CN115925268A - Preparation method of graphene-coated glass micro powder - Google Patents
Preparation method of graphene-coated glass micro powder Download PDFInfo
- Publication number
- CN115925268A CN115925268A CN202211663323.XA CN202211663323A CN115925268A CN 115925268 A CN115925268 A CN 115925268A CN 202211663323 A CN202211663323 A CN 202211663323A CN 115925268 A CN115925268 A CN 115925268A
- Authority
- CN
- China
- Prior art keywords
- graphene
- coated glass
- micropowder
- glass micropowder
- graphene oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 50
- 239000011521 glass Substances 0.000 title claims abstract description 41
- 239000000843 powder Substances 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 239000004033 plastic Substances 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 239000002344 surface layer Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000011163 secondary particle Substances 0.000 abstract description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 230000008859 change Effects 0.000 abstract description 2
- 239000000428 dust Substances 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- 230000002745 absorbent Effects 0.000 abstract 1
- 239000002250 absorbent Substances 0.000 abstract 1
- 239000006260 foam Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- 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
- Y02E60/10—Energy storage using batteries
Landscapes
- Glass Compositions (AREA)
Abstract
The invention discloses a preparation method of graphene-coated glass micro powder, which comprises the following steps of dispersing graphene oxide in pure water; adding low-melting-point glass micro powder and uniformly stirring; addition of NH 4 HF 2 The solution was stirred and then allowed to stand. Reducing the graphene oxide to form gel carrying glass micropowder; and cleaning the generated graphene gel block with pure water, and drying to obtain the graphene-coated glass micropowder. The product can be used as a phase change heat absorbent to fill gaps of a lithium ion battery, and the graphene is coated to reduce the number of gapsPossibility of inhalation by the human body. The graphene coated glass micropowder secondary particles generated by the method cannot generate dust. The generated secondary particles of the graphene coated glass micropowder belong to pure inorganic materials, and the service life is long.
Description
Technical Field
The invention relates to the field of refractory materials, in particular to a phase-change heat-absorbing material, and especially relates to a preparation method of graphene-coated glass micro powder.
Background
In a lithium ion battery fire, a single battery thermally runaway emits a large amount of heat, and the process of heating other batteries to spread a thermal runaway state is an important development stage of the fire. The thermal runaway transmission can be delayed by additionally arranging the clamping plates among the batteries, and the clamping plates are designed to be hollow and filled with a substance (CN _ 115404046) capable of absorbing a large amount of heat.
The low melting point glass can absorb a large amount of heat through phase change, and the transformation temperature (Tg) of the lead-free low melting point glass can be lowered to 310 ℃ through formula adjustment o C. Grinding the glass into nano-scale particles, the Tg is further reduced due to the increase of the surface energy, but the density of the superfine glass micropowder is generally less than 3 g cm -3 The air-permeable fabric is easy to fly with the wind, and has certain threat to the health of human body in the use process.
Disclosure of Invention
The invention aims to provide a preparation method of graphene-coated glass micropowder, aiming at the problem that superfine low-melting-point glass micropowder is easy to scatter.
The technical scheme provided by the invention is as follows: a preparation method of graphene-coated glass micropowder comprises the following steps:
(1) Graphene oxide was dispersed in pure water.
(2) Adding low-melting-point glass micropowder and stirring.
(3) Addition of NH 4 HF 2 The solution was stirred and then allowed to stand. The graphene oxide is reduced to form a gel with glass micropowder.
(4) And cleaning the generated graphene gel block with pure water, and drying to obtain the graphene-coated glass micropowder.
Preferably, the concentration of the graphene oxide in the step (1) is 1 g L -1 。
Preferably, the glass micropowder d in the step (2) 50 = 50 nm。
Preferably, the drying temperature in the step (4) is 120 DEG o C。
In the present invention, NH 4 HF 2 The graphene oxide is firstly reduced to be converted into gel or graphene foam (graphene foam), and then the fluorine remained on the surface of the graphene oxide can also improve the affinity of the graphene oxide with the surface of the glass, so that the graphene oxide is coated on the surface of the glass.
The invention has the advantages that:
the generated secondary particles of the graphene coated glass micropowder cannot generate dust;
the generated secondary particles of the graphene coated glass micropowder belong to pure inorganic materials, and the service life is long.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. The experimental procedures used in the following examples are all conventional procedures unless otherwise specified. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example 1.
50 g 1: the preparation method of 1000 graphene coated glass micropowder comprises the following steps:
(1) Dispersing 50 mg graphene oxide in 50 mL pure water in a polytetrafluoroethylene beaker;
(2) 50 g d 50 Adding low-melting-point glass micropowder of = 50 nm into the solution, and stirring for 0.5 h to obtain a co-dispersion liquid;
(3) While stirring, 10 g L of 10 mL was added to the co-dispersion -1 NH of 4 HF 2 Continuously stirring the solution for 0.5 h, and standing the solution for 24 h at 25 ℃; gradually reducing the graphene oxide, self-assembling the graphene oxide into gel, and wrapping and clamping the glass micro powder in the gel;
(4) And (3) pumping out water on the surface layer by using a plastic dropper, adding 50 mL pure water to clean the graphene gel block generated once, sucking water on the surface of the obtained graphene gel block by using the plastic dropper, drying 8 h in a 120 ℃ drying oven, and crushing the product by using a plastic forceps to obtain the graphene-coated glass micropowder.
The above examples are merely illustrative for clearly illustrating the present invention and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the scope of the invention.
Claims (5)
1. A preparation method of graphene-coated glass micropowder is characterized by comprising the following steps:
(1) Dispersing graphene oxide in pure water;
(2) Adding low-melting-point glass micro powder and uniformly stirring;
(3) Addition of NH 4 HF 2 Stirring the solution and then standing; reducing the graphene oxide to form gel carrying glass micropowder;
(4) And cleaning the generated graphene gel block with pure water, and drying to obtain the graphene-coated glass micropowder.
2. The method for preparing graphene-coated glass micropowder according to claim 1, wherein the graphene oxide concentration in the step (1) is 1 g L -1 Fine glass powder d 50 = 50 nm。
3. The method for preparing graphene-coated glass micropowder according to claim 1, wherein the standing condition in the step (3) is 24 h at 25 ℃.
4. The method for preparing graphene-coated glass micropowder according to claim 1, wherein in the step (4), the drying temperature is 120 ℃.
5. The method for producing a graphene-coated glass micropowder according to any one of claims 1 to 4, wherein 50 g 1: the preparation method of 1000 graphene coated glass micropowder comprises the following steps:
(1) Dispersing 50 mg graphene oxide in 50 mL pure water in a polytetrafluoroethylene beaker;
(2) 50 g d 50 Adding low-melting-point glass micropowder of = 50 nm into the solution, and stirring for 0.5 h to obtain a co-dispersion liquid;
(3) While stirring, 10 g L of 10 mL was added to the co-dispersion -1 NH of (2) 4 HF 2 Continuously stirring the solution for 0.5 h, and standing the solution for 24 h at 25 ℃; gradually reducing the graphene oxide, self-assembling the graphene oxide into gel, and wrapping and clamping the glass micro powder in the gel;
(4) And (3) pumping out water on the surface layer by using a plastic dropper, adding 50 mL pure water to clean the generated graphene gel block once, sucking water on the surface of the obtained graphene gel block by using the plastic dropper, drying 8 h in a 120 ℃ oven, and crushing the product by using a plastic forceps to obtain the graphene-coated glass micropowder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211663323.XA CN115925268A (en) | 2022-12-23 | 2022-12-23 | Preparation method of graphene-coated glass micro powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211663323.XA CN115925268A (en) | 2022-12-23 | 2022-12-23 | Preparation method of graphene-coated glass micro powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115925268A true CN115925268A (en) | 2023-04-07 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211663323.XA Pending CN115925268A (en) | 2022-12-23 | 2022-12-23 | Preparation method of graphene-coated glass micro powder |
Country Status (1)
| Country | Link |
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| CN (1) | CN115925268A (en) |
Citations (8)
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|---|---|---|---|---|
| CN106517215A (en) * | 2016-10-26 | 2017-03-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of graphene-coated silicon dioxide nanoparticles |
| CN106746688A (en) * | 2017-03-22 | 2017-05-31 | 西北大学 | A kind of lead-free glass powder based on graphene modified and preparation method thereof and electric slurry |
| US20180226172A1 (en) * | 2016-05-16 | 2018-08-09 | Nantong T-Sun New Energy Co.,Ltd. | Solar cell front side silver paste doped with modified grapheme and preparation method thereof |
| CN109897532A (en) * | 2019-03-08 | 2019-06-18 | 西安热工研究院有限公司 | A kind of graphene coating material and preparation method thereof protected in advance for four main tubes of boiler high temperature corrosion |
| CN112573508A (en) * | 2020-12-28 | 2021-03-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method, product and application of graphene-coated core-shell stannous oxide @ tin oxide material |
| CN112569516A (en) * | 2020-12-28 | 2021-03-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of graphene-coated hollow glass bead three-phase fire extinguishing agent and product thereof |
| CN112996153A (en) * | 2019-12-12 | 2021-06-18 | 上海烯有新材料有限公司 | Graphene heating plate and preparation method and application thereof |
| US20210230054A1 (en) * | 2017-10-26 | 2021-07-29 | Shenzhen University | Method for preparing hollow glass microbeads coated with graphene oxide |
-
2022
- 2022-12-23 CN CN202211663323.XA patent/CN115925268A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20180226172A1 (en) * | 2016-05-16 | 2018-08-09 | Nantong T-Sun New Energy Co.,Ltd. | Solar cell front side silver paste doped with modified grapheme and preparation method thereof |
| CN106517215A (en) * | 2016-10-26 | 2017-03-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of graphene-coated silicon dioxide nanoparticles |
| CN106746688A (en) * | 2017-03-22 | 2017-05-31 | 西北大学 | A kind of lead-free glass powder based on graphene modified and preparation method thereof and electric slurry |
| US20210230054A1 (en) * | 2017-10-26 | 2021-07-29 | Shenzhen University | Method for preparing hollow glass microbeads coated with graphene oxide |
| CN109897532A (en) * | 2019-03-08 | 2019-06-18 | 西安热工研究院有限公司 | A kind of graphene coating material and preparation method thereof protected in advance for four main tubes of boiler high temperature corrosion |
| CN112996153A (en) * | 2019-12-12 | 2021-06-18 | 上海烯有新材料有限公司 | Graphene heating plate and preparation method and application thereof |
| CN112573508A (en) * | 2020-12-28 | 2021-03-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method, product and application of graphene-coated core-shell stannous oxide @ tin oxide material |
| CN112569516A (en) * | 2020-12-28 | 2021-03-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of graphene-coated hollow glass bead three-phase fire extinguishing agent and product thereof |
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