CN102234131B - Preparation method of dendritic lead sulfide material - Google Patents
Preparation method of dendritic lead sulfide material Download PDFInfo
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- CN102234131B CN102234131B CN 201010153848 CN201010153848A CN102234131B CN 102234131 B CN102234131 B CN 102234131B CN 201010153848 CN201010153848 CN 201010153848 CN 201010153848 A CN201010153848 A CN 201010153848A CN 102234131 B CN102234131 B CN 102234131B
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Abstract
The invention provides a method for preparing a lead sulfide material, which comprises the following steps: preparing a reaction mixture of lead nitrate, thiourea, an abietyl surfactant with a molar ratio of 1-2:2-4:0.05-0.15, adding the mixture into a solvent, stirring uniformly to obtain a reaction solution; wherein, the mass ratio of the reaction mixture and the solvent is 1:15-40, and the solvent is one selected from ethanol and deionized water; adding the reaction solution into a sealed high pressure reaction vessel, heating to 160-220 DEG C, performing heat insulation for 12-72 hours, cooling, washing, and drying to obtain the lead sulfide material with a dendritic particle shape.
Description
Technical field
The present invention relates to a kind of method for preparing the lead sulfide material, be specifically related to a kind of method for preparing dendritic lead sulfide material.
Background technology
Lead sulfide is a kind of important semiconductor material, at aspects such as near infrared communication, photoelectric device and solar cells significant application value is arranged.In recent years, it is found that pattern, size and the structure of material directly affect the performance of material, therefore, the special appearance control preparation of material is also become the study hotspot of field of material preparation.People adopt the whole bag of tricks to prepare the lead sulfide material of different morphologies, adopt interpolation tensio-active agent autoclave hydrothermal method to obtain pulmbous sulfide nanospheres (CN101402468A), nanometer rod (CN101049960A), hollow cubic shape nanocrystalline (CN101402467A), single dispersed cubic shape nanocrystalline (CN101402467A), hexagram nanocrystalline (CN101117237A), pyramid rectangular tube (CrystalGrowth﹠amp such as people; Design, the 2009,7,3119th page); Utilize microwave assisting method to prepare sexangle, dendroid and ear shape (Materials Letters, the 2009,63,667th page); Utilize the microemulsion auxiliary law to synthesize flower-like nanometer crystalline substance (Solid State Sciences, 2009,11,976-981 page or leaf).In the whole bag of tricks of each bibliographical information, wherein autoclave hydrothermal method processing unit is simple, controls easily and realize suitability for industrialized production, and the microwave method reaction times is short, usually namely reacts completely at several minutes or dozens of minutes, saves the energy; And auxiliary these methods of tensio-active agent are preferred approach of control material pattern, the tensio-active agent that uses in the above document is the tensio-active agent of Sodium dodecylbenzene sulfonate anion surfactant or hexadecyl trimethyl ammonium bromide cats product or these two kinds of mixing, these two kinds of tensio-active agents are the petroleum chemistry sintetics, and be the chain alkyl structure, have very strong flexibility, have certain defect at control preparation material pattern.Therefore, in petroleum resources day by day exhausted today, it is a kind of inevitable to replace these two kinds of tensio-active agents to become with novel renewable resources derivative tensio-active agent.
Summary of the invention
The invention provides a kind of method for preparing the lead sulfide material, wherein adopt rosin-based surfactant as the tensio-active agent of control material microscopic appearance.Wherein rosin-based surfactant is the product synthetic take the important renewable resources rosin of China as raw material, has raw material and is easy to get, the characteristics such as environmental protection.
According to one embodiment of the invention, the method for preparing dendritic lead sulfide material may further comprise the steps:
Reaction mixture according to the mol ratio of 1-2: 2-4: 0.05-0.15 preparation lead nitrate, thiocarbamide, rosin-based surfactant joins this mixture in the solvent, stirs, and obtains reaction solution; Wherein, the mass ratio of reaction mixture and solvent is 1: 15-40, described solvent are selected from a kind of in ethanol and the deionized water;
Reaction solution is put into the autoclave of sealing, be heated to 160-220 ℃, be incubated 12-72 hour, then obtain product through overcooling, washing, drying.
Wherein, autoclave can use reactor well known to those skilled in the art and not have particular requirement.
According to one embodiment of the invention, wherein used rosin-based surfactant is selected from one or more in the following table surface-active agent:
Rosin-based surfactant (I)
Wherein, the scope of n is: 1≤n≤6,
Rosin-based surfactant (II)
Wherein, the scope of n is: 1≤n≤4,
Rosin-based surfactant (III)
Wherein,
The scope of n is: 1≤n≤10; The scope of m is: 4≤m≤9; R
1=(CH
2)
pCH
3, the scope of p is 1≤p≤4.
Cooling can be naturally cooling, also can be to force cooling.Washing and drying step can adopt various washing drying means well known to those skilled in the art, for example drying can include but not limited to directly the baking oven inner drying, behind suction filtration in baking oven inner drying, infrared drying, microwave drying etc.
Use scanning electron microscope analysis according to the lead sulfide material of embodiment of the present invention preparation.The lead sulfide material be shaped as the dendroid particle.
Description of drawings
With reference to accompanying drawing and following embodiment, the method for preparing the lead sulfide material that the present invention may be better understood.
Fig. 1, Fig. 2 are scanning electron microscope (SEM) photos of the lead sulfide particle for preparing according to one embodiment of present invention;
Fig. 3 is scanning electron microscope (SEM) photo of the lead sulfide particle for preparing according to another embodiment of the invention;
Fig. 4 is scanning electron microscope (SEM) photo of the lead sulfide particle for preparing according to another embodiment of the invention.
Embodiment
Embodiment 1
The lead nitrate aqueous solution and each 4mL of thiourea solution, the 10g/L rosin-based surfactant A ethanolic soln 1.5mL that get 0.4mol/L join in the reactor, add 2.5mL water, the baking oven of after mixing reactor being put into 160 ℃ reacts 12h, be cooled to room temperature, with deionized water and washing with alcohol black precipitate each 3 times, centrifugation obtains black precipitate, obtains the lead sulfide product of pattern such as Fig. 1, Fig. 2 at 80 ℃ of lower dry 8h.
Rosin-based surfactant A rosin-based surfactant B
Embodiment 2
The lead nitrate aqueous solution and each 4mL of thiourea solution, the 10g/L rosin-based surfactant B ethanolic soln 1.8mL that get 0.4mol/L join in the reactor, add 2.2mL water, the baking oven of after mixing reactor being put into 140 ℃ reacts 36h, be cooled to room temperature, with deionized water and washing with alcohol black precipitate each 3 times, centrifugation obtains black precipitate, obtains the lead sulfide product of pattern such as Fig. 3 at 80 ℃ of lower dry 8h.
Embodiment 3
The lead nitrate aqueous solution and each 4mL of thiourea solution, the 10g/L rosin-based surfactant C ethanolic soln 1.2mL that get 0.2mol/L join in the reactor, add 2.8mL water, the baking oven of after mixing reactor being put into 200 ℃ reacts 12h, be cooled to room temperature, with deionized water and washing with alcohol black precipitate each 3 times, centrifugation obtains black precipitate, obtains the lead sulfide product of pattern such as Fig. 4 at 80 ℃ of lower dry 8h.
Rosin-based surfactant C
Wherein,
R
1=(CH
2)
3CH
3
Although above embodiment for example understands specific embodiments of the present invention,, should be understood that these embodiment only are used for illustrating embodiment of the present invention and scope of the present invention are not had any limiting meaning.Claims and any version thereof all should be included in the scope of protection of present invention.
Claims (1)
1. method for preparing the lead sulfide material, may further comprise the steps: the reaction mixture of preparing lead nitrate, thiocarbamide, rosin-based surfactant according to the mol ratio of 1-2: 2-4: 0.05-0.15, this mixture is joined in the solvent, stir, obtain reaction solution; Wherein, the mass ratio of reaction mixture and solvent is 1: 15-40, described solvent are selected from a kind of in ethanol and the deionized water; Reaction solution is put into the autoclave of sealing, be heated to 160-220 ℃, be incubated 12-72 hour, then obtaining particle shape through overcooling, washing, drying is dendritic lead sulfide material,
Wherein, described rosin-based surfactant is selected from any one or its combination of following rosin-based surfactant:
Rosin-based surfactant (I)
Wherein, the scope of n is: 1≤n≤6,
Rosin-based surfactant (II)
Wherein, the scope of n is: 1≤n≤4,
Rosin-based surfactant (III)
Wherein,
The scope of n is: 1≤n≤10; The scope of m is: 4≤m≤9; R
1=(CH
2)
pCH
3, the scope of p is 1≤p≤4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 201010153848 CN102234131B (en) | 2010-04-23 | 2010-04-23 | Preparation method of dendritic lead sulfide material |
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| CN 201010153848 CN102234131B (en) | 2010-04-23 | 2010-04-23 | Preparation method of dendritic lead sulfide material |
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| CN102234131A CN102234131A (en) | 2011-11-09 |
| CN102234131B true CN102234131B (en) | 2013-04-17 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7229602B2 (en) * | 2003-06-05 | 2007-06-12 | National University Of Singapore | Method of preparing metal chalcogenide particles |
| CN101402465A (en) * | 2008-10-28 | 2009-04-08 | 杭州电子科技大学 | Method for producing pulmbous sulfide dendrite from particle adhesion |
-
2010
- 2010-04-23 CN CN 201010153848 patent/CN102234131B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7229602B2 (en) * | 2003-06-05 | 2007-06-12 | National University Of Singapore | Method of preparing metal chalcogenide particles |
| CN101402465A (en) * | 2008-10-28 | 2009-04-08 | 杭州电子科技大学 | Method for producing pulmbous sulfide dendrite from particle adhesion |
Non-Patent Citations (7)
| Title |
|---|
| Ai-Miao Qin et al..Directionally dendritic growth of metal chalcogenide crystals via mild template-free solvothermal method.《Journal of Crystal Growth》.2005,第283卷230-241. |
| Daibin Kuang et al..Surface-Assisted Growth of Novel PbS Dentritic Nanostructures via Facile Hydrothermal Process.《Advanced Materials》.2003,第15卷(第20期),1747-1750. |
| Directionally dendritic growth of metal chalcogenide crystals via mild template-free solvothermal method;Ai-Miao Qin et al.;《Journal of Crystal Growth》;20050707;第283卷;230-241 * |
| Surface-Assisted Growth of Novel PbS Dentritic Nanostructures via Facile Hydrothermal Process;Daibin Kuang et al.;《Advanced Materials》;20031016;第15卷(第20期);1747-1750 * |
| 多树枝结构和立方结构PbS的水热合成及形成机理;王新军等;《无机化学学报》;20090430;第25卷(第4期);685-692 * |
| 王新军等.多树枝结构和立方结构PbS的水热合成及形成机理.《无机化学学报》.2009,第25卷(第4期),685-692. |
| 陈广大等.星形树枝状硫化铅纳米晶的制备.《北京大学学报（自然科学版）》》.2006,第42卷(第4期),427-430. * |
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