CN110092361A - A kind of preparation method and application of the black phosphorus material of hydroxyl modified - Google Patents
A kind of preparation method and application of the black phosphorus material of hydroxyl modified Download PDFInfo
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- CN110092361A CN110092361A CN201910327203.4A CN201910327203A CN110092361A CN 110092361 A CN110092361 A CN 110092361A CN 201910327203 A CN201910327203 A CN 201910327203A CN 110092361 A CN110092361 A CN 110092361A
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- black phosphorus
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- 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
- C01B25/003—Phosphorus
- C01B25/006—Stabilisation
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- 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
- C01B25/02—Preparation of phosphorus
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
Abstract
The invention discloses a kind of preparation method and application of the black phosphorus material for the hydroxyl modified for belonging to two-dimensional material technical field.It specifically includes step: rich hydroxyl inorganic matter and/or rich hydroxy alcohols organic matter is added in black phosphorus powder, through ball milling, washing, centrifugation, the dry black phosphorus material hydroxyl modified is made；Black phosphorus of the present invention is the ultra-fine black phosphorus powder that obtains through high speed ball milling using red phosphorus as raw material；The ball milling carries out under an inert atmosphere.It is preparation method simple process of the present invention, low in cost, easy to spread；Stability of the black phosphorus material produced by the present invention in air and water is strong, dispersing uniformity in water is strong, has extremely low coefficient of friction using the group water solution that the black phosphorus material of prepared hydroxyl modified configures.
Description
Technical field
The invention belongs to two-dimensional material technical field, in particular to the preparation method of the black phosphorus material of a kind of hydroxyl modified and
Using.
Background technique
Black phosphorus is most stable of a kind of form in the common three kinds of allotropes (red phosphorus, white phosphorus and black phosphorus) of phosphorus.Black phosphorus tool
Have with lamellar structure natural as graphite-like, by sp in layer3The phosphorus atoms of hydridization are connected with cellular shredded form, layer and layer
Between with weak Van der Waals force be connected.The unique structure of black phosphorus makes it have good incident photon-to-electron conversion efficiency, higher electron transfer
Rate and fabulous biocompatibility, in thin film transistor (TFT), photodetection, light-controlled electronic element, electroluminescent field, biomedicine
Field all has a good application prospect, however, black phosphorus is also relatively fewer in the application study of lubricating area, presently, there are profit
Sliding product coefficient of friction is generally 0.1 or so.
Currently, the price of black phosphorus is still sufficiently expensive, main cause is preparation condition harshness, and process costs are high.The biography of black phosphorus
Controlling Preparation Method is to use white phosphorus or red phosphorus for raw material, reacts preparation under high temperature (being higher than 200 DEG C) high pressure (being higher than 1.2GPa).
Just occurred preparing the report of black phosphorus in lower pressure, referred to as " mineralising method " about using mineralizer to be catalyzed until 2007.Mine
Change method is needed in preparation using Au, Sn and SnI4As mineralizer, although making the preparation cost of black phosphorus decrease, still
Higher than the cost requirement used as lubricant, the production cost for further decreasing black phosphorus is still one of vital task.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method and application of the black phosphorus material of hydroxyl modified, particular technique sides
Case is as follows:
A kind of preparation method of the black phosphorus material of hydroxyl modified, comprising steps of by rich hydroxyl inorganic matter and/or rich hydroxyl
Alcohol type organic is added in black phosphorus powder, through ball milling, washing, centrifugation, the dry black phosphorus material hydroxyl modified is made.
The black phosphorus powder is the ultra-fine black phosphorus powder that high speed ball milling obtains under an inert atmosphere using red phosphorus as raw material；
Alternatively, the black phosphorus powder is the ball milling under an inert atmosphere using black phosphorus block and/or black phosphorus crystal powder as raw material
Obtained ultra-fine black phosphorus powder.
The inert atmosphere is nitrogen, argon gas or helium.
The ball milling or high speed ball milling, which are able to achieve in the prior art in the device of ball milling or high speed ball milling, to carry out, such as in height
It can be carried out in ball grinder.
During preparing ultra-fine black phosphorus powder as raw material using red phosphorus, the red phosphorus purity is greater than 98.5%, partial size 0.1
~50 μm；In mechanical milling process, the mass ratio of steel ball and red phosphorus is 20:1~50:1；Drum's speed of rotation is 600~1200rpm, ball
Time consuming is 2~48h.
During preparing ultra-fine black phosphorus powder as raw material using black phosphorus block and/or black phosphorus crystal powder, the black phosphorus block
Body and/or black phosphorus crystal powder are commercially available, ball milling speed 200rpm.
The richness hydroxyl inorganic matter includes the one or two of NaOH, KOH；The richness hydroxyl inorganic powder and black phosphorus
Mass ratio be 1:1~4:1.
The richness hydroxy alcohols organic matter includes the one or two of monohydric alcohol, dihydric alcohol；The richness hydroxy alcohols are organic
The mass ratio of object and black phosphorus is 1:1~30:1.
The richness hydroxy alcohols organic matter includes methanol, ethyl alcohol, ethylene glycol, isopropanol, benzyl alcohol, 1,4- butanediol, gathers
One or more of ethylene glycol.
The ball milling of the richness hydroxyl inorganic matter and/or rich hydroxy alcohols organic matter and black phosphorus powder is in inert atmosphere such as nitrogen
It is carried out under gas, argon gas or helium, rotational speed of ball-mill is 600~1200rpm, and Ball-milling Time is 4~12h.
The washing uses methanol or dehydrated alcohol for detergent, to remove rich hydroxyl inorganic powder remaining in product
End.
The centrifugation is centrifuged using 10000~12000rpm takes deposit, repeated washing-centrifuge separation 1~3
It is secondary.
The drying mode is preferably dried in vacuo, and vacuum drying temperature is 40~60 DEG C.
The black phosphorus material of hydroxyl modified made from the preparation method, hydroxyl is by forming P-OH key with black phosphorus surface dangling bond
Modification is on black phosphorus surface.
Further, in mechanical milling process, black phosphorus surface defect increases, and black phosphorus surface dangling bond increases, in rich hydroxyl environment
In, hydroxyl modified forms P-OH key, obtains the black phosphorus material of hydroxyl modified in dangling bond.
The black phosphorus material of hydroxyl modified made from the preparation method can be placed 30 days in air, place 18 in water
It, no decomposition or other change of properties occur.
The black phosphorus material of hydroxyl modified made from the preparation method stable and uniform can disperse in aqueous solution.
The black phosphorus material of the hydroxyl modified is used to prepare thin-film-transistor material, the negative electrode material of battery, Flexible Displays
Material, LED material, optical switch material, biosensor material, optical dynamic therapy reagent or photo-thermal therapy reagent, water based lubrication
Additive.
The black phosphorus material of the hydroxyl modified is dissolved in deionized water, obtained group water solution is added as water based lubrication
Agent stablizes coefficient of friction and is not more than 0.01.
The invention has the benefit that
(1) it is initial feed that the present invention, which selects red phosphorus powder, in sealing ball grinder, by the high velocity impact of abrading-ball, is cut
It cuts, red phosphorus is promoted to be converted into black phosphorus, there is simple process, advantage low in cost, easy to spread；
(2) present invention is carried out using black phosphorus powder with the organic matter rich in hydroxyl inorganic matter or rich in alcohols hydroxyl secondary
High speed ball milling substitutes common ultrasonic disperse stripping means, on the one hand can be realized by high speed ball milling to the two of black phosphorus powder
On the other hand secondary refinement can be realized by hydroxyl or hydroxyl and be modified the hydroxylating of black phosphorus, improve black phosphorus material in air
With the stability in water, dispersing uniformity in water；
(3) there is ultralow coefficient of friction using the group water solution of the black phosphorus material configuration of the obtained hydroxyl modified of the present invention,
Stablize coefficient of friction less than 0.01；The black phosphorus material of hydroxyl modified i.e. of the present invention has important application as Water-based Lubricating Additives
Value has great potential on developing extremely low coefficient of friction water based lubrication liquid product, can effectively reduce the energy in friction process
Source consumption and the wasting of resources.
Detailed description of the invention
Attached drawing 1 is the XRD spectrum of powder obtained by red phosphorus original powder end and 1 step of embodiment (1) high-energy ball milling.
Specific embodiment
The present invention provides a kind of preparation method and application of the black phosphorus material of hydroxyl modified, with reference to the accompanying drawing and implement
The present invention is described further for example.
Embodiment 1
The black phosphorus material of hydroxyl modified is prepared as steps described below:
(1) weighing purity is 99%, and average grain diameter is that 7 μm of 2 grams of red phosphorus powder (about 1.8 yuan/gram of price) are put into high energy ball
Mass ratio, that is, ratio of grinding media to material of grinding jar ball milling, steel ball and red phosphorus is 30:1, is sealed after nitrogen is passed through in ball grinder, then opens
Begin to carry out ball milling, rotational speed of ball-mill 800rpm, every ball milling 1h ball mill suspends 20min, and Ball-milling Time is for 24 hours, after ball milling
Obtain ultra-fine black phosphorus powder.
(2) ball grinder in opening steps (1) in the glove box for being connected with nitrogen, is added 2g into ultra-fine black phosphorus powder
NaOH powder is sealed after being passed through nitrogen in ball grinder, is then placed in ball mill, starts second stage ball milling, and ball milling turns
Speed is 600rpm, Ball-milling Time 6h.
(3) after second stage ball milling, ball grinder is opened in glove box, ethanol solution is added, to step (2) ball milling
Product is washed, and is then centrifuged at 10000rpm, and basic sediment, repeated washing-centrifugal separation processes are taken
Three times, the powder after washing is finally dried in vacuo 12h at 40 DEG C of vacuum oven；The black of hydroxyl modified is obtained after drying
Phosphate material.
Fig. 1 is the XRD spectrum of ultra-fine black phosphorus powder obtained by red phosphorus original powder end and step (1) high-energy ball milling, and interior illustration is red
The digital photograph of phosphor powder and black phosphorus powder；Black phosphorus object phase is detected after ball milling in powder, the peak of its excess phase is not detected,
Show that black phosphorus can be prepared by red phosphorus by high-energy ball milling method, greatly reduces the production cost of black phosphorus.
The black phosphorus material of gained hydroxyl modified is dissolved in deionized water, configures the hydroxylating black phosphorus aqueous dispersion of 0.5mg/ml
Liquid carries out coefficient of friction detection, and abrading-ball is 4.76mm silicon nitride bead, and opposite grinding pair is quartz glass.The result shows that group water solution
Stabilization coefficient of friction less than 0.01.
Embodiment 2
The black phosphorus material of hydroxyl modified is prepared as steps described below:
(1) weighing purity is 99%, and average grain diameter is that 7 μm of 2 grams of red phosphorus powder (about 1.8 yuan/gram of price) are put into high energy ball
Grinding jar ball milling, ratio of grinding media to material 30:1 are sealed after being passed through nitrogen in ball grinder, then begin to carry out ball milling, rotational speed of ball-mill
For 800rpm, every ball milling 1h ball mill suspends 20min, Ball-milling Time 30h, obtains ultra-fine black phosphorus powder after ball milling.
(2) 10g second is added into ultra-fine black phosphorus powder for the ball grinder in opening steps (1) in the glove box for being connected with nitrogen
Glycol organic matter is sealed after being passed through nitrogen in ball grinder, is then placed in ball mill, starts second stage ball milling, ball milling
Revolving speed is 800rpm, Ball-milling Time 6h.
(3) after second stage ball milling, ball grinder is opened in glove box, methanol solution is added, to step (2) ball milling
Product is washed afterwards, is centrifuged at 10000rpm after washing, and bottom precipitation, repeated washing-centrifugation point are taken
Three times from step, 12h finally is dried in vacuo at 40 DEG C in a vacuum drying oven；The black phosphorus material of hydroxyl modified is obtained after drying
Material.
The black phosphorus material of gained hydroxyl modified is dissolved in deionized water, configures the hydroxylating black phosphorus aqueous dispersion of 1mg/ml
Liquid carries out coefficient of friction detection, and abrading-ball is 4.76mm silicon nitride bead, and opposite grinding pair is quartz glass.The result shows that group water solution
Stabilization coefficient of friction less than 0.01.
Embodiment 3
Using commercially available black phosphorus block or black phosphorus crystal powder as raw material, hydroxyl can be equally prepared using the method for the present invention
Change black phosphorus material, specifically prepare as steps described below:
(1) it weighs the black phosphorus powder commercially available from 1g and is put into high-energy ball milling tank ball milling, be sealed after being passed through nitrogen in ball grinder,
It then begins to carry out ball milling, obtains ultra-fine black phosphorus powder after rotational speed of ball-mill 200rpm, ball milling 2h.
(2) ball grinder in opening steps (1) in the glove box for being connected with nitrogen, is added 3g into ultra-fine black phosphorus powder
NaOH powder is sealed after being passed through nitrogen in ball grinder, is then placed in ball mill, starts second stage ball milling, and ball milling turns
Speed is 600rpm, Ball-milling Time 6h.
(3) after second stage ball milling, ball grinder is opened in glove box, ethanol solution is added, to step (2) ball milling
Product is washed, and is then centrifuged at 10000rpm, and basic sediment, repeated washing-centrifugal separation processes are taken
Three times, the powder after washing is finally dried in vacuo 12h at 40 DEG C of vacuum oven；The black of hydroxyl modified is obtained after drying
Phosphate material.
The black phosphorus material of gained hydroxyl modified is dissolved in deionized water, configures the hydroxylating black phosphorus aqueous dispersion of 0.8mg/ml
Liquid carries out coefficient of friction detection, and abrading-ball is 4.76mm silicon nitride bead, and opposite grinding pair is quartz glass.The result shows that group water solution
Stabilization coefficient of friction less than 0.01.
Embodiment 4
Difference of the present embodiment compared to embodiment 1 is to adjust the mass ratio of black phosphorus powder and inorganic base, specific to make
It is standby that steps are as follows:
(1) weighing purity is 99%, and average grain diameter is that 7 μm of 1 gram of red phosphorus powder (about 1.8 yuan/gram of price) are put into high energy ball
Mass ratio, that is, ratio of grinding media to material of grinding jar ball milling, steel ball and red phosphorus is 30:1, is sealed after nitrogen is passed through in ball grinder, then opens
Begin to carry out ball milling, rotational speed of ball-mill 800rpm, every ball milling 1h ball mill suspends 20min, and Ball-milling Time is for 24 hours, after ball milling
Obtain ultra-fine black phosphorus powder.
(2) ball grinder in opening steps (1) in the glove box for being connected with nitrogen, is added 4g into ultra-fine black phosphorus powder
NaOH powder is sealed after being passed through nitrogen in ball grinder, is then placed in ball mill, starts second stage ball milling, and ball milling turns
Speed is 600rpm, Ball-milling Time 6h.
(3) after second stage ball milling, ball grinder is opened in glove box, ethanol solution is added, to step (2) ball milling
Product is washed, and is then centrifuged at 10000rpm, and basic sediment, repeated washing-centrifugal separation processes are taken
Three times, the powder after washing is finally dried in vacuo 12h at 40 DEG C of vacuum oven；The black of hydroxyl modified is obtained after drying
Phosphate material.
The black phosphorus material of gained hydroxyl modified is dissolved in deionized water, water base point of hydroxylating black phosphorus of 0.5mg/ml is configured
Dispersion liquid carries out coefficient of friction detection, and abrading-ball is 4.76mm silicon nitride bead, and opposite grinding pair is quartz glass.The result shows that water base molten
The stabilization coefficient of friction of liquid is minimum to can reach 0.0006 less than 0.01.
Claims (10)
1. a kind of preparation method of the black phosphorus material of hydroxyl modified, which is characterized in that comprising steps of by rich hydroxyl inorganic matter
And/or rich hydroxy alcohols organic matter is added in black phosphorus powder, through ball milling, washing, centrifugation, the dry black phosphorus hydroxyl modified is made
Material.
2. preparation method according to claim 1, which is characterized in that the black phosphorus powder is using red phosphorus as raw material, lazy
The ultra-fine black phosphorus powder that high speed ball milling obtains under property atmosphere；
Alternatively, the black phosphorus powder is using black phosphorus block and/or black phosphorus crystal powder as raw material, ball milling is obtained under an inert atmosphere
Ultra-fine black phosphorus powder.
3. preparation method according to claim 2, which is characterized in that prepare the mistake of ultra-fine black phosphorus powder using red phosphorus as raw material
Cheng Zhong, the red phosphorus purity are greater than 98.5%, and partial size is 0.1~50 μm, and the mass ratio of steel ball and red phosphorus is 20:1~50:1, ball
Mill speed is 600~1200rpm, and Ball-milling Time is 2~48h.
4. preparation method according to claim 1, which is characterized in that the richness hydroxyl inorganic matter includes NaOH, KOH
It is one or two kinds of；The mass ratio of the richness hydroxyl inorganic powder and black phosphorus powder is 1:1~4:1.
5. preparation method according to claim 1, which is characterized in that it is described richness hydroxy alcohols organic matter include monohydric alcohol,
The one or two of dihydric alcohol；The mass ratio of the richness hydroxy alcohols organic matter and black phosphorus powder is 1:1~30:1.
6. preparation method according to claim 5, which is characterized in that the richness hydroxy alcohols organic matter includes methanol, second
One or more of alcohol, ethylene glycol, isopropanol, benzyl alcohol, 1,4- butanediol, polyethylene glycol.
7. preparation method according to claim 1, which is characterized in that the ball milling carries out under an inert atmosphere, and ball milling turns
Speed is 600~1200rpm, and Ball-milling Time is 4~12h；The washing uses methanol or dehydrated alcohol for detergent, uses
10000~12000rpm, which is centrifuged, takes deposit；The drying mode be vacuum drying, vacuum drying temperature be 40~
60℃。
8. the black phosphorus material of hydroxyl modified made from a kind of any one of claim 1-7 preparation method, which is characterized in that hydroxyl
Base is by forming the modification of P-OH key on black phosphorus surface with black phosphorus surface dangling bond.
9. the application of the black phosphorus material of hydroxyl modified described in claim 8, which is characterized in that the black phosphorus material of the hydroxyl modified
Thin-film-transistor material, the negative electrode material of battery, flexible display material, LED material, optical switch material, biology is used to prepare to pass
Sensor material, optical dynamic therapy reagent, photo-thermal therapy reagent, Water-based Lubricating Additives.
10. application according to claim 9, which is characterized in that the black phosphorus material of the hydroxyl modified is dissolved in deionization
Water, obtained group water solution are used as Water-based Lubricating Additives, stablize coefficient of friction and are not more than 0.01.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591806A (en) * | 2019-09-24 | 2019-12-20 | 清华大学 | Water-based lubricating fluid and preparation method thereof |
| CN111303974A (en) * | 2020-03-26 | 2020-06-19 | 袁全 | Wear-resistant ecological environment-friendly lubricating oil and preparation method thereof |
| CN111394152A (en) * | 2020-03-26 | 2020-07-10 | 西安建筑科技大学 | Composite lubricant containing nano graphene oxide/black phosphorus nanosheets and preparation method thereof |
| CN111875342A (en) * | 2020-08-06 | 2020-11-03 | 南京理工大学 | Novel nano aerogel building thermal insulation material and preparation method thereof |
| CN112110430A (en) * | 2020-09-23 | 2020-12-22 | 中国矿业大学 | Method for improving solubility of black phosphorus of two-dimensional material |
| WO2021114909A1 (en) * | 2019-12-12 | 2021-06-17 | 深圳瀚光科技有限公司 | Photodynamic therapy system, preparation method therefor, and use thereof in photodynamic therapy |
| CN113213441A (en) * | 2021-05-12 | 2021-08-06 | 贵州民族大学 | Preparation method of alcoholized black phosphorus stably dissolved in aqueous solution |
| CN113773892A (en) * | 2021-08-09 | 2021-12-10 | 清华大学 | Preparation method of lipophilic black phosphorus lubricating oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591806A (en) * | 2019-09-24 | 2019-12-20 | 清华大学 | Water-based lubricating fluid and preparation method thereof |
| CN110591806B (en) * | 2019-09-24 | 2020-12-01 | 清华大学 | Water-based lubricating fluid and preparation method thereof |
| WO2021114909A1 (en) * | 2019-12-12 | 2021-06-17 | 深圳瀚光科技有限公司 | Photodynamic therapy system, preparation method therefor, and use thereof in photodynamic therapy |
| CN111303974A (en) * | 2020-03-26 | 2020-06-19 | 袁全 | Wear-resistant ecological environment-friendly lubricating oil and preparation method thereof |
| CN111394152A (en) * | 2020-03-26 | 2020-07-10 | 西安建筑科技大学 | Composite lubricant containing nano graphene oxide/black phosphorus nanosheets and preparation method thereof |
| CN111394152B (en) * | 2020-03-26 | 2021-11-23 | 西安建筑科技大学 | Composite lubricant containing nano graphene oxide/black phosphorus nanosheets and preparation method thereof |
| CN111303974B (en) * | 2020-03-26 | 2022-04-15 | 江苏智摩金属抗磨修复有限责任公司 | Wear-resistant ecological environment-friendly lubricating oil and preparation method thereof |
| CN111875342A (en) * | 2020-08-06 | 2020-11-03 | 南京理工大学 | Novel nano aerogel building thermal insulation material and preparation method thereof |
| CN112110430A (en) * | 2020-09-23 | 2020-12-22 | 中国矿业大学 | Method for improving solubility of black phosphorus of two-dimensional material |
| CN112110430B (en) * | 2020-09-23 | 2021-11-09 | 中国矿业大学 | Method for improving solubility of black phosphorus of two-dimensional material |
| CN113213441A (en) * | 2021-05-12 | 2021-08-06 | 贵州民族大学 | Preparation method of alcoholized black phosphorus stably dissolved in aqueous solution |
| CN113773892A (en) * | 2021-08-09 | 2021-12-10 | 清华大学 | Preparation method of lipophilic black phosphorus lubricating oil |
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Application publication date: 20190806 |