CN116832738A - Wire-discharge plasma device for removing structure guiding agent - Google Patents
Wire-discharge plasma device for removing structure guiding agent Download PDFInfo
- Publication number
- CN116832738A CN116832738A CN202310533764.6A CN202310533764A CN116832738A CN 116832738 A CN116832738 A CN 116832738A CN 202310533764 A CN202310533764 A CN 202310533764A CN 116832738 A CN116832738 A CN 116832738A
- Authority
- CN
- China
- Prior art keywords
- metal electrode
- molecular sieve
- zeolite molecular
- wire
- voltage pulse
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000002184 metal Substances 0.000 claims abstract description 52
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 51
- 239000010457 zeolite Substances 0.000 claims abstract description 51
- 239000002808 molecular sieve Substances 0.000 claims abstract description 43
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 239000010409 thin film Substances 0.000 claims abstract 2
- 238000000034 method Methods 0.000 abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000003889 chemical engineering Methods 0.000 abstract description 2
- 230000004907 flux Effects 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- 239000010408 film Substances 0.000 abstract 1
- 239000012528 membrane Substances 0.000 description 8
- 239000000758 substrate Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma Technology (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention belongs to the technical field of preparation of chemical engineering zeolite molecular sieves, and discloses a wire-discharge plasma device for removing a structure directing agent. Adopting a parallel plane metal electrode structure, wherein one metal electrode covers an insulating medium and is grounded, and the other metal electrode is connected with the positive electrode of the microsecond high-voltage pulse power supply and the surface of the metal electrode is completely exposed; an atmospheric air gap is formed between the two metal electrodes; placing a sample to be treated on a metal electrode covered with an insulating medium; a microsecond high voltage pulse is applied between the two metal electrodes to generate a wire-discharge plasma, depending on the air gap and the thickness of the zeolite molecular sieve thin film layer. The invention can generate plasma wires in the atmosphere air environment, and the discharge pulse current reaches 3-8 amperes; the structure guiding agent in the zeolite molecular sieve can be removed within 10 minutes, so that the nitrogen flux reaches 10 ‑ 6 mol·m ‑2 ·s ‑1 ·Pa ‑1 The above; the molecular sieve film is not locally broken in the treatment process.
Description
Technical Field
The invention relates to the technical field of preparation of chemical engineering zeolite molecular sieves, in particular to a wire-discharge plasma device for removing a structure guiding agent.
Background
Zeolite is a microporous aluminosilicate crystal, a good molecular sieve, and is widely used in molecular separation, chemical catalysis and low-k dielectric materials. Typically, zeolite molecular sieve membranes are prepared on the surface of a carrier substrate, which requires the addition of a structure directing agent to form micropores for a particular application. After the zeolite film is prepared, the structure guiding agent remains in the holes of the zeolite film to block the holes, and the structure guiding agent in the zeolite film must be removed by adopting a proper method. The most commonly used method for removing the structure directing agent from the zeolite membrane is calcination: the prepared zeolite film is put into an oven and calcined at a high temperature of 400 to 600 degrees celsius for a period of hours or even days. Not only is the calcination process energy and time consuming, but it is also prone to localized cracking of the zeolite membrane due to differences in thermal expansion coefficients between the substrate and the membrane. When the zeolite film is used as a catalytic material, micropores do not need to be completely penetrated, only the structure guiding agent on the surface of the zeolite film is removed, and the local cracks of the zeolite film do not influence the catalytic performance. The zeolite film is used as a catalytic material, and some other methods have been discussed to remove the surface structure directing agent, such as ozone treatment, uniform dielectric barrier discharge plasma treatment, and ultraviolet assisted treatment. However, when zeolite membranes are used as molecular sieves for molecular separation, it is necessary to completely penetrate the micropores, and local cracks caused by calcination treatment may cause the zeolite molecular sieves to degrade or even lose molecular separation properties. Therefore, there is a need to develop a method for rapidly removing the structure directing agent in the pores of the zeolite molecular sieve membrane with low energy consumption and capable of inhibiting local cracking of the zeolite membrane.
Disclosure of Invention
The invention provides a wire-discharge plasma device for removing a structure guiding agent, which can be used for removing the structure guiding agent in a planar carrier zeolite molecular sieve film. And a parallel planar metal electrode structure is adopted, wherein one metal electrode is covered with an insulating medium and grounded, and the other metal electrode is completely exposed in surface and is connected with the positive electrode of the microsecond high-voltage pulse power supply. An atmospheric air gap is formed between the electrodes, a zeolite molecular sieve sample of the planar carrier to be treated is placed on the metal electrode covered with the insulating medium, and the distance between the surface of the sample and the surface of the exposed metal electrode is 1-4 mm. And microsecond high-voltage pulse is applied between the two metal electrodes to generate wire discharge plasma, the zeolite molecular sieve of the planar carrier is treated, and the structure guiding agent in the zeolite molecular sieve film is removed, so that micropores in the zeolite molecular sieve are communicated, and the zeolite molecular sieve has molecular separation performance.
The technical scheme adopted by the invention is as follows: a wire-discharge plasma device for removing structure directing agent comprises a metal electrode a1, a metal electrode b6 and a microsecond high-voltage pulse power supply 7; the metal electrode a1 and the metal electrode b6 form a parallel plane metal electrode structure, and are placed in an atmospheric air environment at a certain distance to form an atmospheric air gap 2 with a certain thickness; the metal electrode b6 covers the insulating medium 5 and is grounded after being connected with the negative electrode of the microsecond high-voltage pulse power supply 7 in parallel; the surface of the metal electrode a1 is completely exposed and is connected with the positive electrode of the microsecond high-voltage pulse power supply 7; placing a zeolite molecular sieve sample 4 of a plane carrier to be treated on a metal electrode b 6; a microsecond high voltage pulse is applied between the metal electrode a1 and the metal electrode b6 to generate wire discharge plasma 3, and the planar carrier zeolite molecular sieve sample 4 to be treated is treated.
The microsecond high voltage pulse is based on the thickness of the atmospheric air gap 2 and the thickness of the zeolite molecular sieve film layer of the zeolite molecular sieve sample 4 of the plane carrier to be treated, and the amplitude of the microsecond high voltage pulse is 15-40kV, and the frequency of the microsecond high voltage pulse is 200-1000Hz.
The distance between the upper surface of the to-be-treated planar carrier zeolite molecular sieve sample 4 and the lower surface of the metal electrode a1 is 1-4 mm.
The invention has the beneficial effects that: the wire-discharge plasma device for removing the structure directing agent can generate wire-discharge plasma in an atmospheric air environment, and the discharge pulse current can reach 3-8 amperes; the planar carrier zeolite molecular sieve film is treated, the structure guiding agent in the planar carrier zeolite molecular sieve can be removed within 10 minutes, the holes of the planar carrier zeolite molecular sieve are communicated, and the nitrogen flux reaches 10 -6 mol·m -2 ·s -1 ·Pa -1 The above; no local cracking of the molecular sieve membrane was caused during the 10 minutes treatment.
Drawings
Fig. 1 is a schematic diagram of a wire-discharge plasma device for removing a structure directing agent according to the present invention.
In the figure: 1-a metal electrode a; 2-atmosphere air gap; 3-wire discharge plasma; 4-a sample of the planar carrier zeolite molecular sieve to be treated; 5-an insulating medium; 6-metal electrode b; 7-microsecond high voltage pulse power supply.
Detailed Description
A wire-discharge plasma device for removing a structure guiding agent comprises two metal electrodes, an insulating medium 5 (quartz glass, acrylic or nylon and the like), an atmospheric air gap 2, a microsecond high-voltage pulse power supply 7 and a planar carrier zeolite molecular sieve film sample 4 to be treated; one of the metal electrodes b6 covers the insulating medium 5 and is grounded, the other metal electrode a1 is connected with the positive electrode of the microsecond high-voltage pulse power supply 7, and the surface of the metal electrode b is completely exposed; the two metal electrodes are placed in an atmospheric air environment at a certain distance to form an atmospheric air gap 2 with a certain thickness; the thickness of the atmospheric air gap 2 is adjusted according to the thickness of the zeolite molecular sieve film of the planar carrier to be treated, the zeolite molecular sieve sample 4 of the planar carrier to be treated is placed on the metal electrode b6 covered with the insulating medium 5, and the distance between the surface of the sample and the surface of the exposed metal electrode a1 is 1-4 mm; according to the thickness of the atmospheric air gap 2 and the thickness of the zeolite molecular sieve film layer, microsecond high-voltage pulse with the amplitude of 15-40kV and the frequency of 200-1000Hz is applied between two metal electrodes to generate wire discharge plasma 3, and the planar carrier zeolite molecular sieve film is processed.
The size specifications (diameter and thickness) of the planar carrier substrate used in the preparation of the zeolite molecular sieve film are different, and the thicknesses of the prepared film layers are also different. The following describes in detail embodiments of the present invention by taking as an example a practical sample of a molecular sieve film grown to a thickness of 1 μm on a planar carrier substrate of 18mm diameter and 1mm thickness, with reference to the technical scheme and the accompanying drawings. Other specifications of flat carrier zeolite molecular sieve samples can be implemented by appropriate adjustment with reference to the specific example.
Example 1
For an actual zeolite molecular sieve sample with a1 micron thick film grown on a planar carrier substrate of 18mm diameter and 1mm thickness, two metal electrodes of 12mm effective diameter were placed in an atmospheric air environment with a 4mm electrode spacing. The surface of the grounded metal electrode was covered with quartz glass having a diameter of 30mm and a thickness of 1 mm. An actual zeolite molecular sieve sample with a diameter of 18mm and a thickness of 1mm on which a1 μm thick film was grown on a planar carrier substrate was placed on quartz glass so that the distance between the zeolite molecular sieve film surface and the exposed metal electrode surface not covered with the insulating medium was 3mm. The bare metal electrode which is not covered with the insulating medium is connected with the anode of a microsecond high-voltage pulse power supply, microsecond high-voltage pulse with the amplitude of 28kV, the pulse width of 1 microsecond and the frequency of 500Hz is applied between the two metal electrodes, wire-shaped discharge plasma is generated in an atmospheric air gap between the electrodes, and the planar carrier zeolite molecular sieve sample is treated for 5-10 minutes according to the relative humidity of the atmospheric air, so that the removal of the structure guiding agent is completed.
Claims (3)
1. A wire-discharge plasma device for removing a structure directing agent, which is characterized by comprising a metal electrode a (1), a metal electrode b (6) and a microsecond high-voltage pulse power supply (7); the metal electrode a (1) and the metal electrode b (6) form a parallel plane metal electrode structure, and the metal electrode a and the metal electrode b are placed in an atmospheric air environment at a certain distance to form an atmospheric air gap (2) with a certain thickness; the metal electrode b (6) covers the insulating medium (5) and is grounded after being connected with the negative electrode of the microsecond high-voltage pulse power supply (7) in parallel; the surface of the metal electrode a (1) is completely exposed and is connected with the positive electrode of the microsecond high-voltage pulse power supply (7); placing a zeolite molecular sieve sample (4) of a plane carrier to be treated on a metal electrode b (6); and (3) applying microsecond high-voltage pulse between the metal electrode a (1) and the metal electrode b (6) to generate wire-discharge plasma, and treating the planar carrier zeolite molecular sieve sample (4) to be treated.
2. The wire-discharge plasma device for removing a structure directing agent according to claim 1, wherein the microsecond high voltage pulse is set to have an amplitude of 15-40kV and a frequency of 200-1000Hz according to the thickness of the atmospheric air gap (2) and the thickness of the zeolite molecular sieve thin film layer of the planar carrier zeolite molecular sieve sample (4) to be treated.
3. The wire-discharge plasma device for removing a structure directing agent according to claim 1 or 2, wherein the upper surface of the flat carrier zeolite molecular sieve sample (4) to be treated is spaced from the lower surface of the metal electrode a (1) by 1-4 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310533764.6A CN116832738A (en) | 2023-05-12 | 2023-05-12 | Wire-discharge plasma device for removing structure guiding agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310533764.6A CN116832738A (en) | 2023-05-12 | 2023-05-12 | Wire-discharge plasma device for removing structure guiding agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116832738A true CN116832738A (en) | 2023-10-03 |
Family
ID=88160546
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310533764.6A Pending CN116832738A (en) | 2023-05-12 | 2023-05-12 | Wire-discharge plasma device for removing structure guiding agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116832738A (en) |
-
2023
- 2023-05-12 CN CN202310533764.6A patent/CN116832738A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP3823037B2 (en) | Discharge plasma processing equipment | |
| EP2033207B1 (en) | Method for cleaning, etching, activation and subsequent treatment of glass surfaces, glass surfaces coated by metal oxides, and surfaces of other sio2-coated materials | |
| EP3442005B1 (en) | Method for manufacturing composite wafer provided with oxide single crystal thin film | |
| JP2010103455A (en) | Plasma processing apparatus | |
| US20060234472A1 (en) | Method and device for pre-treating surfaces of substrates to be bonded | |
| JP2005523584A5 (en) | ||
| CN116832738A (en) | Wire-discharge plasma device for removing structure guiding agent | |
| JP2002237463A (en) | Manufacturing method and device of semiconductor element | |
| JP2007080898A (en) | Electrostatic chuck, thin-film manufacturing apparatus provided therewith, thin-film manufacturing method, and substrate surface treatment method | |
| JP2003133291A (en) | Discharge plasma treatment apparatus and discharge plasma treatment method using it | |
| JP2000068252A (en) | Apparatus and method of plasma treatment | |
| EA028651B1 (en) | Pair of electrodes for dielectric barrier discharge (dbd) plasma process | |
| JP2837700B2 (en) | Method for forming diamond-like thin film | |
| WO2002103770A1 (en) | Apparatus and method for cleaning the surface of a substrate | |
| JP4809973B2 (en) | Method and apparatus for manufacturing semiconductor device | |
| JP2003129246A (en) | Discharge plasma treatment apparatus | |
| US20070034155A1 (en) | Apparatus for processing substrate and apparatus for processing electron source substrate | |
| JPH05102068A (en) | Forming method for electrode of electronic device using diamond | |
| JPH1161404A (en) | Electrostatic attracting device, its production and working device using the same | |
| JP2013008770A (en) | Deposit cleaning method for film deposition apparatus | |
| JP4420116B2 (en) | Plasma processing apparatus and plasma processing method | |
| KR20130037447A (en) | Surface treatment method of polypropylene using plasma | |
| JPH05213695A (en) | Method for depositing thin diamond film | |
| WO2007114242A1 (en) | Method and apparatus for removing film on strip body by using plasma | |
| JP3251465B2 (en) | Plasma processing equipment for carbon film formation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |