CN109999851A - Selenizing stainless steel material and the preparation method and application thereof - Google Patents
Selenizing stainless steel material and the preparation method and application thereof Download PDFInfo
- Publication number
- CN109999851A CN109999851A CN201910377705.8A CN201910377705A CN109999851A CN 109999851 A CN109999851 A CN 109999851A CN 201910377705 A CN201910377705 A CN 201910377705A CN 109999851 A CN109999851 A CN 109999851A
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- Prior art keywords
- stainless steel
- selenizing
- steel material
- preparation
- selenium
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- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 74
- 239000010935 stainless steel Substances 0.000 title claims abstract description 70
- 239000000463 material Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000007789 sealing Methods 0.000 claims abstract description 11
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 7
- 239000011669 selenium Substances 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 230000015556 catabolic process Effects 0.000 claims abstract description 3
- 238000006731 degradation reaction Methods 0.000 claims abstract description 3
- 230000005518 electrochemistry Effects 0.000 claims abstract description 3
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 claims 1
- 239000010959 steel Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000010453 quartz Substances 0.000 description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 13
- 239000010963 304 stainless steel Substances 0.000 description 6
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000004575 stone Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229940075397 calomel Drugs 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 229910018162 SeO2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- JPJALAQPGMAKDF-UHFFFAOYSA-N selenium dioxide Chemical compound O=[Se]=O JPJALAQPGMAKDF-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000012795 verification Methods 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0573—Selenium; Compounds thereof
-
- B01J35/33—
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
- C25B11/061—Metal or alloy
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a kind of preparation methods of selenizing stainless steel material, the following steps are included: stainless steel material and selenium source are added in heating container, 1~2h is calcined in sealing in an inert gas atmosphere, calcination temperature is 450~650 DEG C, obtains the selenizing stainless steel material.The invention also discloses the selenizing stainless steel material as well as electrolysis water that are prepared by the method, electrochemistry formated, degradation of organic substances catalyst application.It is poor, at high cost to solve the problems, such as that the preparation of current selenizing stainless steel electrode expends raw material, selenizing efficiency for the preparation method of selenizing stainless steel material of the invention.
Description
Technical field
The present invention relates to electrolysis water catalyst technical fields, and in particular to a kind of selenizing stainless steel material and preparation method thereof
And application.
Background technique
With the continuous development of society, the extensive concern of people has been obtained for energy demand and problem of environmental pollution.
Currently, the sharply reduction of fossil fuel and greenhouse effects bring great difficulty to the development of our mankind.Exploitation cleaning
Renewable energy is extremely urgent.And the energy of the Hydrogen Energy as clean and effective, while burning will not generate greenhouse effects, cause
The exploratory development energetically of people.There are many method of hydrogen making, and water electrolysis hydrogen production is due to product purity height, operation side
Just quick, while the advantages such as pollution are not likely to produce by the concern of people.
At present during electro-catalysis, there is also many problems for water electrolysis hydrogen production, and if overpotential is big, stability is poor, cost
It is higher.Since electrolysis water is to be made of two half-reactions of HER and OER, and OER needs to overcome biggish energy during the reaction
It builds, voltage needed for electrolysis water will be effectively reduced in the performance for improving OER electrode, significantly improve water electrolysis hydrogen production efficiency.So far,
Maximally efficient business OER catalyst be with Ru base (Chem.4.1-15.2019) and Ir base (Adv.Mater.2017,29,
1702385) compound formed.But the disadvantages of these noble metals are expensive, scarcity of resources and poor long-time stability is very
Large-scale commercial applications are hindered in big degree.Therefore, the OER catalyst for developing new and effective economy becomes especially to weigh
It wants.It has been widely studied currently based on the elctro-catalyst (Mn, Fe, Co and Ni) etc. of first row transition metal, oxide, hydrogen
Oxide and layered double-hydroxide have excellent performance, and a kind of material of the stainless steel as iron content nickel, production are simple
Just, cheap, while commercialization is had been carried out, it is modified, its OER catalytic performance is improved, to realize efficient electricity
Xie Shui provides selection.
Application No. is the Chinese patents of CN106268876A to disclose a kind of selenizing stainless steel foam electrolysis water catalysis material
Preparation method, be to calcine stainless steel foam substrate and selenium powder or selenate.But this preparation method compares
Consuming raw material, selenizing efficiency are poor, and the performance of obtained catalysis electrode is also bad.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation methods of selenizing stainless steel material, to solve current selenium
The preparation for changing stainless steel electrode expends raw material, the problem that selenizing efficiency is poor, at high cost.
In order to solve the above-mentioned technical problems, the present invention provides a kind of preparation methods of selenizing stainless steel material, including with
Lower step:
Stainless steel material and selenium source are added in heating container, sealing, calcine 1~2h, calcining in an inert gas atmosphere
Temperature is 450~650 DEG C, obtains the selenizing stainless steel material.
In preferred embodiments of the present invention, the stainless steel is 316 stainless steels, 316L stainless steel or 304 stainless steels.
In preferred embodiments of the present invention, the stainless steel material is sheet or netted.
In preferred embodiments of the present invention, the selenium source is selenium powder, selenate or seleno oxide, and the seleno oxide can be
SeO2。
In preferred embodiments of the present invention, the heating container is quartz boat, energy high temperature resistant, and stability at high temperature
It is good, it does not react with stainless steel or selenium powder.
In preferred embodiments of the present invention, the amount of the selenium powder is 50~350mg.It is highly preferred that the amount of the selenium powder is
250g。
In preferred embodiments of the present invention, calcination temperature is 550 DEG C, calcination time 1h.
In present pre-ferred embodiments, the sealing specifically: vacuum sealing tube machine is sealed or used using graphite plate
It is sealed under protection of liquid nitrogen.
Another aspect of the present invention additionally provides the selenizing stainless steel material being prepared by the method.
In addition, the present invention also provides the selenizing stainless steel material as electrolysis water, electrochemistry formated, degradation it is organic
The application of the catalyst of object.
Beneficial effects of the present invention:
1, compared with prior art, the present invention is calcined by the way of sealing, and selenizing is high-efficient, and original is greatly saved
Material selenium source, reduces costs, efficient and economical, and is easy to industrialized production.
2, selenizing stainless steel electrode prepared by the present invention, the selenizing that catalytic performance is significantly better than existing method preparation are stainless
Steel electrode.3 2.3 × 3cm are used using method of the invention by experimental verification2Stainless steel be added 250mg selenium powder, institute
The OER performance of obtained selenizing stainless steel electrode 100mA/cm in 1MKOH2Under current density, overpotential is only 278mv；And
Existing patent uses 1cm2Selenizing stainless steel electrode prepared by 1g selenium powder is added in stainless steel, and OER performance is in 1M KOH
100mA/cm2Current density under, overpotential then needs 301mv.
Detailed description of the invention
Fig. 1 is the XRD diagram of selenizing stainless steel material prepared by embodiment 1；
Fig. 2 is the SEM figure of selenizing stainless steel material prepared by embodiment 1；
Fig. 3 is the stainless steel of non-selenizing, using selenizing stainless steel electro-catalysis material graphite plate sealing and prepared when blow-by
The OER performance comparison figure of material.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings and specific examples, so that those skilled in the art can be with
It more fully understands the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1
It is not 2.3 × 3cm by 3 Line Integrals2304 stainless steel materials and 250mg selenium powder be put into quartz boat, using stone
Black plate is fully sealed, and then quartz boat is put into tube furnace, and under nitrogen protection atmosphere, 1h is calcined at 550 DEG C, system
Obtain selenizing stainless steel material.
Using obtained selenizing stainless steel material as working electrode, carbon-point is to electrode, and calomel electrode is reference electrode, is adopted
The test of OER material property is carried out in 1M KOH with three-electrode system.The result shows that sealing selenizing stainless steel electrode is with excellent
Different production oxygen performance, in 100mA/cm2Current density under its overpotential only need 278mv, while stability is relatively good.
Embodiment 2
It is not 2.3 × 3cm by 3 Line Integrals2304 stainless steel materials and 250mg selenium powder be put into quartz boat, using stone
Black plate is fully sealed, and then quartz boat is put into tube furnace, and under nitrogen protection atmosphere, 1h is calcined at 600 DEG C, system
Obtain selenizing stainless steel material.In 100mA/cm2Current density under its overpotential only need 280mV.
Embodiment 3
It is not 2.3 × 3cm by 3 Line Integrals2304 stainless steel materials and 250mg selenium powder be put into quartz boat, using stone
Black plate is fully sealed, and then quartz boat is put into tube furnace, and under nitrogen protection atmosphere, 1h is calcined at 450 DEG C, system
Obtain selenizing stainless steel material.In 100mA/cm2Current density under its overpotential only need 318mV.
Embodiment 4
It is not 2.3 × 3cm by 3 Line Integrals2304 stainless steel materials and 100mg selenium powder be put into quartz boat, using stone
Black plate is fully sealed, and then quartz boat is put into tube furnace, and under nitrogen protection atmosphere, 1h is calcined at 550 DEG C, system
Obtain selenizing stainless steel material.In 100mA/cm2Current density under its overpotential only need 324mV.
Embodiment 5
It is not 2.3 × 3cm by 3 Line Integrals2304 stainless steel materials and 350mg selenium powder be put into quartz boat, using stone
Black plate is fully sealed, and then quartz boat is put into tube furnace, and under nitrogen protection atmosphere, 1h is calcined at 550 DEG C, system
Obtain selenizing stainless steel material.In 100mA/cm2Current density under its overpotential only need 285mV.
Comparative example
By 3 2.3 × 3cm2304 stainless steels and 250mg selenium powder be put into quartz boat, then quartz boat is put into tube furnace
In, under nitrogen protection atmosphere, 1h is calcined at 550 DEG C, selenizing stainless steel material is made.
Test and characterization
Fig. 1 is the XRD diagram of selenizing stainless steel material prepared by embodiment 1 and common 304 stainless steel.It can from figure
Out, selenium powder is reacted with stainless steel, generates new substance, produces new peak.While the skeleton structure of stainless steel is still
It is so intact.
Fig. 2 is the SEM figure of selenizing stainless steel material prepared by embodiment 1.It can be seen from the figure that the selenizing of preparation is stainless
Steel catalysis material is graininess.
It works using the selenizing stainless steel material that the stainless steel of non-selenizing, embodiment 1 and comparative example 1 obtain as oxygen is produced
Electrode, carbon-point are to electrode, and calomel electrode is reference electrode, and OER material property is carried out in 1M KOH using three-electrode system
Assessment.
Selenizing (comparative example) when Fig. 3 is the stainless steel of non-selenizing and seals (embodiment 1) and blow-by using graphite plate
The OER performance comparison figure of selenizing stainless steel electrocatalysis material prepared by stainless steel.The result shows that, stainless steel is good after selenizing in figure
In untreated stainless steel, while the selenizing stainless steel obtained after sealing is better than unencapsulated stainless steel.Seal the stainless steel of selenizing
In 100mA/cm2Current density under overpotential be only 278mv, the stainless steel of unsealing selenizing is 324mv.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention
It encloses without being limited thereto.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in the present invention
Protection scope within.Protection scope of the present invention is subject to claims.
Claims (8)
1. a kind of preparation method of selenizing stainless steel material, which comprises the following steps:
Stainless steel material and selenium source are added in heating container, 1~2h, calcination temperature are calcined in sealing in an inert gas atmosphere
It is 450~650 DEG C, obtains the selenizing stainless steel material.
2. the preparation method of selenizing stainless steel material as described in claim 1, which is characterized in that the stainless steel is not 316 not
Become rusty steel, 316L stainless steel or 304 stainless steels.
3. the preparation method of selenizing stainless steel material as described in claim 1, which is characterized in that the stainless steel material is piece
Shape is netted.
4. the preparation method of selenizing stainless steel material as described in claim 1, which is characterized in that the selenium powder is selenium powder, selenium
Hydrochlorate or seleno oxide.
5. the preparation method of selenizing stainless steel material as claimed in claim 4, which is characterized in that the amount of the selenium powder be 50~
350mg。
6. the preparation method of selenizing stainless steel material as described in claim 1, which is characterized in that the sealing specifically: make
It is sealed with graphite plate or is sealed under protection of liquid nitrogen using vacuum sealing tube machine.
7. the selenizing stainless steel material that the method as described in any one of claim 1~6 power is prepared.
8. selenizing stainless steel material as claimed in claim 7 as electrolysis water, electrochemistry formated, degradation of organic substances catalyst
Using.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910377705.8A CN109999851A (en) | 2019-04-30 | 2019-04-30 | Selenizing stainless steel material and the preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910377705.8A CN109999851A (en) | 2019-04-30 | 2019-04-30 | Selenizing stainless steel material and the preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109999851A true CN109999851A (en) | 2019-07-12 |
Family
ID=67176113
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910377705.8A Pending CN109999851A (en) | 2019-04-30 | 2019-04-30 | Selenizing stainless steel material and the preparation method and application thereof |
Country Status (1)
| Country | Link |
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| CN (1) | CN109999851A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114855209A (en) * | 2022-04-16 | 2022-08-05 | 苏州科技大学 | Stainless steel selenide/platinum composite electrode and preparation method and application thereof |
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Application publication date: 20190712 |