CN108584970A - The preparation method of the high temperature negative expansion micro-nano rice flour of one type beta-eucryptite structure - Google Patents
The preparation method of the high temperature negative expansion micro-nano rice flour of one type beta-eucryptite structure Download PDFInfo
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- CN108584970A CN108584970A CN201810451136.2A CN201810451136A CN108584970A CN 108584970 A CN108584970 A CN 108584970A CN 201810451136 A CN201810451136 A CN 201810451136A CN 108584970 A CN108584970 A CN 108584970A
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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
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
Abstract
The present invention is the preparation method of the high temperature negative expansion micro-nano rice flour of a type β eucryptite structures, use natural spodumene ore, lithium carbonate and aluminium oxide for raw material, it is divided into target components according to eucryptite group to be matched, it pours into solvent, it is stirred into uniform sizing material, dry removal solvent, obtains uniformly mixed material system；Material system is placed in sintering furnace and carries out high temperature solid state reaction, after high temperature solid state reaction several hours, material is obtained through being quickly cooled down, which is subjected to ultra-fine grinding, classification, obtained superfine-material powder；Superfine-material powder feed is heat-treated in high temperature fluidized bed；Afterwards by powder drop, super extra gravity settling detaches after upper layer suspended nitride is diluted with water-soluble solvent, and extraction sediment is to get to class β eucryptite micro-nano powders.The method of the present invention is simple, and production cost is low, and obtained product negative thermal expansion coefficient is had excellent performance.
Description
Technical field
The invention belongs to inorganic non-metallic technical field of function materials, and in particular to the high temperature of a type beta-eucryptite structure
The preparation method of negative expansion micro-nano rice flour.
Background technology
The generally existing of expanding with heat and contract with cold of material in nature, and phenomenon of expanding with heat and contract with cold influences deeply nowadays integrated circuit
Far, when the coefficient of thermal expansion between ic substrate and chip material mismatches, thermal stress is will produce, so as to cause semiconductor
The chip service life.For this purpose, by select the material of related low-expansion coefficient or negative thermal expansion coefficient come compound circuit board then seem to
It closes important.Herein, material volume reduces as local environment temperature increases, i.e., the coefficient of thermal expansion of material is such less than zero
Material is referred to as negative thermal expansion material, wherein most typical represent is exactly beta-eucryptite.
Eucryptite is a kind of lithium aluminosilicate mineral, and molecular formula is LiAlSiO4 or Li2O Al2O3 2SiO2, is in round and smooth more
Lumps or star spot shape it is embedding be distributed in spodumene crystal or intercrystalline voids and crack in.One distinguishing feature of beta-eucryptite is
With anisotropic coefficient of thermal expansion.It is by force α c=- 176 × 10-7/ DEG C very much along C axis negative expansions effect, is slight along a axis
Be just expanded to a=92 α × 10-7/ DEG C, therefore material made of being accumulated by tiny crystals total shows as negative expansion macroscopical
Coefficient.
Since the beta-eucryptite mineral reserve quantity in nature is few, low output, therefore beta-eucryptite industrially is mostly
Artificial synthesized.Common beta-eucryptite synthetic method mainly has:High-temperature solid phase reaction method, sol-gel method, high score subnet
Network gel method and glass crystallization method etc..Currently, compare concentration is sol-gel method for research, and on sol-gel method basis
On some new preparation methods for growing up.
2010, XiaL. etc.（ChemCatChem, 2014, 6(12): 3409-3418.）With boehmite sol (
AlOOH), Ludox, 3 9H2O and LiNO3 of Al (NO3) are that raw material is aged after lithium-aluminium-Ludox is made, and are sintered,
It can get the beta-eucryptite powder of single crystalline phase.Meanwhile with the raising of heat treatment temperature, beta-eucryptite mutually increases, cristobalite
It mutually reduces, the negative expansion of beta-eucryptite gradually counteracts the positive expansion of residual glass phase, and the coefficient of thermal expansion of sample is gradually reduced.
2001, (the Materials Science and Engineering such as Ghosh: C, 2001, 16(1-2):
It 113-117.) then replaces metal alkoxide as raw material using the formates of metal, replaces ethyl alcohol as reaction medium using water, synthesize β-
Eucryptite powder.This effective, low cost sol-gel technology is referred to as " aqueous sol-gel method ".
Above method cost is higher, and economic transfer efficiency is relatively low, and difficulty is big and is difficult extensive go into operation.
Invention content
The technical problem to be solved by the present invention is in view of the problems of the existing technology, provide a type beta-eucryptite knot
The preparation method of the high temperature negative expansion micro-nano rice flour of structure.
The technical problem to be solved by the present invention is to what is realized by technical solution below, the present invention is a type β-
The preparation method of the high temperature negative expansion micro-nano rice flour of eucryptite structure, its main feature is that：Its step are as follows：
（a）Use natural spodumene ore, lithium carbonate and aluminium oxide for raw material, with mortar grinder at powder after, according to eucryptite
Group is divided into target components and is matched, and pours into solvent, is stirred into uniform sizing material, and dry removal is molten at room temperature or 60 DEG C
Agent obtains uniformly mixed material system；
（b）Material system is placed in sintering furnace and carries out high temperature solid state reaction, setting program Elevated Temperature Conditions and sintering duration,
After high temperature solid state reaction several hours, material is obtained through being quickly cooled down, which is subjected to ultra-fine grinding, classification, obtains grain size
For 10 μm ~ 30 μm of superfine-material powder；
（c）By superfine-material powder feed in high temperature fluidized bed, fluidized-bed temperature is maintained at certain numerical value, and material is through several small
When heat treatment after leave fluid bed；
（d）By powder under dispersant effect, by mechanical lapping, then settle；By the pulp separation of sedimentation layering, respectively
To concentration slurry and the upper layer suspended nitride of sinking；It is put into after upper layer suspended nitride is diluted 10 times ~ 30 times with water-soluble solvent super
In gravitational separation device, constant speed 3000r/min ~ 12000r/min, the separation of timing 3min ~ 60min super extra gravity settlings, extraction precipitation
Object is to get to class beta-eucryptite micro-nano powder.
In the preparation method of the high temperature negative expansion micro-nano rice flour of class beta-eucryptite structure of the present invention：Step（a）In
The mass ratio of the natural spodumene ore, lithium carbonate and aluminium oxide is 1：3~4：3~4.
In the preparation method of the high temperature negative expansion micro-nano rice flour of class beta-eucryptite structure of the present invention：Step（a）In
The solvent is water, and drying time is 12h ~ for 24 hours.
In the preparation method of the high temperature negative expansion micro-nano rice flour of class beta-eucryptite structure of the present invention：Step（b）In
Temperature programming condition is that 800 DEG C of heating rates are warming up to from 50 DEG C is 2.5 DEG C/min ~ 3.5 DEG C/min, after risen from 800 DEG C
Temperature to 1400 DEG C ~ 1500 DEG C progress solid phase reactions, heating rate is 1.5 DEG C/min ~ 2 DEG C/min；At 1400 DEG C ~ 1500 DEG C
The high temperature solid state reaction duration is 4h ~ 6h.
In the preparation method of the high temperature negative expansion micro-nano rice flour of class beta-eucryptite structure of the present invention：Step（b）In
The method for being quickly cooled down to obtain material be material is poured into the steel or iron ware that fill tap water at room temperature it is fast at room temperature
Quickly cooling is but.
In the preparation method of the high temperature negative expansion micro-nano rice flour of class beta-eucryptite structure of the present invention：Step（c）In
Fluidized-bed temperature is 1280 DEG C ~ 1320 DEG C, and material residence time in fluid bed is 3h ~ 6h.
In the preparation method of the high temperature negative expansion micro-nano rice flour of class beta-eucryptite structure of the present invention：Step（d）In
The mechanical lapping is to be ground using Ball-stirring mill, planetary mills or sand mill.
In the preparation method of the high temperature negative expansion micro-nano rice flour of class beta-eucryptite structure of the present invention：Step（d）In
The dispersant and water-soluble solvent is deionized water.
The present invention is main lithium, aluminium, silicon, oxygen element source using the natural spodumene ore of low cost, can significantly reduce cost,
And be combined by high temperature solid-state frit reaction and high temperature crystallization technology, can produce on a large scale 600 DEG C of temperature and with
Under mean thermal expansion coefficients be about -3.6 × 10-6℃-1Class beta-eucryptite structure high temperature negative expansion micro-nano powder.
Compared with prior art, the method for the present invention is simple, and production cost is low, and obtained product negative thermal expansion coefficient performance is excellent
It is different.
Description of the drawings
Fig. 1 is the XRD diffracting spectrums of preparation-obtained class beta-eucryptite micro-nano powder.
Fig. 2 is the coefficient of thermal expansion test result collection of illustrative plates of preparation-obtained class beta-eucryptite micro-nano powder.
Specific implementation mode
The specific technical solution of the present invention is further described referring to the drawings, in order to which those skilled in the art is into one
Step ground understands the present invention, without constituting the limitation to its right.
Embodiment 1, the preparation method of the high temperature negative expansion micro-nano rice flour of a type beta-eucryptite structure, its step are as follows：
（a）Using natural spodumene ore（Li2O-Al2O3-6~8SiO2）, lithium carbonate（Li2CO3）And aluminium oxide（Al2O3）For original
Material, with mortar grinder at powder after, be divided into target components according to eucryptite group and matched, natural spodumene ore（Li2O-
Al2O3-6~8 SiO2）, lithium carbonate（Li2CO3）And aluminium oxide（Al2O3）Mass ratio be 1：3~4：3 ~ 4, it pours into aqueous solvent,
It is stirred into uniform sizing material, dry removal solvent at room temperature or 60 DEG C, drying time is 12h ~ for 24 hours, is obtained uniformly mixed
Material system；
（b）Material system is placed in sintering furnace and carries out high temperature solid state reaction, setting program Elevated Temperature Conditions and sintering duration,
After high temperature solid state reaction several hours, material is obtained through being quickly cooled down, wherein temperature programming condition is to be warming up to 800 from 50 DEG C
DEG C heating rate is 2.5 DEG C/min ~ 3.5 DEG C/min, after 1400 DEG C ~ 1500 DEG C progress solid phase reactions are warming up to from 800 DEG C,
Heating rate is 1.5 DEG C/min ~ 2 DEG C/min；The high temperature solid state reaction duration is 4h ~ 6h at 1400 DEG C ~ 1500 DEG C；It will
The material carries out ultra-fine grinding, classification, obtains the superfine-material powder that grain size is 10 μm ~ 30 μm；It is wherein quickly cooled down to obtain object
The method of material is to pour into material in the steel or iron ware that fill tap water at room temperature to be quickly cooled down at room temperature.
（c）By superfine-material powder feed in high temperature fluidized bed, fluidized-bed temperature is 1280 DEG C ~ 1320 DEG C, and material is through 3h
Fluid bed is left after ~ 6h heat treatments；
（d）By powder under the action of dispersant deionized water, mechanical grinding is carried out by using Ball-stirring mill, planetary mills or sand mill
Mill, then settles；By the pulp separation of sedimentation layering, sinking concentration slurry and upper layer suspended nitride are respectively obtained；Upper layer is hanged
Laitance material is put into after diluting 10 times ~ 30 times with deionized water in hypergravity separator, constant speed 3000r/min ~ 12000r/min,
Timing 3min ~ 60min super extra gravity settlings detach, and extraction sediment is to get to class beta-eucryptite micro-nano powder.
Embodiment 2, the preparation method of the high temperature negative expansion micro-nano rice flour of a type beta-eucryptite structure, its step are as follows：
Take natural spodumene ore（Li2O-Al2O3-6~8 SiO2）：Lithium carbonate（Li2CO3）：Aluminium oxide（Al2O3）= 1：3：3
Powder is poured into water by quality proportioning, makes system at the slurry with certain fluidity, and is thoroughly mixed uniformly, 60 DEG C
It fully goes to remove water after lower dry 12h, obtains uniformly mixed material system.It is 2.5 that homogeneous material, which is placed in temperature programming condition,
DEG C/min after 50 DEG C are warming up to 800 DEG C, 1.5 DEG C/min of heating rate under the conditions of 800 DEG C are warming up to 1400 DEG C, carry out
Solid phase fusion reacts, and material is poured into the stainless steel for filling tap water at room temperature after lasting 6h heat preservations at 1400 DEG C
It is quickly cooled down in container, to obtained material, carries out ball milling ultra-fine grinding, classification, then the grain size that classification is obtained is 10 μm ~ 30
μm superfine-material powder feed is high temperature fluidized bed in 1280 DEG C, and stream material leaves fluid bed after 3h is heat-treated, and powder is existed
In water, with mechanical ball mill, then settle；By the pulp separation of sedimentation layering, respectively obtains lower layer's concentration slurry and upper layer suspends
Slurry；Hypergravity separator, super extra gravity settling separation are put into after suspended nitride is diluted 10 times with water, extraction precipitation obtains not
With the class beta-eucryptite micro-nano powder of grain size.
The XRD diffracting spectrums of preparation-obtained class beta-eucryptite micro-nano powder are as shown in Figure 1.The crystal of product powder
The feature crystalline phase of diffracting spectrum and beta-eucryptite（Eucryptite, PDF#75-2330）It coincide, specific peak and corresponding crystalline substance
Facial index is presented in fig. 1, it can be verified that there are beta-eucryptite crystal form in the class beta-eucryptite micro-nano powder being prepared,
Guarantee is provided for its negative expansion property.
Embodiment 3, the preparation method of the high temperature negative expansion micro-nano rice flour of a type beta-eucryptite structure, its step are as follows：
Take natural spodumene ore（Li2O-Al2O3-6~8 SiO2）：Lithium carbonate（Li2CO3）：Aluminium oxide（Al2O3）= 1：3.5：
The proportioning of 3.5 amount of substance, powder is poured into water, and makes system at the slurry with certain fluidity, and be thoroughly mixed
Uniformly, moisture removal is fully removed after dry 12h, obtains mixing uniform material system.Homogeneous material is placed in temperature programming condition
Be 3.5 DEG C/min after 50 DEG C are warming up to 800 DEG C, 2 DEG C/min of heating rate under the conditions of 800 DEG C are warming up to 1450 DEG C, into
Row solid phase fusion reacts, and material is poured into the stainless steel for filling tap water at room temperature after lasting 5h heat preservations at 1450 DEG C
It is quickly cooled down in container, to obtained material, carries out ball milling ultra-fine grinding, classification, then it is 10 μm ~ 30 that classification, which is obtained grain size,
μm superfine-material powder feed it is high temperature fluidized bed in 1300 DEG C, stream material leaves fluid bed after 6h is heat-treated, by powder
In water, it with mechanical ball mill, then settles；By the pulp separation of sedimentation layering, respectively obtains lower layer's concentration slurry and upper layer is outstanding
Laitance material；Hypergravity separator, super extra gravity settling separation are put into after suspended nitride is diluted 20 times with water, extraction precipitation obtains
Class beta-eucryptite micro-nano powder.
The coefficient of thermal expansion test result collection of illustrative plates of preparation-obtained class beta-eucryptite micro-nano powder is as shown in Fig. 2.
By measuring obtained coefficient of thermal expansion figure, it can be seen that the coefficient of expansion of obtained class beta-eucryptite micro-nano powder exists
At 600 DEG C or less, numerical value at 400 DEG C always 0 hereinafter, wherein nearby reach minimum -4.7 × 10-6℃-1, product is put down
The equal coefficient of expansion is about -3.6 × 10-6℃-1, product shows excellent.
Embodiment 4, the preparation method of the high temperature negative expansion micro-nano rice flour of a type beta-eucryptite structure, its step are as follows：
Take natural spodumene ore（Li2O-Al2O3-6~8 SiO2）：Lithium carbonate（Li2CO3）：Aluminium oxide（Al2O3）= 1：4：4 matter
The proportioning of amount, powder is poured into water, and makes system at the slurry with certain fluidity, and is thoroughly mixed uniformly, room temperature
Moisture removal is fully removed after lower drying for 24 hours, obtains mixing the material system having.Then homogeneous material is placed in temperature programming condition
Be 3.0 DEG C/min after 50 DEG C are warming up to 800 DEG C, 2 DEG C/min of heating rate under the conditions of 800 DEG C are warming up to 1500 DEG C, into
Row solid phase fusion reacts, and material is poured into the stainless steel for filling tap water at room temperature after lasting 4h heat preservations at 1500 DEG C
It is quickly cooled down in container, to obtained material, carries out ball milling ultra-fine grinding, classification, then it is 10 μm ~ 30 that classification, which is obtained grain size,
μm superfine-material powder feed it is high temperature fluidized bed in 1320 DEG C, stream material leaves fluid bed after 4h is heat-treated, by powder
In water, it with mechanical ball mill, then settles；By the pulp separation of sedimentation layering, respectively obtains lower layer's concentration slurry and upper layer is outstanding
Laitance material；Hypergravity separator, super extra gravity settling separation are put into after suspended nitride is diluted 30 times with water, extraction precipitation obtains
Class beta-eucryptite micro-nano powder.
Claims (8)
1. the preparation method of the high temperature negative expansion micro-nano rice flour of a type beta-eucryptite structure, which is characterized in that its step are as follows：
Use natural spodumene ore, lithium carbonate and aluminium oxide for raw material, with mortar grinder at powder after, according to eucryptite component
It is matched, is poured into solvent for target components, be stirred into uniform sizing material, dry removal solvent at room temperature or 60 DEG C obtains
To uniformly mixed material system；
Material system is placed in sintering furnace and carries out high temperature solid state reaction, setting program Elevated Temperature Conditions and sintering duration are high
After warm solid phase reaction several hours, material is obtained through being quickly cooled down, which is subjected to ultra-fine grinding, classification, obtains 10 μ of grain size
The superfine-material powder of m ~ 30 μm；
By superfine-material powder feed in high temperature fluidized bed, fluidized-bed temperature is maintained at certain numerical value, and material was through several hours warm
Fluid bed is left after processing；
By powder under dispersant effect, by mechanical lapping, then settle；By the pulp separation of sedimentation layering, respectively obtain
Sink concentration slurry and upper layer suspended nitride；It is put into after upper layer suspended nitride is diluted 10 times ~ 30 times with water-soluble solvent overweight
In power separator, constant speed 3000r/min ~ 12000r/min, the separation of timing 3min ~ 60min super extra gravity settlings, extraction precipitation
Object is to get to class beta-eucryptite micro-nano powder.
2. preparation method according to claim 1, it is characterised in that：Step（a）Described in natural spodumene ore, carbonic acid
The mass ratio of lithium and aluminium oxide is 1：3~4：3~4.
3. preparation method according to claim 1, it is characterised in that：Step（a）Described in solvent be water, drying time is
12h ~24h。
4. preparation method according to claim 1, it is characterised in that：Step（b）Program Elevated Temperature Conditions are to be risen from 50 DEG C
Temperature to 800 DEG C of heating rates are 2.5 DEG C/min ~ 3.5 DEG C/min, after be warming up to 1400 DEG C ~ 1500 DEG C from 800 DEG C and consolidated
Phase reaction, heating rate are 1.5 DEG C/min ~ 2 DEG C/min；The high temperature solid state reaction duration is 4h at 1400 DEG C ~ 1500 DEG C
~6h。
5. preparation method according to claim 1, it is characterised in that：Step（b）In be quickly cooled down to obtain the method for material
It is to pour into material in the steel or iron ware that fill tap water at room temperature to be quickly cooled down at room temperature.
6. preparation method according to claim 1, it is characterised in that：Step（c）Middle fluidized-bed temperature is 1280 DEG C ~ 1320
DEG C, material residence time in fluid bed is 3h ~ 6h.
7. preparation method according to claim 1, it is characterised in that：Step（d）Described in mechanical lapping be using stir
Mill, planetary mills or sand mill are ground.
8. preparation method according to claim 1, it is characterised in that：Step（d）Described in dispersant and water solubility
Solvent is deionized water.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112250078A (en) * | 2020-10-29 | 2021-01-22 | 淄博辰东新材料有限公司 | Ultralow-expansion-coefficient eucryptite and preparation method thereof |
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| CN101439932A (en) * | 2008-12-26 | 2009-05-27 | 中国地质科学院尾矿利用技术中心 | Low-expansion glass-ceramics with lithia ore tailings as principal raw material and manufacturing method thereof |
| CN104803666A (en) * | 2015-04-16 | 2015-07-29 | 南京理工大学 | LiAlSiO4 microspheres with negative thermal expansion coefficient and preparation method of LiAlSiO4 microspheres |
| CN106111103A (en) * | 2016-06-26 | 2016-11-16 | 桂林理工大学 | LiAlSiO4application as visible light-responded photocatalyst |
| CN106379908A (en) * | 2015-10-23 | 2017-02-08 | 北京中材人工晶体研究院有限公司 | Simple, convenient and environment-friendly preparation method for beta-eucryptite powder |
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2018
- 2018-05-11 CN CN201810451136.2A patent/CN108584970A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101439932A (en) * | 2008-12-26 | 2009-05-27 | 中国地质科学院尾矿利用技术中心 | Low-expansion glass-ceramics with lithia ore tailings as principal raw material and manufacturing method thereof |
| CN104803666A (en) * | 2015-04-16 | 2015-07-29 | 南京理工大学 | LiAlSiO4 microspheres with negative thermal expansion coefficient and preparation method of LiAlSiO4 microspheres |
| CN106379908A (en) * | 2015-10-23 | 2017-02-08 | 北京中材人工晶体研究院有限公司 | Simple, convenient and environment-friendly preparation method for beta-eucryptite powder |
| CN106111103A (en) * | 2016-06-26 | 2016-11-16 | 桂林理工大学 | LiAlSiO4application as visible light-responded photocatalyst |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112250078A (en) * | 2020-10-29 | 2021-01-22 | 淄博辰东新材料有限公司 | Ultralow-expansion-coefficient eucryptite and preparation method thereof |
| CN112250078B (en) * | 2020-10-29 | 2023-01-31 | 淄博辰东新材料有限公司 | Ultralow-expansion-coefficient eucryptite and preparation method thereof |
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