CN107215851A - A kind of high heat insulation nano ceramic powder and its production and use - Google Patents
A kind of high heat insulation nano ceramic powder and its production and use Download PDFInfo
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- CN107215851A CN107215851A CN201610162831.8A CN201610162831A CN107215851A CN 107215851 A CN107215851 A CN 107215851A CN 201610162831 A CN201610162831 A CN 201610162831A CN 107215851 A CN107215851 A CN 107215851A
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- ceramic powder
- high heat
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- heat insulation
- titanium
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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
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/58007—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides
- C04B35/58014—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides based on titanium nitrides, e.g. TiAlON
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention discloses a kind of preparation method and purposes of high heat insulation nano ceramic powder.Described nano-powder refers to titanium nitride nanopower, and its rejection rate to infrared band is higher than 90%.The preparation method of the nano-powder is first to dissolve in the compound containing titanium source in effumability solvent；The compound containing nitrogen source is mixed into afterwards；Presoma to mixing under an inert atmosphere, carry out high-temperature heat treatment and obtain titanium nitride nanopower finally.Titanium nitride nanopower of the present invention, under ultraviolet light, with excellent stability and infrared light barrier property, can be applied to prepare energy-saving coatings, energy-conservation pad pasting, plastics modifier etc.；Moreover, preparation method of the present invention is simple, cost is low, and the cycle is short, it is easy to large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method and purposes of high heat insulation nano ceramic powder, belong to technical field of function materials.
Background technology
The research of environment amenable thermal isolation film is the hot research for optimizing China's building energy saving field, and the Innovation Input of large quantities of institutes and high-tech enterprise has been attracted in scientific circles and industrial quarters, and the preparation of high heat-insulated powder is the emphasis and difficult point in the field all the time.
At present, in terms of Nano Semiconductor Oxide being focused primarily on based on the heat-insulated powder of nano ceramics, such as tin indium oxide, tin-antiomony oxide, aluminum zinc oxide, gallium oxide aluminium, aluminum oxide cadmium, tin oxide cadmium, but these conductor oxidates are often in atmosphere and unstable, particularly when temperature is higher than 100 DEG C, it is easy to shine into the failure of these Nano Semiconductor Oxides；At the same time, these conductor oxidates do not have very strong weatherability, it is easily apt to deteriorate under the radiation of strong ultraviolet light when particularly incorporating in organic matter, therefore prepare the high heat-insulated nano-ceramic powder of high stable and just become the focus and difficult point of high heat-insulated powder.
In nitride, especially titanium nitride, it is a kind of very promising high heat-insulated semiconductor nano powder of preparation, there is very excellent barriering efficiency to the near infrared band of 760-1500 nano wavebands, and rarely have the method for inexpensively preparing this titanium nitride nanopower on a large scale at present, most of method is in the stage of experiment development or high investment, does not have also cost input few and the extensive method for preparing titanium nitride nano ceramic powder.
Therefore, if extensive prepare high difficult point of the heat-insulated titanium nitride nano ceramic powder as the heat-insulated field.
The content of the invention
The present invention in view of the above-mentioned problems existing in the prior art and demand, it is an object of the invention to provide a kind of preparation method and purposes for being prepared on a large scale high heat insulation nano ceramic powder, to meet the application requirement of energy-saving material.
For achieving the above object, the technical solution adopted by the present invention is as follows：A kind of high heat insulation nano ceramic powder, the nano-ceramic powder refers to titanium nitride nano ceramic powder, and its rejection rate to infrared band is higher than 90%.
The high heat insulation nano ceramic powder, it is characterised in that rejection rate of the nano-ceramic powder at 950 nano wavebands is higher than 95%.
The preparation method of described high heat insulation nano ceramic powder, comprises the following steps：
A) raw material containing titanium is added in the solvent of effumability；
B) raw material containing nitrogen is added to above-mentioned solvent, stirred to clarify transparent；
c）Volatile solvent in said mixture is evaporated, solid precipitation is obtained；
d）Obtained solid is heat-treated in inert atmosphere or reducing atmosphere.
The raw material of titanium is selected from the Organic Ingredients or inorganic raw material of titanium in the preparation method of described high heat insulation nano ceramic powder, the step a).
The preparation method of described high heat insulation nano ceramic powder, the Organic Ingredients of the titanium includes tetraethyl titanate, metatitanic acid orthocarbonate, butyl titanate or isopropyl titanate,
The preparation method of described high heat insulation nano ceramic powder, the inorganic raw material of the titanium includes：Titanium trifluoride, titanium tetrafluoride, titanium trichloride or titanium tetrachloride.
The preparation method of described high heat insulation nano ceramic powder, the volatile solvent includes：Methanol, ethanol, propyl alcohol, butanol, methyl acetate, ethyl acetate, butyl acetate, chloroform, tetrachloromethane, acetone, methyl ether or ether.
The preparation method of described high heat insulation nano ceramic powder, nitrogenous raw material described in the step b includes dimethylamine, trimethylamine, diethanol amine, triethanolamine, ethamine, ethylenediamine, propane diamine, hexamethylene diamine, tertiary amines, quaternary ammonium, hexamethyl triethylammonium tetrakis, urea or thiocarbamide.
The preparation method of described high heat insulation nano ceramic powder, described step d）Inert gas used includes nitrogen, argon gas, hydrogen, nitrogen and hydrogen mixture, argon hydrogen gaseous mixture, ammonia, nitrogen ammonia gaseous mixture, argon ammonia gaseous mixture.
Heat treatment temperature in the preparation method of described high heat insulation nano ceramic powder, step d) is 400~1500 DEG C, and heat treatment time is 5~1200 minutes.
The preparation method of described high heat insulation nano ceramic powder, the special treatment temperature is 500 to 1200 DEG C, and heat treatment time is 30~600 minutes.
There is coating or film prepared by high heat insulation nano ceramic powder described in any one.
Application of the described coating or film in energy-conservation pad pasting, energy-saving glass, plastics, weaving.
The present invention is adapted to the composite nano powder that a large-scale industrial production has infrared high obstructing performance.Composite nano powder prepared by the present invention can be used for preparing energy-saving coatings, energy-conservation pad pasting, energy-saving glass or other energy-saving electric components.
Brief description of the drawings
The crystal structure collection of illustrative plates of Fig. 1 titanium nitride nanopowers
The Optical transmission spectrum figure of Fig. 2 titanium nitride nano splits.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.
Embodiment
1
10 kg tetraethyl titanates, 20 kg methanol are weighed, 20 kg ethylenediamines, stirring are until clear transparent solutions, obtain solid matter by the way of vacuum distillation.Liquid obtained by distillation can be recycled.
Resulting solid precursor is put into annealing furnace, high-purity argon gas is passed through as protective atmosphere, temperature is slowly raised with 2-4 DEG C of speed per minute, 120 minutes is incubated at 800 DEG C or so, cools down afterwards, both can obtain the Nano titanium nitride powder of black.
The Nano titanium nitride of black is characterized using X-ray diffractometer and transmission electron microscope.
The crystal structure collection of illustrative plates of Fig. 1 titanium nitride nanopowers, the Optical transmission spectrum figure of Fig. 2 titanium nitride nano splits.
Embodiment
2
10 kg tetraethyl titanates, 20 kg ethanol are weighed, 20 kg propane diamine, stirring are until clear transparent solutions, obtain solid matter by the way of vacuum distillation.Liquid obtained by distillation can be recycled.
Resulting solid precursor is put into annealing furnace, high-purity argon gas is passed through as protective atmosphere, temperature is slowly raised with 2-4 DEG C of speed per minute, 120 minutes is incubated at 800 DEG C or so, cools down afterwards, both can obtain the Nano titanium nitride powder of black.
The Nano titanium nitride of black is characterized using X-ray diffractometer and transmission electron microscope.
Resulting XRD schemes similar with embodiment 1 with TEM.
Embodiment
3
10 kg butyl titanates, 20 kg isopropanols are weighed, 20 kg diethanol amine, stirring are until clear transparent solutions, obtain solid matter by the way of vacuum distillation.Liquid obtained by distillation can be recycled.
Resulting solid precursor is put into annealing furnace, high-purity argon gas is passed through as protective atmosphere, temperature is slowly raised with 2-4 DEG C of speed per minute, 120 minutes is incubated at 900 DEG C or so, cools down afterwards, both can obtain the Nano titanium nitride powder of black.
The Nano titanium nitride of black is characterized using X-ray diffractometer and transmission electron microscope.
Resulting XRD schemes similar with embodiment 1 with TEM.
Embodiment
4
10 kg titanium tetrachlorides, 20 kg ethanol are weighed, 40 kg urea, stirring are until clear transparent solutions, obtain solid matter by the way of vacuum distillation.Liquid obtained by distillation can be recycled.
Resulting solid precursor is put into annealing furnace, high-purity argon gas is passed through as protective atmosphere, temperature is slowly raised with 2-4 DEG C of speed per minute, 240 minutes is incubated at 800 DEG C or so, cools down afterwards, both can obtain the Nano titanium nitride powder of black.
The Nano titanium nitride of black is characterized using X-ray diffractometer and transmission electron microscope.
Resulting XRD schemes similar with embodiment 1 with TEM.
Embodiment
5
10 kg titanium tetrafluorides, 20 kg ethanol are weighed, 20 kg ethylenediamines, stirring are until clear transparent solutions, obtain solid matter by the way of vacuum distillation.Liquid obtained by distillation can be recycled.
Resulting solid precursor is put into annealing furnace, high-purity argon gas is passed through as protective atmosphere, temperature is slowly raised with 2-4 DEG C of speed per minute, 120 minutes is incubated at 800 DEG C or so, cools down afterwards, both can obtain the Nano titanium nitride powder of black.
The Nano titanium nitride of black is characterized using X-ray diffractometer and transmission electron microscope.
Resulting XRD schemes similar with embodiment 1 with TEM.
Embodiment
6
10 kg tetraethyl titanates, 20 kg ethanol are weighed, 20 kg propane diamine, stirring are until clear transparent solutions, obtain solid matter by the way of vacuum distillation.Liquid obtained by distillation can be recycled.
Resulting solid precursor is put into annealing furnace, high-purity argon gas is passed through as protective atmosphere, temperature is slowly raised with 2-4 DEG C of speed per minute, 120 minutes is incubated at 800 DEG C or so, cools down afterwards, both can obtain the Nano titanium nitride powder of black.
The Nano titanium nitride of black is characterized using X-ray diffractometer and transmission electron microscope.
Resulting XRD schemes similar with embodiment 1 with TEM.
Finally be necessary described herein be：Above example is served only for being described in more detail technical scheme; it is not intended that limiting the scope of the invention, some nonessential modifications and adaptations that those skilled in the art makes according to the above of the present invention belong to protection scope of the present invention.
Claims (13)
1. a kind of high heat insulation nano ceramic powder, it is characterised in that the nano-ceramic powder refers to titanium nitride nano ceramic powder, its rejection rate to infrared band is higher than 90%.
2. high heat-insulated rice ceramic powder as claimed in claim 1, it is characterised in that rejection rate of the nano-ceramic powder at 950 nano wavebands is higher than 95%.
3. the preparation method of high heat insulation nano ceramic powder as claimed in claim 1, it is characterised in that comprise the following steps：
A) raw material containing titanium is added in the solvent of effumability；
B) raw material containing nitrogen is added to above-mentioned solvent, stirred to clarify transparent；
c）Volatile solvent in said mixture is evaporated, solid precipitation is obtained；
d）Obtained solid is heat-treated in inert atmosphere or reducing atmosphere.
4. the preparation method of high heat insulation nano ceramic powder as claimed in claim 3, it is characterised in that the raw material of titanium is selected from the Organic Ingredients or inorganic raw material of titanium in the step a).
5. the preparation method of high heat insulation nano ceramic powder as claimed in claim 4, it is characterised in that the Organic Ingredients of the titanium includes tetraethyl titanate, metatitanic acid orthocarbonate, butyl titanate or isopropyl titanate.
6. the preparation method of high heat insulation nano ceramic powder as claimed in claim 4, it is characterised in that the inorganic raw material of the titanium includes：Titanium trifluoride, titanium tetrafluoride, titanium trichloride or titanium tetrachloride.
7. the preparation method of high heat insulation nano ceramic powder as claimed in claim 4, it is characterised in that tell that volatile solvent includes：Methanol, ethanol, propyl alcohol, butanol, methyl acetate, ethyl acetate, butyl acetate, chloroform, tetrachloromethane, acetone, methyl ether or ether.
8. the preparation method of high heat insulation nano ceramic powder as claimed in claim 4, it is characterized in that, nitrogenous raw material described in the step b includes dimethylamine, trimethylamine, diethanol amine, triethanolamine, ethamine, ethylenediamine, propane diamine, hexamethylene diamine, tertiary amines, quaternary ammonium, hexamethyl triethylammonium tetrakis, urea or thiocarbamide.
9. the preparation method of high heat insulation nano ceramic powder as claimed in claim 4, it is characterised in that described step d）Inert gas used includes nitrogen, argon gas, hydrogen, nitrogen and hydrogen mixture, argon hydrogen gaseous mixture, ammonia, nitrogen ammonia gaseous mixture, argon ammonia gaseous mixture.
10. the preparation method of high heat insulation nano ceramic powder as claimed in claim 4, it is characterised in that：Heat treatment temperature in step d) is 400~1500 DEG C, and heat treatment time is 5~1200 minutes.
11. the preparation method of high heat insulation nano ceramic powder as claimed in claim 4, it is characterised in that：The special treatment temperature is 500 to 1200 DEG C, and heat treatment time is 30~600 minutes.
12. a kind of coating or film with the preparation of high heat insulation nano ceramic powder with described in any one of claim 1~11.
13. the application of coating as claimed in claim 12 or film in energy-conservation pad pasting, energy-saving glass, plastics, weaving.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108585876A (en) * | 2018-03-26 | 2018-09-28 | 青岛桥海陶瓷新材料科技有限公司 | The preparation method of titanium nitride nanopower |
| CN108975339A (en) * | 2018-08-29 | 2018-12-11 | 龙岩学院 | A kind of transition metal carbide powder and transition metal carbide-nitridation composite powder preparation process |
| CN111517800A (en) * | 2020-04-20 | 2020-08-11 | 中国科学院合肥物质科学研究院 | Method for preparing high-purity superfine zirconium boride powder by grinding aid auxiliary sanding |
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| JPS63190703A (en) * | 1987-02-03 | 1988-08-08 | Nikon Corp | Thin filmy titanium nitride base substance |
| CN101298321A (en) * | 2008-05-30 | 2008-11-05 | 河南大学 | Preparation of titanium nitride nanopower |
| CN101462701A (en) * | 2009-01-09 | 2009-06-24 | 北京科技大学 | Method for preparing titanium nitride ceramic powder |
| CN101880445A (en) * | 2004-03-30 | 2010-11-10 | 嘉洛斯欧洲有限公司 | Polymer materials and additive thereof |
| CN103569977A (en) * | 2013-10-16 | 2014-02-12 | 河北联合大学 | Preparation method of TiN powder |
| CN103864030A (en) * | 2012-12-11 | 2014-06-18 | 浙江海洋学院 | Nanometer titanium nitride powder preparation method |
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2016
- 2016-03-22 CN CN201610162831.8A patent/CN107215851A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63190703A (en) * | 1987-02-03 | 1988-08-08 | Nikon Corp | Thin filmy titanium nitride base substance |
| CN101880445A (en) * | 2004-03-30 | 2010-11-10 | 嘉洛斯欧洲有限公司 | Polymer materials and additive thereof |
| CN101298321A (en) * | 2008-05-30 | 2008-11-05 | 河南大学 | Preparation of titanium nitride nanopower |
| CN101462701A (en) * | 2009-01-09 | 2009-06-24 | 北京科技大学 | Method for preparing titanium nitride ceramic powder |
| CN103864030A (en) * | 2012-12-11 | 2014-06-18 | 浙江海洋学院 | Nanometer titanium nitride powder preparation method |
| CN103569977A (en) * | 2013-10-16 | 2014-02-12 | 河北联合大学 | Preparation method of TiN powder |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108585876A (en) * | 2018-03-26 | 2018-09-28 | 青岛桥海陶瓷新材料科技有限公司 | The preparation method of titanium nitride nanopower |
| CN108585876B (en) * | 2018-03-26 | 2021-02-02 | 青岛桥海陶瓷新材料科技有限公司 | Preparation method of titanium nitride nano powder |
| CN108975339A (en) * | 2018-08-29 | 2018-12-11 | 龙岩学院 | A kind of transition metal carbide powder and transition metal carbide-nitridation composite powder preparation process |
| CN108975339B (en) * | 2018-08-29 | 2021-12-28 | 龙岩学院 | Preparation process of transition metal carbide powder and transition metal carbide-nitride composite powder |
| CN111517800A (en) * | 2020-04-20 | 2020-08-11 | 中国科学院合肥物质科学研究院 | Method for preparing high-purity superfine zirconium boride powder by grinding aid auxiliary sanding |
| CN111517800B (en) * | 2020-04-20 | 2022-04-01 | 中国科学院合肥物质科学研究院 | Method for preparing high-purity superfine zirconium boride powder by grinding aid auxiliary sanding |
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Application publication date: 20170929 |