CN102398042A - Preparation method of nanometer gold bar mainly made of (200) crystal face - Google Patents
Preparation method of nanometer gold bar mainly made of (200) crystal face Download PDFInfo
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Abstract
The invention discloses a preparation method of a nanometer gold bar mainly made of (200) crystal face. The method is: adding certain amount of surface active agent, silver salt solution and weak reductant into gold salt solution so as to synthesize growth solution, thus while gold salt is under protection of surface active agent, Au+ or Au3+ is reduced to gold atom by the weak reductant in the growth solution; then adding gold seed into the growth solution, wherein the gold seed is synthesized by adding certain amount of surface active agent and reductant into the gold salt solution, under the induction of silver ion, the surface active agent carrying gold atoms is absorbed on the gold seed which is taken as a growing point, so that a nanometer gold bar mainly made of (200) crystal face is obtained. The method needs temperate condition and is easy to operate, capable of producing nanometer gold bar mainly made of (200) crystal face with controllable shape and size, good water-solubility and sound dispersibility with a high yield. It can be applied into fields of biological analysis, biomedical diagnosis and imaging, biomedical cure, environmental science and analytical science.
Description
Technical field
The present invention relates to the synthetic field of nano material, particularly relating to a kind of is high yield synthetic and the preparation method and the application thereof of master's nm of gold rod with (200) crystal face.
Background technology
Nm of gold has good optics, magnetics, catalytic property and architectural characteristic, can combine with multiple large biological molecule, and not influence its biologically active.Nm of gold with unique physical chemistry attribute and superior biocompatibility is widely used in immune labeled and food security fast detecting field.The different structure of nm of gold and pattern make it present multifarious physicochemical properties.Therefore synthetic nm of gold with novel structure and different-shape is applied to biomedicine and environment food safety detection field, has important and practical meanings.
At present, several different methods can be used to the nm of gold of synthetic different structure and different-shape, like spherical, wire, triangle, cube, polygon and bar-shaped nm of gold.Synthetic the receiving much attention of nm of gold rod wherein; Because its ultra-violet absorption spectrum and fluorescence spectrum all with the excellent length of gold and the line of apsides than relevant, its anisotropy and unique spectral signature are widely used in antibody recognition, nano material assembling, cancer cell imaging and fields such as treatment and DNA analysis.In addition, the nm of gold rod has the response time fast on dynamics, and this unique character makes the nm of gold rod be specially adapted to make biology sensor, is being with a wide range of applications aspect biomedical quick diagnosis and the treatment.
The synthetic method of nm of gold rod mainly contains electrochemical reducing (J.Phys.Chem.B, 1997,101,6661; Langmuir, 1999,15,701) and seed mediated growth method (J.Mater.Chem., 2002,12,2909; Chem.Mater., 2003,15,1957).Use seed mediated growth method synthesis of nano gold rod, receive influence of various factors,, also have the component ratio of various reactants in the system and the reaction rate between them such as size, surfactant, reducing agent and the temperature of gold seeds.The combined influence of above factor makes that the nm of gold that is difficult to a large amount of synthetic size and dimension homogeneous is excellent.In addition, synthetic at present nm of gold rod is main with (111) crystal face, the torpescence yet relative (200) crystal face of (111) crystal face is stable.Therefore, how to prepare that to have more active be that master's nm of gold rod remains a challenge with (200) crystal face.
Summary of the invention
Technical purpose of the present invention is to the above-mentioned state of the art, and the preparation method that a kind of experiment condition is gentle, be easy to repetition, simple and easy to do nm of gold rod is provided, and what can produced in high yields go out pattern, controllable size is that master's nm of gold is excellent with (200) crystal face.
The present invention realizes that the technical scheme that above-mentioned technical purpose adopts is: a kind of is the preparation method of master's nm of gold rod with (200) crystal face, comprises the steps:
Step 1, preparation are the growth-promoting media of master's nm of gold rod with (200) crystal face:
In golden salting liquid, stir adding an amount of surfactant and silver salt solution, stir an amount of weak reductant of adding then fast, then adjust pH value to 5.0～8.0 of mixed solution, obtaining with (200) crystal face is master's the excellent growth-promoting media of nm of gold;
Described surfactant is a quaternary cationics, and its molecular formula is CH
3(CH
2)
mNX (CH
3)
n(CH
2)
p(C
6H
5)
q, m=7～15 wherein, n=2 or 3, p=0 or 1, q=0 or 1, X=Cl, Br, I or F;
Described weak reductant is hydroxylamine hydrochloride (NH
2OHHCl), ascorbic acid (C
6H
8O
6), D-arabo-ascorbic acid (C
6H
8O
6), sodium ascorbate (C
6H
7NaO
6), sodium isoascorbate (C
6H
7NaO
6), Calcium Ascorbate (C
12H
14CaO
122H
2O), monohydrate potassium (C
6H
8O
7H
2O), two hydration trisodium citrate salt (C
6H
5Na
3O
72H
2O), DisodiumHydrogen Citrate salt (C
6H
6Na
2O
71.5H
2O), potassium citrate (K
3C
6H
5O
7H
2O), calcium citrate (Ca
3(C
6H
5O
7)
24H
2O), citric acid hydrogen diamine (C
6H
14N
2O
7) in one or several mixture;
Step 2, preparation are the gold seeds of master's nm of gold rod with (200) crystal face:
In golden salting liquid, stir an amount of surfactant of adding, stir an amount of reducing agent of adding then fast, obtaining with (200) crystal face is master's the excellent gold seeds of nm of gold;
Described surfactant is a quaternary cationics, and its molecular formula is CH
3(CH
2)
mNX (CH
3)
n(CH
2)
p(C
6H
5)
q, m=7～15 wherein, n=2 or 3, p=0 or 1, q=0 or 1, X=Cl, Br, I or F.
Described reducing agent is one or several the mixture in sodium borohydride, potassium borohydride, lithium borohydride, sodium cyanoborohydride, sodium triacetoxy borohydride, tetra-n-butyl tetrahydrochysene ammonium borate, hydroxylamine hydrochloride, citric acid, citrate and ascorbic acid and the ascorbate;
Step 3, preparation are master's nm of gold rod with (200) crystal face:
The gold seeds that step (2) is prepared adds in the growth-promoting media that step (1) prepares fast, in being higher than the environment of room temperature, keeps in Dark Place 12～36 hours, and obtaining with (200) crystal face is that master's nm of gold is excellent.
Described golden salt includes but not limited to one or more in chlorauride, aurous chloride, chlorine carboxyl gold, gold bromide, chlorine (dimethyl sulfuration) gold, dimethylphenylphosphine chlorauride, methyl (triphenylphosphine) gold, chloro tri-tert phosphatization gold, gold chloride, potassium chloroaurate and the sodium chloraurate.
Described silver salt includes but not limited to one or more in silver nitrate, silver acetate, trifluoroacetic acid silver, trifluoro-methane sulfonic acid silver, hexafluoro-antimonic acid silver and the silver tetrafluoroborate.
Described surfactant comprises but is not limited in softex kw, DTAC and the dodecyl benzyl dimethyl ammonium chloride one or more.
Provided by the invention is that concrete course of reaction comprises among master's the preparation method of nm of gold rod with (200) crystal face:
(1) golden salt is under the protective effect of surfactant, the gold (Au of its monovalence or trivalent
+Or Au
3+) in growth-promoting media, be reduced into the gold atom (Au of zeroth order by weak reductant
0), the pH value of regulating growth-promoting media then is in 5.0～8.0 scopes;
(2) at silver ion (Ag
+) inducing action under, be growing point with the gold seeds, surfactant carries the gold atom (Au of zeroth order
0) be adsorbed on gradually on the gold seeds growing point, after 12～36 hours, just the high yield acquisition is master's nm of gold rod with (200) crystal face.
What utilize that preparation method provided by the invention obtains is that master's nm of gold rod is specifically tested through following with (200) crystal face:
(1) observe through SEM (SEM) figure and transmission electron microscope (TEM) figure, the radical length scope that obtains this nm of gold rod is 10～100nm, and the transverse width scope is 2～20nm;
(2) observe through high resolution transmission electron microscopy (HRTEM) and SEAD (SAED), the lattice that obtains this nm of gold rod is clear, and the lattice fringe spacing is about 0.205nm, matches with the interplanar distance of face-centered cubic gold (200) crystal face mutually;
(3) observe through SEAD (SAED), obtain the symmetric crystal lattice that this nm of gold rod has height, confirmed that this nm of gold rod is monocrystalline;
(4) through SEAD (SAED) crystal structure and the power spectrum of this nm of gold rod are further studied, proved that further this nm of gold rod is main with (200) crystal face;
(5) through X-ray diffractometer the total quality and the purity of this nm of gold rod are studied; Show that this nm of gold rod is pure face-centred cubic structure; (200) crystal face is about 1.65 with the ratio of the diffracted intensity of (111) crystal face, proves that once more this nm of gold rod is main with (200) crystal face.
(6) through X-ray energy spectrum (EDS) element in this nm of gold rod is analyzed, it is single to obtain this nm of gold rod composition;
Therefore, provided by the invention is that the preparation method of master's nm of gold rod has the following advantages with (200) crystal face:
(1) preparation condition is gentle, the preparation method is simple; Can produced in high yields go out pattern and controllable size; And size homogeneous, good water solubility, good dispersion is master's nm of gold rod with (200) crystal face; And workable, good reproducibility, have universality, can prepare in enormous quantities, can satisfy the demand of different subjects and technical field;
(2) the nm of gold rod for preparing is main with (200) crystal face, and is active strong, is more suitable for being used for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Description of drawings
Fig. 1 is preparation technology's flow chart of master's nm of gold rod with (200) crystal face for the present invention;
Fig. 2 (a) is the excellent scanning electron microscope diagram of nm of gold for preparing among the embodiment 1;
Fig. 2 (b) is the excellent transmission electron microscope figure of nm of gold for preparing among the embodiment 1;
Fig. 3 (a) is the excellent high resolution transmission electron microscopy figure of single nm of gold for preparing among the embodiment 1;
Fig. 3 (b) is the excellent SEAD figure of single nm of gold for preparing among the embodiment 1;
Fig. 4 (a) is the diffraction surfaces analysis chart of the SEAD figure of Fig. 2 (b) nm of gold rod;
Fig. 4 (b) is the excellent X-ray energy spectrum of nm of gold for preparing among the embodiment 1;
Fig. 5 is the excellent X-ray diffraction spectrum of nm of gold for preparing among the embodiment 1;
Fig. 6 is the ultraviolet-visible absorption spectroscopy of the nm of gold rod solution for preparing among the embodiment 1.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done to describe in further detail, it is pointed out that the following stated embodiment is intended to be convenient to understanding of the present invention, and it is not played any qualification effect.
Embodiment 1:
In the present embodiment, be that the preparation process of master's nm of gold rod comprises the steps: with (200) crystal face
(1) preparation is the growth-promoting media of master's nm of gold rod with (200) crystal face:
Be higher than in the environment of room temperature in temperature, getting the 1mL molar concentration is the four hydration gold chloride (HAuCl of 5mM
44H
2O) solution, adding the 5mL molar concentration respectively is the softex kw (CH of 0.2M
3(CH
2)
15NBr (CH
3)
3) solution and 100uL molar concentration be the silver nitrate (AgNO of 0.01M
3) solution, stir 10min; Adding the 1mL molar concentration then rapidly is the hydroxylamine hydrochloride (NH of 0.1M
2OHHCl) solution continues to stir 2min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 5.68, synthetic (200) crystal face that makes 7.1mL is the main excellent growth-promoting media of nm of gold.
(2) preparation is the gold seeds of master's nm of gold rod with (200) crystal face:
Be higher than in the environment of room temperature in temperature, getting the 5mL molar concentration is the four hydration gold chloride (HAuCl of 0.5mM
44H
2O) solution, adding the 5mL molar concentration is the softex kw (CH of 0.2M
3(CH
2)
15NBr (CH
3)
3) solution, stir 10min; Adding the 600uL molar concentration then rapidly is the sodium borohydride (NaBH of 0.01M
4) solution, continue to stir 2min, making with (200) crystal face is the gold seeds of master's nm of gold rod, keeps in Dark Place.
(3) preparation is master's nm of gold rod with (200) crystal face:
Get the gold seeds of 15uL step (2) preparation, add fast in the growth-promoting media of step (1) preparation, place temperature to be higher than the environment of room temperature, kept in Dark Place 24 hours, making with (200) crystal face is master's nm of gold rod.
It is above-mentioned that what prepare is that master's the test performance of nm of gold rod is following with (200) crystal face:
(1) Fig. 2 (a) is SEM (SEM) figure of this nm of gold rod, and Fig. 2 (b) is transmission electron microscope (TEM) figure of this nm of gold rod.As can be seen from the figure, the radical length scope of this nm of gold rod is 10～100nm, and the transverse width scope is 2～20nm.
(2) use high resolution transmission electron microscopy (HRTEM) and SEAD (SAED) that the single nm of gold rod of picked at random is studied, see Fig. 3.Fig. 3 (a) is high resolution transmission electron microscopy (HRTEM) figure of single nm of gold rod, and it is the about 0.205nm of lattice fringe spacing clearly, matches with the interplanar distance of face-centered cubic gold (200) crystal face mutually.Fig. 3 (b) is the SEAD figure (SAED) of single nm of gold rod, and the diffraction spot from figure can know that synthetic nm of gold rod has the symmetric crystal lattice of height, has confirmed that this nm of gold rod is monocrystalline.
(3) use SEAD (SAED) that the crystal structure and the power spectrum of this nm of gold rod are further studied, see Fig. 4.The diffraction ring that occurs among Fig. 4 (a) is respectively (111), (200), (220), (311), (222) and (400) crystal face (with reference to goldstandard spectrum JCPDS file No.4-0783) from inside to outside through calculating four diffraction surfaces.Wherein the diffraction ring of (200) crystal face is the brightest, proves that further this nm of gold rod is main with (200) crystal face.In addition; Fig. 4 (b) is the X-ray energy spectrum (EDS) of this nm of gold rod; Analyze and confirm: only contain gold dollar element (Au) in this nm of gold rod; Wherein the signal of carbon (C) and copper (Cu) element is from doing the ultrathin carbon films that has copper mesh that transmission electron microscope (TEM) when test use, and the content of silver components is because too low and do not measured simultaneously.
(4) in order to study the total quality and the purity of this nm of gold rod, use X-ray diffractometer (XRD) to characterize this nm of gold rod, see Fig. 5.Visible from Fig. 5; Locate the strong sharp-pointed diffraction maximum of comparison at 44.35 °; Can know through looking into JCPDS standard card: this diffraction maximum is corresponding to (200) crystal face of face-centered cubic gold; Wherein 38.34 °, 64.72 °, 77.61 °, 81.89 ° and 98.26 ° of diffraction maximums of locating correspond respectively to (111), (220), (311), (222) and (400) crystal face of gold, do not find the diffraction maximum of other impurity, show that this nm of gold rod is pure face-centred cubic structure; (200) crystal face is about 1.65 with the ratio of the diffracted intensity of (111) crystal face, proves that once more this nm of gold rod is main with (200) crystal face.
(5) Fig. 6 is UV, visible light absorption (UV-vis) spectrum of this nm of gold rod.As shown in Figure 6, this nm of gold rod has two plasma resonance absworption peaks: an absorbing wavelength is between 500～550, and another absorbing wavelength is between 700～830nm.
Embodiment 2:
In the present embodiment, be that the preparation process of master's nm of gold rod comprises the steps: with (200) crystal face
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the four hydration gold chloride (HAuCl of 100mL 5mM
44H
2O) solution adds the softex kw (CH of 500mL 0.2M respectively
3(CH
2)
15NBr (CH
3)
3) silver nitrate (AgNO of solution and 10mL 0.01M
3) solution, stir 10min; Hydroxylamine hydrochloride (the NH that adds 100mL0.1M then rapidly
2OHHCl) solution continues to stir 2min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 5.0, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
This step (2) is identical with step (2) among the embodiment 1.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 1.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 12 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 3:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the two hydration potassium chloroaurate (KAuCl of 100mL 5mM
42H
2O) solution adds the dodecyl benzyl dimethyl ammonium chloride (CH of 500mL 0.2M respectively
3(CH
2)
11NCl (CH
3)
2CH
2C
6H
5) silver nitrate (AgNO of solution and 10mL 0.01M
3) solution, stir 10min; Hydroxylamine hydrochloride (the NH that adds 100mL 0.1M then rapidly
2OHHCl) solution continues to stir 2min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 6.08, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the gold chloride (HAuCl of 1mL 0.5mM
4) solution, the DTAC (CH of adding 1mL 0.2M
3(CH
2)
11NCl (CH
3)
3) solution, stir 10min.Potassium borohydride (the KBH that adds 120uL 0.01M then rapidly
4) solution, continue to stir 2min, making synthetic (200) crystal face is the main excellent gold seeds of nm of gold, keeps in Dark Place.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 1.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 36 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 4:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the two hydration potassium chloroaurate (KAuCl of 100mL 5mM
42H
2O) solution adds the DTAC (CH of 500mL 0.2M respectively
3(CH
2)
11NCl (CH
3)
3) silver nitrate (AgNO of solution and 10mL 0.01M
3) solution, stir 10min; Hydroxylamine hydrochloride (the NH that adds 10mL 0.1M then rapidly
2OHHCl) solution continues to stir 2min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 6.55, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the chlorauride (AuCl of 1mL 0.2M
3) solution, the dodecyl benzyl dimethyl ammonium chloride (CH of adding 1mL0.2M
3(CH
2)
11NCl (CH
3)
2CH
2C
6H
5) solution, stir 10min; Potassium borohydride (the KBH that adds 120uL 0.01M then rapidly
4) solution, continue to stir 2min, making synthetic (200) crystal face is the main excellent gold seeds of nm of gold, keeps in Dark Place.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 1.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 14 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 5:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the two hydration sodium chloraurate (NaAuCl of 100mL 5mM
42H
2O) solution adds the softex kw (CH of 500mL 0.2M respectively
3(CH
2)
15NBr (CH
3)
3) silver acetate (CH of solution and 10mL 0.01M
3COOAg) solution stirs 10min; Ascorbic acid (the C that adds 100mL 1mM then rapidly
6H
8O
6) solution, continue to stir 2min; Use cushioning liquid that the pH value of growth-promoting media is transferred to 6.88, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the two hydration potassium chloroaurate (KAuCl of 1mL 0.2M
42H
2O) solution, the 0.2M DTAC (CH of adding 1mL
3(CH
2)
11NCl (CH
3)
3) solution, stir 10min; Potassium borohydride (the KBH that adds the 0.01M of 120uL then rapidly
4) solution, continue to stir 2min, making synthetic (200) crystal face is the main excellent gold seeds of nm of gold, keeps in Dark Place.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 1.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 20 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 6:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the gold chloride (HAuCl of 100mL 5mM
4) solution, add the DTAC (CH of 500mL 0.2M respectively
3(CH
2)
11NCl (CH
3)
3) silver tetrafluoroborate (AgBF of solution and 10mL 0.01M
4) solution, stir 10min; Ascorbic acid (the C that adds 1mL 0.01M then rapidly
6H
8O
6) solution, continue to stir 2min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 7.88, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the two hydration sodium chloraurate (NaAuCl of 1mL 0.2M
42H
2O) solution, the dodecyl benzyl dimethyl ammonium chloride (CH of adding 1mL 0.2M
3(CH
2)
11NCl (CH
3)
2CH
2C
6H
5) solution, stir 10min; Sodium borohydride (the NaBH that adds 120uL 0.01M then rapidly
4) solution, continue to stir 2min, making synthetic (200) crystal face is the main excellent gold seeds of nm of gold, keeps in Dark Place.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 1.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 22 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 7:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get aurous chloride (AuCl) solution of 100mL 5mM, add the DTAC (CH of 500mL 0.2M respectively
3(CH
2)
11NCl (CH
3)
3) the trifluoroacetic acid silver (CF of solution and 10mL 0.01M
3COOAg) solution stirs 10min; Monohydrate potassium (the C that adds 100mL0.1M then rapidly
6H
8O
7H
2O) solution continues to stir 2min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 8.0, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get aurous chloride (AuCl) solution of 1mL 0.5mM, add the softex kw (CH of 1mL 0.2M
3(CH
2)
15NBr (CH
3)
3) solution, stir 10min.Potassium borohydride (the KBH that adds 120uL 0.01M then rapidly
4) solution, continue to stir 2min, making synthetic (200) crystal face is the main excellent gold seeds of nm of gold, keeps in Dark Place.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 1.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 30 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 8:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the chlorauride (AuCl of 100mL 5mM
3) solution, add the DTAC (CH of 500mL 0.2M respectively
3(CH
2)
11NCl (CH
3)
3) the hexafluoro-antimonic acid silver (AgSbF of solution and 10mL0.01M
4) solution, stir 10min; Calcium citrate (the Ca that adds 100mL 1mM then rapidly
3(C
6H
5O
7)
24H
2O) solution continues to stir 2min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 7.0, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the gold chloride (HAuCl of 1mL 0.5mM
4) solution, the DTAC (CH of adding 1mL 0.2M
3(CH
2)
11NCl (CH
3)
3) solution, stir 10min.Potassium borohydride (the KBH that adds 120uL 0.01M then rapidly
4) solution, continue to stir 2min, making synthetic (200) crystal face is the main excellent gold seeds of nm of gold, keeps in Dark Place.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 1.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 34 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 9:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the gold chloride (HAuCl of 100mL 5mM
4) solution, add the dodecyl benzyl dimethyl ammonium chloride (CH of 500mL 0.2M respectively
3(CH
2)
11NCl (CH
3)
2CH
2C
6H
5) trifluoro-methane sulfonic acid silver (CF of solution and 10mL 0.01M
3SO
3Ag) solution stirs 10min; Sodium ascorbate (the C that adds 100mL 0.1M then rapidly
6H
7NaO
6) solution, continue to stir 2min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 7.4, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
This step (2) is identical with step (2) among the embodiment 5.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 1.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 25 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 10:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the three hydration gold chloride (HAuCl of 100mL 5mM
43H
2O) solution adds the DTAC (CH of 500mL 0.2M respectively
3(CH
2)
11NCl (CH
3)
3) silver tetrafluoroborate (AgBF of solution and 10mL 0.01M
4) solution, stir 10min; The two hydration trisodium citrate salt (C that add 100mL 0.1M then rapidly
6H
5Na
3O
72H
2O) solution continues to stir 2min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 5.8, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
This step (2) is identical with step (2) among the embodiment 1;
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 1.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 33 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 11:
In the present embodiment, be that the preparation process of master's nm of gold rod comprises the steps: with (200) crystal face
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the four hydration gold bromide (AuBr of 100mL 5mM
3) solution, add the softex kw (CH of 500mL 0.2M respectively
3(CH
2)
15NBr (CH
3)
3) silver nitrate (AgNO of solution and 10mL 0.01M
3) solution, stir 10min; D-arabo-ascorbic acid (the C that adds 100mL 0.1M then rapidly
6H
8O
6) solution, continue to stir 5min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 5.0, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the four hydration gold bromide (AuBr of 1mL 0.5mM
3) solution, the DTAC (CH of adding 1mL 0.2M
3(CH
2)
11NCl (CH
3)
3) solution, stir 10min.Lithium borohydride (the LiBH that adds 120uL 0.01M then rapidly
4) solution, continue to stir 15min, making synthetic (200) crystal face is the main excellent gold seeds of nm of gold, keeps in Dark Place.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 1.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 32 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 12:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get chlorine carboxyl gold (CAuClO) solution of 100mL 5mM, add the dodecyl benzyl dimethyl ammonium chloride (CH of 500mL 0.2M respectively
3(CH
2)
11NCl (CH
3)
2CH
2C
6H
5) silver nitrate (AgNO of solution and 10mL 0.01M
3) solution, stir 10min; Sodium ascorbate (the C that adds 100mL 0.1M then rapidly
6H
7NaO
6) solution, continue to stir 3min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 6.0, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get chlorine carboxyl gold (CAuClO) solution of 1mL 0.5mM, add the DTAC (CH of 1mL 0.2M
3(CH
2)
11NCl (CH
3)
3) solution, stir 12min.Sodium cyanoborohydride (the CH that adds 120uL 0.01M then rapidly
3BNNa) solution continues to stir 2min, and making synthetic (200) crystal face is the main excellent gold seeds of nm of gold, keeps in Dark Place.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 2mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 16 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 13:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get chlorine (dimethyl sulfuration) the gold ((CH of 100mL 5mM
3)
2SAuCl) solution adds the DTAC (CH of 500mL 0.2M respectively
3(CH
2)
11NCl (CH
3)
3) silver nitrate (AgNO of solution and 10mL 0.01M
3) solution, stir 10min; DisodiumHydrogen Citrate salt (the C that adds 10mL 0.01M then rapidly
6H
6Na
2O
71.5H
2O) solution continues to stir 2min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 7.55, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get chlorine (dimethyl sulfuration) the gold ((CH of 1mL 0.2M
3)
2SAuCl) solution, the dodecyl benzyl dimethyl ammonium chloride (CH of adding 1mL 0.2M
3(CH
2)
11NCl (CH
3)
2CH
2C
6H
5) solution, stir 5min; Sodium triacetoxy borohydride (the C that adds 120uL 0.01M then rapidly
6H
10BNaO
6) solution, continue to stir 2min, making synthetic (200) crystal face is the main excellent gold seeds of nm of gold, keeps in Dark Place.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 1.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 15 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 14:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the dimethylphenylphosphine chlorauride (C of 100mL 5mM
8H
11AuClP) solution adds the softex kw (CH of 500mL 0.2M respectively
3(CH
2)
15NBr (CH
3)
3) silver acetate (CH of solution and 10mL 0.01M
3COOAg) solution stirs 10min; Sodium isoascorbate (the C that adds 100mL 1mM then rapidly
6H
7NaO
6) solution, continue to stir 2min; Use cushioning liquid that the pH value of growth-promoting media is transferred to 7.88, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the dimethylphenylphosphine chlorauride (C of 1mL 0.2M
8H
11AuClP) solution, the 0.2M DTAC (CH of adding 1mL
3(CH
2)
11NCl (CH
3)
3) solution, stir 10min; The tetra-n-butyl tetrahydrochysene ammonium borate (C that adds the 0.01M of 120uL then rapidly
16H
40BN) solution continues to stir 4min, and making synthetic (200) crystal face is the main excellent gold seeds of nm of gold, keeps in Dark Place.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 1.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 23 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 15:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get methyl (triphenylphosphine) the gold ((C of 100mL 5mM
6H
5)
3PAuCH
3) solution, add the DTAC (CH of 500mL 0.2M respectively
3(CH
2)
11NCl (CH
3)
3) silver tetrafluoroborate (AgBF of solution and 10mL 0.01M
4) solution, stir 10min; Calcium Ascorbate (the C that adds 1mL 0.01M then rapidly
12H
14CaO
122H
2O) solution continues to stir 2min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 8.0, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get methyl (triphenylphosphine) the gold ((C of 1mL 0.2M
6H
5)
3PAuCH
3) solution, the dodecyl benzyl dimethyl ammonium chloride (CH of adding 1mL 0.2M
3(CH
2)
11NCl (CH
3)
2CH
2C
6H
5) solution, stir 10min; The tetra-n-butyl tetrahydrochysene ammonium borate (C that adds 120uL 0.01M then rapidly
16H
40BN) solution continues to stir 2min, and making synthetic (200) crystal face is the main excellent gold seeds of nm of gold, keeps in Dark Place.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 1.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 28 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 16:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get chloro tri-tert phosphatization the gold ((C of 100mL 5mM
4H
9)
3PAuCl) solution adds the DTAC (CH of 500mL 0.2M respectively
3(CH
2)
11NCl (CH
3)
3) the trifluoroacetic acid silver (CF of solution and 10mL 0.01M
3COOAg) solution stirs 10min; Citric acid hydrogen diamine (the C that adds 100mL 0.1M then rapidly
6H
14N
2O
7) solution, continue to stir 5min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 6.48, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get chloro tri-tert phosphatization the gold ((C of 1mL 0.5mM
4H
9)
3PAuCl) solution, the softex kw (CH of adding 1mL 0.2M
3(CH
2)
15NBr (CH
3)
3) solution, stir 10min.Potassium borohydride (the KBH that adds 120uL 0.01M then rapidly
4) solution, continue to stir 2min, making synthetic (200) crystal face is the main excellent gold seeds of nm of gold, keeps in Dark Place.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 1.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 36 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 17:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the chlorauride (AuCl of 100mL 5mM
3) solution, add the DTAC (CH of 500mL 0.2M respectively
3(CH
2)
11NCl (CH
3)
3) the hexafluoro-antimonic acid silver (AgSbF of solution and 10mL0.01M
4) solution, stir 10min; DisodiumHydrogen Citrate salt (the C that adds 100mL 0.1M then rapidly
6H
6Na
2O
71.5H
2O) solution continues to stir 6min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 5.5, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the gold chloride (HAuCl of 1mL 0.5mM
4) solution, the DTAC (CH of adding 1mL 0.2M
3(CH
2)
11NCl (CH
3)
3) solution, stir 10min.Ascorbic acid (the C that adds 1mL 1M then rapidly
6H
8O
6) solution, continue to stir 10min, making synthetic (200) crystal face is the main excellent gold seeds of nm of gold, keeps in Dark Place.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 2.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 24 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 18:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get chlorine (dimethyl sulfuration) the gold ((CH of 100mL 5mM
3)
2SAuCl) solution adds the dodecyl benzyl dimethyl ammonium chloride (CH of 500mL 0.2M respectively
3(CH
2)
11NCl (CH
3)
2CH
2C
6H
5) trifluoro-methane sulfonic acid silver (CF of solution and 10mL 0.01M
3SO
3Ag) solution stirs 8min; Sodium isoascorbate (the C that adds 100mL 0.1M then rapidly
6H
7NaO
6) solution, continue to stir 12min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 7.8, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
This step (2) is identical with step (2) among the embodiment 6.
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 3.5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 25 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 19:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get the four hydration gold chloride (HAuCl of 100mL 5mM
44H
2O) solution adds the DTAC (CH of 500mL 0.2M respectively
3(CH
2)
11NCl (CH
3)
3) silver tetrafluoroborate (AgBF of solution and 10mL 0.01M
4) solution, stir 6min; Potassium citrate (the K that adds 100mL 0.1M then rapidly
3C
6H
5O
7H
2O) solution continues to stir 2min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 6.8, synthetic (200) crystal face that makes 710mL is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
This step (2) is identical with step (2) among the embodiment 1;
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 5mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 36 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Embodiment 20:
(1) synthetic (200) crystal face is the main excellent growth-promoting media preparation of nm of gold:
Be higher than in the environment of room temperature in temperature, get methyl (triphenylphosphine) the gold ((C of 100mL 5mM
6H
5)
3PAuCH
3) solution, add the softex kw (CH of 5mL 0.2M respectively
3(CH
2)
15NBr (CH
3)
3) silver nitrate (AgNO of solution and 10mL 0.01M
3) solution, stir 10min; Potassium citrate (the K that adds 10mL 0.01M then rapidly
3C
6H
5O
7H
2O) solution continues to stir 2min; Then use cushioning liquid that the pH value of growth-promoting media is transferred to 6.6, making synthetic (200) crystal face is the main excellent growth-promoting media of nm of gold.
(2) synthetic (200) crystal face is the main excellent gold seeds preparation of nm of gold:
This step (2) is identical with step (2) among the embodiment 17;
(3) synthetic (200) crystal face is the main excellent preparation of nm of gold:
Get the gold seeds of 10mL step (2) preparation, add the growth-promoting media of step (1) preparation fast, place temperature to be higher than the environment of room temperature, kept in Dark Place 26 hours, making with (200) crystal face is master's nm of gold rod.
Adopt with embodiment 1 in identical method of testing what prepare is that master's nm of gold rod is tested with (200) crystal face to above-mentioned, obtaining this nm of gold rod, to have with (200) crystal face be master's mono-crystalline structures, size homogeneous, composition are simple.Therefore, be main with (200) crystal face in the mono-crystalline structures of this nm of gold rod, active strong, be suitable for fields such as bioanalysis, biomedical diagnostic and imaging, biomedical treatment, environmental science and analysis science.
Above-described embodiment specifies technical scheme of the present invention; Be understood that the above is merely specific embodiment of the present invention; Be not limited to the present invention; The all any modifications in principle scope of the present invention, made and improvement etc. all should be included within protection scope of the present invention.
Claims (4)
1. one kind is the preparation method of master's nm of gold rod with (200) crystal face, it is characterized in that: comprise the steps:
Step 1, preparation are the growth-promoting media of master's nm of gold rod with (200) crystal face:
In golden salting liquid, stir adding an amount of surfactant and silver salt solution, stir an amount of weak reductant of adding then fast, then adjust pH value to 5.0～8.0 of mixed solution, obtaining with (200) crystal face is master's the excellent growth-promoting media of nm of gold;
Described surfactant is a quaternary cationics, and its molecular formula is CH
3(CH
2)
mNX (CH
3)
n(CH
2)
p(C
6H
5)
q, m=7～15 wherein, n=2 or 3, p=0 or 1, q=0 or 1, X=Cl, Br, I or F;
Described weak reductant is one or several the mixture in hydroxylamine hydrochloride, ascorbic acid, D-arabo-ascorbic acid, sodium ascorbate, sodium isoascorbate, Calcium Ascorbate, monohydrate potassium, two hydration trisodium citrate salt, DisodiumHydrogen Citrate salt, potassium citrate, calcium citrate, the citric acid hydrogen diamine;
Step 2, preparation are the gold seeds of master's nm of gold rod with (200) crystal face:
In golden salting liquid, stir an amount of surfactant of adding, stir an amount of reducing agent of adding then fast, obtaining with (200) crystal face is master's the excellent gold seeds of nm of gold;
Described surfactant is a quaternary cationics, and its molecular formula is CH
3(CH
2)
mNX (CH
3)
n(CH
2)
p(C
6H
5)
q, m=7～15 wherein, n=2 or 3, p=0 or 1, q=0 or 1, X=Cl, Br, I or F.
Described reducing agent is one or several the mixture in sodium borohydride, potassium borohydride, lithium borohydride, sodium cyanoborohydride, sodium triacetoxy borohydride, tetra-n-butyl tetrahydrochysene ammonium borate, hydroxylamine hydrochloride, citric acid, citrate and ascorbic acid and the ascorbate;
Step 3, preparation are master's nm of gold rod with (200) crystal face:
The gold seeds that step (2) is prepared adds in the growth-promoting media that step (1) prepares fast, in being higher than the environment of room temperature, keeps in Dark Place 12～36 hours, and obtaining with (200) crystal face is that master's nm of gold is excellent.
2. according to claim 1 is the preparation method of master's nm of gold rod with (200) crystal face, and it is characterized in that: described golden salt is one or more in chlorauride, aurous chloride, chlorine carboxyl gold, gold bromide, chlorine (dimethyl sulfuration) gold, dimethylphenylphosphine chlorauride, methyl (triphenylphosphine) gold, chloro tri-tert phosphatization gold, gold chloride, potassium chloroaurate and the sodium chloraurate.
3. according to claim 1 and 2 is the preparation method of master's nm of gold rod with (200) crystal face, and it is characterized in that: described silver salt is one or more in silver nitrate, silver acetate, trifluoroacetic acid silver, trifluoro-methane sulfonic acid silver, hexafluoro-antimonic acid silver and the silver tetrafluoroborate.
4. according to claim 1 and 2 is the preparation method of master's nm of gold rod with (200) crystal face, and it is characterized in that: described surfactant comprises one or more in softex kw, DTAC and the dodecyl benzyl dimethyl ammonium chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110363934 CN102398042B (en) | 2011-11-16 | 2011-11-16 | Preparation method of nanometer gold bar mainly made of (200) crystal face |
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| CN103203459A (en) * | 2013-03-08 | 2013-07-17 | 华南师范大学 | Method for preparing gold nano-rods |
| CN103878382A (en) * | 2012-12-20 | 2014-06-25 | 江南大学 | Preparation method for special-shaped gold nanocrystals and application on detection of tripolycyanamide by using surface enhanced Raman scattering |
| CN104209533A (en) * | 2014-07-21 | 2014-12-17 | 苏州大学 | Method for rapidly preparing gold nanorod |
| CN104249159A (en) * | 2013-06-26 | 2014-12-31 | 梁萍 | Method for largely preparing gold nanorods |
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| CN103878382A (en) * | 2012-12-20 | 2014-06-25 | 江南大学 | Preparation method for special-shaped gold nanocrystals and application on detection of tripolycyanamide by using surface enhanced Raman scattering |
| CN103203459B (en) * | 2013-03-08 | 2015-05-06 | 华南师范大学 | Method for preparing gold nano-rods |
| CN103203459A (en) * | 2013-03-08 | 2013-07-17 | 华南师范大学 | Method for preparing gold nano-rods |
| CN104249159A (en) * | 2013-06-26 | 2014-12-31 | 梁萍 | Method for largely preparing gold nanorods |
| CN104209533A (en) * | 2014-07-21 | 2014-12-17 | 苏州大学 | Method for rapidly preparing gold nanorod |
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| CN104907578A (en) * | 2015-04-29 | 2015-09-16 | 福州大学 | Method for preparing gold nanorods |
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| CN105499598A (en) * | 2015-12-10 | 2016-04-20 | 上海交通大学 | Preparation method for gold nano-rods |
| CN105665748A (en) * | 2016-04-25 | 2016-06-15 | 辽宁石化职业技术学院 | Method for preparing high-purity superfine silver powder |
| CN105665748B (en) * | 2016-04-25 | 2018-01-19 | 辽宁石化职业技术学院 | A kind of preparation method of high pure and ultra-fine silver powder |
| CN106077705A (en) * | 2016-08-19 | 2016-11-09 | 东华大学 | A kind of preparation method of gold nanorods |
| CN108043195A (en) * | 2017-11-13 | 2018-05-18 | 广州泓生物科技有限公司 | A kind of nanogold gas purification liquid and preparation method and application |
| CN108097979A (en) * | 2017-12-18 | 2018-06-01 | 苏州中科纳福材料科技有限公司 | A kind of preparation method of metal nanoparticle |
| CN111085692A (en) * | 2019-12-27 | 2020-05-01 | 季华实验室 | Irregular alloy nano material synthesis method based on high-temperature water phase reaction |
| CN114082936A (en) * | 2021-11-19 | 2022-02-25 | 杭州电子科技大学 | Synthesis method of gold nanorods with good monodispersity |
| CN114082936B (en) * | 2021-11-19 | 2024-05-24 | 杭州电子科技大学 | Gold nanorod synthesis method with good monodispersity |
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