CN112030118A - Preparation method of deuterated polyethylene nanowire array target - Google Patents
Preparation method of deuterated polyethylene nanowire array target Download PDFInfo
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- CN112030118A CN112030118A CN202010757274.0A CN202010757274A CN112030118A CN 112030118 A CN112030118 A CN 112030118A CN 202010757274 A CN202010757274 A CN 202010757274A CN 112030118 A CN112030118 A CN 112030118A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/12—Organic material
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Abstract
The invention belongs to the technical field of nuclear technology application, and discloses deuterated polyethylene ((CD)2)n) A method for preparing a nanowire array target. The method is to prepare (CD) by adopting a dissolution-polymerization method2)nFlat target, then (CD) by hot extrusion-etching2)nA planar target is etched into the mold of the desired nanoarray. The nanowire array target prepared by the method is orderly arranged, good in uniformity, smooth and clean in nanowire surface and good in method repeatability.
Description
Technical Field
The invention belongs to the technical field of nuclear technology application, and particularly relates to deuterated polyethylene ((CD)2)n) A method for preparing a nanowire array target.
Background
The target can be prepared by a variety of methods including chemical vapor deposition, physical vapor deposition, roll milling, and the like. Currently, nuclear physics research needs to prepare a deuterated polyethylene ((CD)2)n) The nanowire array target is not reported in the prior published reports, so that a method for preparing the array target is urgently needed.
Disclosure of Invention
Objects of the invention
To enable the preparation of deuterated polyethylene ((CD)2)n) The invention discloses a nanowire array target and provides a preparation method which is orderly arranged, good in uniformity, smooth and clean in nanowire surface and good in method repeatability.
(II) technical scheme
To solve the problems of the prior art, the present disclosure employs a two-step process for preparing (CD)2)nThe technical scheme of the nanowire array target is as follows:
a process for preparing the deuterated polyethene nanowire array target includes dissolving-polymerizing (CD)2)nFlat target, then (CD) by hot extrusion-etching2)nA planar target is etched into the mold of the desired nanoarray.
Preferably, a method for preparing a deuterated polyethylene nanowire array target, the method comprising the steps of:
(1) preparation of (CD) by solution-polymerization2)nPlanar target
a. Will (CD)2)nPutting the material and the xylene solution into a container, and stirring in the heating process;
b. wait for (CD)2)nAfter all the materials are dissolved and form colloidal turbid liquid, pouring the colloidal turbid liquid into a flat-bottom quartz glass vessel;
c: placing the quartz glass ware obtained in the step b on a platform, uniformly heating the colloidal suspension in the quartz glass ware until the dimethylbenzene is fully volatilized, and (CD)2)nFully polymerizing in a supersaturated atmosphere of xylene;
d: after the xylene solution is completely volatilized, uniform (CD) is formed on the bottom surface of the quartz vessel2) n planar target films obtained by peeling the planar target films from the bottom of the vessel (CD)2) n planar target films;
(2) hot extrusion-etching method for preparing (CD)2)nNanowire array target
e: placing an array target die made of aluminum oxide on a base with a smooth surface; the array target die is of a cuboid structure, the structure is provided with pore channels with nanometer-scale pore diameters which are arranged into a certain array, and the arrangement mode and the pore channel diameter of the array are determined by the required physical experiment; the pore canal extends downwards in the Y-axis direction and is not a through hole;
f: covering the planar target film obtained in the step d in the step (1) on the pore channel of the array target mold, and placing the porous target film in a vacuum chamber; heating the planar target film until the planar target film becomes a flowable colloid; the colloid flows into the pore channels of the array target mould under the action of gravity, wherein the volume of the colloid target mould is larger than the sum of the volumes of all the pore channels, and the redundant part of the colloid target mould can form a plane deuterated polyethylene film integrated with the nanowires;
g: and f, corroding the alumina framework of the array target die obtained in the step f by using a copper sulfate solution to obtain the required deuterated polyethylene nanowire array target.
Preferably, a planar target film is overlaid on the channels of the array target mold in step f, and also weighted to allow faster flow into the channels of the array target mold.
Preferably, the volume sum (CD) of the xylene solution in step a2)nThe volume-mass ratio of the mass of the material is 1: 1.
Preferably, the pore diameter of the pore channel is 100-800 nm, and the depth of the pore channel in the Y-axis direction is 5-50 μm.
Preferably, in step c, the uniform heating is performed by reversely buckling a heat-conducting container above the quartz glass vessel, and heating the heat-conducting container from top to bottom by using an infrared lamp.
Preferably, in the step c, the suspension is uniformly heated to reach a temperature of 110-130 ℃.
Preferably, the concentration of the copper sulfate in the step g is 1-2 mol/L.
Preferably, the pressure in the vacuum chamber in step f is not more than 5 x 10-1Pa；
Preferably, in the step f, the heating temperature is 100-110 ℃.
(III) advantageous effects
The deuterated polyethylene nanowire array target prepared by the method can be used for preparing a deuterated polyethylene target film with the diameter of nanometer magnitude and the height of micrometer magnitude and arranged according to a certain array, and each nanowire has a smooth surface and can vertically stand on a plane deuterated polyethylene film connected with the nanowire in an integrated manner. In the preparation process, a dissolution-polymerization method is adopted to prepare a planar deuterated polyethylene target film with the polymerization degree and the uniformity meeting the requirements, then the planar polyethylene target film is pressed into a mold with the required specification by a hot extrusion-etching method, simultaneously, an aluminum oxide is skillfully designed to be used as a mold frame, and the aluminum oxide is corroded after the etching is finished to prepare the nanowire array target film.
Detailed Description
The present disclosure will be further illustrated with reference to specific examples.
Example 1
A process for preparing the deuterated polyethene nanowire array target includes dissolving-polymerizing (CD)2)nFlat target, then (CD) by hot extrusion-etching2)nA planar target is etched into the mold of the desired nanoarray. The method comprises the following steps:
(1) preparation of (CD) by solution-polymerization2)nPlanar target
a. Will (CD)2)nPutting the material and the xylene solution into a container, and stirring in the heating process; volume sum of xylene solution (CD)2)nThe volume-mass ratio of the mass of the material is 1: 1.
b. Wait for (CD)2)nAfter all the materials are dissolved and form colloidal turbid liquid, pouring the colloidal turbid liquid into a flat-bottom quartz glass vessel;
c: placing the quartz glass ware obtained in the step b on a platform, uniformly heating the colloidal suspension in the quartz glass ware until the dimethylbenzene is fully volatilized, and (CD)2)nFully polymerizing in a supersaturated atmosphere of xylene; the uniform heating mode is that a beaker is reversely buckled above a quartz glass vessel, an infrared lamp is utilized to heat the beaker from top to bottom to 120 ℃, the heating mode enables the xylene solution to slowly volatilize, and the prepared target film has a flat and smooth surface and no air holes. The use of flat-bottomed quartz glassware and a platform ensured the level of the colloidal suspension to produce target films of uniform thickness.
d: after the xylene solution is completely volatilized, the mixture is put into quartzForming a uniform target film on the bottom surface of the vessel, and peeling off the planar target film from the bottom of the vessel to obtain the final product (CD)2) n planar target films;
(2) hot extrusion-etching method for preparing (CD)2)nNanowire array target
e: placing an array target die made of aluminum oxide on a base with a smooth surface; the structure is a cuboid structure, the structure is provided with pore channels with nanometer-scale pore diameters which are arranged into a certain array, and the arrangement mode and the pore channel diameter of the array are determined by the required physical experiment; the pore canal extends downwards in the Y-axis direction, but the depth of a through hole which is not penetrated, namely the through hole, is less than the height of the mold; the pore diameter of the pore channel is 400nm, and the depth of the pore channel in the Y-axis direction is 30 mu m. The pitch between the channels was 5 μm.
f: covering the pore channels of the array target mold with the planar target film obtained in step (1) and weighting the planar target film to enable faster flow into the pore channels of the array target mold. Placing the mold in a vacuum chamber with a vacuum degree of 4 × 10-1Pa; heating the planar target film to 110 ℃ until the planar target film becomes flowable colloid; the colloid flows into the pore channels of the array target mould under the action of gravity, wherein the volume of the colloid target mould is larger than the sum of the volumes of all the pore channels, and a plane deuterated polyethylene film integrated with the nanowires can be formed by the redundant colloid target mould above the pore channels;
g: and f, corroding the alumina frame of the array target die obtained in the step f by using 1mol/L copper sulfate solution to obtain the required deuterated polyethylene nanowire array target.
The prepared nanowire array target is orderly arranged and has good uniformity.
Example 2
Unlike example 1, the pore diameter of the pore channel in the array target mold was 100nm, and the depth of the pore channel in the Y-axis direction was 5 μm. In step c, the suspension is heated uniformly to a temperature of 110 ℃. The concentration of the copper sulfate in the step g is 2 mol/L. In step f, the heating temperature was 110 ℃.
Example 3
Unlike example 1, the pore diameter of the channels in the array target mold was 800nm, and the depth of the channels in the Y-axis direction was 50 μm. In step c, the suspension is heated uniformly to a temperature of 120 ℃.
Claims (10)
1. A process for preparing the deuterated polyethene nano-wire array target includes such steps as preparing planar target by dissolving-polymerizing method, and hot extruding-etching to obtain (CD)2)nA planar target is etched into the mold of the desired nanoarray.
2. The method of claim 1, wherein the method comprises the steps of:
(1) preparation of (CD) by solution-polymerization2)nPlanar target
a. Will (CD)2)nPutting the material and the xylene solution into a container, and stirring in the heating process;
b. wait for (CD)2)nAfter all the materials are dissolved and form colloidal turbid liquid, placing the colloidal turbid liquid into a flat-bottom quartz glass vessel;
c: placing the quartz glass ware obtained in the step b on a platform, uniformly heating the colloidal suspension in the quartz glass ware until the dimethylbenzene is fully volatilized, and (CD)2)nFully polymerizing in a supersaturated atmosphere of xylene;
d: after the xylene solution is completely volatilized, uniform (CD) is formed on the bottom surface of the quartz vessel2) n planar target films obtained by peeling the planar target films from the bottom of the vessel (CD)2) n planar target films;
(2) hot extrusion-etching method for preparing (CD)2)nNanowire array target
e: placing an array target die made of aluminum oxide on a base with a smooth surface; the array target die is of a cuboid structure, the structure is provided with pore channels with nanometer-scale pore diameters which are arranged into a certain array, and the arrangement mode and the pore channel diameter of the array are determined by the required physical experiment; the pore canal extends downwards in the Y-axis direction and is not a through hole;
f: covering the planar target film obtained in the step d in the step (1) on the pore channel of the array target mold, and placing the porous target film in a vacuum chamber; heating the planar target film until the planar target film becomes a flowable colloid; the colloid flows into the pore channels of the array target mould under the action of gravity, wherein the volume of the colloid target mould is larger than the sum of the volumes of all the pore channels;
g: and f, corroding the alumina framework of the array target die obtained in the step f by using a copper sulfate solution to obtain the required deuterated polyethylene nanowire array target.
3. The method of claim 2, wherein a planar target film is coated on the channels of the array target mold in step f, and a weight is further added on the planar target film.
4. The method of claim 2, wherein the volume sum of the xylene solution in step a and (CD) is greater than the volume sum of the xylene solution in step a2)nThe volume-mass ratio of the mass of the material is 1: 1.
5. The method of claim 2, wherein the pore diameter of the pore channel is 100-800 nm, and the depth of the pore channel in the Y-axis direction is 5-50 μm.
6. The method of claim 2, wherein the uniform heating in step c is performed by reversing a heat conducting container over the quartz glass vessel and heating the heat conducting container from top to bottom using an infrared lamp.
7. The method of claim 2, wherein in step c, the suspension is uniformly heated to a temperature of 110-130 ℃.
8. The method of claim 2, wherein the copper sulfate concentration in step g is 1-2 mol/L.
9. The method of claim 2, wherein the pressure in the vacuum chamber in step f is no greater than 5 x 10-1Pa。
10. The method of claim 2, wherein the heating temperature in step f is 100-110 ℃.
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