CN110981212B - Method for manufacturing single-layer TCTS anti-relaxation coating in alkali metal gas chamber - Google Patents
Method for manufacturing single-layer TCTS anti-relaxation coating in alkali metal gas chamber Download PDFInfo
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- CN110981212B CN110981212B CN201911309484.7A CN201911309484A CN110981212B CN 110981212 B CN110981212 B CN 110981212B CN 201911309484 A CN201911309484 A CN 201911309484A CN 110981212 B CN110981212 B CN 110981212B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
- C03C17/30—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B05D1/00—Processes for applying liquids or other fluent materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
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- C03C2218/11—Deposition methods from solutions or suspensions
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Abstract
A TCTS solution and an alkali metal air chamber after hydroxylation treatment are both placed in a heated state, a peristaltic pump is utilized to enable the alkali metal air chamber to be fully filled with the TCTS solution, TCTS molecules in the TCTS solution and hydroxyl on the inner wall of the air chamber are subjected to dehydration condensation reaction to form a TCTS coating which is combined with the inner wall of the air chamber through silicon-oxygen bonds, application of the coating at higher temperature is guaranteed, such as a SERF magnetometer and the like, the application field of the anti-relaxation coating is widened, meanwhile, the thickness of the formed coating is larger due to the fact that the length of the TCTS molecules is longer, and even the single-layer TCTS coating can meet or even improve the anti-relaxation performance of the alkali metal air chamber. TCTS is triacontyltrichlorosilane.
Description
Technical Field
The invention relates to a technology for manufacturing an anti-relaxation coating on the inner wall of an alkali metal air chamber, in particular to a method for manufacturing a single-layer TCTS anti-relaxation coating in the alkali metal air chamber. TCTS is triacontyltrichlorosilane.
Background
With the continuous widening of the application field of the alkali metal air chamber, the anti-relaxation coating has more advantages compared with buffer gas, and at present, two factors for limiting the wide application of the anti-relaxation coating are mainly used, namely, the preparation of the high-temperature resistant anti-relaxation coating, such as an Octadecyl Trichlorosilane (OTS) coating and the like, has poor anti-relaxation performance and poor consistency of the preparation of the coating. And the coatings with stronger anti-relaxation performance, such as olefin, paraffin and the like, have lower working temperature and narrow application range. Based on the above problems, researchers have conducted extensive research. It has been found that, although the single layer TCTS (triacontyltrichlorosilane) coating has a similar morphology to the single layer OTS coating, its anti-relaxation effect is close to that of the dual layer OTS coating, which is similar in thickness. In addition, the relaxation resistance of the dual-layer OTS coating is much better than that of the single-layer OTS coating, and therefore, it is generally believed that the thickness of the coating has a greater effect on the relaxation resistance than the morphology of the coating, and the thicker the coating, the better the relaxation resistance. The thickness is critical to the performance impact of the anti-relaxation coating. The research on the anti-relaxation performance of the TCTS single-layer coating in the alkali metal gas chamber has important significance on the understanding of the anti-relaxation mechanism of the coating. At present, the TCTS coating is manufactured on a glass sheet or a silicon sheet, the TCTS is solid at room temperature, the melting point of the TCTS is as high as 82 ℃, the manufacturing difficulty of the TCTS anti-relaxation coating in the gas chamber is high, and the single-layer TCTS coating needs to be formed in a nitrogen or anhydrous environment, so that the manufacturing of the single-layer TCTS coating in the alkali metal gas chamber is further increased. The inventor believes that if the TCTS solution and the hydroxylated alkali metal gas chamber are both in a heated state, the alkali metal gas chamber is fully filled with the TCTS solution by using a peristaltic pump, and TCTS molecules in the TCTS solution and hydroxyl on the inner wall of the gas chamber form a TCTS coating which is bonded to the inner wall of the gas chamber by silicon-oxygen bonds through dehydration condensation reaction, the application of the coating at higher temperature is ensured, such as a SERF magnetometer and the like, the application field of the anti-relaxation coating is widened, meanwhile, the coating thickness is larger because the chain length of the TCTS molecules is longer (OTS is octadecyltrichlorosilane which is commonly used, and TCTS is triacontyltrichlorosilane of the invention), and even a single-layer TCTS coating can meet or even improve the anti-relaxation performance of the alkali metal gas chamber. In view of the above, the present inventors have completed the present invention.
Disclosure of Invention
Aiming at the defects or shortcomings in the prior art, the invention provides a method for manufacturing a single-layer TCTS anti-relaxation coating in an alkali metal gas chamber, wherein a TCTS solution and the alkali metal gas chamber subjected to hydroxylation treatment are both placed in a heated state, a peristaltic pump is utilized to ensure that the TCTS solution is fully absorbed in the alkali metal gas chamber, TCTS molecules in the TCTS solution and hydroxyl on the inner wall of the gas chamber form a TCTS coating combined with the inner wall of the gas chamber through a silicon-oxygen bond through dehydration condensation reaction, the application of the coating at higher temperature is favorably ensured, such as a SERF magnetometer and the like, the application field of the anti-relaxation coating is widened, meanwhile, the coating thickness is larger due to the longer chain length of the TCTS molecules, and even the single-layer TCTS coating can meet or even improve the anti-relaxation performance of the alkali metal gas chamber. TCTS is triacontyltrichlorosilane.
The technical scheme of the invention is as follows:
a single-layer TCTS anti-relaxation coating manufacturing method in an alkali metal air chamber is characterized by comprising the following steps of placing a first container with a prepared TCTS solution and the alkali metal air chamber with the inner wall subjected to hydroxylation in a heated state, placing a lower tail pipe of the alkali metal air chamber in the TCTS solution, connecting an upper tail pipe of the alkali metal air chamber with a left section air suction port of a silicone tube of a peristaltic pump, starting the peristaltic pump to enable the alkali metal air chamber to be filled with the TCTS solution, and forming the TCTS coating which is combined with the inner wall of the air chamber through a silicon-oxygen bond through dehydration condensation reaction between TCTS molecules in the TCTS solution and hydroxyl on the inner wall of the air chamber.
The solvent of the TCTS solution is dicyclohexyl, the solute is TCTS, and the concentration of the TCTS is 1 mM.
The right section of the silicone tube is provided with an exhaust port with a first valve and a nitrogen inlet with a second valve.
The peristaltic pump makes TCTS solution quilt after the alkali metal air chamber is inhaled fully, TCTS solution is in persist in the alkali metal air chamber is no less than 3 hours, then the export of nitrogen cylinder is connected to silicone tube right side section port, utilizes the peristaltic pump with nitrogen pump in the alkali metal air chamber, will TCTS solution in the alkali metal air chamber is followed tail pipe discharge down in the first container, behind the TCTS solution in the alkali metal air chamber was evacuated, will the tail pipe is arranged in the bicyclohexane as the washing liquid down, through the circulating pump go into the bicyclohexane with nitrogen gas in the nitrogen cylinder is right the inner wall in alkali metal air chamber is used the bicyclohexane washs 3 ~ 5 times, nitrogen gas is used for empting the bicyclohexane.
The bicyclohexane is formulated in a second container.
The heating state is realized by an oven, the alkali metal air chamber and the first container are both arranged in the oven, and the temperature in the oven is 85 +/-2 ℃.
And a transverse section radially extends from the side wall of the upper tail pipe, and the port of the transverse section is connected with the air suction port of the left section of the silicone tube.
The hydroxylation treatment adopts a piranha solution, an upper tail pipe of an alkali metal air chamber is connected with a peristaltic pump, a lower tail pipe of the alkali metal air chamber is arranged in the piranha solution, the piranha solution is fully absorbed in the alkali metal air chamber through the peristaltic pump and is kept for not less than 1 hour, then the piranha solution is discharged in a nitrogen pumping mode, the piranha solution in the alkali metal air chamber is emptied and then is placed in deionized water, the inner wall of the alkali metal air chamber is cleaned by the deionized water in a circulating pumping mode, the nitrogen is used for emptying the deionized water, the cleaned alkali metal air chamber is placed in a vacuum oven for drying, and the dried alkali metal air chamber is taken out from the vacuum oven and is firstly filled with the nitrogen into the vacuum oven for vacuum breaking.
The first container is a beaker.
The second container is a beaker.
The invention has the following technical effects: the invention relates to a method for preparing a monolayer TCTS anti-relaxation coating in an alkali metal gas chamber. Before the air chamber is taken out of the vacuum oven, nitrogen is adopted to break vacuum instead of air, so that the inside of the alkali metal air chamber can not be attached with water molecules of the atmospheric environment, and the formation of a single-layer coating is ensured. Preparing 1mM TCTS solution, placing the TCTS solution in a dicyclohexyl solution, placing the solution in an oven at 85 ℃, dissolving TCTS, symmetrically distributing two tail pipes in an alkali metal gas chamber, placing one tail pipe in the TCTS solution, connecting the other tail pipe with a peristaltic pump, and sucking the TCTS solution into the gas chamber by the peristaltic pump. After the TCTS solution is left in the alkali metal gas chamber for 3 hours, one end of the peristaltic pump is connected with a tail pipe of the alkali metal gas chamber, and the other end of the peristaltic pump is connected with nitrogen, so that the TCTS solution is discharged. After the TCTS solution is discharged, the inside of the air chamber is cleaned for 3-5 times by adopting dicyclohexyl in an oven, unreacted TCTS molecules remained in the alkali metal air chamber are removed as soon as possible, and the formation of a multi-layer crosslinked coating caused by the adhesion of water molecules on the inner wall of the air chamber for too long time is avoided. The method is simple and feasible to operate, not only forms a single-layer TCTS coating, but also does not need to create an anhydrous external environment, can effectively accelerate the coating manufacturing process and reduce the coating manufacturing difficulty on the premise of effectively ensuring the coating manufacturing consistency.
Drawings
FIG. 1 is a schematic diagram of the layout of an apparatus for implementing a method for forming a single TCTS anti-relaxation coating in an alkali metal chamber according to the present invention.
The reference numbers are listed below: 1-an alkali metal gas cell; 2-upper tail pipe; 3-lower tail pipe; 4-TCTS solution; 5-beaker or first container; 6-baking oven; 7-left section of silicone tube; 8-a peristaltic pump; 9-right section of silicone tube; and (3) a 10-nitrogen cylinder (when the nitrogen cylinder is connected with the right section of the silicone tube, the port of the right section of the silicone tube is a nitrogen inlet for inputting nitrogen into the air chamber, and when the nitrogen cylinder is not connected with the right section of the silicone tube, the port of the right section of the silicone tube is an exhaust port).
Detailed Description
The invention is described below with reference to the accompanying drawing (fig. 1).
FIG. 1 is a schematic diagram of the layout of an apparatus for implementing a method for forming a single TCTS anti-relaxation coating in an alkali metal chamber according to the present invention. Referring to fig. 1, a method for manufacturing a single-layer TCTS anti-relaxation coating in an alkali metal gas chamber includes the following steps of placing a first container 5 with a TCTS solution 4 and an alkali metal gas chamber 1 with an inner wall subjected to hydroxylation in a heated state, placing a lower tail pipe 3 of the alkali metal gas chamber 1 in the TCTS solution 4, connecting an upper tail pipe 2 of the alkali metal gas chamber 1 to an air suction port of a left section 7 of a silicone tube of a peristaltic pump 8, using a port of a right section 9 of the silicone tube of the peristaltic pump 8 as an air exhaust port, starting the peristaltic pump 8 to enable the alkali metal gas chamber 1 to be fully filled with the TCTS solution 4, and forming a TCTS coating which is bonded to the inner wall of the gas chamber through a silicon-oxygen bond through a dehydration condensation reaction between TCTS molecules in the TCTS solution 4 and hydroxyl groups on the inner wall of the gas chamber. The solvent of the TCTS solution 4 is dicyclohexyl, the solute is TCTS, and the concentration of TCTS is 1 mM. The right section 9 of the silicone tube is provided with an exhaust port with a first valve and a nitrogen inlet with a second valve (for example, a three-way structure). After the peristaltic pump 8 enables the TCTS solution 4 to be fully absorbed by the alkali metal air chamber 1, the TCTS solution is stored in the alkali metal air chamber 1 for at least 3 hours, then the port 9 of the right section of the silicone tube is connected with the outlet of the nitrogen cylinder 10, nitrogen is pumped into the alkali metal air chamber 1 by the peristaltic pump 8, the TCTS solution in the alkali metal air chamber 1 is discharged into the first container 5 from the lower tail tube 3, the lower tail tube 3 is placed in the dicyclohexyl serving as a cleaning liquid after the TCTS solution in the alkali metal air chamber 1 is emptied, the inner wall of the alkali metal air chamber 1 is cleaned by the dicyclohexyl for 3-5 times by the nitrogen circularly pumped into the dicyclohexyl and the nitrogen cylinder 10, and the nitrogen is used for emptying the dicyclohexyl. The bicyclohexane is formulated in a second container. The heating state is realized by an oven 6, the alkali metal air chamber 1 and the first container 5 are both arranged in the oven 6, and the temperature in the oven 6 is 85 +/-2 ℃. A transverse section (for example, the upper part of the transverse section is bent rightwards) radially extends out of the side wall of the upper tail pipe 2, and the port of the transverse section is connected with a suction port of the left section 7 of the silicone tube (the suction port sucks gas in the air chamber through a peristaltic pump when TCTS solution is required to enter the air chamber, negative pressure is generated in the air chamber, however, when the air chamber is required to be filled with nitrogen, the suction port fills the nitrogen in a nitrogen bottle into the air chamber, the assisting air chamber empties the TCTS solution and fills the space in the air chamber with the nitrogen, and the like during cleaning operation). The hydroxylation treatment adopts a piranha solution (the piranha solution is a mixture of 98 mass percent of concentrated sulfuric acid and 30 mass percent of hydrogen peroxide solution, the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide solution is 7:3 or 3:1), an upper tail pipe 2 of an alkali metal gas chamber 1 is connected with a peristaltic pump, a lower tail pipe 3 of the alkali metal gas chamber 1 is placed in the piranha solution, the piranha solution is filled in the alkali metal gas chamber 1 through the peristaltic pump and is kept for not less than 1 hour, then the piranha solution is discharged by pumping nitrogen, after the piranha solution in the alkali metal gas chamber is emptied, the lower tail pipe is placed in deionized water, the deionized water is used for cleaning the inner wall of the alkali metal gas chamber 1 by using the deionized water in a circulating pumping manner, and the nitrogen is used for emptying the deionized water, and (3) placing the cleaned alkali metal gas chamber 1 in a vacuum oven for drying, and filling nitrogen into the vacuum oven for vacuum breaking (or using dry inert gas for vacuum breaking) when taking out the dried alkali metal gas chamber 1 from the vacuum oven. The first container is a beaker. The second container is a beaker.
A single-layer TCTS anti-relaxation coating in an alkali metal gas chamber is prepared by hydroxylating the interior of the gas chamber by piranha solution and drying in a vacuum oven. Before the air chamber is taken out of the vacuum oven, nitrogen is adopted to break vacuum instead of air, so that the inside of the alkali metal air chamber can not be attached with water molecules of the atmospheric environment, and the formation of a single-layer coating is ensured. Preparing 1mM of TCTS solution, placing the TCTS solution in a bicyclohexane solution, placing the solution 4 in an oven 6 at 85 ℃, dissolving TCTS, symmetrically distributing an upper tail pipe 2 and a lower tail pipe 3 in an alkali metal gas chamber 1, placing the lower tail pipe 3 in the TCTS solution 4, connecting the upper tail pipe 2 with a peristaltic pump 8 through a left section 7 of a silicone tube, and pouring the TCTS solution 4 into the alkali metal gas chamber 1 by adopting the peristaltic pump 8. And after the TCTS solution 4 is left in the alkali metal air chamber 1 for three hours, connecting the left section 7 of the silicone tube with the upper tail pipe 2 of the alkali metal air chamber 1, connecting the right section 9 of the silicone tube with the nitrogen cylinder 10, discharging the TCTS solution 4, and then cleaning the inside of the alkali metal air chamber 1 by adopting dicyclohexyl for 3-5 times.
A method for preparing a single-layer TCTS anti-relaxation coating is characterized by comprising the formation of the single-layer TCTS coating in an alkali metal gas chamber. The alkali metal gas cell has a curved upper tailpipe and a vertical lower tailpipe. When the dried alkali metal gas chamber in the vacuum oven is taken out, the vacuum is broken by adopting nitrogen. The solvent for the TCTS solution was dicyclohexyl and was 1 mM. And placing the alkali metal gas chamber and the TCTS solution in an oven at 85 ℃ to finish the coating manufacture. After the TCTS solution was removed, the solution inside the chamber was washed with dicyclohexyl in an oven at 85 ℃ as soon as possible. And the TCTS solution is discharged by adopting nitrogen and the used dicyclohexyl is cleaned, so that the adhesion of water molecules in the air on the inner wall of the air chamber is avoided, and a cross-linked coating is further formed. The method is simple and feasible to operate, a single-layer TCTS coating is formed, no anhydrous external environment is required to be created, the coating manufacturing flow can be effectively accelerated on the premise of effectively ensuring the coating manufacturing consistency, and the coating manufacturing difficulty is reduced.
It is pointed out here that the above description is helpful for the person skilled in the art to understand the invention, but does not limit the scope of protection of the invention. Any such equivalents, modifications and/or omissions as may be made without departing from the spirit and scope of the invention may be resorted to.
Claims (10)
1. A single-layer TCTS anti-relaxation coating manufacturing method in an alkali metal gas chamber is characterized by comprising the following steps of putting a first container with a TCTS solution and the alkali metal gas chamber with the inner wall subjected to hydroxylation in a heated state, putting a lower tail pipe of the alkali metal gas chamber in the TCTS solution, connecting an upper tail pipe of the alkali metal gas chamber with a left section air suction port of a silicone tube of a peristaltic pump, starting the peristaltic pump to enable the alkali metal gas chamber to be fully filled with the TCTS solution, and enabling TCTS molecules in the TCTS solution and hydroxyl on the inner wall of the gas chamber to form a TCTS coating which is combined with the inner wall of the gas chamber through a silicon-oxygen bond through dehydration condensation reaction;
the TCTS is triacontyltrichlorosilane.
2. The method for preparing a single-layer TCTS anti-relaxation coating in an alkali metal gas chamber as claimed in claim 1, wherein the solvent of the TCTS solution is dicyclohexyl, the solute is TCTS, and the concentration of TCTS is 1 mM.
3. The method for preparing single-layer TCTS anti-relaxation coating in alkali metal gas chamber as claimed in claim 1, wherein the right section of silicone tube is provided with an exhaust port with a first valve and a nitrogen inlet port with a second valve.
4. The method for preparing a single-layer TCTS anti-relaxation coating in an alkali metal gas chamber according to claim 1, wherein the TCTS solution is fully absorbed by the alkali metal gas chamber through the peristaltic pump, the TCTS solution is remained in the alkali metal gas chamber for not less than 3 hours, then the right end of the silicone tube is connected with the outlet of a nitrogen gas bottle, nitrogen is pumped into the alkali metal gas chamber through the peristaltic pump, the TCTS solution in the alkali metal gas chamber is discharged into the first container from the lower tail tube, the lower tail tube is placed in the dicyclohexyl serving as a cleaning solution after the TCTS solution in the alkali metal gas chamber is emptied, and the inner wall of the alkali metal gas chamber is cleaned with the dicyclohexyl for 3-5 times through the nitrogen circularly pumped into the dicyclohexyl and the nitrogen gas bottle, wherein the nitrogen is used for emptying the dicyclohexyl.
5. The method of claim 4, wherein the dicyclohexyl is dispensed in a second container as a cleaning solution.
6. The method of claim 1, wherein said heating is performed in an oven, said alkali gas chamber and said first container are both placed in said oven, and the temperature in said oven is 85 ℃ ± 2 ℃.
7. The method for preparing a single-layer TCTS anti-relaxation coating in an alkali metal gas chamber as claimed in claim 1, wherein a transverse section extends from the side wall of the upper tail tube in the radial direction, and the port of the transverse section is connected with the air suction port of the left section of the silicone tube.
8. The method for preparing the single-layer TCTS anti-relaxation coating in the alkali metal gas chamber according to claim 1, wherein the hydroxylation treatment is performed by using a piranha solution, an upper tail pipe of the alkali metal gas chamber is connected with a peristaltic pump, a lower tail pipe of the alkali metal gas chamber is placed in the piranha solution, the piranha solution is filled in the alkali metal gas chamber and is kept for not less than 1 hour, then the piranha solution is discharged by pumping nitrogen, the piranha solution in the alkali metal gas chamber is discharged, the lower tail pipe is placed in deionized water, the inner wall of the alkali metal gas chamber is cleaned by using the deionized water by circularly pumping the deionized water and the nitrogen, the nitrogen is used for discharging the deionized water, the cleaned alkali metal gas chamber is placed in a vacuum oven to be dried, and when the dried alkali metal gas chamber is taken out of the vacuum oven, the nitrogen is firstly filled in the vacuum oven And (4) carrying out vacuum.
9. The method of making a single layer TCTS anti-relaxation coating in an alkali metal gas cell as claimed in claim 1, wherein said first container is a beaker.
10. The method of making a single layer TCTS anti-relaxation coating within an alkali metal gas cell as claimed in claim 5, wherein said second container is a beaker.
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