CN105621488A - Method for producing infrared absorbing powder - Google Patents
Method for producing infrared absorbing powder Download PDFInfo
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- CN105621488A CN105621488A CN201410615412.6A CN201410615412A CN105621488A CN 105621488 A CN105621488 A CN 105621488A CN 201410615412 A CN201410615412 A CN 201410615412A CN 105621488 A CN105621488 A CN 105621488A
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- infrared ray
- ray absorbing
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- 239000000843 powder Substances 0.000 title claims abstract description 133
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 claims abstract description 61
- 238000001354 calcination Methods 0.000 claims abstract description 39
- 150000003839 salts Chemical class 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 12
- 239000010937 tungsten Substances 0.000 claims abstract description 12
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 7
- 150000001340 alkali metals Chemical group 0.000 claims description 24
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical group O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 23
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 239000003638 chemical reducing agent Substances 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 150000001720 carbohydrates Chemical class 0.000 claims description 6
- 239000000571 coke Substances 0.000 claims description 6
- MIDXCONKKJTLDX-UHFFFAOYSA-N 3,5-dimethylcyclopentane-1,2-dione Chemical compound CC1CC(C)C(=O)C1=O MIDXCONKKJTLDX-UHFFFAOYSA-N 0.000 claims description 3
- 229930091371 Fructose Natural products 0.000 claims description 3
- 239000005715 Fructose Substances 0.000 claims description 3
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- 150000001450 anions Chemical class 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 3
- 235000013736 caramel Nutrition 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- 239000003610 charcoal Substances 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- 238000007602 hot air drying Methods 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 abstract 4
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 28
- 239000000243 solution Substances 0.000 description 25
- 229910052792 caesium Inorganic materials 0.000 description 21
- 238000001228 spectrum Methods 0.000 description 15
- 238000006722 reduction reaction Methods 0.000 description 9
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 239000013078 crystal Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 description 4
- 238000004880 explosion Methods 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- PYMIHQBVZWBTEV-UHFFFAOYSA-N oxotungsten;potassium Chemical compound [K].[W]=O PYMIHQBVZWBTEV-UHFFFAOYSA-N 0.000 description 2
- -1 tungsten ion Chemical class 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- YOUIDGQAIILFBW-UHFFFAOYSA-J Tungsten(IV) chloride Inorganic materials Cl[W](Cl)(Cl)Cl YOUIDGQAIILFBW-UHFFFAOYSA-J 0.000 description 1
- AIPOWKNDIGTUAO-UHFFFAOYSA-N [O].[Cl].[W] Chemical compound [O].[Cl].[W] AIPOWKNDIGTUAO-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 description 1
- NCMHKCKGHRPLCM-UHFFFAOYSA-N caesium(1+) Chemical compound [Cs+] NCMHKCKGHRPLCM-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- BGRYSGVIVVUJHH-UHFFFAOYSA-N prop-2-ynyl propanoate Chemical compound CCC(=O)OCC#C BGRYSGVIVVUJHH-UHFFFAOYSA-N 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- YXPHMGGSLJFAPL-UHFFFAOYSA-J tetrabromotungsten Chemical compound Br[W](Br)(Br)Br YXPHMGGSLJFAPL-UHFFFAOYSA-J 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- WQJQOUPTWCFRMM-UHFFFAOYSA-N tungsten disilicide Chemical compound [Si]#[W]#[Si] WQJQOUPTWCFRMM-UHFFFAOYSA-N 0.000 description 1
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 1
- KPGXUAIFQMJJFB-UHFFFAOYSA-H tungsten hexachloride Chemical compound Cl[W](Cl)(Cl)(Cl)(Cl)Cl KPGXUAIFQMJJFB-UHFFFAOYSA-H 0.000 description 1
- NXHILIPIEUBEPD-UHFFFAOYSA-H tungsten hexafluoride Chemical compound F[W](F)(F)(F)(F)F NXHILIPIEUBEPD-UHFFFAOYSA-H 0.000 description 1
- 229910021342 tungsten silicide Inorganic materials 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for preparing infrared absorption powder, which comprises the steps of dissolving tungsten-containing salts in water to form a solution; drying the solution to obtain a powder; and calcining the powder in a negative pressure environment to obtain the infrared absorption powder. The method for preparing the infrared absorption powder can also improve the production efficiency of the infrared absorption powder.
Description
Technical field
The present invention relates to the manufacture method of a kind of infrared ray absorbing powder, the manufacture method of espespecially a kind of infrared ray absorbing powder improving production efficiency and safety.
Background technology
Owing to tungsten oxide caesium has visible ray penetrance and the infrared ray shielding of excellence, tungsten oxide caesium is generally applied to make infrared absorbing film, to provide infrared ray absorbing and the function such as heat insulation. It is said that in general, in order to make infrared absorbing film, tungsten oxide caesium is first to be ground into nano_scale particle with powder kenel, is further dispersed in resinous substrates to form infrared absorbing film. In the prior art, the method manufacturing tungsten oxide caesium powder has two kinds, and first method is by tungstenic material and the Material Containment containing caesium in the chamber being filled with hydrogen, and is heated obtaining tungsten oxide caesium powder; And second method is that tungstenic material and the aqueous solution containing caesium material add reducing agent, and it is placed in the hydrothermal reactor of High Temperature High Pressure and carries out reduction reaction to obtain tungsten oxide caesium powder. But, the first method manufacturing tungsten oxide caesium powder likely can cause hydrogen explosion because of high temperature, increase the danger producing tungsten oxide caesium powder, and the method that the second manufactures tungsten oxide caesium powder must carry out reduction reaction in hydrothermal reactor, its production efficiency is relatively low, it is impossible to produce tungsten oxide caesium powder in large quantities.
Summary of the invention
The present invention provides the manufacture method of a kind of infrared ray absorbing powder improving production efficiency and safety, with the problem solving prior art.
The manufacture method of infrared ray absorbing powder of the present invention comprises soluble in water for tungstenic salt to form a solution; Dry this solution to obtain a powder; And this powder is carried out calcination processing to obtain this infrared ray absorbing powder in a subnormal ambient.
In an embodiment of the present invention, this manufacture method mixes a reducing agent in this powder before being separately included in and carrying out this calcination processing.
In an embodiment of the present invention, this reducing agent is selected from the group that is made up of sucrose, glucose, caramel, fructose and the carbohydrate containing carbohydrate.
In an embodiment of the present invention, this manufacture method be separately included in when carrying out calcination processing put one containing carbon feedstock by this powder.
In an embodiment of the present invention, should be selected from, containing carbon feedstock, the group that is made up of coke, activated carbon, Linesless charcoal and carbon black.
In an embodiment of the present invention, this powder is to carry out calcination processing between 650 degree and 850 degree Celsius.
In an embodiment of the present invention, the air pressure of this subnormal ambient is less than 160mm-Hg.
In an embodiment of the present invention, by soluble in water for this tungstenic salt with formed this solution for by soluble in water to alkali metal group metallic salt and this tungstenic salt to form this solution.
This alkali metal group metallic salt is by chemical formula M in an embodiment of the present inventionpN represents, M is alkali metal group element, and N is the anion with negative valency, 1��p��12.
In an embodiment of the present invention, this infrared ray absorbing powder is by chemical formula MxWO3-yRepresenting, M is alkali metal group element, and W is tungsten, and O is oxygen, 0.001 < x < 1,0��y < 0.8.
In an embodiment of the present invention, dry that the mode of this solution comprises spray drying, lyophilization, heat drying, microwave drying, vacuum drying, rotary heating dry and/or hot air drying.
In an embodiment of the present invention, this infrared ray absorbing powder is tungsten oxide powder, by chemical formula WOzRepresenting, W is tungsten, and O is oxygen, wherein 2.2��z��2.99.
Compared to prior art, the manufacture method of infrared ray absorbing powder of the present invention is to carry out calcination processing in subnormal ambient, to improve reducing environment when forming infrared ray absorbing powder. Owing to the manufacture method of infrared ray absorbing powder of the present invention need not carry out in the chamber be filled with hydrogen, therefore the manufacture method of infrared ray absorbing powder of the present invention does not have the problem of hydrogen explosion, and then increases the safety producing infrared ray absorbing powder. Furthermore, the manufacture method of infrared ray absorbing powder of the present invention is to carry out reduction reaction in calcining furnace, its volume of production can more than the volume of production carrying out reduction reaction in hydrothermal reactor, therefore, the manufacture method of infrared ray absorbing powder of the present invention can also improve the production efficiency of infrared ray absorbing powder.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the manufacture method of infrared ray absorbing powder of the present invention.
Fig. 2 is the flow chart of the manufacture method of infrared ray absorbing powder of the present invention.
Fig. 3 is the XRD figure spectrum of the first embodiment of infrared ray absorbing powder of the present invention.
Fig. 4 is the XRD figure spectrum of the second embodiment of infrared ray absorbing powder of the present invention.
Fig. 5 is the XRD figure spectrum of the 3rd embodiment of infrared ray absorbing powder of the present invention.
Fig. 6 is the XRD figure spectrum of the 4th embodiment of infrared ray absorbing powder of the present invention.
Fig. 7 is the XRD figure spectrum of the 5th embodiment of infrared ray absorbing powder of the present invention.
Description of reference numerals:
100, vacuum calcining stove;
110, containing cesium salt class;
120, tungstenic salt;
130, water;
A, solution;
B, powder;
C, reducing agent;
D, infrared ray absorbing powder;
210 to 230, step.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the invention will be further described, so that those skilled in the art can be better understood from the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Refer to Fig. 1. Fig. 1 is the schematic diagram of the manufacture method of infrared ray absorbing powder of the present invention. As it is shown in figure 1, the manufacture method of infrared ray absorbing powder of the present invention is first will to be dissolved in water 130 to form a solution A containing cesium salt class 110 and tungstenic salt 120. Cesium carbonate salt and cesium chloride salt can be chosen from containing cesium salt class 110. Tungstenic salt 120 can be wolframic acid, ammonium metatungstate, positive ammonium tungstate, ammonium paratungstate, alkali metal group tungstates, tungsten silicide, tungsten sulfide, chlorine oxygen tungsten, pure oxygen tungsten, tungsten hexachloride, tungsten tetrachloride, tungsten bromide, tungsten fluoride, tungsten carbide, oxidation of coal tungsten and other salt containing tungsten. After forming solution A, the manufacture method of infrared ray absorbing powder of the present invention can dry solution A to obtain a powder B. Dry that the mode of solution comprises spray drying, lyophilization, heat drying, microwave drying, vacuum drying, rotary heating dry and/or hot air drying etc. Can be uniformly dispersed containing cesium salt class and tungstenic salt in powder B. After obtaining powder B, the manufacture method of infrared ray absorbing powder of the present invention can add a reducing agent C, and mixes reducing agent C in powder B. Reducing agent C can be selected from the group being made up of sucrose, glucose, caramel, fructose and the carbohydrate containing carbohydrate. Finally, powder B can be carried out calcination processing to obtain infrared ray absorbing powder D by the manufacture method of infrared ray absorbing powder of the present invention in a subnormal ambient (such as in a vacuum calcining stove 100), that is tungsten oxide caesium powder.
In embodiments of the present invention, the air pressure of subnormal ambient when carrying out calcination processing is less than 160mm-Hg, so can reduce oxygen content in reaction chamber, and then improves reducing environment when powder B forms infrared ray absorbing powder. According to above-mentioned configuration, when manufacture method of the present invention is when carrying out calcination processing to powder B, it is not necessary to carry out in the chamber be filled with hydrogen, therefore manufacture method of the present invention does not have the problem of hydrogen explosion, and then increases the safety producing infrared ray absorbing powder. Furthermore, manufacture method of the present invention is to carry out reduction reaction in vacuum calcining stove 100, and its volume of production can more than the volume of production carrying out reduction reaction in hydrothermal reactor, say, that manufacture method of the present invention can improve the production efficiency of infrared ray absorbing powder.
It addition, in the manufacture method of infrared ray absorbing powder of the present invention, the mol ratio of the tungsten ion in solution A and cesium ion is 1:0.33, and powder B carries out calcination processing between 650 degree and 850 degree Celsius. Tungsten oxide caesium powder can by chemical formula CsxWO3-yRepresenting, Cs is caesium, and W is tungsten, and O is oxygen, 0.001 < x < 1,0��y < 0.8.
On the other hand, in embodiments of the present invention, reducing agent C is not necessarily intended in addition powder B, and powder B can also be directly placed in vacuum calcining stove 100 and carry out reduction reaction. Furthermore, in order to improve reducing environment further, the manufacture method of infrared ray absorbing powder of the present invention can put one containing carbon feedstock by powder B when carrying out calcination processing. The group being made up of coke, activated carbon, Linesless charcoal, carbon black can be selected from containing carbon feedstock.
Refer to the flow chart that Fig. 2, Fig. 2 are the manufacture methods of infrared ray absorbing powder of the present invention. Flow process such as the following step of the manufacture method of infrared ray absorbing powder of the present invention:
Step 210: will be soluble in water to form a solution containing cesium salt class and tungstenic salt;
Step 220: dry this mixed solution to obtain a powder; And
Step 230: this powder is carried out calcination processing to obtain this infrared ray absorbing powder in a subnormal ambient.
The flow process of the manufacture method of infrared ray absorbing powder of the present invention can also comprise other step, for instance can separately comprise mixing one reducing agent step in this powder between step 220 and step 230. Furthermore, when carrying out calcination processing in step 230, one can be put containing carbon feedstock by this powder.
For example, in the first embodiment of the invention, the manufacture method of infrared ray absorbing powder of the present invention is to be dissolved in deionized water by cesium carbonate salt and tungstates to form solution A. Solution A can be heated to 120 degree Celsius further and obtain powder B with complete transpiring moisture. Powder B is sufficiently mixed and is placed in reducing agent C in vacuum calcining stove again. The chamber of vacuum calcining stove under the subnormal ambient of 0mm-Hg, can heat to 750 degree Celsius with the heating rate of 15 degree Celsius of per minute afterwards. The chamber of vacuum calcining stove can naturally cool to room temperature after maintaining 10 hours at 750 degree Celsius again, so namely can obtain tungsten oxide caesium powder.
Refer to the XRD figure spectrum that Fig. 3, Fig. 3 are the first embodiments of infrared ray absorbing powder of the present invention. As it is shown on figure 3, analyze obtained XRD figure spectrum via X-ray diffractometer, the tungsten oxide caesium powder of first embodiment of the invention is hexagonal crystal system Cs0.33WO3Structure.
In second embodiment of the invention, the manufacture method of infrared ray absorbing powder of the present invention is to be dissolved in deionized water by cesium carbonate salt and tungstates to form solution A. Solution A can be heated to 120 degree Celsius further and obtain powder B with complete transpiring moisture. Powder B is directly placed in vacuum calcining stove again, and appropriate coke can be placed in by powder B. The chamber of vacuum calcining stove under the subnormal ambient of 0mm-Hg, can heat to 850 degree Celsius with the heating rate of 15 degree Celsius of per minute afterwards. The chamber of vacuum calcining stove can naturally cool to room temperature after maintaining 6 hours at 850 degree Celsius again, so namely can obtain tungsten oxide caesium powder.
Refer to the XRD figure spectrum that Fig. 4, Fig. 4 are the second embodiments of infrared ray absorbing powder of the present invention. As shown in Figure 4, analyzing obtained XRD figure spectrum via X-ray diffractometer, the tungsten oxide caesium powder of second embodiment of the invention is hexagonal crystal system Cs0.33WO3Structure.
In third embodiment of the invention, the manufacture method of infrared ray absorbing powder of the present invention is to be dissolved in deionized water to form solution A by cesium carbonate salt and ammonium metatungstate salt. Solution A can be heated to 120 degree Celsius further and obtain powder B with complete transpiring moisture. Powder B is directly placed in vacuum calcining stove again. The chamber of vacuum calcining stove under the subnormal ambient of 0mm-Hg, can heat to 800 degree Celsius with the heating rate of 5 degree Celsius of per minute afterwards. The chamber of vacuum calcining stove can naturally cool to room temperature after maintaining 6 hours at 800 degree Celsius again, so namely can obtain tungsten oxide caesium powder.
Refer to the XRD figure spectrum that Fig. 5, Fig. 5 are the 3rd embodiments of infrared ray absorbing powder of the present invention. As it is shown in figure 5, analyze obtained XRD figure spectrum via X-ray diffractometer, the tungsten oxide caesium powder of third embodiment of the invention is hexagonal crystal system Cs0.33WO3Structure.
On the other hand, in other embodiments of the present invention, (that is other alkali metal group metallic salt and tungstenic salt 120 can be dissolved in water 130 to form solution A by step 210) can be replaced by other alkali metal group metallic salt containing cesium salt class 110. Alkali metal group metallic salt is by chemical formula MpN represents, M is that alkali metal group element includes Li, Na, K, Rb, Cr or above-mentioned combination, and N is anion or the anion radical of band negative valency, 1��p��12. Alkali metal group metallic salt MpN can be alkali metal group carbonate, alkali metal group bicarbonate, alkali metal group nitrate, alkali metal group nitrite, alkali metal group hydroxide, alkali metal group halide salt, alkali metal group sulfate, alkali metal group sulphite and other at least one of which containing alkali metal group metallic salt. In other words, the infrared ray absorbing powder of above-mentioned formation can be by chemical formula MxWO3-yRepresenting, M is alkali metal group element, and W is tungsten, and O is oxygen, 0.001 < x < 1,0��y < 0.8.
For example, in fourth embodiment of the invention, the manufacture method of infrared ray absorbing powder of the present invention is to be dissolved in deionized water by potassium carbonate salt and tungstates to form solution A. Solution A can be heated to 120 degree Celsius further and obtain powder B with complete transpiring moisture. Powder B is directly placed in vacuum calcining stove again, and appropriate coke can be placed in by powder B. The chamber of vacuum calcining stove under the subnormal ambient of 0mm-Hg, can heat to 700 degree Celsius with the heating rate of 5 degree Celsius of per minute afterwards. The chamber of vacuum calcining stove can naturally cool to room temperature after maintaining 6 hours at 700 degree Celsius again, so namely can obtain tungsten oxide potassium powder.
Refer to the XRD figure spectrum that Fig. 6, Fig. 6 are the 4th embodiments of infrared ray absorbing powder of the present invention. As shown in Figure 6, analyzing obtained XRD figure spectrum via X-ray diffractometer, the tungsten oxide potassium powder of fourth embodiment of the invention is hexagonal crystal system K0.33WO3Structure.
Additionally, in the manufacture method of infrared ray absorbing powder of the present invention, being not necessarily intended to addition containing cesium salt class 110 or alkali metal group metallic salt in water 130, the manufacture method of infrared ray absorbing powder of the present invention can also only add tungstenic salt 120 in water 130 to form solution A (that is step 210 can be dissolved in water 130 by tungstenic salt 120 to form solution A).
For example, in fifth embodiment of the invention, the manufacture method of infrared ray absorbing powder of the present invention is to be dissolved in deionized water by tungstates to form solution A. Solution A can be heated to 120 degree Celsius further and obtain powder B with complete transpiring moisture. Powder B is directly placed in vacuum calcining stove again, and appropriate coke can be placed in by powder B. The chamber of vacuum calcining stove under the subnormal ambient of 0mm-Hg, can heat to 750 degree Celsius with the heating rate of 5 degree Celsius of per minute afterwards. The chamber of vacuum calcining stove can naturally cool to room temperature after maintaining 6 hours at 750 degree Celsius again, so namely can obtain tungsten oxide powder. Tungsten oxide powder can by chemical formula WOzRepresenting, W is tungsten, and O is oxygen, wherein 2.2��z��2.99.
Refer to the XRD figure spectrum that Fig. 7, Fig. 7 are the 5th embodiments of infrared ray absorbing powder of the present invention. As it is shown in fig. 7, analyze obtained XRD figure spectrum via X-ray diffractometer, the tungsten oxide powder of fifth embodiment of the invention is hexagonal crystal system WO2.72Structure.
Compared to prior art, the manufacture method of infrared ray absorbing powder of the present invention is to carry out calcination processing in subnormal ambient, to improve reducing environment when forming infrared ray absorbing powder. Owing to the manufacture method of infrared ray absorbing powder of the present invention need not carry out in the chamber be filled with hydrogen, therefore the manufacture method of infrared ray absorbing powder of the present invention does not have the problem of hydrogen explosion, and then increases the safety producing infrared ray absorbing powder. Furthermore, the manufacture method of infrared ray absorbing powder of the present invention is to carry out reduction reaction in calcining furnace, its volume of production can more than the volume of production carrying out reduction reaction in hydrothermal reactor, therefore, the manufacture method of infrared ray absorbing powder of the present invention can also improve the production efficiency of infrared ray absorbing powder.
Embodiment described above is only the preferred embodiment lifted for absolutely proving the present invention, and protection scope of the present invention is not limited to this. Equivalent replacement that those skilled in the art make on basis of the present invention or conversion, all within protection scope of the present invention. Protection scope of the present invention is as the criterion with claims.
Claims (12)
1. the manufacture method of an infrared ray absorbing powder, it is characterised in that comprise:
By soluble in water for tungstenic salt to form a solution;
Dry this solution to obtain a powder; And
This powder is carried out calcination processing to obtain this infrared ray absorbing powder in a subnormal ambient.
2. manufacture method as claimed in claim 1, it is characterised in that separately comprise:
A reducing agent was mixed in this powder before carrying out this calcination processing.
3. manufacture method as claimed in claim 2, it is characterised in that this reducing agent is selected from the group being made up of sucrose, glucose, caramel, fructose and the carbohydrate containing carbohydrate.
4. manufacture method as claimed in claim 1, it is characterised in that separately comprise: put when carrying out calcination processing containing carbon feedstock by this powder.
5. manufacture method as claimed in claim 4, it is characterised in that this is selected from the group being made up of coke, activated carbon, Linesless charcoal and carbon black containing carbon feedstock.
6. manufacture method as claimed in claim 1, it is characterised in that this powder is to carry out calcination processing between 650 degree and 850 degree Celsius.
7. manufacture method as claimed in claim 1, it is characterised in that the air pressure of this subnormal ambient is less than 160mm-Hg.
8. manufacture method as claimed in claim 1, it is characterised in that by soluble in water for this tungstenic salt with formed this solution for by soluble in water to alkali metal group metallic salt and this tungstenic salt to form this solution.
9. manufacture method as claimed in claim 8, it is characterised in that this alkali metal group metallic salt is by chemical formula MpN represents, M is alkali metal group element, and N is the anion with negative valency, 1��p��12.
10. manufacture method as claimed in claim 9, it is characterised in that this infrared ray absorbing powder is by chemical formula MxWO3-yRepresenting, M is alkali metal group element, and W is tungsten, and O is oxygen, wherein 0.001 < x < 1,0��y < 0.8.
11. manufacture method as claimed in claim 1, it is characterised in that dry that the mode of this solution comprises spray drying, lyophilization, heat drying, microwave drying, vacuum drying, rotary heating dry and/or hot air drying.
12. manufacture method as claimed in claim 1, it is characterised in that this infrared ray absorbing powder is tungsten oxide powder, by chemical formula WOzRepresenting, W is tungsten, and O is oxygen, wherein 2.2��z��2.99.
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| TW103135548A TWI607971B (en) | 2014-10-14 | 2014-10-14 | Manufacturing method of infrared absorption powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020158799A (en) * | 2019-03-25 | 2020-10-01 | 国立研究開発法人産業技術総合研究所 | Manufacturing method of noble metal hydrosol |
| CN115003631A (en) * | 2020-01-31 | 2022-09-02 | 住友金属矿山株式会社 | Electromagnetic wave absorbing particles, electromagnetic wave absorbing particle dispersion liquid, and method for producing electromagnetic wave absorbing particles |
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| CN1745149A (en) * | 2003-10-20 | 2006-03-08 | 住友金属矿山株式会社 | Infrared shielding material microparticle dispersion, infrared shield, process for producing infrared shielding material microparticle, and infrared shielding material microparticle |
| CN101428344A (en) * | 2008-12-17 | 2009-05-13 | 四川大学 | Nano-scale wolfram carbine composite powder and method of manufacturing the same |
| JP4666226B2 (en) * | 2006-05-18 | 2011-04-06 | 住友金属鉱山株式会社 | Near-infrared absorption filter for plasma display panel, method for producing the same, and plasma display panel |
| CN103539205A (en) * | 2013-11-15 | 2014-01-29 | 哈尔滨工业大学 | Method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles |
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| US8083847B2 (en) * | 2003-10-20 | 2011-12-27 | Sumitomo Metal Mining Co., Ltd. | Fine particle dispersion of infrared-shielding material, infrared-shielding body, and production method of fine particles of infrared-shielding material and fine particles of infrared-shielding material |
| CN103708558B (en) * | 2013-12-31 | 2015-09-09 | 大连工业大学 | Cs xwO yf zpowder and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1745149A (en) * | 2003-10-20 | 2006-03-08 | 住友金属矿山株式会社 | Infrared shielding material microparticle dispersion, infrared shield, process for producing infrared shielding material microparticle, and infrared shielding material microparticle |
| JP4666226B2 (en) * | 2006-05-18 | 2011-04-06 | 住友金属鉱山株式会社 | Near-infrared absorption filter for plasma display panel, method for producing the same, and plasma display panel |
| CN101428344A (en) * | 2008-12-17 | 2009-05-13 | 四川大学 | Nano-scale wolfram carbine composite powder and method of manufacturing the same |
| CN103539205A (en) * | 2013-11-15 | 2014-01-29 | 哈尔滨工业大学 | Method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles |
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| JP2020158799A (en) * | 2019-03-25 | 2020-10-01 | 国立研究開発法人産業技術総合研究所 | Manufacturing method of noble metal hydrosol |
| JP7182786B2 (en) | 2019-03-25 | 2022-12-05 | 国立研究開発法人産業技術総合研究所 | Method for producing precious metal hydrosol |
| CN115003631A (en) * | 2020-01-31 | 2022-09-02 | 住友金属矿山株式会社 | Electromagnetic wave absorbing particles, electromagnetic wave absorbing particle dispersion liquid, and method for producing electromagnetic wave absorbing particles |
Also Published As
| Publication number | Publication date |
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| CN105621488B (en) | 2017-08-25 |
| TW201613826A (en) | 2016-04-16 |
| TWI607971B (en) | 2017-12-11 |
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