CN102815871A - Preparation method of phosphorus-doped graphite optical lens - Google Patents
Preparation method of phosphorus-doped graphite optical lens Download PDFInfo
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- CN102815871A CN102815871A CN2012103205362A CN201210320536A CN102815871A CN 102815871 A CN102815871 A CN 102815871A CN 2012103205362 A CN2012103205362 A CN 2012103205362A CN 201210320536 A CN201210320536 A CN 201210320536A CN 102815871 A CN102815871 A CN 102815871A
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Abstract
The invention provides a preparation method of a phosphorus-doped graphite optical lens, which comprises the following steps: putting a quartz boat with a clean quartz plate into the middle part of a quartz pipe, putting the quartz pipe in a pipe furnace, and heating the high-temperature part of the quartz pipe to reaction temperature in an argon protective atmosphere; adding methylbenzene and triphenyl phosphorus into a conical flask, and injecting the mixed solution into the quartz pipe through a constant flow pump after the triphenyl phosphorus is completely dissolved, wherein the solution is gasified and carried to the high-temperature region by the argon, and the carbon source methylbenzene and the phosphorus source triphenyl phosphorus are decomposed so as to start growing phosphorus-dope lamellar graphite on the quartz plate surface; and after 5-10 minutes, stopping heating and solution injection, pulling the quartz boat to the pipe opening from the middle part of the quartz pipe, cooling the quartz boat to room temperature in an argon protective atmosphere, and taking out the quartz boat to obtain the phosphorus-doped graphite optical lens with favorable optical and conductive properties.
Description
Technical field
The present invention relates to the graphite material technical field, be specifically related to a kind of preparation method of phosphorus doping graphite optical mirror slip.
Background technology
Graphite is a kind of important carbon material, has the character of a lot of uniquenesses, and as high temperature resistant, the fusing point of graphite is up to 3850 ℃, even through the calcination of ultrahigh-temperature electric arc, the loss of weight is very little, and thermal expansivity is also very little; The favorable conductive thermal conductivity; The electroconductibility of graphite is higher 100 times than general nonmetalliferous ore; Be since in the graphite each carbon atom only form 3 covalent linkage with carbon atom on every side; Each carbon atom also remain 1 not bonding electrons come transmission charge, simultaneously its thermal conductivity surpasses metallic substance such as steel, iron, lead; Good chemicalstability under the normal temperature can be acidproof, alkaline-resisting and the corrosion of organic solvent-resistant; And good lubricity and plasticity-etc.Therefore graphite has in industry such as metallurgical, electrical equipment and machineries and greatly uses, and graphite is still made pencil, prepared Chinese ink, pitch-dark, printing ink and man-made diamond, the indispensable raw material of diamond in addition.Along with development of modern science and technology, the Application Areas of graphite is also constantly being widened, and in development and national economy, plays more and more important effect.
In recent years along with the application of graphite material and going deep into of research; People attempt through in graphite, introducing the structure that other atom changes graphite; Thereby obtain to have the new graphite material of some specific performance; Like atoms such as the B that in graphite, mixes, N, P and S, the introducing of these non-metallic atoms can directly influence the structure and the character of graphite.As in graphite-structure, mixing the N atom, because nitrogen-atoms Duo an outer valence electron than carbon atom, thus after forming conjugated system with the valence electron of graphite carbon, can obviously increase the electric density of graphite carbon, thus the electroconductibility and the catalytic performance of increase graphite; Phosphorus atom and for example; Because the P atomic radius is bigger than carbon atom; After in graphite, mixing phosphorus atom; Because the bond distance of carbon phosphorus key is littler than the carbon-carbon bond than the bond angle of the length of carbon-carbon bond and carbon phosphorus key, tangible projection can appear in graphite surface, and its hydrogen reduction electrocatalysis characteristic in fuel cell also obviously improves simultaneously.
Investigators such as Liu Ruili have reported the preparation of nitrogen doped graphite carbon, do not relate to the preparation of phosphorus doping graphite carbon in the literary composition; Prepare nitrogen phosphorus adulterated multi-walled carbon nano-tubes simultaneously though there is investigator such as Terrones to report the employing ferrocene as catalyzer; And investigator such as Jourdain reported synthetic many walls of phosphorus doping carbon pipe on the NiFe catalyzer of the anodised pellumina load of phosphorated, but the report of at present still without phosphorus adulterated graphite optical mirror slip preparation.
Summary of the invention
Technical problem: the purpose of this invention is to provide a kind of preparation method of phosphorus doping graphite optical mirror slip, fill up the application disappearance of doped graphite, the application of widening graphite material at optical field.
Technical scheme: the preparation method of phosphorus doping graphite optical mirror slip of the present invention comprises the steps:
A, employing chemical Vapor deposition process, the quartz boat that will have a clean quartz plate is put into the silica tube middle part, and silica tube is put into tube furnace, and heating under the protection of argon gas rare gas element makes the temperature at silica tube middle part be increased to temperature of reaction;
B, in container bottle, add 4-10 mL toluene and add 44.1-955 mg triphenyl phosphorus; The vibration, treat that triphenyl phosphorus dissolves fully after, under argon shield; The mixing solutions that will obtain after will dissolving through constant flow pump injects in the silica tube; Taken to the heating zone at silica tube middle part behind the vaporizer by argon gas, carbon source toluene and phosphorus source triphenyl phosphorus decompose, and on quartz plate, begin to generate phosphorus doping graphite;
Stop heating after c, 5-10 minute and in silica tube, inject mixing solutions; And move quartz boat to the mouth of pipe from silica tube middle part; Under argon shield with the quartz boat cool to room temperature; From quartz boat, take out clean quartz plate sample, obtain having the phosphorus doping graphite optical mirror slip of optics and conductivity.
The concentration of described triphenyl phosphorus in toluene solution is 2.5～10 wt%;
Described triphenyl phosphorus is the phosphorus source; Toluene is carbon source; Argon gas is protection gas;
Said temperature of reaction is 900-1200 ℃;
The flow velocity of said argon gas rare gas element is 0.3～0.6 L/min; The flow velocity of said constant flow pump is 2～3 mL/h; The flow velocity of said argon gas is 0.1～0.4 L/min;
Beneficial effect: the present invention is that substrate adopts the CVD method to prepare phosphorus doping graphite optical mirror slip with the quartz, has following advantage:
(1) adopting triphenyl phosphorus is the phosphorus source, and employing toluene is carbon source, can successfully control the content of phosphorus in the phosphorus doping graphite optical mirror slip through controlling the content of triphenyl phosphorus in toluene, thus the optical property of effective modulation graphite;
(2) the phosphorus doping graphite optical mirror slip of preparation, owing to adopt direct decomposition reactant under the comparatively high temps, and the atom after decomposing directly generates the graphite optical mirror slip on the quartz plate surface, used time weak point, the speed of prepared phosphorus doping graphite optical mirror slip is fast.
(3) preparation method of phosphorus doping graphite optical mirror slip is simple, and operation controllability is strong.
Need not any catalyzer when (4) preparing phosphorus doping graphite eyeglass.
Description of drawings
Fig. 1 (a), Fig. 1 (b), Fig. 1 (c) are former quartz plate and the embodiment of the invention 3 prepared phosphorus doping graphite optical mirror slip comparison diagrams.
Fig. 2 (a), Fig. 2 (b) are the ESEM and ability spectrogram of the embodiment of the invention 3 prepared phosphorus doping graphite optical mirror slips.
The ESEM of the upper strata light reflecting material that takes off on the phosphorus doping graphite optical mirror slip that Fig. 3 (a), Fig. 3 (b), Fig. 3 (c) make for the embodiment of the invention 1, element distribute (Elemental mapping) and power spectrum EDS figure.
Embodiment
Further describe embodiments of the invention are done below in conjunction with accompanying drawing:
Embodiment 1,
The quartz boat that will have a clean quartz plate is placed on the silica tube middle part and silica tube is put into tube furnace, is under the protection of argon gas rare gas element of 0.3 L/min at flow velocity, and the temperature of silica tube high-temperature part is elevated to 900 ℃;
The toluene and the triphenyl phosphorus that in container bottle, add 2 mL make consumption 2.5 wt.% of triphenyl phosphorus; Under argon shield, with the flow velocity of 2.0 mL/h this mixing solutions is injected into silica tube through constant flow pump, taken to the high-temperature zone by argon gas behind the vaporizer, decompose in carbon source and phosphorus source, and beginning is growth phosphorus doping graphite on the quartz plate surface;
After 5 minutes; Stop heating; At flow velocity is under the argon shield of 0.1 L/min; Quartz boat is moved on to afterbody mouth of pipe cool to room temperature from the silica tube middle part, from quartz boat, take out clean quartz plate, the content that obtains phosphorus doping graphite optical mirror slip that obtains through power spectrum EDS analysis revealed is 0.30 wt.%.
Embodiment 2,
The quartz boat that will have a clean quartz plate is placed on the silica tube middle part and silica tube is put into tube furnace, is under the protection of argon gas rare gas element of 0.4 L/min at flow velocity, and the temperature of silica tube high-temperature part is elevated to 1000 ℃;
In container bottle, add the toluene of 4 mL, slowly add triphenyl phosphorus again, wherein the consumption of triphenyl phosphorus is 5 wt.% toluene; After treating that triphenyl phosphorus and ferrocene dissolve fully; Under argon shield, with the flow velocity of 2.4 mL/h this mixing solutions is injected into silica tube through constant flow pump, taken to the high-temperature zone by argon gas behind the vaporizer; Decompose in carbon source and phosphorus source, and beginning is growth phosphorus doping graphite on the quartz plate surface;
After 6 minutes; Stop heating; At flow velocity is under the argon shield of 0.2 L/min; Quartz boat is moved on to afterbody mouth of pipe cool to room temperature from the silica tube middle part, from quartz boat, take out clean quartz plate sample, the content that obtains phosphorus in the phosphorus doping graphite optical mirror slip that obtains through power spectrum EDS analysis revealed is 0.56 wt.%.
Embodiment 3,
The quartz boat that will have a clean quartz plate is placed on the silica tube middle part and silica tube is put into tube furnace, is under the protection of argon gas rare gas element of 0.5 L/min at flow velocity, and the temperature of silica tube high-temperature part is elevated to 1100 ℃;
In container bottle, add the toluene of 6 mL, and add triphenyl phosphorus, make wherein consumption 7.5 wt.% of triphenyl phosphorus; After treating that triphenyl phosphorus dissolves fully; Under argon shield, with the flow velocity of 2.7 mL/h this mixing solutions is injected into silica tube through constant flow pump, taken to the high-temperature zone by argon gas behind the vaporizer; Decompose in carbon source and phosphorus source, and beginning is growth phosphorus doping graphite on the quartz plate surface;
After 8 minutes; Stop heating; At flow velocity is under the argon shield of 0.3 L/min; Quartz boat is moved on to afterbody mouth of pipe cool to room temperature from the silica tube middle part, from quartz boat, take out clean quartz plate sample, the content that obtains phosphorus in the phosphorus doping graphite optical mirror slip that obtains through power spectrum EDS analysis revealed is 0.87 wt.%.
Embodiment 4,
The quartz boat that will have a clean quartz plate is placed on the silica tube middle part and silica tube is put into tube furnace, is under the protection of argon gas rare gas element of 0.6 L/min at flow velocity, and the temperature of silica tube high-temperature part is elevated to 1200 ℃;
In container bottle, add the toluene of 10 mL, and add triphenyl phosphorus, wherein consumption 10 wt.% of triphenyl phosphorus; After treating that triphenyl phosphorus dissolves fully; Under argon shield, with the flow velocity of 3.0 mL/h this mixing solutions is injected into silica tube through constant flow pump, taken to the high-temperature zone by argon gas behind the vaporizer; Carbon source toluene and phosphorus source triphenyl phosphorus decompose, and beginning is growth phosphorus doping graphite on the quartz plate surface;
After 10 minutes; Stop heating; At flow velocity is under the argon shield of 0.3 L/min; Quartz boat is moved on to afterbody mouth of pipe cool to room temperature from the silica tube middle part, from quartz boat, take out clean quartz plate sample, the content that obtains phosphorus in the phosphorus doping graphite optical mirror slip that obtains through power spectrum EDS analysis revealed is 1.28 wt.%.
Fig. 1 (a) is water white former quartz plate; Fig. 1 (b) and Fig. 1 (c) they are prepared phosphorus doping graphite optical mirror slip, by Fig. 1 (a), and Fig. 1 (b); Fig. 1 (c) can find out that prepared phosphorus doping graphite optical mirror slip demonstrates optical property preferably.
By Fig. 2 (a); The graphite optical mirror slip that Fig. 2 (b) EDS can spectrogram can confirm this preparation is mainly by the carbon (C on surperficial upper strata; 8.82 wt.%) with the quartz plate of lower floor in element silicon (Si, 32.2 0 wt.%) oxygen element form (O, 45.94 wt.%).
By Fig. 3 (a), ESEM, element that Fig. 3 (b), Fig. 3 (c) are respectively the upper strata light reflecting material that takes off on the phosphorus doping graphite optical mirror slip distribute (Elemental mapping) and power spectrum EDS figure; Picture shows that phosphorus doping graphite optical mirror slip upper strata light reflecting material is that phosphorus mixes graphite; By carbon (C, 96.92 wt.%), oxygen (O; 2.77 wt.%) and three kinds in phosphorus (P, 0.30 wt.%) elementary composition.
Claims (5)
1. the preparation method of a phosphorus doping graphite optical mirror slip is characterized in that comprising the steps:
A, employing chemical Vapor deposition process, the quartz boat that will have a clean quartz plate is put into the silica tube middle part, and silica tube is put into tube furnace, and heating under the protection of argon gas rare gas element makes the temperature at silica tube middle part be increased to temperature of reaction;
B, in container bottle, add 4-10 mL toluene and add 44.1-955 mg triphenyl phosphorus; The vibration, treat that triphenyl phosphorus dissolves fully after, under argon shield; The mixing solutions that will obtain after will dissolving through constant flow pump injects in the silica tube; Taken to the heating zone at silica tube middle part behind the vaporizer by argon gas, carbon source toluene and phosphorus source triphenyl phosphorus decompose, and on quartz plate, begin to generate phosphorus doping graphite;
Stop heating after c, 5-10 minute and in silica tube, inject mixing solutions; And move quartz boat to the mouth of pipe from silica tube middle part; Under argon shield with the quartz boat cool to room temperature; From quartz boat, take out clean quartz plate sample, obtain having the phosphorus doping graphite optical mirror slip of optics and conductivity.
2. the preparation method of phosphorus doping graphite optical mirror slip according to claim 1 is characterized in that: the concentration of described triphenyl phosphorus in toluene solution is 2.5～10 wt%.
3. the preparation method of phosphorus doping graphite optical mirror slip according to claim 1 is characterized in that: described triphenyl phosphorus is the phosphorus source; Toluene is carbon source; Argon gas is protection gas.
4. the preparation method of phosphorus doping graphite optical mirror slip according to claim 1 is characterized in that: said temperature of reaction is 900-1200 ℃.
5. the preparation method of phosphorus doping graphite optical mirror slip according to claim 1 is characterized in that: the flow velocity of said argon gas rare gas element is 0.3～0.6 L/min; The flow velocity of said constant flow pump is 2～3 mL/h; The flow velocity of said argon gas is 0.1～0.4 L/min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1970439A (en) * | 2005-11-25 | 2007-05-30 | 中国科学院金属研究所 | Preparation method of thermolysis carbon ball |
| CN101289181A (en) * | 2008-05-29 | 2008-10-22 | 中国科学院化学研究所 | Doped graphene and method for preparing same |
| CN102001648A (en) * | 2010-10-29 | 2011-04-06 | 华南理工大学 | Method for preparing phosphorus-doped spherical graphite |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1970439A (en) * | 2005-11-25 | 2007-05-30 | 中国科学院金属研究所 | Preparation method of thermolysis carbon ball |
| CN101289181A (en) * | 2008-05-29 | 2008-10-22 | 中国科学院化学研究所 | Doped graphene and method for preparing same |
| CN102001648A (en) * | 2010-10-29 | 2011-04-06 | 华南理工大学 | Method for preparing phosphorus-doped spherical graphite |
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