CN105032385B - A kind of preparation method of metal oxide/Pt nanoparticle composite catalyst - Google Patents
A kind of preparation method of metal oxide/Pt nanoparticle composite catalyst Download PDFInfo
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- CN105032385B CN105032385B CN201510398455.8A CN201510398455A CN105032385B CN 105032385 B CN105032385 B CN 105032385B CN 201510398455 A CN201510398455 A CN 201510398455A CN 105032385 B CN105032385 B CN 105032385B
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Abstract
The invention discloses a kind of preparation method of metal oxide/Pt nanoparticle composite catalyst, this method includes:Platinum nano catalyst particle and metal oxide are grown using Atomic layer deposition method, by changing atomic layer deposition cycles number of times, so that the oxide composite layers and the nano particle of required particle diameter of thickness needed for depositing, both combine to form composite catalyst.Pass through the present invention, the composite catalyst of metal oxide and Pt nanoparticle can accurately be prepared, grappling metal catalysis particles are so as to improve the heat endurance of platinum catalyst at high temperature, and because sull and metal directly have catalyzing cooperation effect, the activity of catalyst can be improved while catalyst anti-agglutinatting property is improved.
Description
Technical field
The invention belongs to composite nano materials preparation field, more particularly, to a kind of metal oxide/Pt nanoparticle
The preparation method of composite catalyst.
Background technology
Catalyst has a wide range of applications and meaning in fields such as the energy, chemical industry, environmental protection.Used in actual catalyst
Cheng Zhong, there is the active reaction center that a big chunk catalyst has used nano particle as catalyst.Because nanometer
Grain typically has higher activity, and is supplied to the progress of catalytic reaction with great specific surface area.
Pt nanoparticle is mainly used in ammoxidation, oil hydrocarbon reforming, unsaturated compound oxidation and added as catalyst
The process such as removing of carbon monoxide, nitrogen oxides in hydrogen, gas, be chemistry, oil and chemical reaction process pass through frequently with one
Plant catalyst.With catalytic activity is high, strong, the easy to make, usage amount of selectivity is few, application field is wide, the features such as renewable.
But used for a long time under the continuous catalytic reaction condition for heating up and cooling, nano particle is easy to migrate
And fusion.The reunion for causing nano particle is grown up and reduces the surface area for being provided to catalytic reaction by this phenomenon, and this is
One main cause of catalyst inactivation.Therefore keep the stability of nano particle pattern and property that there is great value and meaning
Justice.
The main method of current stable nanoparticles catalyst is that metal oxide is added in noble metal nano particles, this
The sintering phenomenon of the nano particle of noble metal catalyst can effectively be suppressed.The method of some current traditional deposition films has
Vapour deposition, liquid deposition etc., compared with these methods, due to the noncontinuity and autoreactivity of atom layer deposition process
From restricted, this deposition process has great advantage in the control of film thickness and uniformity.There are some to grind
Study carefully the aluminum oxide film for attempting to coat one layer of infiltration in the nano grain surface of Metal Palladium using technique for atomic layer deposition, this can have
The sintering of noble metal nano particles is prevented to effect, but does not have the report of metal oxide cladding platinum catalyst also.In this catalysis
In agent system, the thickness and material of oxide skin(coating) are highly important.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of metal oxide/platinum nanometer
The preparation method of grain composite catalyst, its object is to improve the stability of Pt nanoparticle, thus solves Pt nanoparticle and exists
The unstable technical problem of property in use.
To achieve the above object, according to one aspect of the present invention, there is provided a kind of metal oxide/Pt nanoparticle is multiple
Close the preparation method of catalyst, it is characterised in that layer of metal oxide is first deposited in substrate using ald, then is sunk
Product one layer of Pt nanoparticle, or first deposit one layer of Pt nanoparticle, redeposited layer of metal oxide, metal oxide layer and
Pt nanoparticle collectively constitutes required composite catalyst;
Wherein, using metal organic salt and corresponding oxidant as reactant, by the circulation time for controlling ald
The metal oxide layer of thickness needed for number deposition;Reaction is used as using trimethyl (methyl cyclopentadienyl) platinum and oxygen or ozone
Thing, by controlling the cycle-index of ald to deposit the Pt nanoparticle of required particle diameter.
Preferably, it is characterised in that the particle diameter of Pt nanoparticle is 7nm~8nm, and the thickness of metal oxide is 0.9nm
~1.1nm.
Preferably, it is characterised in that the substrate is silicon chip.
Preferably, in the deposition of the metal oxide, the metal organic salt is cobaltocene, and the oxidant is smelly
Oxygen, reaction temperature is 150 DEG C~250 DEG C, and number of deposition cycles is 20~30 times.
Preferably, in the deposition of the metal oxide, the metal organic salt is trimethyl aluminium, and the oxidant is to go
Ionized water, reaction temperature is 70 DEG C~350 DEG C, and number of deposition cycles is 8~10 times.
Preferably, in the preparation of the Pt nanoparticle, reaction temperature is 280 DEG C~300 DEG C, and number of deposition cycles is 90
~110 times.
According to another aspect of the present invention, the metal oxide/Pt nanoparticle prepared in this way is additionally provided multiple
Close catalyst, it is characterised in that the catalytic oxidation for CO.
According to the preparation method of metal oxide/Pt nanoparticle composite catalyst of the present invention, have the following advantages that:
1st, composite catalyst is constituted using reactive metal oxides and nano-catalyst particles, on the one hand can reduces noble metal
Consumption, on the other hand can provide more reaction surfaces, play synergy in catalytic reaction, strengthen platinum catalyst
Low temperature active, improves cold starting performance;
2nd, activating oxide can make catalyst granules have good anti-sintering property, extend the life-span of catalyst,
Reduce use cost;
3rd, realized by adjusting the cycle-index of metal oxide atoms layer deposition to metal oxide layer film thickness
Accurate control, be conducive to improve nano particle catalytic performance.
Brief description of the drawings
Fig. 1 is the comparison that catalyst prepared by embodiment 1-2 and comparative example reacts medium velocity in catalysis CO;
Fig. 2 is the front and rear comparison that medium velocity is reacted in catalysis CO of sintering of catalyst prepared by embodiment 1 and comparative example;
Fig. 3 is the front and rear comparison that medium velocity is reacted in catalysis CO of sintering of catalyst prepared by comparative example and embodiment 3;
Fig. 4 is that the Pt nanocatalysts in comparative example sinter front and rear atomic force microscope images and apparent height curve;
Fig. 5 is the Pt/Co in embodiment 33O4Atomic force microscope images and surface before and after coated catalyst sintering are high
Write music line.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below
Not constituting conflict each other can just be mutually combined.
Embodiment 1Pt/Co3O4The preparation of base type catalyst
(1) it is 5 in the volume ratio of deionized water, ammoniacal liquor and hydrogen peroxide by silicon chip:1:Boiled in 1 mixed solution
20min, then dries up silicon chip using high pure nitrogen.
(2) silicon chip treated in (1) is put into atomic layer deposition apparatus;Using cobaltocene and ozone in silicon chip surface
Grow cobalt oxide.High purity oxygen gas (99.999%) is passed through in ozone generator and generates the ozone that volumetric concentration is about 11%).It is heavy
Cobalt precursor temperature is maintained at 100 DEG C during product.Reaction temperature is 150 DEG C.Carrier gas is still high pure nitrogen, cobalt precursor pulse
Time is 1.6s, and the ozone presoma burst length is 2s, and nitrogen scavenging period is 8s.25 circulations are repeated, are generated on silicon chip
Tricobalt tetraoxide film.
(3) sample of deposition peroxide film in (2) is put into atomic layer deposition apparatus, existed using platinum source and oxygen
Sample surfaces deposit Pt nanoparticle, and platinum source here is trimethyl (methyl cyclopentadienyl) platinum (IV).Whole atomic layer
High Purity Nitrogen (99.999%) is continually fed into during deposition reaction as carrier gas, the pressure in cavity is controlled in below 4mbar.It is former
The range of reaction temperature of sublayer deposition is 300 DEG C.To ensure enough vapour pressures, platinum source is heated to 65 DEG C;To prevent condensation, pipe
Road is heated to 80 DEG C, the platinum presoma burst length be in 1.6s, oxygen precursor arteries and veins the time be 2s, nitrogen scavenging period is
8s.100 circulations are repeated, that is, obtain required Pt/Co3O4Base type catalyst, the oxidation reaction available for catalysis CO.
Embodiment 2Pt/Al2O3The preparation of base type catalyst
Embodiment 1 is repeated with described same steps, difference is, the metal organic salt used in step (2) is front three
Base aluminium, oxidant is deionized water.Reaction temperature is 180 DEG C, and carrier gas is nitrogen, and the presoma burst length of two kinds of presomas is equal
For 0.1s, nitrogen scavenging period is 8s, and number of deposition cycles is 9 times, obtains Pt/Al2O3Base type catalyst, available for being catalyzed
The oxidation reaction of methanol or CO.
The preparation of comparative example Pt nanocatalysts
(1) repeat to implement 1 with described same steps.
(2) silicon chip treated in (1) is put into atomic layer deposition apparatus, it is heavy in silicon chip surface using platinum source and oxygen
Product Pt nanoparticle, platinum source here is trimethyl (methyl cyclopentadienyl) platinum (IV).Whole ald reacted
High Purity Nitrogen (99.999%) is continually fed into journey as carrier gas, the pressure in cavity is controlled in below 4mbar.Ald
Range of reaction temperature is 300 DEG C.To ensure enough vapour pressures, platinum source is heated to 65 DEG C;To prevent condensation, pipeline is heated to
80 DEG C, the platinum presoma burst length is 1.6s, and the time is 2s in oxygen precursor arteries and veins, and nitrogen scavenging period is 8s.Repeat 100 times
Circulation, obtains the superficial growth silicon chip of Pt nanocatalysts.
Embodiment 3Pt/Co3O4The preparation of coated catalyst
The silicon chip of superficial growth Pt nanocatalysts is put into atomic layer deposition apparatus in comparative example;Using cobaltocene and
Ozone is in Pt nanoparticle superficial growth cobalt oxide.High purity oxygen gas (99.999%) is passed through generation volume in ozone generator dense
The ozone of degree about 11%).Cobalt precursor temperature is maintained at 100 DEG C in deposition process.Reaction temperature is 150 DEG C.Carrier gas is still
High pure nitrogen, the cobalt precursor burst length is 1.6s, and the ozone presoma burst length is 2s, and nitrogen scavenging period is 8s.Repeat
25 circulations, generate tricobalt tetraoxide film on Pt nanoparticle, that is, obtain required Pt/Co3O4Coated catalyst, can
Oxidation reaction for being catalyzed CO.
Analysis of experimental results
Using plane catalysis test equipment respectively by the catalyst prepared in embodiment 1-2 and comparative example in catalysis CO reactions
It is middle to be analyzed that (silicon chip is cut into 10 × 20mm2Size), in this experiment used gas componant be 0.5%CO,
4.5%O2, remaining is Ar, and gas flow is stabilized it with MFC as 5sccm, to cavity where catalyst while being passed through gas
Heated, maximum temperature is 300 DEG C.CO conversion ratios and temperature curve are as shown in Figure 1, it can be seen that metal oxide
Base type catalyst is compared with Pt nanocatalysts, and its catalytic performance is greatly enhanced, wherein especially with Co3O4It is catalyzed during as substrate
Performance boost it is larger.
Pt/Co prepared by embodiment 1 and comparative example3O4Base type catalyst and Pt nanocatalysts are sintered at 750 DEG C
Analyzed after 2h with same method, experimental result is as shown in Figure 2.It can be seen that after sintering, the performance of two kinds of catalyst is equal
There are certain reduction, but Pt/Co3O4The performance of base type catalyst is still better than Pt catalyst.
Catalysis before and after the catalyst for again preparing embodiment 3 and comparative example is sintered can be tested, experimental result such as Fig. 3
It is shown, it can be seen that Pt/Co3O4The performance of coated catalyst improves a lot relative to Pt catalyst, is combined and urges after sintering
The performance of agent is also smaller by being influenceed.
The pattern on the surface before and after the sintering of catalyst prepared using atomic force microscope observation embodiment 3 and comparative example,
As a result Fig. 4-5 is seen.Wherein Fig. 4 a, b is the atomic force microscope images and apparent height before and after Pt nanocatalyst sintering processes
Curve;Fig. 5 a, b are Pt/Co3O4Atomic force microscope images and apparent height curve before and after coated catalyst sintering processes.
It can be seen that Pt nanocatalysts are after sintering, agglomeration is serious, and particle diameter becomes uneven, and Pt/Co3O4Cladded type is catalyzed
Particle diameter distribution after agent sintering is then without significant change, it was demonstrated that metal oxide clad greatly improves the thermally-stabilised of catalyst
Property.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, it is not used to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the invention etc., it all should include
Within protection scope of the present invention.
Claims (6)
1. the preparation method of a kind of metal oxide/Pt nanoparticle composite catalyst, it is characterised in that utilize ald
Layer of metal oxide, redeposited one layer of Pt nanoparticle are first deposited in substrate, or first deposits one layer of Pt nanoparticle, then
Layer of metal oxide is deposited, metal oxide layer and Pt nanoparticle collectively constitute required composite catalyst;
Wherein, using metal organic salt and corresponding oxidant as reactant, by controlling the cycle-index of ald to sink
The metal oxide of thickness needed for product;Using trimethyl (methyl cyclopentadienyl) platinum and oxygen or ozone as reactant, pass through
The Pt nanoparticle of particle diameter needed for controlling the cycle-index deposition of ald;
In the deposition of the metal oxide, the metal organic salt is cobaltocene, and reaction temperature is 150 DEG C~250 DEG C.
2. preparation method as claimed in claim 1, it is characterised in that the particle diameter of Pt nanoparticle is 7nm~8nm, metal oxidation
The thickness of thing is 0.9nm~1.1nm.
3. preparation method as claimed in claim 1, it is characterised in that the substrate is silicon chip.
4. preparation method as claimed in claim 1, it is characterised in that the oxidant is ozone, number of deposition cycles is 20~
30 times.
5. preparation method as claimed in claim 1, it is characterised in that in the deposition of the Pt nanoparticle, reaction temperature is 280
DEG C~300 DEG C, number of deposition cycles is 90~110 times.
6. a kind of metal oxide/Pt nanoparticle composite catalyst prepared with claim 4 methods described, its feature exists
In the catalytic oxidation for CO.
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