CN108714626A - A kind of deep cooling asynchronous rolling method preparing noble metal nano-plate - Google Patents
A kind of deep cooling asynchronous rolling method preparing noble metal nano-plate Download PDFInfo
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- CN108714626A CN108714626A CN201810411571.2A CN201810411571A CN108714626A CN 108714626 A CN108714626 A CN 108714626A CN 201810411571 A CN201810411571 A CN 201810411571A CN 108714626 A CN108714626 A CN 108714626A
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- noble metal
- foil
- deep cooling
- lithium
- rolling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/40—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling foils which present special problems, e.g. because of thinness
Abstract
A kind of deep cooling asynchronous rolling method preparing noble metal nano-plate, lithium foil and noble metal foil are sheared into rectangularity, noble metal foil doubling, lithium foil has been coated completely, it is then placed in deep cooling box and is cooled down, it takes out and carries out deep cooling rolling, then doubling overlaps, and is put into deep cooling box and cools down again, further takes out and carries out deep cooling rolling, it repeats 10-20 times, high performance stratiform noble metal/Li metal composite foil is generated, then is cooled down again, using deep cooling asymmetrical rolling, it repeats, until rolled piece thickness is rolled to 5~20 μm, to obtain composite foil；Into the water by composite foil, single noble metal nano-plate is prepared, the present invention is plastically deformed using ultralow temperature, and binding force is relatively weak between lithium metal and metal noble metal, and intermetallic compound is formed to be difficult to.At the same time, in the case of using ultralow temperature, lithium metal all has good plasticity with metal noble metal, to realize that multi-pass is plastically deformed, using the chemical characteristic of lithium, prepares single noble metal nano-plate.
Description
Technical field
The invention belongs to metal material rolling technical field, more particularly to a kind of deep cooling preparing noble metal nano-plate is asynchronous
Milling method.
Background technology
As noble metal, nanometer sheet is with important application prospects in fields such as catalytic chemistries for gold, silver and platinum.Lithium gold
Category is known as new energy materials, is largely existed on earth, has been used as common material, in fields such as lithium batteries
It is used widely.For pure lithium material, in heating, wet environment, it may occur that oxidation is especially directly reacted with water, raw
At lithium hydroxide and hydrogen.
Mainly there is chemical synthesis process for the preparation method of the noble metal nano-plates such as gold, silver and platinum in the past.These methods
A large amount of chemical reagent is needed, pollution may be generated to environment.
Invention content
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of noble metal nano-plates of preparing
Deep cooling asynchronous rolling method,
For this problem, in conjunction with the noble metals such as gold, silver and platinum and lithium metal in ultralow temperature with good
Plastic deformation ability, applicants have invented the asynchronous ply rolling technology of deep cooling, can be used for preparing with noble metal (gold, silver or
Platinum) then into the water by lamellar composite foil/Li metal composite foil chemically reacted using lithium and water, produce hydrogen
Gas, to which the separation of noble metal (gold, silver either platinum) nanometer sheet to be prepared to the single noble metal (gold, silver or platinum) of high quality
Nanometer sheet.
The main object of the present invention is to prepare noble metal (gold, silver or platinum)/Li metal composite foil of high quality, should
Material is laminar composite, be noble metal/lithium/noble metal ... lithium/noble metal multilayer composite foil, the material, lithium with it is expensive
Compound between noble metal (gold, silver or platinum) lithium metal is not formed at metal (gold, silver either platinum) material interface.By the foil of preparation
Material into the water, is chemically reacted by lithium and water, prepares single noble metal nano-plate.
To achieve the goals above, the technical solution adopted by the present invention is：
A kind of deep cooling asynchronous rolling method preparing noble metal nano-plate, includes the following steps：
The first step：Using pure lithium and pure noble metal (gold, silver or platinum) foil as raw material；
Second step：Lithium foil and noble metal foil are sheared into rectangularity size；
Third walks：By noble metal foil doubling, lithium foil has been coated completely；
4th step：It is put into deep cooling box and is cooled down, it is 10 minutes cooling, realize that material temperature is uniformly cooled, deep cooling box
It is cooled down using nitrogen, cooling temperature range is -190 DEG C~-100 DEG C；
5th step：Material is taken out, is 50% or so progress deep cooling rolling with reduction ratio, after rolling, rolled piece temperature
<-50℃；
6th step：Band after rolling is subjected to doubling and is overlapped, is put into deep cooling box and cools down again, cooling time is in 3-
10 minutes；
7th step：Cooling material is subjected to deep cooling rolling again, reduction ratio maintains 50% or so；
The 6th step and the 7th step 10-20 times are repeated, high performance stratiform noble metal/Li metal composite foil is generated；
8th step：Stratiform noble metal/Li metal composite foil is put into deep cooling box and is cooled down again, cooling time is in 3-
10 minutes；
9th step：Using deep cooling asymmetrical rolling, friction speed ratio is 1.0~1.6, and roll reduction is 5~50%；
It repeats the 8th step and the 9th step obtains composite foil until rolled piece thickness is rolled to 5~20 μm；
Tenth step：Into the water by the composite foil of preparation, single noble metal nano-plate is prepared.
Thickness before the pure lithium foil rolling is 50-100 μm, and the thickness before pure noble metal foil rolling is 10-50 μm.
In the second step, the width of noble metal foil is identical as lithium foil, but one times that length is lithium foil；The third step
In, lithium foil is placed on noble metal foil, a broadside of lithium foil is aligned with a broadside of noble metal foil, by noble metal foil along long
The perpendicular bisector doubling for spending direction, has coated lithium foil completely.
Compared with prior art, the beneficial effects of the invention are as follows：
The cardinal principle of the present invention is to be plastically deformed using ultralow temperature, lithium metal and metal noble metal (gold, silver or platinum)
Between binding force it is relatively weak, to form intermetallic compound to be difficult to.At the same time, in the case of using ultralow temperature, lithium metal
Good plasticity is all had with metal noble metal (gold, silver or platinum), to realize that multi-pass is plastically deformed.Utilize the chemistry of lithium
Characteristic prepares single noble metal nano-plate.Fig. 1 show nano-noble metal (gold, silver or platinum)/Li metal composite insulating foil
The deep cooling asymmetrical rolling preparation flow figure of material.It is accumulated and is rolled by multi-pass deep cooling, rolled piece forms the noble metal of layer structure
(gold, silver or platinum)/Li metal composite foil.
Pure noble metal (gold, silver or platinum) and pure lithium material are suitble to using deep cooling ply rolling technology at present.Using the technology, at
Work(it is prepared for noble metal (gold, silver or platinum)/Li metal composite foil.Using the composite foil, prepare single expensive
Metal nano plate, the noble metal nano-plate have broad prospect of application in fields such as catalytic chemistry, biological medicines.
Description of the drawings
Fig. 1 show the deep cooling rolling preparation flow figure of nano lamellar noble metal/Li metal composite foil.
In figure, 1. noble metal foils；2. lithium foil；3. stacking noble metal/lithium composite foil；4. first stage deep cooling box uses
Nitrogen cools down, and temperature is controlled at -190 DEG C to -100 DEG C；5. the noble metal of subzero treatment/lithium composite foil；6. your gold of rolling
Category/lithium composite foil；7. topping roll；8. bottom roll；9. second stage deep cooling box；10. stratiform noble metal/Li metal composite insulating foil
Material；11. the noble metal of asymmetrical rolling/lithium composite foil；12. nitrogen gun, for realizing roll low temperature；13. asynchronous rolling machine
Topping roll；14. the bottom roll of asynchronous rolling machine.
Specific implementation mode
The embodiment that the present invention will be described in detail with reference to the accompanying drawings and examples.
The main object of the present invention is to prepare noble metal (gold, silver or platinum)/Li metal composite foil of high quality, should
Material is laminar composite, be noble metal/lithium/noble metal ... lithium/noble metal multilayer composite foil, the material, lithium with it is expensive
Compound between noble metal (gold, silver or platinum) lithium metal is not formed at metal (gold, silver either platinum) material interface.By the foil of preparation
Material into the water, is chemically reacted by lithium and water, prepares single noble metal nano-plate.
As shown in Figure 1, the specific process step of the present invention is as follows：
The first step：Using pure lithium and pure noble metal (gold, silver or platinum) metal foil as raw material, the thickness before the rolling of lithium foil 2
It it is 50-100 μm, the thickness before noble metal foil 1 rolls is 10-50 μm.
Second step：Noble metal foil 1 and lithium foil 2 are sheared into rectangularity size, the width of noble metal foil 1 is identical as lithium foil 2,
But one times that length is lithium foil 2.
Third walks：Lithium foil 2 is placed on noble metal foil 1, a broadside of lithium foil 2 and a broadside pair of noble metal foil 1
Together, the perpendicular bisector doubling by noble metal foil 1 along its length, has coated lithium foil 2 completely, obtains stacking noble metal/lithium composite insulating foil
Material 3.
4th step：Noble metal/lithium composite foil 3 will be stacked to be put into first stage deep cooling box 4 and cool down, it is 10 points cooling
Clock realizes that material temperature is uniformly cooled, obtains noble metal/lithium composite foil 5 of subzero treatment, first stage deep cooling box 4 is adopted
It is cooled down with nitrogen, cooling temperature range is -190 DEG C~-100 DEG C；
5th step：The noble metal of subzero treatment/lithium composite foil 5 is taken out, using topping roll 7 and bottom roll 8, with pressure
Rate is 50% or so progress deep cooling rolling, after rolling, rolled piece temperature<- 50 DEG C, the noble metal rolled/lithium composite insulating foil
Material 6.
6th step：The noble metal of rolling/lithium composite foil 6 is subjected to doubling along rolling direction and is overlapped, the first rank is put into
It is cooled down again in section deep cooling box 4, cooling time was at 3-10 minutes.
7th step：Cooling material is subjected to deep cooling rolling again, reduction ratio maintains 50% or so.
The 6th step and the 7th step 10-20 times are repeated, high performance stratiform noble metal/Li metal composite foil is generated
10。
8th step：Stratiform noble metal/Li metal composite foil 10 is put into second stage deep cooling box 9 and is cooled down again,
Cooling temperature range is -190 DEG C~-100 DEG C, and cooling time was at 3-10 minutes.
9th step：It takes out stratiform noble metal/Li metal composite foil 10 and carries out deep cooling asymmetrical rolling, friction speed ratio is 1.0
~1.6, roll reduction is 5~50%, obtains noble metal/lithium composite foil 11 of asymmetrical rolling.Before asymmetrical rolling, it need to adopt
It is cooled down with the bottom roll 14 of topping roll 13 and asynchronous rolling machine that nitrogen gun 12 is asynchronous rolling machine, to ensure deep cooling effect.
The 8th step and the 9th step are repeated, until rolled piece thickness is rolled 5~20 μm.
Tenth step：Into the water by the composite foil of preparation, single noble metal (gold, silver or platinum) nanometer is prepared
Piece.
The nanometer sheet is large-sized metal nano plate, has the foreground applied in fields such as catalytic chemistry, bio-pharmaceuticals.
It is two concrete cases of the present invention below.
Application case 1：
Prepared by gold-nano-piece deep cooling asymmetrical rolling, steps are as follows：
The first step：Using lithium foil and goldleaf as raw material, the thickness before lithium rolling is 50 μm, and noble metal (gold, silver or platinum) rolls
Thickness before system is 25 μm.
Second step：Goldleaf and lithium foil are sheared into rectangularity size, the width of goldleaf is identical as lithium foil, still, goldleaf
Length is one times of lithium foil.
Third walks：By goldleaf doubling along its length, lithium foil has been coated completely.
4th step：Material is put into deep cooling box and is cooled down, it is 10 minutes cooling, realize material temperature by uniformly cold.It is deep
Ice chest is cooled down using nitrogen, and cooling temperature range is -150 DEG C.
5th step：Material is taken out, is 50% or so progress deep cooling rolling with reduction ratio.After rolling, rolled piece temperature
<-50℃。
6th step：Band after rolling is subjected to doubling along rolling direction and is overlapped, is put into deep cooling box and cools down again, it is cold
But the time was at 5 minutes.
7th step：Cooling material is subjected to deep cooling rolling again, reduction ratio maintains 50% or so.
The 6th step and the 7th step 15 times are repeated, stratiform gold/Li metal composite foil is generated.
8th step：Composite foil after rolling is put into deep cooling box and is cooled down again, cooling time was at 5 minutes.
9th step：Using deep cooling asymmetrical rolling, friction speed ratio is 1.5, roll reduction 30%.
The 8th step and the 9th step are repeated, until rolled piece thickness is rolled 10 μm.
Tenth step：Into the water by the composite foil of preparation, single gold-nano-piece is prepared.Pass through above-mentioned technique, system
The average thickness of standby gold-nano-piece is 1nm.
Application case 2
Prepared by Nano silver piece deep cooling asymmetrical rolling, steps are as follows：
The first step：Using lithium foil and silver foil as raw material, the thickness before lithium rolling is 100 μm, your silver belongs to (silver, silver or platinum) and rolls
Thickness before system is 30 μm.
Second step：Silver foil and lithium foil are sheared into rectangularity size, the width of silver foil is identical as lithium foil, still, silver foil
Length is one times of lithium foil.
Third walks：By silver foil doubling along its length, lithium foil has been coated completely.
4th step：Material is put into deep cooling box and is cooled down, it is 8 minutes cooling, realize material temperature by uniformly cold.Deep cooling
Case is cooled down using nitrogen, and cooling temperature range is -190 DEG C.
5th step：Material is taken out, is 50% or so progress deep cooling rolling with reduction ratio.After rolling, rolled piece temperature
<-50℃。
6th step：Band after rolling is subjected to doubling along rolling direction and is overlapped, is put into deep cooling box and cools down again, it is cold
But the time was at 8 minutes.
7th step：Cooling material is subjected to deep cooling rolling again, reduction ratio maintains 50% or so.
The 6th step and the 7th step 14 times are repeated, the double silver of stratiform silver/lithium is generated and belongs to composite foils.
8th step：Composite foil after rolling is put into deep cooling box and is cooled down again, cooling time was at 5 minutes.
9th step：Using deep cooling asymmetrical rolling, friction speed ratio is 1.3, roll reduction 25%.
The 8th step and the 9th step are repeated, until rolled piece thickness is rolled 8 μm.
Tenth step：Into the water by the composite foil of preparation, single Nano silver piece is prepared.Pass through above-mentioned technique, system
The average thickness of standby Nano silver piece is 1.8nm.
Claims (4)
1. a kind of deep cooling asynchronous rolling method preparing noble metal nano-plate, which is characterized in that include the following steps：
The first step：Using pure lithium and pure noble metal foil as raw material；
Second step：Lithium foil and noble metal foil are sheared into rectangularity；
Third walks：By noble metal foil doubling, lithium foil has been coated completely；
4th step：It is put into deep cooling box and is cooled down, it is 10 minutes cooling, realize that material temperature is uniformly cooled, deep cooling box uses
Nitrogen is cooled down, and cooling temperature range is -190 DEG C~-100 DEG C；
5th step：Material is taken out, is 50% or so progress deep cooling rolling with reduction ratio, after rolling, rolled piece temperature<-50
℃；
6th step：Band after rolling is subjected to doubling and is overlapped, is put into deep cooling box and cools down again, cooling time is at 3-10 points
Clock；
7th step：Cooling material is subjected to deep cooling rolling again, reduction ratio maintains 50% or so；
The 6th step and the 7th step 10-20 times are repeated, high performance stratiform noble metal/Li metal composite foil is generated；
8th step：Stratiform noble metal/Li metal composite foil is put into deep cooling box and is cooled down again, cooling time is at 3-10 points
Clock；
9th step：Using deep cooling asymmetrical rolling, friction speed ratio is 1.0~1.6, and roll reduction is 5~50%；
It repeats the 8th step and the 9th step obtains composite foil until rolled piece thickness is rolled to 5~20 μm；
Tenth step：Into the water by the composite foil of preparation, single noble metal nano-plate is prepared.
2. preparing the deep cooling asynchronous rolling method of noble metal nano-plate according to claim 1, which is characterized in that the pure lithium
Thickness before foil rolling is 50-100 μm, and the thickness before pure noble metal foil rolling is 10-50 μm.
3. preparing the deep cooling asynchronous rolling method of noble metal nano-plate according to claim 1, which is characterized in that described second
In step, the width of noble metal foil is identical as lithium foil, but one times that length is lithium foil；In the third step, your gold lithium foil is placed on
Belong on foil, a broadside of lithium foil is aligned with a broadside of noble metal foil, by the perpendicular bisector pair of noble metal foil along its length
Folding, has coated lithium foil completely.
4. preparing the deep cooling asynchronous rolling method of noble metal nano-plate according to claim 1, which is characterized in that your gold
Belong to is gold, silver or platinum.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109201740A (en) * | 2018-11-15 | 2019-01-15 | 中南大学 | A kind of multistage deep cooling milling method preparing high density twin medium entropy alloy |
| CN109576454A (en) * | 2018-12-19 | 2019-04-05 | 深圳先进技术研究院 | Preparation method, metal nano plate, purposes and the negative electrode active material of metal nano plate |
| CN110064658A (en) * | 2019-05-31 | 2019-07-30 | 哈尔滨工业大学 | A method of laminated hetero composite metal plate is prepared using from riveting pre-manufactured hole configuration rolling riveting |
| CN110396633A (en) * | 2019-05-20 | 2019-11-01 | 东北大学 | A kind of preparation method of the bimodal tissue medium entropy alloy of Ultra-fine Grained |
| WO2020124452A1 (en) * | 2018-12-19 | 2020-06-25 | 深圳先进技术研究院 | Method for preparing metal nanosheet, metal nanosheet, use, and negative electrode active material |
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| JPH1034205A (en) * | 1996-07-25 | 1998-02-10 | Kawasaki Steel Corp | Manufacture of metallic foil |
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| CN106670233A (en) * | 2016-12-20 | 2017-05-17 | 中南大学 | Cryogenic rolling method for preparing nanometer lithium aluminum bi-metal composite foil |
| CN107185963A (en) * | 2017-06-14 | 2017-09-22 | 中南大学 | A kind of method for preparing high performance Ti 6Al4V sheet alloys |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109201740A (en) * | 2018-11-15 | 2019-01-15 | 中南大学 | A kind of multistage deep cooling milling method preparing high density twin medium entropy alloy |
| CN109576454A (en) * | 2018-12-19 | 2019-04-05 | 深圳先进技术研究院 | Preparation method, metal nano plate, purposes and the negative electrode active material of metal nano plate |
| WO2020124452A1 (en) * | 2018-12-19 | 2020-06-25 | 深圳先进技术研究院 | Method for preparing metal nanosheet, metal nanosheet, use, and negative electrode active material |
| CN110396633A (en) * | 2019-05-20 | 2019-11-01 | 东北大学 | A kind of preparation method of the bimodal tissue medium entropy alloy of Ultra-fine Grained |
| CN110064658A (en) * | 2019-05-31 | 2019-07-30 | 哈尔滨工业大学 | A method of laminated hetero composite metal plate is prepared using from riveting pre-manufactured hole configuration rolling riveting |
| CN110064658B (en) * | 2019-05-31 | 2021-02-09 | 哈尔滨工业大学 | Method for preparing titanium-magnesium composite board through self-riveting prefabricated hole configuration rolling riveting |
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