CN109331665B - Method for producing film containing fine particles - Google Patents
Method for producing film containing fine particles Download PDFInfo
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- CN109331665B CN109331665B CN201811294049.7A CN201811294049A CN109331665B CN 109331665 B CN109331665 B CN 109331665B CN 201811294049 A CN201811294049 A CN 201811294049A CN 109331665 B CN109331665 B CN 109331665B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
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Abstract
The invention provides a preparation method of a film containing particles. The method comprises the following steps: the method comprises the following steps: preparing an organic solution; step two: transferring uranium-containing particles and plutonium-containing particles in a sample into the organic solution; step three: and dispersing the organic solution containing the particles on the surface of the mica sheet to form a film containing the particles. The preparation method of the film containing the particles mainly adds the synthetic camphor into the film-forming organic solution, and the organic solution consisting of the synthetic camphor, the collodion and the isoamyl acetate can generate complex physical and chemical actions with the mica in the drying process, so that the adhesive force of the film containing the particles on mica sheets can be obviously enhanced, the phenomena of warping and falling off of the film containing the particles in the drying process are effectively prevented, and the success rate and the analysis efficiency of particle analysis are obviously improved.
Description
Technical Field
The invention belongs to the field of nuclear guarantee, and particularly relates to a preparation method of a film containing particles.
Background
In the field of nuclear security, particle analysis is an important detection means, and uranium-containing particles and plutonium-containing particles in a wiping sample are analyzed to realize relevant detection. In the analysis process, in order to ensure the controllable position of the particles, the particles need to be carried by a carrier. Currently, the use of film carriers to carry particles is the most common way.
In recent years, collodion film carriers are developed domestically, and the basic preparation method comprises the following steps: firstly, adding particles into a mixed solution of collodion and isoamyl acetate, then spreading the mixed solution on a plane, volatilizing an organic solvent, and drying to form a film to obtain the particle-containing film. The application of the film containing the particles effectively avoids the occurrence of particle loss, simplifies the operation process and avoids positioning errors. However, after long-term use, the film containing the particles has the problems of insufficient adhesive force, easy warping and falling off in the drying and using processes and the like, and reduces the success rate and the analysis efficiency of particle analysis.
Disclosure of Invention
The invention provides a preparation method of a film containing particles, aiming at solving the problems that the existing film containing particles in particle analysis has insufficient adhesive force and is easy to warp and fall off in the drying and using processes. The method comprises the following steps:
the method comprises the following steps: preparing an organic solution, wherein the organic solution consists of synthetic camphor, collodion and isoamyl acetate, and the weight ratio of the synthetic camphor to the collodion in the collodion is 1: 2.5-1: 3.5;
step two: transferring uranium-containing particles and plutonium-containing particles in a sample to the organic solution to obtain a particle-containing organic solution;
step three: and dispersing the organic solution containing the particles on the surface of the mica sheet, and volatilizing the solvent to form a film containing the particles.
According to one embodiment, in the second step, the transferring is performed by: and ultrasonically vibrating the organic solution.
Further, the time of the ultrasonic oscillation is preferably more than 5 minutes.
According to one embodiment, in step three, the thickness of the mica sheets is preferably less than 100 μm.
According to one embodiment, in the third step, the mica sheet surface is preferably a fresh release surface.
Further, it is preferable that the peeling time of the fresh peeled surface is less than 12 hours.
According to one embodiment, in the third step, the dispersion of the particulate organic solution on the surface of the mica platelets is preferably carried out under dust-free conditions.
The preparation method of the film containing the particles mainly adds the synthetic camphor into the film-forming organic solution, and the organic solution consisting of the synthetic camphor, the collodion and the isoamyl acetate can generate complex physical and chemical actions with the mica in the drying process, so that the adhesive force of the film containing the particles on mica sheets can be obviously enhanced, the phenomena of warping and falling off of the film containing the particles in the drying process are effectively prevented, and the success rate and the analysis efficiency of particle analysis are obviously improved.
Detailed Description
The technical scheme of the invention is further specifically described by the following embodiments. In the following detailed description, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of the embodiments of the invention. It may be evident, however, that one or more embodiments may be practiced without these specific details.
The preparation method of the film containing the particles comprises the following steps:
the method comprises the following steps: preparing an organic solution, wherein the organic solution consists of synthetic camphor, collodion and isoamyl acetate, and the weight ratio of the synthetic camphor to the collodion in the collodion is 1: 2.5-1: 3.5;
step two: transferring uranium-containing particles and plutonium-containing particles in a sample to the organic solution to obtain a particle-containing organic solution;
step three: and dispersing the organic solution containing the particles on the surface of the mica sheet, and volatilizing the solvent to form a film containing the particles.
The technical core of the invention is that synthetic camphor is added into film-forming organic solution, and a large number of test results show that: the organic solution composed of the synthetic camphor, the collodion and the isoamyl acetate can generate complex physical and chemical actions with the mica in the drying process, so that the adhesive force of the film containing the particles on the mica sheet can be obviously enhanced, the phenomena of warping and falling of the film containing the particles in the drying process are effectively prevented, and a good effect is achieved.
According to an example, in the second step, the transferring mode is: and ultrasonically vibrating the organic solution. Ultrasonic vibration can separate particles from a wiping sample efficiently, and the transfer efficiency of the particles is obviously improved.
Further, the time of the ultrasonic oscillation is more than 5 minutes.
According to an example, in step three, the thickness of the mica sheets is preferably less than 100 μm. The thickness of the thinner mica sheet is beneficial to cutting, and the edge of the cut mica sheet can be ensured to be tidy.
According to one example, in the third step, the mica sheet surface is preferably a fresh release surface. Practical inspection and application show that the fresh stripping surface of the mica sheet has high cleanliness and good flatness, so that organic solution containing particles dispersed on the surface of the mica sheet can form firm combination with the fresh stripping surface in the drying process, and the adhesion effect of the film containing particles on the mica sheet is obviously improved.
Further, the stripping time of the fresh stripping surface is less than 12 h.
According to one example, in the third step, the dispersion of the organic solution containing particles on the surface of the mica sheet is carried out under dust-free conditions. The reduction of the influence of dust further ensures the effect of the adhesion of the particle-containing film to the mica sheet.
Example 1
The method comprises the following steps: preparing an organic solution, wherein the organic solution consists of synthetic camphor, collodion and isoamyl acetate, and the weight ratio of the synthetic camphor to the collodion in the collodion is 1: 3;
step two: transferring uranium-containing particles and plutonium-containing particles in a sample to the organic solution to obtain a particle-containing organic solution;
step three: and dispersing the organic solution containing the particles on the surface of a mica sheet under a dust-free condition, wherein the thickness of the mica sheet is 90 mu m, the surface of the mica sheet is a fresh stripping surface, and a film containing the particles is formed after the solvent is volatilized.
Example 2
The method comprises the following steps: preparing an organic solution, wherein the organic solution consists of synthetic camphor, collodion and isoamyl acetate, and the weight ratio of the synthetic camphor to the collodion in the collodion is 1: 2.5;
step two: transferring uranium-containing particles and plutonium-containing particles in a sample to the organic solution to obtain a particle-containing organic solution;
step three: and dispersing the organic solution containing the particles on the surface of a mica sheet under a dust-free condition, wherein the thickness of the mica sheet is 75 micrometers, the surface of the mica sheet is a fresh stripping surface, and a film containing the particles is formed after the solvent is volatilized.
Example 3
The method comprises the following steps: preparing an organic solution, wherein the organic solution consists of synthetic camphor, collodion and isoamyl acetate, and the weight ratio of the synthetic camphor to the collodion in the collodion is 1: 3.5;
step two: transferring uranium-containing particles and plutonium-containing particles in a sample to the organic solution to obtain a particle-containing organic solution;
step three: and dispersing the organic solution containing the particles on the surface of a mica sheet under a dust-free condition, wherein the thickness of the mica sheet is 60 mu m, the surface of the mica sheet is a fresh stripping surface, and a film containing the particles is formed after the solvent is volatilized.
Examination of the particle-containing films obtained in examples 1 to 3 above revealed that: the prepared film body of the film containing the particles is uniform and flat, the film forming effect is good, and a plurality of groups of films prepared in parallel are not warped or shed. The preparation method of the film containing the particles is applied to particle analysis, so that the fluency of analysis operation is effectively improved, and the analysis efficiency is improved.
Although a few embodiments in accordance with the present general inventive concept have been shown and described, it would be appreciated by those skilled in the art that changes may be made in these embodiments without departing from the principles and spirit of the general inventive concept, the scope of which is defined in the claims and their equivalents.
Claims (9)
1. A method of making a microparticle-containing film, the method comprising the steps of:
the method comprises the following steps: preparing an organic solution, wherein the organic solution consists of synthetic camphor, collodion and isoamyl acetate, and the weight ratio of the synthetic camphor to the collodion in the collodion is 1: 2.5-1: 3.5;
step two: transferring uranium-containing particles and plutonium-containing particles in a sample to the organic solution to obtain a particle-containing organic solution;
step three: and dispersing the organic solution containing the particles on the surface of the mica sheet, and volatilizing the solvent to form a film containing the particles.
2. The method for producing a microparticle-containing film according to claim 1, wherein: in the second step, the transfer mode is as follows: and ultrasonically vibrating the organic solution.
3. The method for producing a microparticle-containing film according to claim 2, wherein: the time of the ultrasonic oscillation is more than 5 minutes.
4. The method for producing a microparticle-containing film according to any one of claims 1 to 3, wherein: in the third step, the thickness of the mica sheet is less than 100 μm.
5. The method for producing a microparticle-containing film according to any one of claims 1 to 3, wherein: in the third step, the surface of the mica sheet is a fresh stripping surface.
6. The method for producing a microparticle-containing film according to claim 4, wherein: in the third step, the surface of the mica sheet is a fresh stripping surface.
7. The method for producing a microparticle-containing film according to claim 5, wherein: the stripping time of the fresh stripping surface is less than 12 h.
8. The method for producing a microparticle-containing film according to claim 6, wherein: the stripping time of the fresh stripping surface is less than 12 h.
9. The method for producing a microparticle-containing film according to any one of claims 1 to 3 and 6 to 8, wherein: in the third step, the operation process of dispersing the organic solution containing the particles on the surface of the mica sheet is to operate under a dust-free condition.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811294049.7A CN109331665B (en) | 2018-11-01 | 2018-11-01 | Method for producing film containing fine particles |
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| CN201811294049.7A CN109331665B (en) | 2018-11-01 | 2018-11-01 | Method for producing film containing fine particles |
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| CN109331665B true CN109331665B (en) | 2021-01-05 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103728327A (en) * | 2013-12-18 | 2014-04-16 | 中国原子能科学研究院 | Method for measuring uranium isotope ratio in single particles |
| RU2637396C2 (en) * | 2016-04-20 | 2017-12-04 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Method for producing dissipative structures |
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2018
- 2018-11-01 CN CN201811294049.7A patent/CN109331665B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103728327A (en) * | 2013-12-18 | 2014-04-16 | 中国原子能科学研究院 | Method for measuring uranium isotope ratio in single particles |
| RU2637396C2 (en) * | 2016-04-20 | 2017-12-04 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Method for producing dissipative structures |
Non-Patent Citations (1)
| Title |
|---|
| CRM 铀微粒的FT-TIMS 分析方法研究;陈彦等;《原子能科学技术》;20110930;第1031-1033页 * |
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