CN109160501A - The method for preparing transition metal phosphide with microwave plasma CVD - Google Patents
The method for preparing transition metal phosphide with microwave plasma CVD Download PDFInfo
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- CN109160501A CN109160501A CN201811314450.2A CN201811314450A CN109160501A CN 109160501 A CN109160501 A CN 109160501A CN 201811314450 A CN201811314450 A CN 201811314450A CN 109160501 A CN109160501 A CN 109160501A
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- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 24
- 150000003624 transition metals Chemical class 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000005268 plasma chemical vapour deposition Methods 0.000 title claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 27
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims abstract description 19
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims abstract description 9
- 239000000919 ceramic Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000002243 precursor Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 4
- 239000004575 stone Substances 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 229910002804 graphite Inorganic materials 0.000 abstract description 5
- 239000010439 graphite Substances 0.000 abstract description 5
- 239000002105 nanoparticle Substances 0.000 abstract description 4
- 238000012512 characterization method Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 abstract description 2
- 229910017052 cobalt Inorganic materials 0.000 description 13
- 239000010941 cobalt Substances 0.000 description 13
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- ZGDWHDKHJKZZIQ-UHFFFAOYSA-N cobalt nickel Chemical compound [Co].[Ni].[Ni].[Ni] ZGDWHDKHJKZZIQ-UHFFFAOYSA-N 0.000 description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 241000208340 Araliaceae Species 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 2
- 235000003140 Panax quinquefolius Nutrition 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003028 elevating effect Effects 0.000 description 2
- 235000008434 ginseng Nutrition 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- VAKIVKMUBMZANL-UHFFFAOYSA-N iron phosphide Chemical compound P.[Fe].[Fe].[Fe] VAKIVKMUBMZANL-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000259 microwave plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a kind of methods for preparing transition metal phosphide with microwave plasma CVD, include the following steps: that 1) the hydroxide precursor nanometer part of ceramic boat and transition metal equipped with sodium hypophosphite is put into together in cavity on graphite platform, closes the cavity and the cavity is vacuumized；2) it is passed through nitrogen to the cavity, microwave power is adjusted, to generate nitrogen plasma and phosphine plasma；3) flow for adjusting the nitrogen, is maintained at intracavitary air pressure within the scope of 15torr~23torr, and after above-mentioned plasmoid is stable and wraps up above-mentioned example reaction 0.5min~3min, reaction was completed, closes microwave source；4) cooling to the cavity, sample is taken out to get transition metal phosphide is arrived.Transition metal phosphide nano particle diameter prepared by the present invention is small, and crystallinity is high, this improves its catalytic performance and unfailing performance, conducive to the test and characterization of catalytic field, is conducive to study its electric catalyticing characteristic.
Description
Technical field
The present invention relates to field of nano material preparation, and in particular to prepares transition with microwave plasma CVD
The method of metal phosphide.
Background technique
Due to oil-fired quick reduction, Hydrogen Energy receives people as the sustainable energy of cleaning and widely pays close attention to.
However high performance catalyst for preparing hydrogen is usually therefore your non-gold to be developed using rare Pt class as the precious metal material of representative now
The catalyst for preparing hydrogen substitute of category is very important.With the continuous development of catalytic field, transition metal phosphide is due to it
The hydrogen manufacturing performance of stability and high efficiency and gradually attract attention, become the research focus of new material catalytic field, but
It is the problem that the generally existing nano particle diameter of transition metal phosphide for preparing at present is larger, crystallinity is lower, this restrict
The performance of its catalytic performance, unfailing performance also have to be hoisted.
Summary of the invention
To overcome deficiencies of the prior art, the present invention, which provides, a kind of uses microwave plasma CVD
The method for preparing transition metal phosphide, the small, crystallinity by the transition metal phosphide nano particle diameter of this method preparation
It is high.The invention is realized by the following technical scheme: preparing transition metal phosphide with microwave plasma CVD
Method includes the following steps:
1) the hydroxide precursor nanometer part of ceramic boat and transition metal equipped with sodium hypophosphite is put into cavity together
On interior graphite platform, closes the cavity and the cavity is vacuumized；
2) it is passed through nitrogen to the cavity, microwave power is adjusted, to generate nitrogen plasma and phosphine plasma；
3) flow for adjusting the nitrogen, is maintained at intracavitary air pressure within the scope of 15torr~23torr, to above-mentioned etc.
Gas ions are in stable condition and after wrapping up above-mentioned example reaction 0.5min~3min, and reaction was completed, close microwave source；
4) cooling to the cavity, sample is taken out to get transition metal phosphide is arrived.
Preferably, in step 1), the form of the sodium hypophosphite is solid, and being evacuated to vacuum degree is 0.5torr.
Preferably, in step 2), the microwave power is 400W, operating air pressure 17torr.
Preferably, in step 3), the flow of the nitrogen is 30sccm, the intracavitary air pressure be 18torr~
20torr。
Preferably, in step 4), the time of reaction is 1min~2min.
Compared with prior art, the invention has the advantages that
Using microwave plasma method phosphatization, since microwave energy density is big, power is high, and group has greater activity,
Efficiently quick phosphatization can be achieved.The advantage of the method is that phosphatization temperature is low, can quickly prepare, it can be achieved that multiple element
Phosphatization.In addition, plasma is covered on above sodium hypophosphite, provide enough temperature to sodium hypophosphite, plasma from
Heating mode drives sodium hypophosphite to generate phosphine plasma, can realize during the preparation process solid-state phosphorus source quickly to it is equal from
The transformation of daughter state.Due to the etching effect of plasma, have by transition metal phosphide sample surfaces prepared by this method
Porous characteristic, thus have relatively bigger specific surface area, so that the phosphide of this method preparation has compared with traditional
There is different surface state, transition metal phosphide nano particle diameter is small, and crystallinity is high, this improves its catalytic performance and can
By performance, conducive to the test and characterization of catalytic field, it is conducive to study its electric catalyticing characteristic.
Detailed description of the invention
Invention is further described in detail in the following with reference to the drawings and specific embodiments.
Fig. 1 is the XRD spectra of phosphatization cobalt prepared by the embodiment of the present invention 1；
Fig. 2 is the SEM figure of phosphatization cobalt prepared by the embodiment of the present invention 1；
Fig. 3 is the XRD spectra of phosphatization cobalt prepared by the embodiment of the present invention 2 and phosphatization cobalt nickel；
Fig. 4 is the alkaline hydrogen manufacturing electrocatalysis characteristic curve graph (alkali of phosphatization cobalt prepared by the embodiment of the present invention 2 and phosphatization cobalt nickel
Property solution be 1M KOH)；
Fig. 5 is the structural schematic diagram that the embodiment of the present invention prepares transition metal phosphide equipment therefor；.
Corresponding as follows, the 1- chip bench of each label in Fig. 5,2- sample introduction chamber door, 3- cavity, 4- air inlet, the pumping of 5- vacuum pump
Mouthful, 6- compressed rectangular waveguide, 7- quartz glass plate, 8- elevating mechanism.
Specific embodiment
The present invention is further described With reference to embodiment:
Following each embodiments prepare transition metal phosphide equipment therefor, as shown in figure 5, including chip bench 1, sample introduction chamber door
2 and cavity 3, chip bench 1 be located in cavity 3, chip bench 1 is mounted on elevating mechanism 8, cavity 3 be equipped with air inlet 4, vacuum
Pumping port 5, nitrogen are imported by air inlet 4, and vacuum pump bleeding point 5 is connected (for taking out in cavity 3 with vacuum pump by vacuum pipe
Air to vacuum), the top of cavity 3 is equipped with quartz glass plate 7, and (cavity 3 is circle, and the surface of cavity 3 is quartz glass
Plate 7), cavity 3 is connected by the upper half (7 top of quartz glass plate) with compressed rectangular waveguide 6, and compressed rectangular waveguide 6 and microwave are sent out
Raw device is connected (microwave energy that microwave generator generates is entered in cavity 3 by compressed rectangular waveguide 6 through quartz glass plate 7).Make
Used time, microwave is transmitted by rectangular waveguide and is coupled in the cavity, after gas enters cavity, is absorbed microwave energy excitation and is produced
Raw plasma simultaneously drives sodium hypophosphite to generate phosphine plasma.
Embodiment 1
The method that the present embodiment prepares phosphatization cobalt with microwave plasma CVD, comprising the following steps:
1) the hydroxide precursor nanometer sheet of ceramic boat and cobalt equipped with sodium hypophosphite solid (is grown in carbon cloth substrate
On) it is put into graphite platform center in cavity together, vacuum degree 0.5torr is evacuated to cavity.
2) it is passed through nitrogen to cavity, when cavity reaches certain air pressure, adjusts microwave power, inside cavity nitrogen gas is inhaled
It receives microwave and generates nitrogen plasma and phosphine plasma.Technological parameter: microwave power 400W, operating air pressure are
17torr。
3) nitrogen flow is adjusted, intracavitary air pressure is made to keep in a certain range, keeping plasmoid stable and being wrapped in
Example reaction is for a period of time.Technological parameter: nitrogen flow 30sccm, intracavitary air pressure are 18torr-20torr, and the reaction time is
1min-2min。
4) microwave source after reaction, is closed, it is cooling to cavity, sample is taken out, phosphatization cobalt is obtained.Technological parameter: cooling
Temperature is 100 DEG C.
The result tested to phosphatization cobalt obtained is as illustrated in fig. 1 and 2.By the phase structure of phosphatization cobalt obtained by with
Standard X-ray diffraction data pdf 29-0497 comparison, it was demonstrated that be phosphatization cobalt crystal.
Embodiment 2
The method that the present embodiment prepares phosphatization cobalt and phosphatization cobalt nickel with microwave plasma CVD, including it is following
Step:
1) the hydroxide precursor nanometer sheet of ceramic boat and cobalt nickel equipped with sodium hypophosphite solid (is grown in carbon cloth base
On bottom) it is put into graphite platform center in cavity together, vacuum degree 0.5torr is evacuated to cavity.
2) it is passed through nitrogen to cavity, when cavity reaches certain air pressure, adjusts microwave power, inside cavity nitrogen gas is inhaled
It receives microwave and generates nitrogen plasma and phosphine plasma.Technological parameter: microwave power 400W, operating air pressure are
17torr。
3) nitrogen flow is adjusted, intracavitary air pressure is made to keep in a certain range, keeping plasmoid stable and being wrapped in
Example reaction is for a period of time.Technological parameter: nitrogen flow 30sccm, intracavitary air pressure are 18torr-20torr, and the reaction time is
1min-2min。
4) microwave source after reaction, is closed, it is cooling to cavity, sample is taken out, transition metal phosphide is obtained.Technique ginseng
Number: cooling temperature is 100 DEG C.
The result tested to phosphatization cobalt obtained and phosphatization cobalt nickel is as shown in Figures 3 and 4.By the mutually knot of substance obtained
Structure with standard X-ray diffraction data pdf 29-0497 and pdf 71-2336 by comparing, it was demonstrated that for phosphatization cobalt and phosphatization cobalt nickel
Crystal.
Embodiment 3
The method that the present embodiment prepares iron phosphide with microwave plasma CVD, comprising the following steps:
1) by the hydroxide precursor nanometer rods (being grown in carbon cloth substrate) of ceramic boat and iron equipped with sodium hypophosphite
It is put into graphite platform center in cavity together, vacuum degree 0.5torr is evacuated to cavity.
2) it is passed through nitrogen to cavity, when cavity reaches certain air pressure, adjusts microwave power, inside cavity nitrogen and phosphatization
Hydrogen absorbs microwave and generates nitrogen plasma and phosphine plasma.Technological parameter: heating temperature is 300 DEG C, microwave function
Rate is 400W, operating air pressure 17torr.
3) nitrogen flow is adjusted, intracavitary air pressure is made to keep in a certain range, keeping plasmoid stable and being wrapped in
Example reaction is for a period of time.Technological parameter: nitrogen flow 30sccm, intracavitary air pressure are 18torr-20torr, and the reaction time is
1min-2min。
4) microwave source after reaction, is closed, it is cooling to cavity, sample is taken out, transition metal phosphide is obtained.Technique ginseng
Number: cooling temperature is 100 DEG C.
The present invention uses MPCVD method (MPECVD) for the first time, using producing after nitrogen adsorption microwave
Raw plasma and the interaction of sodium hypophosphite solid further generate phosphine plasma, and the plasma of generation carrys out phosphatization
The substrate of transition metal, to prepare the transition metal phosphide of high hydrogen manufacturing performance；The present invention utilizes solid for the first time
Sodium hypophosphite drives the sodium hypophosphite of solid-state phosphorus source to be converted to hydrogen phosphide etc. as phosphorus source, by the nitrogen plasma of microwave-excitation
The form of gas ions realizes phosphorus source by the transformation of solid-state to plasma state.
It should be understood that for those of ordinary skill in the art, it can be modified or changed according to the above description,
And all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Illustrative description is carried out to the invention patent above, it is clear that the realization of the invention patent is not by aforesaid way
Limitation, as long as use the invention patent method concept and technical solution carry out various improvement, or it is not improved will this
The conception and technical scheme of patent of invention directly apply to other occasions, are within the scope of the invention.
Claims (5)
1. the method for preparing transition metal phosphide with microwave plasma CVD, which is characterized in that including as follows
Step:
1) the hydroxide precursor nanometer part of ceramic boat and transition metal equipped with sodium hypophosphite is put into stone in cavity together
On disc, closes the cavity and the cavity is vacuumized；
2) it is passed through nitrogen to the cavity, microwave power is adjusted, to generate nitrogen plasma and phosphine plasma；
3) flow for adjusting the nitrogen, is maintained at intracavitary air pressure within the scope of 15torr~23torr, to above-mentioned plasma
Body is in stable condition and after wrapping up above-mentioned example reaction 0.5min~3min, and reaction was completed, closes microwave source；
4) cooling to the cavity, sample is taken out to get transition metal phosphide is arrived.
2. the form of the sodium hypophosphite is solid the method according to claim 1, wherein in step 1),
Being evacuated to vacuum degree is 0.5torr.
3. the method according to claim 1, wherein the microwave power is 400W, work gas in step 2)
Pressure is 17torr.
4. the method according to claim 1, wherein the flow of the nitrogen is 30sccm, institute in step 3)
The intracavitary air pressure stated is 18torr~20torr.
5. the method according to claim 1, wherein the time of reaction is 1min~2min in step 4).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811314450.2A CN109160501A (en) | 2018-11-06 | 2018-11-06 | The method for preparing transition metal phosphide with microwave plasma CVD |
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| CN201811314450.2A CN109160501A (en) | 2018-11-06 | 2018-11-06 | The method for preparing transition metal phosphide with microwave plasma CVD |
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|---|---|---|---|---|
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