CN100347089C - Synthesis of nanometer block of lead sulfide - Google Patents
Synthesis of nanometer block of lead sulfide Download PDFInfo
- Publication number
- CN100347089C CN100347089C CNB200610002147XA CN200610002147A CN100347089C CN 100347089 C CN100347089 C CN 100347089C CN B200610002147X A CNB200610002147X A CN B200610002147XA CN 200610002147 A CN200610002147 A CN 200610002147A CN 100347089 C CN100347089 C CN 100347089C
- Authority
- CN
- China
- Prior art keywords
- lead sulfide
- nanometers
- nanometer
- dithioglycol
- plumbic acetate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 229940056932 lead sulfide Drugs 0.000 title claims abstract description 48
- 229910052981 lead sulfide Inorganic materials 0.000 title claims abstract description 48
- 230000015572 biosynthetic process Effects 0.000 title 1
- 238000003786 synthesis reaction Methods 0.000 title 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 32
- VYMPLPIFKRHAAC-UHFFFAOYSA-N 1,2-ethanedithiol Chemical compound SCCS VYMPLPIFKRHAAC-UHFFFAOYSA-N 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000010189 synthetic method Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- JEHCHYAKAXDFKV-UHFFFAOYSA-J lead tetraacetate Chemical compound CC(=O)O[Pb](OC(C)=O)(OC(C)=O)OC(C)=O JEHCHYAKAXDFKV-UHFFFAOYSA-J 0.000 claims description 27
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 229960004756 ethanol Drugs 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 229940046892 lead acetate Drugs 0.000 abstract 2
- 239000011259 mixed solution Substances 0.000 abstract 2
- 238000006243 chemical reaction Methods 0.000 description 15
- 230000005540 biological transmission Effects 0.000 description 14
- 239000007788 liquid Substances 0.000 description 14
- 239000000243 solution Substances 0.000 description 11
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- 230000004087 circulation Effects 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 5
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 230000001235 sensitizing effect Effects 0.000 description 2
- 229910001961 silver nitrate Inorganic materials 0.000 description 2
- 150000003464 sulfur compounds Chemical class 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 229910052798 chalcogen Inorganic materials 0.000 description 1
- 150000001787 chalcogens Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical group [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920002717 polyvinylpyridine Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- -1 vinyl pyridine alkane ketone Chemical class 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 239000011701 zinc Chemical group 0.000 description 1
- 229910052725 zinc Chemical group 0.000 description 1
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a synthetic method of nanometer blocks of lead sulfide, which belongs to the technical field of preparing nanometer materials of semiconductors. The present invention is characterized in that the method comprises the following steps: lead acetate and dithioglycol are used as raw materials, and a mixed solution of water and alcohol of sodium hydroxide which comprises the lead acetate and the dithioglycol is prepared; the mixed solution is placed in a reactor and heated for 4 to 48 hours at the temperature of 180 to 220 DEG C; the reacted deposits are orderly washed with deionized water and alcohol, and are put in a drying box to be dried; and then, nanometer blocks of lead sulfide are obtained. The synthetic method has the advantages of easy acquirement of the raw materials, and simple and convenient technique. The synthetic method can synthesize the nanometer blocks of the lead sulfide, the average size of which is from 83 nanometers * 59 nanometers*22 nanometers to 39 nanometers * 10 nanometers * 7 nanometers.
Description
Technical field
A kind of synthetic method of nanometer block of lead sulfide belongs to the preparing technical field of semiconductor nano material.
Background technology
Lead sulfide is that the narrow of a kind of important II-VI family can gap semiconductor material, reduces because its energy gap descends with temperature, utilizes this character, and infrared diode laser in can preparing changes temperature and can regulate wavelength of transmitted light.In addition, the static dielectric of lead sulfide is very big, causes electronics and hole mobility under the low temperature very high.And the optical property of lead sulfide is big owing to uptake factor in its basic absorption frequency scope, the specific refractory power height, and this character makes lead sulfide can be used for preparing infrared eye and laser apparatus.
Thereby the lead sulfide nano structural material can be used as candidate material in following nano electron device and the nano photoelectronic devices, no matter in academic research still in application facet, all have great importance.
In the prior art of our retrieval, there are four about the synthetic patent report of lead sulfide nanostructure:
(1) " organic compounds containing sulfur modified metal-chalcogen compound nanoparticle and its production and use " (applicant: Lanzhou Inst. of Chemical Physics, Chinese Academy of Sciences, contriver: the flourish Zhang Zhijun Xue Qun of Liu Wei people Chen Shuan Yang Sheng base; Application number 98118087), this invention has been narrated a kind of oil soluble and has been contained sulfydryl or organic compound modified metal-chalcogen compound nanoparticle and the synthetic method of thiosalt, invention relates to the compound of novel general formula (I), R is the straight or branched alkyl of (C#-[8]～C#-[18]) in the formula, and M is metallic lead or zinc.
(2) " solvent process for thermosynthesizing of nano sulfur compound capable ", (applicant: China Science ﹠ Technology University, the contriver: the grand money ease of Yu's book is safe, application number 99107093), the solvent process for thermosynthesizing of this invention nano sulfur compound capable, with a kind of II A that is selected from, IVA, V A family and Ag, Ni, the oxalate of the transition element of Sn, with at least a sulphur that is selected from, selenium, the chalcogen simple substance of tellurium, add appropriate organic solvent, in the autoclave of sealing, be not less than 120-200 ℃ in the temperature of reaction lower limit, the upper limit is lower than the decomposition temperature of this system oxalate, and the reaction times is no less than 12-24 hour; Described appropriate organic solvent is chosen from polyamines, pyridine (py), ethylene glycol (EG) or tetrahydrofuran (THF) (THF); The inventive method preparation condition gentleness, operate simple and easy, the productive rate height, product particle size and shape are easy to control, are suitable for producing in batches.
(3) " lead sulfide nano-particle sensitizer and its production and use ", (applicant: Physical Chemistry Technology Inst., Chinese Academy of Sciences, the contriver: Li Jinpei is permitted spring China, application number: 02153758), this invention belongs to the photosensitive silve halide material technical field, particularly a kind of lead sulfide nano-particle sensitizer and its production and use.Water miscible lead salt solution and water miscible sulfocompound solution are dispersed in the water miscible macromolecular compound, in temperature is to mix under 10～100 ℃ of conditions, stir, obtain the sensitizing agent of forming by lead sulfide nanoparticle, water soluble inorganic substance and water-soluble polymer then; Wherein, the concentration of the lead sulfide nanoparticle in the sensitizing agent is 0.00001～0.1 mol, and the concentration of water miscible inorganics is 0.00002～0.2 mol, and the weight percent concentration of water miscible macromolecular compound is 0.1～10%; The particle diameter of described lead sulfide nanoparticle is in 1～20 nanometer.
(4) " liquid phase sandwich-type nanometer colloid particle laser protective material " (applicant: Electronic Engineering College, PLA, the contriver: surplus big refined Sun Xiao spring king is from Rong Tong loyalty, application number: 02157281).This invention is a kind of liquid phase sandwich-type nanometer colloid particle laser protective material and preparation.By Silver Nitrate, or Silver Nitrate and lead nitrate the two one of in the solvent of, ethanol water-soluble, ethylene glycol, benzene, pyridine, tetrahydrofuran (THF) one of them or combination with thioacetamide, one of them is a stablizer with polyvinyl pyridine, vinyl pyridine alkane ketone, polyvinyl alcohol, preparation nanometer colloid particle solution.
The character of nano material and its size, shape are relevant, and we provide a kind of material that is shaped as the lead sulfide of blocky nano-scale, and this is for understanding the relation of its structure and performance, and in the exploitation of the nano electron device in future, provide a kind of possible selection.
Summary of the invention
The object of the present invention is to provide a kind of easy method for preparing nanometer block of lead sulfide.The invention is characterized in, carry out as follows:
1) be raw material with plumbic acetate, dithioglycol, preparation comprises the water-ethanol mixing solutions of the sodium hydroxide of plumbic acetate, dithioglycol; Wherein, described plumbic acetate concentration is 0.133～2.168 mmole/40 milliliter scopes, Pbu
2+: the S molar ratio is 1: 0.75～1: 6 scope, and naoh concentration is 1 mol, and ethanol is dehydrated alcohol;
2) described mixing solutions is positioned in the teflon-lined stainless steel cauldron, 180～220 ℃ of temperature range heating 4～48 hours;
3) throw out that obtains after will reacting is put into loft drier and is carried out drying successively through deionized water and washing with alcohol, promptly obtains nanometer block of lead sulfide.
Raw materials used being easy to get in the synthetic method of the present invention, technology is easy, can synthesize the nanometer block of lead sulfide of size average out to 83 nanometers * 59 nanometers * 22 nanometers～39 nanometers * 10 nanometers * 7 nanometer range.
Description of drawings:
Fig. 1: (a) being embodiment 1X x ray diffration pattern x, (b) is the transmission electron microscope photo of embodiment 1.
Fig. 2: (a) being embodiment 2X x ray diffration pattern x, (b) is the transmission electron microscope photo of embodiment 2.
Fig. 3: be the transmission electron microscope photo of embodiment 3.
Fig. 4: be the transmission electron microscope photo of embodiment 4.
Fig. 5: be the transmission electron microscope photo of embodiment 5.
Fig. 6: be the transmission electron microscope photo of embodiment 6.
Fig. 7: be the transmission electron microscope photo of embodiment 7.
Embodiment:
Below by specific embodiment the present invention further is illustrated.
Embodiment 1:
---with plumbic acetate (Pb (Ac)
23H
2O), dithioglycol (HSCH
2CH
2SH) be raw material, at room temperature, water-dehydrated alcohol (10 milliliters) of preparing the sodium hydroxide (30 milliliters of 1MNaOH solution) that comprises plumbic acetate, dithioglycol is as reaction starting liquid, with plumbic acetate (Pb (Ac)
2) concentration is 0.542 mmole/40 milliliter scopes, Pb
2+/ S molar ratio was at 1: 0.75;
---this reaction starting liquid is placed in the teflon-lined stainless steel cauldron, 220 ℃ of temperature range heating 4 hours;
---the throw out that will obtain after will reacting is put into loft drier and was carried out drying 2 hours for 50 ℃ successively through deionized water and 3 circulations of absolute ethanol washing, promptly obtains nanometer block of lead sulfide.
By Fig. 1 a is the X-ray diffractogram of nanometer block of lead sulfide, can prove conclusively this by figure is the lead sulfide that belongs to the wurtzite-type structure, Fig. 1 b is the transmission electron microscope photo of nanometer block of lead sulfide, as seen from the figure these nanometer block of lead sulfide size average out to 83 nanometers * 58 nanometers * 22 nanometers.
Embodiment 2:
---with plumbic acetate (Pb (Ac)
23H
2O), dithioglycol (HSCH
2CH
2SH) be raw material, at room temperature, water-dehydrated alcohol (10 milliliters) of preparing the sodium hydroxide (30 milliliters of 1MNaOH solution) that comprises plumbic acetate, dithioglycol is as reaction starting liquid, with plumbic acetate (Pb (Ac)
2) concentration is 0.542 mmole/40 milliliter scopes, Pb
2+/ S molar ratio was at 1: 3;
---this reaction starting liquid is placed in the teflon-lined stainless steel cauldron, 220 ℃ of temperature range heating 4 hours;
---the throw out that will obtain after will reacting is put into loft drier and was carried out drying 2 hours for 50 ℃ successively through deionized water and 3 circulations of absolute ethanol washing, promptly obtains nanometer block of lead sulfide.
By Fig. 2 a is the X-ray diffractogram of lead sulfide nano cubic block, can prove conclusively this by figure is the lead sulfide that belongs to the wurtzite-type structure, Fig. 2 b is the transmission electron microscope photo of nanometer block of lead sulfide, as seen from the figure these nanometer block of lead sulfide size average out to 39 nanometers * 10 nanometers * 7 nanometers.
Embodiment 3:
---with plumbic acetate (Pb (Ac)
23H
2O), dithioglycol (HSCH
2CH
2SH) be raw material, at room temperature, water-dehydrated alcohol (10 milliliters) of preparing the sodium hydroxide (30 milliliters of 1MNaOH solution) that comprises plumbic acetate, dithioglycol is as reaction starting liquid, with plumbic acetate (Pb (Ac)
2) concentration is 0.542 mmole/40 milliliter scopes, Pb
2+/ S molar ratio was at 1: 6;
---this reaction starting liquid is placed in the teflon-lined stainless steel cauldron, 220 ℃ of temperature range heating 48 hours;
---the throw out that will obtain after will reacting is put into loft drier and was carried out drying 2 hours for 50 ℃ successively through deionized water and 3 circulations of absolute ethanol washing, promptly obtains nanometer block of lead sulfide.
By Fig. 3 is the transmission electron microscope photo of nanometer block of lead sulfide, as seen from the figure these nanometer block of lead sulfide size average out to 72 nanometers * 41 nanometers * 13 nanometers.
Embodiment 4:
---with plumbic acetate (Pb (Ac)
23H
2O), dithioglycol (HSCH
2CH
2SH) be raw material, at room temperature, water-dehydrated alcohol (10 milliliters) of preparing the sodium hydroxide (30 milliliters of 1MNaOH solution) that comprises plumbic acetate, dithioglycol is as reaction starting liquid, with plumbic acetate (Pb (Ac)
2) concentration is 0.542 mmole/40 milliliter scopes, Pb
2+/ S molar ratio was at 1: 3;
---this reaction starting liquid is placed in the teflon-lined stainless steel cauldron, 180 ℃ of temperature range heating 4 hours;
---the throw out that will obtain after will reacting is put into loft drier and was carried out drying 2 hours for 50 ℃ successively through deionized water and 3 circulations of absolute ethanol washing, promptly obtains nanometer block of lead sulfide.
By Fig. 4 is the transmission electron microscope photo of nanometer block of lead sulfide, as seen from the figure these nanometer block of lead sulfide size average out to 77 nanometers * 57 nanometers * 21 nanometers.
Embodiment 5:
---with plumbic acetate (Pb (Ac)
23H
2O), dithioglycol (HSCH
2CH
2SH) be raw material, at room temperature, water-dehydrated alcohol (10 milliliters) of preparing the sodium hydroxide (30 milliliters of 1MNaOH solution) that comprises plumbic acetate, dithioglycol is as reaction starting liquid, with plumbic acetate (Pb (Ac)
2) concentration is 0.542 mmole/40 milliliter scopes, Pb
2+/ S molar ratio was at 1: 1;
---this reaction starting liquid is placed in the teflon-lined stainless steel cauldron, 200 ℃ of temperature range heating 8 hours;
---the throw out that will obtain after will reacting is put into loft drier and was carried out drying 2 hours for 50 ℃ successively through deionized water and 3 circulations of absolute ethanol washing, promptly obtains nanometer block of lead sulfide.
By Fig. 5 is the transmission electron microscope photo of nanometer block of lead sulfide, as seen from the figure these nanometer block of lead sulfide size average out to 55 nanometers * 27 nanometers * 14 nanometers.
Embodiment 6:
---with plumbic acetate (Pb (Ac)
23H
2O), dithioglycol (HSCH
2CH
2SH) be raw material, at room temperature, water-dehydrated alcohol (10 milliliters) of preparing the sodium hydroxide (30 milliliters of 1MNaOH solution) that comprises plumbic acetate, dithioglycol is as reaction starting liquid, with plumbic acetate (Pb (Ac)
2) concentration is 0.133 mmole/40 milliliter scopes, Pb
2+/ S molar ratio was at 1: 3;
---this reaction starting liquid is placed in the teflon-lined stainless steel cauldron, 220 ℃ of temperature range heating 4 hours;
---the throw out that will obtain after will reacting is put into loft drier and was carried out drying 2 hours for 50 ℃ successively through deionized water and 3 circulations of absolute ethanol washing, promptly obtains nanometer block of lead sulfide.
By Fig. 6 is the transmission electron microscope photo of nanometer block of lead sulfide, as seen from the figure these nanometer block of lead sulfide size average out to 67 nanometers * 450 nanometers * 17 nanometers.
Embodiment 7:
---with plumbic acetate (Pb (Ac)
23H
2O), dithioglycol (HSCH
2CH
2SH) be raw material, at room temperature, water-dehydrated alcohol (10 milliliters) of preparing the sodium hydroxide (30 milliliters of 1MNaOH solution) that comprises plumbic acetate, dithioglycol is as reaction starting liquid, with plumbic acetate (Pb (Ac)
2) concentration is 2.168 mmoles/40 milliliter scopes, Pb
2+/ S molar ratio was at 1: 3;
---this reaction starting liquid is placed in the teflon-lined stainless steel cauldron, 220 ℃ of temperature range heating 4 hours;
---the throw out that will obtain after will reacting is put into loft drier and was carried out drying 2 hours for 50 ℃ successively through deionized water and 3 circulations of absolute ethanol washing, promptly obtains nanometer block of lead sulfide.
By Fig. 7 is the transmission electron microscope photo of nanometer block of lead sulfide, as seen from the figure these nanometer block of lead sulfide size average out to 58 nanometers * 28 nanometers * 12 nanometers.
Claims (1)
1, a kind of synthetic method of nanometer block of lead sulfide is characterized in that, this method is carried out as follows:
1) be raw material with plumbic acetate, dithioglycol, preparation comprises the water-ethanol mixing solutions of the sodium hydroxide of plumbic acetate, dithioglycol; Wherein, described plumbic acetate concentration is 0.133～2.168 mmole/40 milliliter scopes, Pb
2+: the S molar ratio is 1: 0.75～1: 6 scope, and naoh concentration is 1 mol, and ethanol is dehydrated alcohol;
2) described mixing solutions is positioned in the teflon-lined stainless steel cauldron, 180～220 ℃ of temperature range heating 4～48 hours;
3) throw out that obtains after will reacting is put into loft drier and is carried out drying successively through deionized water and washing with alcohol, promptly obtains nanometer block of lead sulfide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610002147XA CN100347089C (en) | 2006-01-19 | 2006-01-19 | Synthesis of nanometer block of lead sulfide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610002147XA CN100347089C (en) | 2006-01-19 | 2006-01-19 | Synthesis of nanometer block of lead sulfide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1817798A CN1817798A (en) | 2006-08-16 |
| CN100347089C true CN100347089C (en) | 2007-11-07 |
Family
ID=36918042
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200610002147XA Expired - Fee Related CN100347089C (en) | 2006-01-19 | 2006-01-19 | Synthesis of nanometer block of lead sulfide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100347089C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805015B (en) * | 2009-02-17 | 2011-12-21 | 国家纳米科学中心 | Preparation method of porous PbS nano sheet |
| CN108793235A (en) * | 2018-09-20 | 2018-11-13 | 昌吉学院 | A method of preparing vulcanized lead using ammonia process of desulfurization waste liquid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1275525A (en) * | 1999-05-27 | 2000-12-06 | 中国科学技术大学 | Solvent thermal synthesis method for nanometer sulfide |
| JP2004352594A (en) * | 2003-05-30 | 2004-12-16 | Hitachi Software Eng Co Ltd | Nanoparticle production method, and nanoparticle produced by the method |
| CN1594100A (en) * | 2004-07-08 | 2005-03-16 | 南京大学 | PbS nano-ribbon and its producing method |
| JP2005325016A (en) * | 2004-04-20 | 2005-11-24 | Samsung Electronics Co Ltd | Manufacturing method of metal nanocrystalline sulfide using thiol compound as sulfur precursor |
-
2006
- 2006-01-19 CN CNB200610002147XA patent/CN100347089C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1275525A (en) * | 1999-05-27 | 2000-12-06 | 中国科学技术大学 | Solvent thermal synthesis method for nanometer sulfide |
| JP2004352594A (en) * | 2003-05-30 | 2004-12-16 | Hitachi Software Eng Co Ltd | Nanoparticle production method, and nanoparticle produced by the method |
| JP2005325016A (en) * | 2004-04-20 | 2005-11-24 | Samsung Electronics Co Ltd | Manufacturing method of metal nanocrystalline sulfide using thiol compound as sulfur precursor |
| CN1594100A (en) * | 2004-07-08 | 2005-03-16 | 南京大学 | PbS nano-ribbon and its producing method |
Non-Patent Citations (1)
| Title |
|---|
| 立方体形PbS纳米晶的制备 褚海斌等.无机化学学报，第20卷第10期 2004 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1817798A (en) | 2006-08-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Song et al. | Preparation of single-crystalline AgIn5S8 octahedrons with exposed {111} facets and its visible-light-responsive photocatalytic H2 production activity | |
| CN1884090A (en) | ZnIn2S4 nano materials and their synthesis method and application | |
| Guo et al. | Hierarchical TiO 2–CuInS 2 core–shell nanoarrays for photoelectrochemical water splitting | |
| CN101214990B (en) | Normal temperature synthesis method for nanometer zinc oxide | |
| CN108893114B (en) | Lead-free halide perovskite quantum dot and preparation method thereof | |
| CN1817799A (en) | Synthesis of TiO2 nanometer particles and bars | |
| CN104785280A (en) | Flaky titanium dioxide/bismuth oxybromide composite photocatalyst and preparation method thereof | |
| CN101074093A (en) | Series of elliptical metal sulfide grain, its production and use | |
| CN100347089C (en) | Synthesis of nanometer block of lead sulfide | |
| CN103191783B (en) | Zinc sulfide-benzoic acid nano composite photocatalytic material and preparation method thereof | |
| CN1693206A (en) | Process for preparing water soluble cadmium telluride quantum point with program controlling microwave | |
| CN101077791A (en) | Method for preparing monodisperse copper sulfide semiconductor nano particles | |
| Sirimekanont et al. | Titanium (IV) oxide composite hollow nanofibres with silver oxide outgrowth by combined sol–gel and electrospinning techniques and their potential applications in energy and environment | |
| CN101066776A (en) | Zinc oxide synthesizing process | |
| CN1314750C (en) | Microwave liquid phase preparation method of polyacrylamide base metal nanometer composite material | |
| CN112898966A (en) | Copper-zinc-indium-sulfur quantum dot, photo-anode, photoelectrochemical cell and preparation method | |
| CN1948167A (en) | Synthesis method of cobaltosic oxide nano-tube | |
| Sedighi et al. | Fabricant and characterization of SrWO4 and novel silver-doped SrWO4 using co-precipitation method: Their photocatalytic performances for methyl orange degradation | |
| CN109574065B (en) | Foliaceous Zn0.2Cd0.8Preparation method of S material | |
| CN104399452A (en) | Method for one-step microwave synthesis of La-Cr co-doped strontium titanate | |
| CN112397659A (en) | Composite material, preparation method thereof and quantum dot light-emitting diode | |
| CN101475148B (en) | Method for preparing CdS or CdSe nano-tube with KCdCl3 nanowire as template | |
| CN101314665B (en) | Photoelectric nano-composite material and preparation thereof | |
| CN1286730C (en) | Bar type zinc oxide granule, preparation method and usage | |
| CN1673091A (en) | Prepn process of nano copper iodide powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20071107 Termination date: 20110119 |