CN102815749A - Preparation method of molybdenum dioxide nanorod - Google Patents
Preparation method of molybdenum dioxide nanorod Download PDFInfo
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Abstract
The invention discloses a preparation method of a molybdenum dioxide nanorod. The preparation method comprises the following steps of: by taking sodium molybdate as a molybdenum source, acetic oxide as an additive, dimethylformamide as a solvent, concentrated hydrochloric acid as an acidifier, and tetrabutylammonium bromide as a settling agent, through a simple experiment device and reaction steps, controlling concentration of molybdate suspension, an additive amount of the additive, a pH value of the solution and the amount of the settling agent, recrystalizing and purifying to obtain precursor tetrabutyl ammonium hexamolybdate; and thermally treating the precursor tetrabutyl ammonium hexamolybdate in a quartz tube under an inert atmosphere to have decomposition to obtain a monoclinic phase molybdenum dioxide nanorod. The method, prepared by the invention, has the advantages of low cost and high reaction yield, and capability of overcoming the vices of expensive instrument device, rigorous reaction conditions and reduction at high temperature with H2 with safety hidden trouble of the conventional preparation method.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of preparation method of molybdenum dioxide nanometer rod.
Background technology
The transition metal oxide molybdenum dioxide belongs to oblique system, has distored rutile crystal structure.Because its particular structural; Molybdenum dioxide has high conductivity, HMP, high chemical stability, its efficiently charge transmission make it extensive in aspect application prospects such as catalyzer, transmitter, electrochromic display device, recording materials, electric chemical super capacitor, ionization cell and field emmision materials.
The molybdenum dioxide preparation of nanomaterials is existing at present reports.People such as Wang Zhonglin (Advanced Materials, 2003,15:1835) metal molybdenum is heated to 1100 ℃ in vacuum oven, feed shielding gas Ar then, on monocrystal silicon substrate, obtain the molybdenum dioxide nano-wire array; People such as Liu Huarong (Solid State Sciences; 2006; 8:526) with the molybdic oxide be raw material; Prepared molybdenum dioxide through gammairradiation and hydrogen shield pyroprocessing bonded method, these two kinds of preparing methods need expensive plant and instrument and harsh preparation condition, have limited the application of molybdenum dioxide.People such as Shi Yifeng (Nano Letters, 2009,9:4215) with the phospho-molybdic acid be presoma, mesoporous silicon oxide KIT-6 is a hard template, the H 10%
2The mesoporous nano molybdenum dioxide that has prepared high-sequential under the atmosphere through gaseous techniques; This molybdenum dioxide has the reversible charging and discharging capacity up to 750mAh/g; It is the lithium-ion secondary cell anode material of potentialization; This preparation method possibly cause material damage when existing the molybdenum dioxide material to separate with template, and is difficult to realize shortcoming such as batch process.People such as Hu Bin (ACS Nano, 2009,3:478) with MoO
3Nano belt is a raw material, uses H under the high temperature
2Reduce and successfully prepared the molybdenum dioxide nanometer rod, product pattern heterogeneity, particularly H that this method obtains
2Security at high temperature makes this method have various hidden danger.
There is apparatus expensive mostly in above compound method, and synthesis temperature is high, and energy consumption is big, and synthesis condition is harsh, need employ the H that has potential safety hazard
2Problem.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of molybdenum dioxide nanometer rod has solved existing method and has prepared the molybdenum dioxide nanometer rod, apparatus expensive, and synthesis temperature is high, and energy consumption is big, and synthesis condition is harsh, and there is the problem of potential safety hazard in product pattern heterogeneity.
The technical scheme that the present invention adopted is, a kind of preparation method of molybdenum dioxide nanometer rod specifically implements according to following steps:
Step 1: with Sodium orthomolybdate grind into powder at ambient temperature, be dissolved in the N, it is 0.1-0.4molL that magnetic agitation obtains concentration
-1Suspension liquid, continuing in suspension liquid, to add acetic anhydride under the condition of stirring, stir 10min;
Step 2: continuing in the suspension liquid that step 1 obtains, slowly to add concentrated hydrochloric acid under the condition of stirring, after concentrated hydrochloric acid adds; Suspension liquid becomes yellow solution, and the adularescent deposition produces continuation stirring 15min; After stirring end; The yellow solution that contains white precipitate that obtains is filtered, and the filtering white precipitate obtains yellow transparent filtrating;
Step 3: under the situation of magnetic agitation, be 0.3-0.5molL with concentration
-1The dimethyl formamide solution of Tetrabutyl amonium bromide join in the yellow transparent filtrating that step 2 obtains, up to there being yellow mercury oxide to produce, continue vigorous stirring 30min, it is fully precipitated;
Step 4: after stirring end; The solution that contains yellow mercury oxide that step 3 is obtained filters; Obtaining the yellow mercury oxide product, earlier with ethanol lotion 3-5 time, use ether lotion 3-5 time again, is that solvent carries out the recrystallization purification with acetone with yellow solid product with the yellow solid product that obtains at last; After accomplishing, recrystallization, obtains presoma six molybdic acid TBuAs with yellow crystals product collection, dried in vacuum;
Step 5: the presoma six molybdic acid TBuAs that step 4 recrystallization is obtained are placed in the silica tube in the tube furnace heat-treats, and obtains monocline phase molybdenum dioxide nanometer rod.
Characteristics of the present invention also are,
The volume ratio of acetic anhydride and suspension liquid is 1:10-1:30 in the step 1 wherein.
The add-on of concentrated hydrochloric acid in the step 2 wherein makes the pH value of solution transfer to 0.5-1.5.
The volume ratio of the dimethyl formamide solution of the Tetrabutyl amonium bromide that adds in the step 3 wherein and yellow transparent filtrating is 1:1-1:2.
Thermal treatment in the step 5 wherein is at N
2Carry out in the atmosphere, temperature 600-700 ℃, insulation 2-3h, naturally cools to room temperature then by temperature rise rate 25-35 ℃/min.
The invention has the beneficial effects as follows, at first be the molybdenum source with the Sodium orthomolybdate, and acetic anhydride is an additive; N is a solvent, and concentrated hydrochloric acid is a souring agent, and Tetrabutyl amonium bromide is a precipitation agent; Through simple experimental apparatus and reactions step; Through control molybdate suspension liquid concentration, additive add-on, the potential of hydrogen of solution and the consumption of precipitation agent, and carry out recrystallization and purify, obtain presoma six molybdic acid TBuAs.Secondly the presoma six molybdic acid TBuAs that obtain are heat-treated under inert atmosphere in silica tube, it is decomposed, obtain monocline phase molybdenum dioxide nanometer rod.This method raw materials cost is low, and reaction yield is high.Process method of the present invention has overcome the H that potential safety hazard is arranged under existing preparing method's plant and instrument costliness, severe reaction conditions and the employing high temperature
2Carry out the reductive drawback, change gas phase reduction process into the precursor thermal decomposition method, promptly utilize solution deposit synthesis of nano particle size to control easily, equipment is simple, the synthetic precursor six molybdic acid TBuAs of the advantage that cost is low; Utilize the thermal decomposition method charging capacity big, sufficient reacting, the synthetic molybdenum dioxide nanometer rod of the advantage that productive rate is high.Through the presoma thermal decomposition method, can realize fully that maroscopic quantity prepares the molybdenum dioxide nanometer rod, reduced preparation cost, significant for the industrialization preparation of molybdenum dioxide nanometer rod with application.
Description of drawings
Fig. 1 is the molybdenum dioxide nanometer rod TEM figure of the embodiment of the invention 1 preparation;
Fig. 2 is the molybdenum dioxide nanometer rod XRD figure of the embodiment of the invention 1 preparation;
Fig. 3 is the ED figure of the molybdenum dioxide nanometer rod of the embodiment of the invention 1 preparation.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
The present invention prepares the method for molybdenum dioxide nanometer rod, and the preparation process was divided into for two steps.At first utilizing the precipitator method to prepare precursor six molybdic acid TBuAs, promptly is the molybdenum source with the Sodium orthomolybdate, and acetic anhydride is an additive; N is a solvent, and concentrated hydrochloric acid is a souring agent, and Tetrabutyl amonium bromide is a precipitation agent; The acetone crystalline solvent of attaching most importance to utilizes simple experimental apparatus and reactions step, through the consumption of control molybdate suspension liquid concentration, additive add-on, concentrated hydrochloric acid and precipitation agent; And carry out recrystallization and purify, obtain presoma six molybdic acid TBuAs.Secondly with the presoma six molybdic acid TBuAs that obtain in silica tube at rare gas element N
2Heat-treat under the protection, it is decomposed, obtain the molybdenum dioxide nanometer rod.
Concrete operations technology is, Sodium orthomolybdate grinds to form the thinner powder of granularity at ambient temperature, pours into to fill in the N beaker, and it is 0.1-0.4molL that magnetic agitation obtains concentration
-1Suspension liquid, in suspension liquid, add the 1-3ml acetic anhydride then, continue to stir 10min; Continuing under the condition of stirring, in above-mentioned suspension liquid, adding concentrated hydrochloric acid it is carried out acidifying, after concentrated hydrochloric acid adds; Suspension liquid becomes the yellow transparent solution that contains white precipitate; The add-on of concentrated hydrochloric acid finally makes the pH value of solution after the acidifying be 0.5-1.5, continues to stir 15min; After stirring end, the yellow souring soln that contains white precipitate that obtains is filtered, the elimination white depositions obtains yellow transparent filtrating; Under the situation of magnetic agitation, be 0.3-0.5molL with concentration
-1The dimethyl formamide solution of Tetrabutyl amonium bromide joins in the yellow filtrate of acquisition, has yellow mercury oxide to generate in the filtrating, continues vigorous stirring 30min, and it is fully precipitated; The solution of abundant post precipitation is filtered; Obtain the yellow mercury oxide product; Earlier with ethanol lotion 3-5 time, use ether lotion 3-5 time again, with acetone is solvent carry out recrystallization with this yellow solid product at last with the yellow solid product that obtains, after the recrystallization completion with the yellow crystals product collection; Dry under vacuum condition, i.e. the presoma six molybdic acid TBuAs of acquisition preparation molybdenum dioxide nanometer rod; The six molybdic acid TBuAs that recrystallization is obtained are placed in the silica tube in the tube furnace, give silica tube with the logical rare gas element N of the speed of 400ml/min
2, behind the 30min, to 600-700 ℃, insulation 2-3h is then at N with the temperature rise rate heated quarty tube of 25-35 ℃/min
2Naturally cool to room temperature in the atmosphere, can obtain monocline phase molybdenum dioxide nanometer rod powder.The key that obtains pure molybdenum dioxide nanometer rod is to obtain pure precursor six molybdic acid TBuAs.If during with the N suspension liquid of concentrated hydrochloric acid acidifying sodium wolframate; The pH value of yellow solution that finally contains white precipitate is at 0.5-1.5, will can not obtain pure six molybdic acid TBuAs deposition after in filtering the yellow filtrate that the back obtains, adding the dimethyl formamide solution of precipitation agent Tetrabutyl amonium bromide.In addition, the purity and the recrystallizing technology of the precursor six molybdic acid TBuAs of acquisition are closely related, and bad if recrystallization process is handled, the precursor of acquisition finally can not obtain pure molybdenum dioxide nanometer rod not by effective purification.
Embodiment 1
Sodium wolframate is dissolved in the N after grinding, and it is 0.1molL that magnetic agitation obtains concentration
-1The Sodium orthomolybdate suspension liquid; Continuing under the condition of stirring, in the Sodium orthomolybdate suspension liquid, adding the 1ml acetic anhydride, after continuing to stir 10min; In above-mentioned suspension liquid, slowly add concentrated hydrochloric acid it is carried out acidifying, after concentrated hydrochloric acid added, suspension liquid became the yellow solution that contains white precipitate, and the add-on of concentrated hydrochloric acid makes finally that the pH value of solution is 1.5 after the acidifying, continues stirring 15min; After stirring end, the yellow solution that contains white precipitate after the acidifying is filtered, the elimination white precipitate obtains yellow transparent filtrating; Under the situation of magnetic agitation, be 0.3molL with concentration
-1The dimethyl formamide solution of Tetrabutyl amonium bromide join in the yellow transparent filtrating of acquisition, have yellow mercury oxide to produce, continue vigorous stirring 30min, it is fully precipitated; The solution of abundant post precipitation is filtered; Obtain the yellow mercury oxide product, the yellow solid product that obtains earlier with ethanol lotion 3 times, is used the ether lotion 5 times again; Be that solvent carries out recrystallization with acetone with this yellow solid product at last; After recrystallization is accomplished the yellow crystals that obtains is collected, dry under vacuum condition, promptly obtain precursor six molybdic acid TBuAs; The presoma six molybdic acid TBuAs that recrystallization is obtained are placed in the silica tube in the tube furnace, give silica tube with the logical rare gas element N of the speed of 400ml/min
2, behind the 30min, with the temperature rise rate heated quarty tube to 600 of 25 ℃/min ℃, insulation 3h is then at N
2Naturally cool to room temperature in the atmosphere, can obtain monocline phase molybdenum dioxide nanometer rod powder.
Fig. 2 is the molybdenum dioxide nanometer rod XRD figure of preparation; The position of each diffraction peak of XRD figure of synthetic product and relative intensity all with JCPDS card NO.78-1070 (a=0.5620nm; B=0.4860nm, c=0.5630nm) in full accord, show that product is the molybdenum dioxide of monocline phase.Fig. 1 is the molybdenum dioxide nanometer rod TEM figure of preparation, and the molybdenum dioxide that as can be seen from the figure obtains is a club shaped structure, nanometer rod shape rule, smooth surface, length 0.6-1.2um, diameter 40-80nm.Fig. 3 is the ED figure of the molybdenum dioxide nanometer rod of preparation, and ED figure is diffraction spot clearly, shows that the synthetic product is a single crystal structure.Compare with other preparing methods, the inventive method equipment is simple, and productive rate is high, and cost is low, no potential safety hazard.
Embodiment 2
Sodium wolframate is dissolved in the N after grinding, and it is 0.4molL that magnetic agitation obtains concentration
-1The Sodium orthomolybdate suspension liquid; Continuing under the condition of stirring, in the Sodium orthomolybdate suspension liquid, adding the 3ml acetic anhydride, after continuing to stir 10min; In above-mentioned suspension liquid, slowly add concentrated hydrochloric acid it is carried out acidifying, after concentrated hydrochloric acid added, suspension liquid became the yellow solution that contains white precipitate, and the add-on of concentrated hydrochloric acid makes finally that the pH value of solution is 0.5 after the acidifying, continues stirring 15min; After stirring end, the yellow solution that contains white precipitate after the acidifying is filtered, the elimination white precipitate obtains yellow transparent filtrating; Under the situation of magnetic agitation, be 0.5molL with concentration
-1The dimethyl formamide solution of Tetrabutyl amonium bromide join in the yellow transparent filtrating of acquisition, have yellow mercury oxide to produce, continue vigorous stirring 30min, it is fully precipitated; The solution of abundant post precipitation is filtered; Obtain the yellow mercury oxide product, the yellow solid product that obtains earlier with ethanol lotion 5 times, is used the ether lotion 3 times again; Be that solvent carries out recrystallization with acetone with this yellow solid product at last; Collect the yellow crystals that recrystallization obtains, dry under vacuum condition, promptly obtain precursor six molybdic acid TBuAs; The presoma six molybdic acid TBuAs that recrystallization is obtained are placed in the silica tube in the tube furnace, give silica tube with the logical rare gas element N of the speed of 400ml/min
2, behind the 30min, with the temperature rise rate heated quarty tube to 700 of 35 ℃/min ℃, insulation 2h is then at N
2Naturally cool to room temperature in the atmosphere, can obtain monocline phase molybdenum dioxide nanometer rod powder.
Embodiment 3
Sodium wolframate is dissolved in the N after grinding, and it is 0.3molL that magnetic agitation obtains concentration
-1The Sodium orthomolybdate suspension liquid; Continuing under the condition of stirring, in the Sodium orthomolybdate suspension liquid, adding the 2ml acetic anhydride, after continuing to stir 10min; In above-mentioned suspension liquid, slowly add concentrated hydrochloric acid it is carried out acidifying, after concentrated hydrochloric acid added, suspension liquid became the yellow solution that contains white precipitate, and the add-on of concentrated hydrochloric acid makes finally that the pH value of solution is 1.0 after the acidifying, continues stirring 15min; After stirring end, the yellow solution that contains white precipitate after the acidifying is filtered, the elimination white depositions obtains yellow transparent filtrating; Under the situation of magnetic agitation, be 0.4molL with concentration
-1The dimethyl formamide solution of Tetrabutyl amonium bromide join in the yellow transparent filtrating of acquisition, have yellow mercury oxide to produce, continue vigorous stirring 30min, it is fully precipitated; The solution of abundant post precipitation is filtered; Obtain the yellow mercury oxide product, the yellow solid product that obtains earlier with ethanol lotion 4 times, is used the ether lotion 4 times again; Be that solvent carries out recrystallization with acetone with this yellow solid product at last; Collect the yellow crystals product that obtains behind the recrystallization, dry under vacuum condition, promptly obtain preparation precursor six molybdic acid TBuAs; The presoma six molybdic acid TBuAs that recrystallization is obtained are placed in the silica tube in the tube furnace, give silica tube with the logical rare gas element N of the speed of 400ml/min
2, behind the 30min, with the temperature rise rate heated quarty tube to 650 of 30 ℃/min ℃, insulation 2.5h is then at N
2Naturally cool to room temperature in the atmosphere, can obtain monocline phase molybdenum dioxide nanometer rod powder.
Embodiment 4
Sodium wolframate is dissolved in the N after grinding, and it is 0.2molL that magnetic agitation obtains concentration
-1The Sodium orthomolybdate suspension liquid; Continuing under the condition of stirring, in the Sodium orthomolybdate suspension liquid, adding the 2.5ml acetic anhydride, after continuing to stir 10min; In above-mentioned suspension liquid, slowly add concentrated hydrochloric acid it is carried out acidifying, after concentrated hydrochloric acid added, suspension liquid became the yellow solution that contains white precipitate, and the add-on of concentrated hydrochloric acid makes finally that the pH value of solution is 1.2 after the acidifying, continues stirring 15min; After stirring end, the yellow solution that contains white precipitate after the acidifying is filtered, the elimination white precipitate obtains yellow transparent filtrating; Under the situation of magnetic agitation, be 0.35molL with concentration
-1The dimethyl formamide solution of Tetrabutyl amonium bromide join in the yellow transparent filtrating of acquisition, have yellow mercury oxide to produce, continue vigorous stirring 30min, it is fully precipitated; The solution of abundant post precipitation is filtered; Obtain the yellow mercury oxide product, the yellow solid product that obtains earlier with ethanol lotion 5 times, is used the ether lotion 4 times again; Be that solvent carries out recrystallization with acetone with this yellow solid product at last; After recrystallization is accomplished the yellow crystals that obtains is collected, dry under vacuum condition, promptly obtain precursor six molybdic acid TBuAs; The presoma six molybdic acid TBuAs that recrystallization is obtained are placed in the silica tube in the tube furnace, give silica tube with the logical rare gas element N of the speed of 400ml/min
2, behind the 30min, with the temperature rise rate heated quarty tube to 680 of 28 ° of C/min ℃, insulation 2.2h is then at N
2Naturally cool to room temperature in the atmosphere, can obtain monocline phase molybdenum dioxide nanometer rod powder.
Claims (5)
1. the preparation method of a molybdenum dioxide nanometer rod is characterized in that, specifically implements according to following steps:
Step 1: with Sodium orthomolybdate grind into powder at ambient temperature, be dissolved in the N, it is 0.1-0.4molL that magnetic agitation obtains concentration
-1Suspension liquid, continuing in suspension liquid, to add acetic anhydride under the condition of stirring, stir 10min;
Step 2: continuing in the suspension liquid that step 1 obtains, slowly to add concentrated hydrochloric acid under the condition of stirring, after concentrated hydrochloric acid adds; Suspension liquid becomes yellow solution, and the adularescent deposition produces continuation stirring 15min; After stirring end; The yellow solution that contains white precipitate that obtains is filtered, and the filtering white precipitate obtains yellow transparent filtrating;
Step 3: under the situation of magnetic agitation, be 0.3-0.5molL with concentration
-1The dimethyl formamide solution of Tetrabutyl amonium bromide join in the yellow transparent filtrating that step 2 obtains, up to there being yellow mercury oxide to produce, continue vigorous stirring 30min, it is fully precipitated;
Step 4: after stirring end; The solution that contains yellow mercury oxide that step 3 is obtained filters; Obtaining the yellow mercury oxide product, earlier with ethanol lotion 3-5 time, use ether lotion 3-5 time again, is that solvent carries out the recrystallization purification with acetone with yellow solid product with the yellow solid product that obtains at last; After accomplishing, recrystallization, obtains presoma six molybdic acid TBuAs with yellow crystals product collection, dried in vacuum;
Step 5: the presoma six molybdic acid TBuAs that step 4 recrystallization is obtained are placed in the silica tube in the tube furnace heat-treats, and obtains monocline phase molybdenum dioxide nanometer rod.
2. the preparation method of molybdenum dioxide nanometer rod according to claim 1 is characterized in that, the volume ratio of acetic anhydride and suspension liquid is 1:10-1:30 in the described step 1.
3. the preparation method of molybdenum dioxide nanometer rod according to claim 1 is characterized in that, the add-on of concentrated hydrochloric acid in the described step 2 makes the pH value of solution transfer to 0.5-1.5.
4. the preparation method of molybdenum dioxide nanometer rod according to claim 1 is characterized in that, the volume ratio of the dimethyl formamide solution of the Tetrabutyl amonium bromide that adds in the described step 3 and yellow transparent filtrating is 1:1-1:2.
5. the preparation method of molybdenum dioxide nanometer rod according to claim 1 is characterized in that, the thermal treatment in the described step 5 is at N
2Carry out in the atmosphere, temperature 600-700 ℃, insulation 2-3h, naturally cools to room temperature then by temperature rise rate 25-35 ℃/min.
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| CN105568201A (en) * | 2015-12-18 | 2016-05-11 | 合肥中澜新材料科技有限公司 | Anti-crack wear-resistant coating of engine cylinder inner wall and preparation method thereof |
| CN105986218A (en) * | 2015-12-18 | 2016-10-05 | 合肥中澜新材料科技有限公司 | Engine steam cylinder inner wall wear-resisting coating good in lubricating and preparing method of coating |
| CN111621645A (en) * | 2020-06-09 | 2020-09-04 | 西安迈斯拓扑科技有限公司 | Irradiation from accelerator100Mo production99mRecovery from Tc process effluent100Method for Mo |
| CN112299483A (en) * | 2020-10-29 | 2021-02-02 | 中国科学院过程工程研究所 | Nano molybdenum dioxide and preparation method and application thereof |
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