CN108193268A - A kind of crystalline material and its preparation method and application - Google Patents
A kind of crystalline material and its preparation method and application Download PDFInfo
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- CN108193268A CN108193268A CN201711351658.7A CN201711351658A CN108193268A CN 108193268 A CN108193268 A CN 108193268A CN 201711351658 A CN201711351658 A CN 201711351658A CN 108193268 A CN108193268 A CN 108193268A
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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
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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
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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Abstract
The invention discloses a kind of crystalline material, chemical formula Mg11(HPO3)8(OH)6, 0.2~2.5 μm of UV, visible light near infrared band reflectivity is more than 88%, while it is more than 0.90 in 2.5~25 μm of mid and far infrared wave band emissivity.The invention also discloses the preparation methods of above-mentioned crystalline material：Based on four water magnesium acetates, phosphorous acid starting material, while hexamethylene amine template is added, Mg is prepared by hydrothermal synthesis method11(HPO3)8(OH)6Crystal powder.The crystalline material of the present invention can combine well to be reflected and radiates comprehensive performance, and practical cooling-down effect can be applied than common 2~10 DEG C of heat-reflecting material titanium dioxide in the market in heat reflection infra-red radiation field well.
Description
Technical field
The present invention relates to crystalline material, more particularly to it is a kind of have simultaneously UV, visible light near-infrared high reflectance and in it is remote red
Outer high-emissivity material and preparation method thereof.
Background technology
Global warming is a severe environmental problem, be can not be underestimated.Unquestionably, the continuous of huge greenhouse gases is brought
Increased energy consumption becomes main cause.The energy usage amount of China increased to from 0.59 hundred million tons of standard coal equivalents of 1980
29.2 hundred million tons in 2009.2011, building energy consumption accounted for the 27.5% of whole total energy consumptions, and to the year two thousand twenty, this ratio will
Rise to 35%.There is no the passive cooling of any electric power input or cooling that may be consumed to global energy and generate significant impact.
Ultraviolet-visible-the near infrared region of passive cooling or cooling material in solar energy has high reflectivity, simultaneously
Self-energy can be passed through to air infrared window as much as possible in a manner of infra-red radiation in 8~13um wave bands again, efficiently
Air outer layer is emitted to, achievees the purpose that comprehensive cooling or refrigeration so as to reflect and emit to combine.
In the research passively cooled down in the daytime, Aaswath P.Raman describe one kind by seven layers of HfO2And SiO2Composition
Integrated photon solar reflector and hot emitter, they reflect 97% incident sunlight, while strong in air transparent window
It is strong to be selectively emitted.Eden Rephaeli companies use five layers of a- quartz, SiC, MgF2, TiO2It is unique micro- with Ag etc.
Shape devises passive cooling device.Test device has low absorptivity in solar spectrum, has high emission in atmospheric window
Rate.To sum up largely research all concentrates in the design of device passive radiating area of current daytime, i.e. the knot in reflecting layer and emission layer
It closes.Wherein most is complicated, by technology of preparing.
Invention content
In order to overcome the disadvantages mentioned above of the prior art with insufficient, the purpose of the present invention is to provide a kind of crystalline material,
0.2~2.5 μm of UV, visible light near infrared band reflectivity is up to more than 88%, while it is in 2.5~25 μm of mid and far infrared wave bands
Emissivity is up to more than 0.90.
It is simple for process another object of the present invention is to provide a kind of preparation method of crystalline material.
It is still another object of the present invention to provide the applications of above-mentioned crystalline material.
The purpose of the present invention is achieved through the following technical solutions：
A kind of crystalline material, chemical formula Mg11(HPO3)8(OH)6。
The crystalline material, 0.2~2.5 μm of UV, visible light near infrared band reflectivity are more than 88%, while its
It is more than 0.90 in 2.5~25 μm of mid and far infrared wave band emissivity.
A kind of preparation method of crystalline material, includes the following steps：
(1) it is 1 according to mol ratio:0.5~1.5 weighs four acetate hydrate magnesium and phosphorous acid, adds in deionized water dissolving,
Stirring 15~30 minutes, obtains solution；
(2) hexamethylene amine template is added in the solution obtained in step (1), continues stirring 0.5~1.5 hour, obtains breast
Turbid；The volume ratio of the hexamethylene amine template and emulsion is 1:4.8~1:12；
(3) mixed liquor that step (2) obtains is reacted in autoclave, and reaction temperature is 140~180 DEG C；
(4) it after reacting 2000 minutes, is filtered after obtained solution cooling, grinds, obtain after obtained solid is dried
Powdered crystalline material, chemical formula Mg11(HPO3)8(OH)6。
The preparation method of the crystalline material, step (1) described stirring, specially：By the way of magnetic agitation, turn
Speed is 200~400r/min.
The preparation method of the crystalline material, step (3) described mixed liquor are reacted in autoclave, specifically
For：
The emulsion being stirred is added in composite high pressure reaction kettle, by composite high pressure reaction kettle be placed in drying box into
Row reaction.
The preparation method of the crystalline material, step (4) described drying, specially：It is dried in 80~110 DEG C.
The application of the crystalline material, as heat reflection infrared radiant material.
The application of the crystalline material, with Mg11(HPO3)8(OH)6Heat reflection infrared radiating coating is made for color stuffing.
Compared with prior art, the present invention has the following advantages and beneficial effect：
(1) crystalline material of the invention, while there is higher UV, visible light near-infrared high reflectance and mid and far infrared height
Emissivity material, 0.2~2.5 μm of UV, visible light near infrared band reflectivity is up to more than 88%, while it is at 2.5~25 μm
Mid and far infrared wave band emissivity is up to more than 0.90.
(2) preparation method of crystalline material of the invention, preparation process is simple, the excellent material performance that is prepared,
(3) crystalline material of the invention can combine and reflect and radiate comprehensive performance well, and practical cooling-down effect compares market
Upper common 2~10 DEG C of heat-reflecting material titanium dioxide, can apply well in heat reflection infra-red radiation field.
Description of the drawings
Fig. 1 is Mg prepared by the embodiment of the present invention 111(HPO3)8(OH)6Refine XRD diagram.
Fig. 2 a are the micrograph of the hair of the body surface of silver-colored ant in desert.
Fig. 2 b are Mg prepared by the embodiment of the present invention 111(HPO3)8(OH)6Surface surface sweeping electron microscope.
Fig. 3 is Mg prepared by the embodiment of the present invention 111(HPO3)8(OH)6With most common heat-reflecting material two in the market
The cooling-down effect comparison diagram of titanium oxide.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1
It is 0.5 by mol ratio:1 weighs tetra- acetate hydrate magnesium of 2.144g and 1.64g phosphorous acid solid powders, is poured into
In beaker, with deionized water dissolving, magnetic stir bar stirring is added in, rotating speed adds in 5ml rings after being adjusted to 400 revs/min, 15 minutes
Hexylamine is stirred for 15 minutes after covering preservative film, obtains uniform emulsion, wherein, the volume of cyclohexylamine and the body of emulsion
Product is than being 1:12；Uniform emulsion is put into reaction kettle, then reaction kettle is placed in an oven, setting oven temperature is 140
DEG C, 2000 minutes reaction time.It takes out after complete reaction, it is small to be dried at 80 DEG C 5 by washing filtering for the sample on filter paper
When, the sample of uniform particle diameter is can obtain after grinding.
2.5~25 μm of mid and far infrared wave band emissivity test results of the sample are 0.914,0.2~2.5 μm of UV, visible light
Near infrared band reflectivity is 0.87.
Fig. 1 is the refine XRD analog result figures of sample manufactured in the present embodiment.With Co in ICSD databases11(HPO3)8
(OH)6Crystal structure (ICSD#72431) for modeling basis, Co atoms are replaced with into Mg atoms, pass through Rietveld refine sides
Method obtains its analogue value and experiment value error Rwp=8.98%, and credible result degree is higher.Refine XRD has found that the substance of synthesis is
A kind of newly synthesized crystalline material, chemical formula Mg11(HPO3)8(OH)6。
Fig. 2 a are the face shape appearance figure of sample manufactured in the present embodiment.It was found that its surface topography is similar to silver-colored ant (quilt in desert
Prove simultaneously there is visible ray high reflectance and infrared high emissivity) body surface (Fig. 2 b), this is also Mg11(HPO3)8
(OH)6With good heat reflection and the reason of radiation effect.
Fig. 3 is Mg manufactured in the present embodiment11(HPO3)8(OH)6With most common heat-reflecting material titanium dioxide in the market
Cooling-down effect comparison diagram.With Mg11(HPO3)8(OH)6After making coating for color stuffing, it is anti-with most common heat in the market to test it
It penetrates material silica titanium coating and is cooling Experimental comparison, cooling-down effect is sunny when than titanium dioxide 2~10
℃。
Embodiment 2
It is 1 by mol ratio:1 weighs tetra- acetate hydrate magnesium of 4.289g and 1.64g phosphorous acid solid powders, is poured into burning
In cup, with deionized water dissolving, magnetic stir bar stirring is added in, rotating speed is adjusted to 300 revs/min, 12.5ml is added in after 15 minutes
Cyclohexylamine is stirred for 15 minutes after covering preservative film, obtains uniform emulsion, wherein, the volume of cyclohexylamine and emulsion
Volume ratio is 1:4.8；Uniform emulsion is put into reaction kettle, then reaction kettle is placed in an oven, setting oven temperature is
160 DEG C, 2000 minutes reaction time.It takes out after complete reaction, the sample on filter paper is dried 3 by washing filtering at 100 DEG C
Hour, the sample of uniform particle diameter is can obtain after grinding.
2.5~25 μm of mid and far infrared wave band emissivity test results of the sample are 0.928,0.2~2.5 μm of UV, visible light
Near infrared band reflectivity is 0.88.
Mg manufactured in the present embodiment11(HPO3)8(OH)6Test result it is similar to Example 1, details are not described herein.
Embodiment 3
It is 2 by mol ratio:1 weighs tetra- acetate hydrate magnesium of 8.578g and 1.64g phosphorous acid solid powders, is poured into burning
In cup, with deionized water dissolving, magnetic stir bar stirring is added in, rotating speed is adjusted to 200 revs/min, adds in 10ml rings after twenty minutes
Hexylamine is stirred for 20 minutes after covering preservative film, obtains uniform emulsion, wherein, the volume of cyclohexylamine and the body of emulsion
Product is than being 1:6；Uniform emulsion is put into reaction kettle, then reaction kettle is placed in an oven, setting oven temperature is 180
DEG C, 2000 minutes reaction time.It takes out after complete reaction, it is small to be dried at 110 DEG C 2 by washing filtering for the sample on filter paper
When, the sample of uniform particle diameter is can obtain after grinding.
2.5~25 μm of mid and far infrared wave band emissivity test results of the sample are 0.933,0.2~2.5 μm of UV, visible light
Near infrared band reflectivity is 0.89.
Mg manufactured in the present embodiment11(HPO3)8(OH)6Test result it is similar to Example 1, details are not described herein.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by the embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (8)
- A kind of 1. crystalline material, which is characterized in that chemical formula Mg11(HPO3)8(OH)6。
- 2. crystalline material according to claim 1, which is characterized in that its 0.2~2.5 μm of UV, visible light near infrared band is anti- It is more than 88% to penetrate rate, while it is more than 0.90 in 2.5~25 μm of mid and far infrared wave band emissivity.
- 3. a kind of preparation method of crystalline material, which is characterized in that include the following steps：(1) it is 1 according to mol ratio：0.5~1.5 weighs four acetate hydrate magnesium and phosphorous acid, adds in deionized water dissolving, stirring 15~30 minutes, obtain solution；(2) hexamethylene amine template is added in the solution obtained in step (1), continues stirring 0.5~1.5 hour, obtains emulsion； The volume ratio of the hexamethylene amine template and emulsion is 1:4.8~1:12；(3) mixed liquor that step (2) obtains is reacted in autoclave, and reaction temperature is 140~180 DEG C；(4) it after reacting 2000 minutes, is filtered after obtained solution cooling, is ground after obtained solid is dried, obtain powder Shape crystalline material, chemical formula Mg11(HPO3)8(OH)6。
- 4. the preparation method of crystalline material according to claim 1, which is characterized in that step (1) described stirring, specifically For：By the way of magnetic agitation, rotating speed is 200~400r/min.
- 5. the preparation method of crystalline material according to claim 1, which is characterized in that step (3) described mixed liquor is in height It is reacted in pressure reaction kettle, specially：The emulsion being stirred is added in composite high pressure reaction kettle, composite high pressure reaction kettle is placed in drying box and is carried out instead It should.
- 6. the preparation method of crystalline material according to claim 1, which is characterized in that step (4) described drying, specifically For：It is dried in 80~110 DEG C.
- 7. the application of crystalline material described in claim 1, which is characterized in that as heat reflection infrared radiant material.
- 8. the application of crystalline material according to claim 7, which is characterized in that with Mg11(HPO3)8(OH)6For color stuffing system Make heat reflection infrared radiating coating.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711351658.7A CN108193268B (en) | 2017-12-15 | 2017-12-15 | Crystal material and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711351658.7A CN108193268B (en) | 2017-12-15 | 2017-12-15 | Crystal material and preparation method and application thereof |
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| CN108193268A true CN108193268A (en) | 2018-06-22 |
| CN108193268B CN108193268B (en) | 2020-08-18 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109837589A (en) * | 2019-03-29 | 2019-06-04 | 华南理工大学 | A kind of passive refrigerating crystal, passively refrigeration coating and its preparation method and application |
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|---|---|---|---|---|
| US20100018435A1 (en) * | 2008-07-28 | 2010-01-28 | Vorderbruggen Mark Alan | Compositions and methods to prevent corrosion by co2 on cement compositions |
| CN104692353A (en) * | 2015-01-30 | 2015-06-10 | 南京理工大学 | Porous near-infrared reflective heat insulation material and preparation method thereof |
| CN107215894A (en) * | 2017-06-09 | 2017-09-29 | 北京华腾新材料股份有限公司 | A kind of heat-insulated granules of pigments of bismoclite near-infrared high reflection and preparation method |
-
2017
- 2017-12-15 CN CN201711351658.7A patent/CN108193268B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100018435A1 (en) * | 2008-07-28 | 2010-01-28 | Vorderbruggen Mark Alan | Compositions and methods to prevent corrosion by co2 on cement compositions |
| CN104692353A (en) * | 2015-01-30 | 2015-06-10 | 南京理工大学 | Porous near-infrared reflective heat insulation material and preparation method thereof |
| CN107215894A (en) * | 2017-06-09 | 2017-09-29 | 北京华腾新材料股份有限公司 | A kind of heat-insulated granules of pigments of bismoclite near-infrared high reflection and preparation method |
Non-Patent Citations (1)
| Title |
|---|
| M. P. ATTFIELD, ET AL.: "Synthesis and structures of two isostructural phosphite, Fe11(HPO3)8(OH)6 and Mn11(HPO3)8(OH)6", 《ACTA CRYSTALLOGRAPHICA SECTION C》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109837589A (en) * | 2019-03-29 | 2019-06-04 | 华南理工大学 | A kind of passive refrigerating crystal, passively refrigeration coating and its preparation method and application |
| CN109837589B (en) * | 2019-03-29 | 2020-10-27 | 华南理工大学 | Passive refrigeration crystal, passive refrigeration coating, and preparation method and application thereof |
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