CN107954467B - A kind of silver-colored, bismuth doping cadmium oxide near-infrared high reflection raw powder's production technology - Google Patents
A kind of silver-colored, bismuth doping cadmium oxide near-infrared high reflection raw powder's production technology Download PDFInfo
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- CN107954467B CN107954467B CN201711070059.8A CN201711070059A CN107954467B CN 107954467 B CN107954467 B CN 107954467B CN 201711070059 A CN201711070059 A CN 201711070059A CN 107954467 B CN107954467 B CN 107954467B
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Abstract
The invention discloses a kind of silver, bismuths to adulterate cadmium oxide near-infrared high reflection raw powder's production technology, belongs to cadmium oxide near-infrared high reflection powder technology field.The following steps are included: (1) chooses primary raw material cadmium salt, and silver salt and bismuth salt are chosen collectively as doped raw material, by cadmium salt, doped raw material 1:(0.01~0.10 in molar ratio) it is added in reaction dissolvent and carries out mixing treatment；(2) it is gradually added into diluted alkaline into precursor solution, adjusts the pH to 8~9 of precursor solution；(3) precursor solution is placed in the closed hydrothermal reaction kettle with blender, under the conditions of 120~260 DEG C, is stirred to react 5~20h；(4) reaction precipitate is carried out after sufficiently washing, dry, crushing is calcined to get target product is arrived.Preparation process of the present invention is simple, consumes energy low, and equipment is simple, and product purity is high, can directly applicable industry metaplasia produce；And obtained silver, bismuth doping cadmium oxide diameter of particle is small, narrowly distributing is not easy to reunite, and stability is good.
Description
Technical field
The present invention relates to a kind of silver, bismuths to adulterate cadmium oxide near-infrared high reflection raw powder's production technology, and it is close to belong to cadmium oxide
Infrared high reflection powder technology field.
Background technique
Bismuth ion is the third class near infrared band active ions of discovery after transition metal ions and rare earth ion.
Such as 1999, Murata etc. had found the broad-band illumination of near infrared band in the zeolite that bismuth adulterates.Subsequent 2001,
Fujimoto etc. has also discovered this phenomenon in the sillico aluminate glass that bismuth adulterates.So far, using bismuth as the close of the P p-block element p of representative
IR fluorescence phenomenon has come into the sight of people, has obtained extensive concern, opens newly for the application of near infrared band fluorescence
Field.The near-infrared fluorescent phenomenon that the material of especially bismuth doping generates, it will bring another revolution to optical communication.Silver from
Son has near-infrared reflection function, while also having ultraviolet absorption ability.Cadmium oxide, as the transparent conductive oxide more early found,
Its forbidden bandwidth is small, there is high visible light transmittance.Therefore, using silver, bismuth adulterates cadmium oxide, promotes its near-infrared reflection energy
Power.
The near infrared reflectivity of the infrared heat insulation nano material prepared at present is not high, and production cost is relatively high, does not answer
For large-scale industrial production.
Summary of the invention
Technical problem to be solved by the present invention lies in: a kind of silver-colored, bismuth doping cadmium oxide near-infrared high reflection powder is provided
Preparation method, the near infrared reflectivity that it solves the infrared heat insulation nano material prepared at present is not high, and production cost is opposite
It is higher, be applied to large-scale industrial production the problem of.
The technical problems to be solved by the invention take following technical scheme to realize:
A kind of silver-colored, bismuth doping cadmium oxide near-infrared high reflection raw powder's production technology, comprising the following steps:
(1) primary raw material cadmium salt is chosen, and chooses silver salt and bismuth salt collectively as doped raw material, wherein in doped raw material
Molar ratio containing silver salt and bismuth salt is 1:(0.1~10), by cadmium salt, doped raw material 1:(0.01~0.10 in molar ratio) addition
Mixing treatment is carried out into reaction dissolvent, precursor solution is made in 1~3h of ultrasonic mixing；
(2) it is gradually added into diluted alkaline into precursor solution, adjusts the pH to 8~9 of precursor solution；
(3) precursor solution is placed in the closed hydrothermal reaction kettle with blender, under the conditions of 120~260 DEG C, is stirred
Mix 5~20h of reaction；
(4) reaction precipitate is carried out after sufficiently washing, dry, crushing is calcined to get target product is arrived.
As preferred embodiment, cadmium salt is caddy, in cadmium nitrate, cadmium iodide, cadmium bromide, cadmium sulfate in the step (1)
Any one, bismuth salt is bismuth chloride, bismuth nitrate, any one in bismuth sulfate, and silver salt is silver nitrate.
As preferred embodiment, in the step (1) reaction dissolvent be deionized water or dehydrated alcohol any one, react molten
Agent quality is 1~2 times of cadmium salt and doped raw material gross mass.
As preferred embodiment, in the step (2) diluted alkaline be sodium hydroxide, potassium hydroxide, ammonium hydroxide any one.
As preferred embodiment, in the step (4) washing deionized water, dehydrated alcohol any one, drying is 80
Under the conditions of~150 DEG C, dry 6~for 24 hours, crushing is to crush 5~30min under the conditions of 2000~15000r/min, calcining be
In argon gas or nitrogen protection atmosphere, under the conditions of 300~750 DEG C of temperature, 3~10h is calcined.
The beneficial effects of the present invention are: preparation process of the present invention is simple, consume energy low, equipment is simple, and product purity is high, can be straight
Connect the production of applicable industry metaplasia；And be experimentally confirmed, obtained silver, bismuth doping cadmium oxide diameter of particle is small, narrowly distributing, the group of being not easy
Poly-, stability is good, and near infrared reflectivity is more than 89%；Silver or bismuth individually adulterate cadmium oxide and are lower than to the albedo of near-infrared
Silver-colored, bismuth co-doped miscellaneous cadmium oxide nano material, and its outdoor weathe resistance is not as good as silver, bismuth co-doped miscellaneous cadmium oxide.
Specific embodiment
In order to be easy to understand to technical means, creative features, achievable purpose and effectiveness of the invention, further below
Illustrate the present invention.
Embodiment 1
A kind of silver-colored, bismuth doping cadmium oxide near-infrared high reflection raw powder's production technology, comprising the following steps:
(1) primary raw material caddy is chosen, and chooses silver nitrate and bismuth chloride collectively as doped raw material, wherein adulterating
Molar ratio containing silver nitrate and bismuth chloride in raw material is 1:0.1, and by caddy, doped raw material, 1:0.02 is added in molar ratio
Mixing treatment is carried out in reaction dissolvent, reaction dissolvent is deionized water, and reaction dissolvent quality is cadmium salt and doped raw material gross mass
1 times, ultrasonic mixing 1h, be made precursor solution；
(2) it is gradually added into sodium hydroxide into precursor solution, adjusts the pH to 8.5 of precursor solution；
(3) precursor solution is placed in the closed hydrothermal reaction kettle with blender, under the conditions of 150 DEG C, stirring is anti-
Answer 6h；
(4) after reaction precipitate being carried out sufficiently washing with deionized water, under the conditions of 100 DEG C, dry 8h；In pulverizer
In, to crush 10min under 5000r/min speed conditions；In argon atmosphere, 400 DEG C of calcining 4h to get arrive target product.It is real
Apply example 2
A kind of silver-colored, bismuth doping cadmium oxide near-infrared high reflection raw powder's production technology, comprising the following steps:
(1) primary raw material cadmium iodide is chosen, and chooses silver nitrate and bismuth chloride collectively as doped raw material, wherein adulterating
Molar ratio containing silver nitrate and bismuth chloride in raw material is 1:2, and by cadmium iodide, doped raw material, 1:0.01 is added to instead in molar ratio
It answers and carries out mixing treatment in solvent, reaction dissolvent is deionized water, and reaction dissolvent quality is cadmium iodide and doped raw material gross mass
1 times, ultrasonic mixing 2h, be made precursor solution；
(2) it is gradually added into ammonium hydroxide into precursor solution, adjusts the pH to 9 of precursor solution；
(3) precursor solution is placed in the closed hydrothermal reaction kettle with blender, under the conditions of 150 DEG C, stirring is anti-
Answer 6h；
(4) after reaction precipitate being carried out sufficiently washing with deionized water, under the conditions of 90 DEG C, dry 20h；In pulverizer
In, to crush 5min under 6000r/min speed conditions；In argon atmosphere, 300 DEG C of calcining 6h to get arrive target product.
Embodiment 3
A kind of silver-colored, bismuth doping cadmium oxide near-infrared high reflection raw powder's production technology, comprising the following steps:
(1) primary raw material cadmium nitrate is chosen, and chooses silver nitrate and bismuth chloride collectively as doped raw material, wherein adulterating
Molar ratio containing silver nitrate and bismuth chloride in raw material is 1:0.2, and by cadmium nitrate, doped raw material, 1:0.04 is added in molar ratio
Mixing treatment is carried out in reaction dissolvent, reaction dissolvent is dehydrated alcohol, and reaction dissolvent quality is cadmium nitrate and the total matter of doped raw material
Precursor solution is made in 1.2 times, ultrasonic mixing 3h of amount；
(2) it is gradually added into potassium hydroxide into precursor solution, adjusts the pH to 9 of precursor solution；
(3) precursor solution is placed in the closed hydrothermal reaction kettle with blender, under the conditions of 120 DEG C, stirring is anti-
Answer 20h；
(4) after reaction precipitate being carried out sufficiently washing with deionized water, under the conditions of 120 DEG C, dry 10h；It is crushing
In machine, to crush 30min under 2000r/min speed conditions；In nitrogen atmosphere, 750 DEG C of calcining 3h to get arrive target product.
Embodiment 4
A kind of silver-colored, bismuth doping cadmium oxide near-infrared high reflection raw powder's production technology, comprising the following steps:
(1) primary raw material cadmium nitrate is chosen, and chooses silver nitrate and bismuth nitrate collectively as doped raw material, wherein adulterating
Molar ratio containing silver nitrate and bismuth nitrate in raw material is 1:5, and by cadmium nitrate, doped raw material, 1:0.1 is added to instead in molar ratio
It answers and carries out mixing treatment in solvent, reaction dissolvent is deionized water, and reaction dissolvent quality is cadmium nitrate and doped raw material gross mass
1.6 times, ultrasonic mixing 3h, be made precursor solution；
(2) it is gradually added into sodium hydroxide into precursor solution, adjusts the pH to 8 of precursor solution；
(3) precursor solution is placed in the closed hydrothermal reaction kettle with blender, under the conditions of 250 DEG C, stirring is anti-
Answer 5h；
(4) after reaction precipitate being carried out sufficiently washing with deionized water, under the conditions of 150 DEG C, dry 6h；In pulverizer
In, to crush 5min under 15000r/min speed conditions；In argon atmosphere, 300 DEG C of calcining 10h to get arrive target product.
Embodiment 5
A kind of silver-colored, bismuth doping cadmium oxide near-infrared high reflection raw powder's production technology, comprising the following steps:
(1) primary raw material caddy is chosen, and chooses silver nitrate and bismuth chloride collectively as doped raw material, wherein adulterating
Molar ratio containing silver nitrate and bismuth chloride in raw material is 1:9, and by caddy, doped raw material, 1:0.06 is added to instead in molar ratio
It answers and carries out mixing treatment in solvent, reaction dissolvent is deionized water, and reaction dissolvent quality is caddy and doped raw material gross mass
1.2 times, ultrasonic mixing 2h, be made precursor solution；
(2) it is gradually added into sodium hydroxide into precursor solution, adjusts the pH to 8 of precursor solution；
(3) precursor solution is placed in the closed hydrothermal reaction kettle with blender, under the conditions of 120 DEG C, stirring is anti-
Answer 20h；
(4) after reaction precipitate being carried out sufficiently washing with deionized water, under the conditions of 110 DEG C, dry 12h；It is crushing
In machine, to crush 12min under 8000r/min speed conditions；In nitrogen atmosphere, 500 DEG C of calcining 7h to get arrive target product.
Embodiment 6
A kind of silver-colored, bismuth doping cadmium oxide near-infrared high reflection raw powder's production technology, comprising the following steps:
(1) primary raw material caddy is chosen, and chooses silver nitrate and bismuth sulfate collectively as doped raw material, wherein adulterating
Molar ratio containing silver nitrate and bismuth sulfate in raw material is 1:10, and by caddy, doped raw material, 1:0.08 is added in molar ratio
Mixing treatment is carried out in reaction dissolvent, reaction dissolvent is deionized water, and reaction dissolvent quality is caddy and the total matter of doped raw material
Precursor solution is made in 1.4 times, ultrasonic mixing 2.5h of amount；
(2) it is gradually added into potassium hydroxide into precursor solution, adjusts the pH to 8.5 of precursor solution；
(3) precursor solution is placed in the closed hydrothermal reaction kettle with blender, under the conditions of 200 DEG C, stirring is anti-
Answer 8h；
(4) after reaction precipitate being carried out sufficiently washing with deionized water, under the conditions of 140 DEG C, dry 6h；In pulverizer
In, to crush 10min under 10000r/min speed conditions；In argon atmosphere, 600 DEG C of calcining 6h to get arrive target product.
Embodiment 7
A kind of silver-colored, bismuth doping cadmium oxide near-infrared high reflection raw powder's production technology, comprising the following steps:
(1) primary raw material caddy is chosen, and chooses silver nitrate and bismuth nitrate collectively as doped raw material, wherein adulterating
Molar ratio containing silver nitrate and bismuth nitrate in raw material is 1:3, and by caddy, doped raw material, 1:0.04 is added to instead in molar ratio
It answers and carries out mixing treatment in solvent, reaction dissolvent is dehydrated alcohol, and reaction dissolvent quality is caddy and doped raw material gross mass
1.2 times, ultrasonic mixing 1.5h, be made precursor solution；
(2) it is gradually added into ammonium hydroxide into precursor solution, adjusts the pH to 8 of precursor solution；
(3) precursor solution is placed in the closed hydrothermal reaction kettle with blender, under the conditions of 180 DEG C, stirring is anti-
Answer 10h；
(4) after reaction precipitate being carried out sufficiently washing with dehydrated alcohol, under the conditions of 120 DEG C, dry 8h；In pulverizer
In, to crush 6min under 12000r/min speed conditions；In nitrogen atmosphere, 700 DEG C of calcining 4h to get arrive target product.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, without departing from the spirit and scope of the present invention, this hair
Bright to will also have various changes and improvements, these changes and improvements are both fallen in the scope of protection of present invention.The present invention claims
Protection scope is defined by the appending claims and its equivalent thereof.
Claims (2)
1. a kind of silver, bismuth adulterate cadmium oxide near-infrared high reflection raw powder's production technology, which comprises the following steps:
(1) primary raw material cadmium salt is chosen, and chooses silver salt and bismuth salt collectively as doped raw material, is wherein contained in doped raw material
The molar ratio of silver salt and bismuth salt is 1:(0.1~10), by cadmium salt, doped raw material 1:(0.01~0.10 in molar ratio) be added to it is anti-
It answers and carries out mixing treatment in solvent, precursor solution is made in 1~3h of ultrasonic mixing；
(2) it is gradually added into diluted alkaline into precursor solution, adjusts the pH to 8~9 of precursor solution；
(3) precursor solution is placed in the closed hydrothermal reaction kettle with blender, under the conditions of 120~260 DEG C, stirring is anti-
Answer 5~20h；
(4) reaction precipitate is carried out after sufficiently washing, dry, crushing is calcined to get target product is arrived；
Cadmium salt is caddy, cadmium nitrate, cadmium iodide, cadmium bromide, any one in cadmium sulfate in the step (1), and bismuth salt is chlorine
Change bismuth, bismuth nitrate, any one in bismuth sulfate, silver salt is silver nitrate；
In the step (1) reaction dissolvent be deionized water or dehydrated alcohol any one, reaction dissolvent quality is cadmium salt and mixes
1~2 times of miscellaneous total mass of raw material；
In the step (4) washing deionized water, dehydrated alcohol any one, drying be under the conditions of 80~150 DEG C, it is dry
6~for 24 hours, crushing is to crush 5~30min, calcining is in argon gas or nitrogen protection atmosphere under the conditions of 2000~15000r/min
In, under the conditions of 300~750 DEG C of temperature, calcine 3~10h.
2. a kind of silver, bismuth adulterate cadmium oxide near-infrared high reflection raw powder's production technology according to claim 1, feature exists
In: in the step (2) diluted alkaline be sodium hydroxide, potassium hydroxide, ammonium hydroxide any one.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1796271A (en) * | 2004-12-24 | 2006-07-05 | 同济大学 | Method for preparing Nano lead telluride doped with silver and stibium or silver and bismuth |
| CN106430293A (en) * | 2016-09-28 | 2017-02-22 | 沪本新材料科技（上海）有限公司 | Preparation method of novel bismuth-doped tin dioxide powder with high near-infrared reflectivity |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1796271A (en) * | 2004-12-24 | 2006-07-05 | 同济大学 | Method for preparing Nano lead telluride doped with silver and stibium or silver and bismuth |
| CN106430293A (en) * | 2016-09-28 | 2017-02-22 | 沪本新材料科技（上海）有限公司 | Preparation method of novel bismuth-doped tin dioxide powder with high near-infrared reflectivity |
Non-Patent Citations (1)
| Title |
|---|
| Ag或Bi掺杂玻璃可调节宽带发光性能与机理研究;刘雪云;《中国博士学位论文全文数据库 工程科技Ⅰ辑》;20170515(第5期);1 |
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