucible is placed in tube-type atmosphere furnace,
Logical nitrogen excludes air, and in a nitrogen atmosphere, by iron pentacarbonyl and preimpregnation magnesium carbonate whisker mass ratio 5:1, iron pentacarbonyl is added
It adds in crucible, is warming up to 250~300 DEG C, after 2~3h of insulation reaction, stopping is passed through nitrogen and opens atmospheric communicating pipe, with 10
DEG C/min rate is warming up to 950~1000 DEG C, heat preservation 1~2h of calcining then stops heating and standing being cooled to room temperature, can make
It is standby to obtain a kind of iron coated magnesium oxide fixed whisker.
Example 1
Magnesite is chosen first, and placing it in hydraulic breaker and being crushed to partial size is 1cm ore particles, then by ore
Particle is placed in ball grinder, 3~5h of ball milling at 350~400r/min, is crossed 90~100 meshes, is collected to obtain giobertite powder；
The giobertite powder of above-mentioned preparation is placed in Muffle furnace, at 150~200 DEG C preheat 10~15min, then with 10 DEG C/
Min rate is warming up to 850~1000 DEG C, and after 1~2h is calcined in heat preservation, standing is cooled to room temperature, and is milled and is prepared into calcined magnesite
Calcined magnesite stone powder and 40% sulfuric acid of mass fraction are stirred and are placed in 45~50 DEG C by stone powder, in mass ratio 1:8
25~30min of lower heating water bath then stands and is cooled to room temperature, filters and collect filtrate and obtain Adlerika；In mass ratio 1:
8, ammonium carbonate is added in the Adlerika of above-mentioned preparation, is stirred 45~60min at 55~60 DEG C, filtered and receive
Collect filter cake, filter cake and iron pentacarbonyl are stirred by 1:1 in mass ratio, then the rotary evaporated to dryness at 95~100 DEG C, preparation
Magnesium carbonate whisker must be presoaked；The preimpregnation magnesium carbonate whisker of above-mentioned preparation is placed in crucible, crucible is placed in tube-type atmosphere furnace,
Logical nitrogen excludes air, and in a nitrogen atmosphere, by iron pentacarbonyl and preimpregnation magnesium carbonate whisker mass ratio 5:1, iron pentacarbonyl is added
It adds in crucible, is warming up to 250~300 DEG C, after 2~3h of insulation reaction, stopping is passed through nitrogen and opens atmospheric communicating pipe, with 10
DEG C/min rate is warming up to 950~1000 DEG C, heat preservation 1~2h of calcining then stops heating and standing being cooled to room temperature, can make
It is standby to obtain a kind of iron coated magnesium oxide fixed whisker.
3:2 in mass ratio mixes portland cement with tap water, stirs 1h with 120r/min, obtains stirring thing, then to
Iron coated magnesium oxide fixed whisker produced by the present invention is added in stirring thing, control additive amount is 5%, and it is mixed that addition finishes stirring
It closes uniformly, and mixture is put into mold, the compression moulding at 20 DEG C, then steam 8h at 180 DEG C, can be prepared by test block.
Magnesia crystal whisker of the present invention is uniformly dispersed in the base, can effectively enhance the bending strength and impact strength of test block, test block it is curved
Qu Qiangdu reaches 260kg/m2, impact strength reach 20.5kg/m2, it is worthy to be popularized and uses.
Example 2
Magnesite is chosen first, and placing it in hydraulic breaker and being crushed to partial size is 1cm ore particles, then by ore
Particle is placed in ball grinder, 3~5h of ball milling at 350~400r/min, is crossed 90~100 meshes, is collected to obtain giobertite powder；
The giobertite powder of above-mentioned preparation is placed in Muffle furnace, at 150~200 DEG C preheat 10~15min, then with 10 DEG C/
Min rate is warming up to 850~1000 DEG C, and after 1~2h is calcined in heat preservation, standing is cooled to room temperature, and is milled and is prepared into calcined magnesite
Calcined magnesite stone powder and 40% sulfuric acid of mass fraction are stirred and are placed in 45~50 DEG C by stone powder, in mass ratio 1:8
25~30min of lower heating water bath then stands and is cooled to room temperature, filters and collect filtrate and obtain Adlerika；In mass ratio 1:
8, ammonium carbonate is added in the Adlerika of above-mentioned preparation, is stirred 45~60min at 55~60 DEG C, filtered and receive
Collect filter cake, filter cake and iron pentacarbonyl are stirred by 1:1 in mass ratio, then the rotary evaporated to dryness at 95~100 DEG C, preparation
Magnesium carbonate whisker must be presoaked；The preimpregnation magnesium carbonate whisker of above-mentioned preparation is placed in crucible, crucible is placed in tube-type atmosphere furnace,
Logical nitrogen excludes air, and in a nitrogen atmosphere, by iron pentacarbonyl and preimpregnation magnesium carbonate whisker mass ratio 5:1, iron pentacarbonyl is added
It adds in crucible, is warming up to 250~300 DEG C, after 2~3h of insulation reaction, stopping is passed through nitrogen and opens atmospheric communicating pipe, with 10
DEG C/min rate is warming up to 950~1000 DEG C, heat preservation 1~2h of calcining then stops heating and standing being cooled to room temperature, can make
It is standby to obtain a kind of iron coated magnesium oxide fixed whisker.
3:2 in mass ratio mixes portland cement with tap water, stirs 2h with 140r/min, obtains stirring thing, then to
Iron coated magnesium oxide fixed whisker produced by the present invention is added in stirring thing, control additive amount is 6%, and it is mixed that addition finishes stirring
It closes uniformly, and mixture is put into mold, the compression moulding at 25 DEG C, then steam 9h at 190 DEG C, can be prepared by test block.
Magnesia crystal whisker of the present invention is uniformly dispersed in the base, can effectively enhance the bending strength and impact strength of test block, test block it is curved
Qu Qiangdu reaches 280kg/m2, impact strength reach 31.6kg/m2, it is worthy to be popularized and uses.
Example 3
Magnesite is chosen first, and placing it in hydraulic breaker and being crushed to partial size is 1cm ore particles, then by ore
Particle is placed in ball grinder, 3~5h of ball milling at 350~400r/min, is crossed 90~100 meshes, is collected to obtain giobertite powder；
The giobertite powder of above-mentioned preparation is placed in Muffle furnace, at 150~200 DEG C preheat 10~15min, then with 10 DEG C/
Min rate is warming up to 850~1000 DEG C, and after 1~2h is calcined in heat preservation, standing is cooled to room temperature, and is milled and is prepared into calcined magnesite
Calcined magnesite stone powder and 40% sulfuric acid of mass fraction are stirred and are placed in 45~50 DEG C by stone powder, in mass ratio 1:8
25~30min of lower heating water bath then stands and is cooled to room temperature, filters and collect filtrate and obtain Adlerika；In mass ratio 1:
8, ammonium carbonate is added in the Adlerika of above-mentioned preparation, is stirred 45~60min at 55~60 DEG C, filtered and receive
Collect filter cake, filter cake and iron pentacarbonyl are stirred by 1:1 in mass ratio, then the rotary evaporated to dryness at 95~100 DEG C, preparation
Magnesium carbonate whisker must be presoaked；The preimpregnation magnesium carbonate whisker of above-mentioned preparation is placed in crucible, crucible is placed in tube-type atmosphere furnace,
Logical nitrogen excludes air, and in a nitrogen atmosphere, by iron pentacarbonyl and preimpregnation magnesium carbonate whisker mass ratio 5:1, iron pentacarbonyl is added
It adds in crucible, is warming up to 250~300 DEG C, after 2~3h of insulation reaction, stopping is passed through nitrogen and opens atmospheric communicating pipe, with 10
DEG C/min rate is warming up to 950~1000 DEG C, heat preservation 1~2h of calcining then stops heating and standing being cooled to room temperature, can make
It is standby to obtain a kind of iron coated magnesium oxide fixed whisker.
3:2 in mass ratio mixes portland cement with tap water, stirs 2h with 160r/min, obtains stirring thing, then to
Iron coated magnesium oxide fixed whisker produced by the present invention is added in stirring thing, control additive amount is 7%, and it is mixed that addition finishes stirring
It closes uniformly, and mixture is put into mold, the compression moulding at 30 DEG C, then steam 10h at 200 DEG C, can be prepared by test block.
Magnesia crystal whisker of the present invention is uniformly dispersed in the base, can effectively enhance the bending strength and impact strength of test block, test block it is curved
Qu Qiangdu reaches 300kg/m2, impact strength reach 42.3kg/m2, it is worthy to be popularized and uses.
Claims (1)
1. a kind of preparation method of fixed sections coated magnesium oxide whisker, it is characterised in that specific preparation step are as follows:
(1) magnesite is chosen, placing it in hydraulic breaker and being crushed to partial size is 1cm ore particles, then by ore particles
It is placed in ball grinder, 3~5h of ball milling at 350~400r/min, crosses 90~100 meshes, collect to obtain giobertite powder；
(2) the giobertite powder of above-mentioned preparation is placed in Muffle furnace, 10~15min is preheated at 150~200 DEG C, then
850~1000 DEG C are warming up to 10 DEG C/min rate, after 1~2h is calcined in heat preservation, standing is cooled to room temperature, and is milled and is prepared into calcining
Calcined magnesite stone powder and 40% sulfuric acid of mass fraction are stirred and are placed in 45 by giobertite powder, in mass ratio 1:8
25~30min of heating water bath at~50 DEG C then stands and is cooled to room temperature, filters and collect filtrate and obtain Adlerika；
(3) ammonium carbonate is added in the Adlerika of above-mentioned preparation by 1:8 in mass ratio, is stirred at 55~60 DEG C
45~60min filters and collects filter cake, in mass ratio 1:1, filter cake and iron pentacarbonyl are stirred, then at 95~100 DEG C
Rotary evaporated to dryness is prepared into preimpregnation magnesium carbonate whisker；
(4) the preimpregnation magnesium carbonate whisker of above-mentioned preparation is placed in crucible, crucible is placed in tube-type atmosphere furnace, led to nitrogen and exclude
By iron pentacarbonyl and preimpregnation magnesium carbonate whisker mass ratio 5:1, iron pentacarbonyl is added in crucible in a nitrogen atmosphere for air,
It is warming up to 250~300 DEG C, after 2~3h of insulation reaction, stopping is passed through nitrogen and opens atmospheric communicating pipe, with 10 DEG C/min rate
950~1000 DEG C are warming up to, heat preservation 1~2h of calcining then stops heating and standing being cooled to room temperature, can be prepared into fixed
Iron coated magnesium oxide whisker.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6838004B1 (en) * | 1999-09-07 | 2005-01-04 | Industrial Science & Technology Network, Inc. | Nanopore reactive adsorbents for the high-efficiency removal of waste species |
| CN101353784A (en) * | 2008-09-19 | 2009-01-28 | 高晢 | Method for coating target medicament particle with soft magnetic nanofilm |
| CN101974740A (en) * | 2010-10-29 | 2011-02-16 | 北京矿冶研究总院 | Preparation method of zinc oxide whisker loaded copper and silver |
| CN102887506A (en) * | 2012-09-28 | 2013-01-23 | 南京大学 | Method for preparing iron coated multi-layer graphene nano composite material by performing gaseous decomposition on pentacarbonyl iron |
-
2016
- 2016-11-10 CN CN201610990418.0A patent/CN106702489B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6838004B1 (en) * | 1999-09-07 | 2005-01-04 | Industrial Science & Technology Network, Inc. | Nanopore reactive adsorbents for the high-efficiency removal of waste species |
| CN101353784A (en) * | 2008-09-19 | 2009-01-28 | 高晢 | Method for coating target medicament particle with soft magnetic nanofilm |
| CN101974740A (en) * | 2010-10-29 | 2011-02-16 | 北京矿冶研究总院 | Preparation method of zinc oxide whisker loaded copper and silver |
| CN102887506A (en) * | 2012-09-28 | 2013-01-23 | 南京大学 | Method for preparing iron coated multi-layer graphene nano composite material by performing gaseous decomposition on pentacarbonyl iron |
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