CN101376745A - Method for synthesizing molybdena-polyaniline polyaniline composite single crystal nanowire - Google Patents
Method for synthesizing molybdena-polyaniline polyaniline composite single crystal nanowire Download PDFInfo
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Abstract
The invention relates to the technical field of nanometer materials, in particular to a synthesizing method of a molybdena-polyaniline compound monocrystalline nano-line which includes the following steps: molybdate is dissolved in water; the mol concentration of molybdenum atoms is 0.05 to 1.0 mol/L; aniline monomers are injected in the liquid of the molybdate; the mol ratio of the aniline monomers to the molybdenum atoms in the liquid of the molybdate is 4.0-1.0 : 1; inorganic acid is added in the liquid; the pH value is adjusted between 2 and 5 until a white deposit appears and then the liquid is manufactured into a reaction liquid; the reaction liquid is transferred into an oil bath with a temperature between 30 and 60 DEG C for reacting for 2 to 12 hours; then the product is washed, extracted, filtered and dried. The invention has the advantages as follows: the prepared compound nano-line has a regular organic-inorganic compound nanometer periodical structure, has the characteristics of controllable physicochemical properties, large specific surface area as well as controllable thickness and length as well as can be applied to a plurality of fields; the yield can achieve more than 95 percent; the preparation condition is simple and is easily controlled; the preparation efficiency is high; the product quality and the finished product rate are high; besides, the invention has excellent application and industrialization prospects.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire.
Background technology
Hybrid inorganic-organic materials refers to the hydridization of organic and inorganic material under nanoscale, a series of matrix materials that combine inorganic materials, organic materials, nano material good characteristic of having derived thus.Closely contact the inferior nano periodic structure of formation by weak interaction (Van der Waals force, hydrogen bond, electrostatic attraction or hydrophilic hydrophobic interaction) between the organic and inorganic two-phase, be inferior nanometer sheet or the nano wire (less than 10nm) that the embedding of organic molecule is divided into inorganic skeleton periodic arrangement, cause material quantum effect (QCE) obviously to strengthen, the energy level band gap widens, for example CdSe (en)
0.5Compared 1.0eV high than the energy level band gap of CdSe.And, by adjusting the kind and the ratio of organism, inorganics, can regulate and control the physico-chemical property of matrix material, for example (W.T.Yao such as optics, electricity, S.H.Yu, X.Y.Huang, J.Jiang, L.Q.Zhao, L.Pan, J.Li Adv.Mater.2005,17,2799; Y.J.Dong, Q.Peng, Y.D.Li Inorg.Chem.Commun.2004,7,370; W.T.Yao, S.H.Yu, Q.S.Wu, Adv.Fun.Mater.2007,17,623; Q.S.Gao, P.Chen, Y, H.Zhang, Y.Tang, Adv.Mater.2008,20,1837).
The hybrid inorganic-organic monodimension nanometer material is one of research field that wherein is even more important, and its distinctive one dimension Nano structure has caused the characteristic of nano materials such as small-size effect, surface effects, has good assembling performance, and abundant physical and chemical performance; Simultaneously, periodic inferior nanostructure modulation character such as inorganic materials electricity, optics, magnetics.Therefore, the research of hybrid inorganic-organic monodimension nanometer material will greatly change key areas such as traditional material science, micro-nano electronics, nonlinear optics, magneticsubstance and medical science.
Molybdenum oxide is important semiconductor material, at embedded photoluminescent material, electrode materials, there is purposes widely in field such as catalysis, sensing, and the unidimensional nanotopography can be strengthened the above-mentioned character of molybdenum oxide, and the molybdenum oxide nano wire that for example has big outside surface is because of embodying higher capacity and good cyclicity in anode material for lithium-ion batteries.Polyaniline is important conducting polymer, and itself and molybdenum oxide are carried out the compound conductive capability that will improve material at inferior nanoscale, and derives numerous special physicochemical property.Therefore, synthetic molybdena-polyaniline polyaniline composite nano-line will enrich the synthetic of organic and inorganic one-dimensional material, help the more powerful nano-device of design function.Yet, still have nothing to do at present and report in molybdena-polyaniline polyaniline composite nano-line synthetic.
At present, the molybdena-polyaniline polyaniline matrix material that is successfully synthesized mainly is massive material or composite membrane etc., the main method that adopts the back to embed, promptly aniline monomer is embedded the interlayer of molybdenum oxide by the method for repeatedly ion-exchange, and then the method by oxypolymerization is with aniline polymerization (Kerr, T.A.; Wu, H.; Nazar, F.Chem.Mater.1996,8,2005; Wang, J.Z.; Matsubara, I.; Murayama, N.; Woosuck, S.; Izu, N.ThinSolid Films 2006,514,329; Liu, X.X.; Bian, L.J.; Zhang, L.; Zhang, L.J.J.Solid State Electrochem.2007,11,1279; N.Ballav, M.Biswas, Mater.Lett.2006,60,514).There are shortcomings such as complex steps, complicated operation, product be impure in this method, has limited the scale operation and the application of molybdena-polyaniline polyaniline matrix material; The product yardstick that obtains simultaneously is not a nano material greater than several microns, can't use in emerging fields such as nano-device, micro-nano electronics.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire of simple and easy to control, economical rationality; Another technical problem to be solved is to provide the molybdena-polyaniline polyaniline composite single crystal nanowire that makes at synthetic method.
The present invention solves the problems of the technologies described above the technical scheme of being taked: a kind of synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire comprises the steps: in regular turn
(1) with the molybdate molybdate solution that obtains soluble in water, the volumetric molar concentration of molybdenum atom is 0.05～1.0mol/L;
(2) aniline monomer is injected above-mentioned molybdate solution, the mol ratio of molybdenum atom is 4.0～1.0:1 in aniline monomer and the molybdate solution;
(3) dropping inorganic acid in the solution is regulated pH to 2～5, to the white precipitate appearance, makes reaction solution;
(4) reaction solution moves in 30～60 ℃ the oil bath, reacted 2～12 hours, product;
(5) product washing suction filtration, oven dry, concrete, washing can be adopted absolute ethanol washing number time, and bake out temperature obtains molybdena-polyaniline polyaniline composite single crystal nanowire about 50 ℃.
Utilize obtain molybdena-polyaniline polyaniline composite single crystal nanowire one step of synthetic method of the present invention, to strengthen the physico-chemical property of molybdena-polyaniline polyaniline matrix material and in the application in fields such as electrochemistry, sensing, embedded photoluminescent material, synthetic method makes things convenient for, easily controls simultaneously, meets requirement of large-scale production.
In the above-mentioned steps (1), in the molybdate solution, the volumetric molar concentration of molybdenum atom is specifically as follows 0.05,0.1, and 0.15,0.2,0.25,0.3,0.35,0.4,0.45,0.5,0.55,0.6,0.65,0.7,0.75,0.8,0.85,0.9,0.95 or 1.0mol/L.
The mol ratio of molybdenum atom is specifically as follows 4.0,3.5 in aniline monomer and the molybdate solution, and 3.0,2.5,2.0,1.5 or 1.0:1.
Dropping inorganic acid, regulating pH specifically can be down to 2,2.5, and 3,3.5,4,4.5 or 5.
Oil bath temperature is specifically as follows 30,35,40,45,50,55 or 60 ℃; Reaction times is specifically as follows 2,3,5,6,8,10 or 12 hours.
On the basis of such scheme, the molybdate in the step (1) is ammonium molybdate, Sodium orthomolybdate or potassium molybdate.
On the basis of such scheme, the aniline monomer in the step (2) is aniline, p-diaminodiphenyl or monomethylaniline.
On the basis of such scheme, the mineral acid in the step (3) is hydrochloric acid, nitric acid or sulfuric acid.
Preferred synthetic method is provided:
On the basis of such scheme, the preferred concentration range for of molybdate solution is provided, molybdate solution in the step (1), the volumetric molar concentration of molybdenum atom is preferably 0.25～0.5mol/L.
On the basis of such scheme, provide aniline monomer and molybdate solution preferred mol ratio, the mol ratio of molybdenum atom is preferably 3.5～2.5:1 in middle aniline monomer of step (2) and the molybdate solution.
On the basis of such scheme, the preferred hydrochloric acid of mineral acid in the step (3), volumetric molar concentration is 1.0～2.5mol/L, the volumetric molar concentration of hydrochloric acid is specifically as follows 1.0,1.2, and 1.5,1.8,2.0,2.2 or 2.5mol/L.
On the basis of such scheme, dropping inorganic acid is regulated the pH value preferably to 3～5, especially is best with pH=4.5, and promptly the pH value of reaction solution is preferably 4.5.
Preferred ammonium molybdate (NH in the described molybdate
4)
6Mo
7O
244H
2O, purity 99.99%.
Preferred aniline in the described organic amine, analytical pure;
Temperature of reaction is preferably 50 ℃, and the reaction times is preferably 6～12 hours.
The molybdena-polyaniline polyaniline composite nano-line of the inventive method preparation, its composition mainly comprises inorganic part (MoO
x), and organic moiety: as polyaniline, polyphenylmethyl amine; Wherein, be the molybdena-polyaniline polyaniline composite nano-line that monomer makes by aniline, be a kind of new crystalline phase, belong to oblique system.
The invention has the beneficial effects as follows:
The composite nano-line of the inventive method preparation has the compound inferior nano periodic structure of regular organic and inorganic, regulatable physico-chemical property, big specific surface area and thickness, the regulatable characteristic of length, therefore this compound molybdena-polyaniline polyaniline nano wire can be in a lot of fields, in for example nano-device design, electrode materials, microcosmic conduction and advanced optics, electricity and magnetics material synthetic using value arranged;
The productive rate of synthetic method of the present invention is very high, reaches more than 95%, and preparation condition is simple and easy to control, and the processing condition cost is low, the preparation efficiency height, and quality product and yield rate height have good application and industrialization prospect.
Description of drawings
Fig. 1 is scanning electron microscope (SEM) figure of molybdena-polyaniline polyaniline composite nano-line product A of the present invention.
Fig. 2 is transmission electron microscope (TEM) figure of product A of the present invention.
Fig. 3 is X-ray powder diffraction (XRD) figure of product A of the present invention.
Fig. 4 is Raman spectrum (Raman) figure of product A of the present invention.
Fig. 5 is infrared spectra (IR) figure of product A of the present invention.
Fig. 6 is x-ray photoelectron power spectrum (XPS) figure of product A of the present invention.
Fig. 7 is scanning electron microscope (SEM) figure of product B of the present invention.
Fig. 8 is scanning electron microscope (SEM) figure of products C of the present invention.
Fig. 9 is transmission electron microscope (TEM) figure of products C of the present invention.
Figure 10 is X-ray powder diffraction (XRD) figure of products C of the present invention.
Figure 11 is scanning electron microscope (SEM) figure of product D of the present invention.
Figure 12 is scanning electron microscope (SEM) figure of product E of the present invention
Embodiment
A kind of synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire comprises the steps:
(1) with 1.24g ammonium molybdate (NH
4)
6Mo
7O
244H
2O is dissolved in and obtains ammonium molybdate solution (the about 0.35mol/L of molybdenum atom volumetric molar concentration) in the 20mL distilled water;
(2) 1.95g aniline is injected above-mentioned ammonium molybdate solution (aniline and the about 2.86:1 of molybdenum atom mol ratio);
(3) dropwise add the hydrochloric acid of 1.0mol/L in the solution, regulate pH to 4.5, occur to white precipitate, make reaction solution;
(4) reaction solution is transferred in 50 ℃ the oil bath, reacted 6 hours, product;
(5) product is through absolute ethanol washing several and suction filtration, and 50 ℃ of oven dry obtain molybdena-polyaniline polyaniline composite nano-line product A.
The scanning electron microscope of product A (SEM) figure absorbs on Philips XL30 D6716 instrument, and as shown in Figure 1, product A has one dimension wire pattern.
The transmission electron microscope of product A (TEM) figure absorbs on JEOL JEM-2010 instrument, as shown in Figure 2, observes the inferior nano periodic structure of existence～1.39nm in the nano wire.
The X-ray powder diffraction of product A (XRD) figure carries out on Rigaku D/Max-IIA type X-ray diffractometer, product A to gained characterizes, as shown in Figure 3, the XRD stave of product A reveals the characteristic peak of monocline (P21/c (14)), be confirmed to be a kind of structure (P21/c (14) of novelty by analysis
,
,
, β=114.6 °).
Shown in Fig. 4 Raman spectrum, there is the vibration absorption peak of polyaniline and molybdenum oxygen octahedra in the product A, and shown in Fig. 5 infrared spectrogram, corresponding absorption peak arranged, explanation is a molybdena-polyaniline polyaniline compound structure.Shown in the x-ray photoelectron power spectrum of Fig. 6, showing has Mo in the product A
5+There is amine molybdate catalysis with strong oxidation capacity the has been described polymerization of aniline.
Embodiment 2
A kind of synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire comprises the steps:
(1) with ammonium molybdate (NH
4)
6Mo
7O
244H
2O is dissolved in and obtains ammonium molybdate solution (the molybdenum atom volumetric molar concentration is 0.05mol/L) in the 20mL distilled water;
(2) (aniline and molybdenum atom mol ratio are 3.5～2.5:1) aniline to be injected above-mentioned ammonium molybdate solution;
(3) dropwise add the hydrochloric acid of 1.0mol/L in the solution, regulate pH to 3～5, occur to white precipitate, make reaction solution;
(4) reaction solution is transferred in 50 ℃ the oil bath, reacted 6 hours, product;
(5) product is through absolute ethanol washing several and suction filtration, and 50 ℃ of oven dry obtain molybdena-polyaniline polyaniline composite nano-line product A '.
Embodiment 3
A kind of synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire comprises the steps:
(1) with ammonium molybdate (NH
4)
6Mo
7O
244H
2O is dissolved in and obtains ammonium molybdate solution (the molybdenum atom volumetric molar concentration is 1.0mol/L) in the 20mL distilled water;
(2) (aniline and molybdenum atom mol ratio are 3.5～2.5:1) aniline to be injected above-mentioned ammonium molybdate solution;
(3) dropwise add the hydrochloric acid of 1.0mol/L in the solution, regulate pH to 3～5, occur to white precipitate, make reaction solution;
(4) reaction solution is transferred in 50 ℃ the oil bath, reacted 6 hours, product;
(5) product is through absolute ethanol washing several and suction filtration, and 50 ℃ of oven dry obtain molybdena-polyaniline polyaniline composite nano-line product A ".
A kind of synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire comprises the steps:
(1) with 1.24g ammonium molybdate (NH
4)
6Mo
7O
244H
2O is dissolved in and obtains ammonium molybdate solution (the about 0.35mol/L of molybdenum atom volumetric molar concentration) in the 20mL distilled water;
(2) aniline is injected above-mentioned ammonium molybdate solution (aniline and molybdenum atom mol ratio are 4:1);
(3) dropwise add the hydrochloric acid of 1.0mol/L in the solution, regulate pH to 3～5, occur to white precipitate, make reaction solution;
(4) reaction solution is transferred in 50 ℃ the oil bath, reacted 6 hours, product;
(5) product is through absolute ethanol washing several and suction filtration, and 50 ℃ of oven dry obtain molybdena-polyaniline polyaniline composite nano-line product A ' ".
A kind of synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire comprises the steps:
(1) with 1.24g ammonium molybdate (NH
4)
6Mo
7O
244H
2O is dissolved in and obtains ammonium molybdate solution (the about 0.35mol/L of molybdenum atom volumetric molar concentration) in the 20mL distilled water;
(2) aniline is injected above-mentioned ammonium molybdate solution (aniline monomer and molybdenum atom mol ratio are 1:1);
(3) dropwise add the hydrochloric acid of 1.0mol/L in the solution, regulate pH to 3～5, occur to white precipitate, make reaction solution;
(4) reaction solution is transferred in 50 ℃ the oil bath, reacted 6 hours, product;
(5) product is through absolute ethanol washing several and suction filtration, and 50 ℃ of oven dry obtain molybdena-polyaniline polyaniline composite nano-line product A " ".
A kind of synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire comprises the steps:
(1) with 1.24g ammonium molybdate (NH
4)
6Mo
7O
244H
2O is dissolved in and obtains ammonium molybdate solution (the about 0.35mol/L of molybdenum atom volumetric molar concentration) in the 20mL distilled water;
(2) 1.95g aniline is injected above-mentioned ammonium molybdate solution (aniline and the about 2.86:1 of molybdenum atom mol ratio);
(3) dropwise add the hydrochloric acid of 1.0mol/L in the solution, regulate pH to 2～3, occur to white precipitate, make reaction solution;
(4) reaction solution is transferred in 50 ℃ the oil bath, reacted 6 hours, product;
(5) product is through absolute ethanol washing several and suction filtration, and 50 ℃ of oven dry obtain molybdena-polyaniline polyaniline composite nano-line product B.
Shown in Fig. 7 scanning electron microscope (SEM) figure, instrument proves and utilizes Sodium orthomolybdate with embodiment 1, also getable nano wire product, but show that acid strong excessively (pH＜3) can not get pure nanowire product, and can produce block impurity.
Embodiment 7
A kind of synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire comprises the steps:
(1) with Sodium orthomolybdate Na
2MoO
42H
2O is dissolved in and obtains sodium molybdate solution (the about 0.35mol/L of molybdenum atom volumetric molar concentration) in the 20mL distilled water;
(2) aniline is injected above-mentioned sodium molybdate solution (aniline and the about 2.86:1 of molybdenum atom mol ratio);
(3) dropwise add the hydrochloric acid of 1.0mol/L in the solution, regulate pH to 3～5, occur to white precipitate, make reaction solution;
(4) reaction solution is transferred in 50 ℃ the oil bath, reacted 6 hours, product;
(5) product is through absolute ethanol washing several and suction filtration, and 50 ℃ of oven dry obtain molybdena-polyaniline polyaniline composite nano-line products C.
As Fig. 8～shown in Figure 10, laboratory apparatus is all with embodiment 1, and products C has one dimension wire pattern, and the principal character peak basically identical of the XRD figure (Fig. 3) of diffraction pattern and A can think that product A and products C are same substances in the XRD figure of products C (Figure 10).
Embodiment 8
A kind of synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire comprises the steps:
(1) with 1.24g ammonium molybdate (NH
4)
6Mo
7O
244H
2O is dissolved in and obtains ammonium molybdate solution (the about 0.35mol/L of molybdenum atom volumetric molar concentration) in the 20mL distilled water;
(2) (p-diaminodiphenyl and molybdenum atom mol ratio are 3.5～2.5:1) p-diaminodiphenyl to be injected above-mentioned ammonium molybdate solution;
(3) dropwise add the hydrochloric acid of 1.0mol/L in the solution, regulate pH to 3～5, occur to white precipitate, make reaction solution;
(4) reaction solution is transferred in 50 ℃ the oil bath, reacted 6 hours, product;
(5) product is through absolute ethanol washing several and suction filtration, and 50 ℃ of oven dry obtain molybdena-polyaniline polyaniline composite Nano line products D.
As shown in figure 11, instrument is with embodiment 1, and the character of product D is similar to the product A of embodiment 1.
Embodiment 9
A kind of synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire comprises the steps:
(1) with 1.24g ammonium molybdate (NH
4)
6Mo
7O
244H
2O is dissolved in and obtains ammonium molybdate solution (the about 0.35mol/L of molybdenum atom volumetric molar concentration) in the 20mL distilled water;
(2) o-toluidine is injected above-mentioned ammonium molybdate solution (o-toluidine and molybdenum atom mol ratio about 3.5～2.5:1);
(3) dropwise add the hydrochloric acid of 1.0mol/L in the solution, regulate pH to 3～5, occur to white precipitate, make reaction solution;
(4) reaction solution is transferred in 50 ℃ the oil bath, reacted 6 hours, product;
(5) product is through absolute ethanol washing several and suction filtration, and 50 ℃ of oven dry obtain molybdena-polyaniline polyaniline composite nano-line product E.
As shown in figure 12, instrument is with embodiment 1, and the character of product E is similar to the product A of embodiment 1.
Reference examples
A kind of synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire comprises the steps:
(1) with 1.24g ammonium molybdate (NH
4)
6Mo
7O
244H
2O is dissolved in and obtains molybdate solution (the about 0.35mol/L of molybdenum atom volumetric molar concentration) in the 20mL distilled water;
(2) aniline is injected molybdate solution (aniline and the about 2.86:1 of molybdenum atom mol ratio);
(3) dropwise add the hydrochloric acid of 1.0mol/L in the solution, regulate pH to 6, can not get white precipitate.
Because class molybdena-polyaniline polyaniline composite single crystal nanowire of the present invention has novel structure and the adjustable optical property that becomes, very big specific surface area and length, the regulatable character of thickness, in therefore this molybdena-polyaniline polyaniline composite nano-line for example nano-device design and assembling in a lot of fields, electrode materials, sensing, microcosmic conduction and advanced optics, electricity and magnetics material synthetic using value is arranged.In addition, because the product composite nano-line has one-dimentional structure and is good crystal, it can also have some other application, for example can be used as presoma and prepares for example MoO of other one-dimentional structures
2/ C composite Nano rod etc.; Lead that can utilize the one-dimentional structure of the regulatable physico-chemical property of crystal and itself to make to play conduction between the nano-device and connecting device etc.Because this product has above potential using value, and preparation condition is simple and easy to control, the processing condition cost is low, the preparation efficiency height, and quality product and yield rate height, so this product has good application and industrialization prospect.
Claims (9)
1, a kind of synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire comprises the steps: in regular turn
(1) with the molybdate molybdate solution that obtains soluble in water, the volumetric molar concentration of molybdenum atom is 0.05～1.0mol/L;
(2) aniline monomer is injected above-mentioned molybdate solution, the mol ratio of molybdenum atom is 4.0～1.0:1 in aniline monomer and the molybdate solution;
(3) dropping inorganic acid in the solution is regulated pH to 2～5, to the white precipitate appearance, makes reaction solution;
(4) reaction solution moves in 30～60 ℃ the oil bath, reacted 2～12 hours, product;
(5) product washing suction filtration, oven dry obtains molybdena-polyaniline polyaniline composite single crystal nanowire.
2, the synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire according to claim 1 is characterized in that: the molybdate in the described step (1) is ammonium molybdate, Sodium orthomolybdate or potassium molybdate.
3, the synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire according to claim 1 and 2 is characterized in that: the molybdate solution in the described step (1), the volumetric molar concentration of molybdenum atom are 0.25～0.5mol/L.
4, the synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire according to claim 1 is characterized in that: the aniline monomer in the described step (2) is aniline, p-diaminodiphenyl or monomethylaniline.
5, according to the synthetic method of claim 1 or 4 described molybdena-polyaniline polyaniline composite single crystal nanowires, it is characterized in that: the mol ratio of molybdenum atom is 3.5～2.5:1 in aniline monomer in the described step (2) and the molybdate solution.
6, the synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire according to claim 1 is characterized in that: the mineral acid in the described step (3) is hydrochloric acid, nitric acid or sulfuric acid.
7, according to the synthetic method of claim 1 or 6 described molybdena-polyaniline polyaniline composite single crystal nanowires, it is characterized in that: the mineral acid in the described step (3) is a hydrochloric acid, and volumetric molar concentration is 1.0～2.5mol/L.
8, the synthetic method of molybdena-polyaniline polyaniline composite single crystal nanowire according to claim 1 is characterized in that: in the step (3), regulate pH value to 3～5.
9, the molybdena-polyaniline polyaniline composite single crystal nanowire that makes at the described synthetic method of one of claim 1 to 8.
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