CN113337120A - Preparation method of graphene radiation-proof material and radiation-proof garment - Google Patents
Preparation method of graphene radiation-proof material and radiation-proof garment Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000000463 material Substances 0.000 title claims abstract description 61
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000010008 shearing Methods 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 20
- 239000004917 carbon fiber Substances 0.000 claims abstract description 20
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 19
- 239000010439 graphite Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 15
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000741 silica gel Substances 0.000 claims abstract description 12
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 230000005855 radiation Effects 0.000 claims description 12
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 6
- 230000001680 brushing effect Effects 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims 2
- 230000000694 effects Effects 0.000 abstract description 11
- 239000012535 impurity Substances 0.000 abstract description 7
- 230000003471 anti-radiation Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
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- 239000012258 stirred mixture Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 210000000349 chromosome Anatomy 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229910003472 fullerene Inorganic materials 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 206010050296 Intervertebral disc protrusion Diseases 0.000 description 1
- 208000028571 Occupational disease Diseases 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000012217 deletion Methods 0.000 description 1
- 230000037430 deletion Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 210000002865 immune cell Anatomy 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention provides a preparation method of a graphene radiation-proof material and radiation-proof clothes, which specifically comprise the following steps: mixing the proportioned graphite, graphene and carbon fiber materials, and then carrying out shearing treatment under the conditions that the shearing frequency is 3000-50000 r/min and the shearing time is 1-5 h; uniformly stirring the sheared mixture, cyclohexane and silica gel at the temperature of 0-80 ℃ to prepare a radiation-proof material; according to the invention, three materials are uniformly mixed, and simultaneously, graphene is converted into three dimensions from a two-dimensional material, so that a more excellent shielding effect is realized; meanwhile, the content of impurities is effectively controlled in the shearing process, the problem of impurities is solved in batches, and the working efficiency of material treatment is improved.
Description
Technical Field
The invention relates to a radiation-proof material, in particular to a preparation method of a graphene radiation-proof material and radiation-proof clothes.
Background
Graphite and graphene-related materials are widely used in battery electrode materials, semiconductor devices, transparent display screens, sensors, capacitors, transistors, and the like. But at present, no product which meets the market requirements is available in the aspect of medical appliances.
Graphene is currently the most attractive new material. Since the preparation of graphene by Novoselov and Geim in 2004, the appearance of graphene immediately arouses wide attention of the scientific community, the novel carbon fiber material becomes another research hotspot in the fields of materials and physics after fullerene and carbon nano tube, and various scholars develop a great deal of research on the structure and performance of graphene. Graphene is a monoatomic thick carbon film with high crystallinity and capable of stably existing, is a two-dimensional crystal formed by carbon atom six-membered rings closely, has a honeycomb lattice structure with a repeating cycle, can be warped into zero-dimensional fullerene, and is rolled into a one-dimensional carbon nanotube or stacked into three-dimensional graphite. Due to the special structure, graphene has many excellent properties, the electron transport speed of the graphene is 100 times that of Si, and the theoretical specific surface area is as high as 2600m2(iv) g, hardness greater than diamond without loss of toughness. The performances of the graphene nanocomposite material are also outstanding, the electromagnetic shielding threshold content of the graphene/epoxy resin composite material is only 0.52 vol.%, and when the graphene content is 8.8 vol.%, the composite material can obtain 21dB shielding efficiency under the test condition of 8.2-12.4GHz (X-band).
Along with the rapid development of the medical industry, detection rooms of various hospitals are more and more, and the detection rooms facilitate physical examination and medical treatment of people and simultaneously silently breed a plurality of hazards such as leakage of X-ray radiation. Research shows that if a person does not wear any protection, immune cells in the human body can be damaged if the person receives X-ray radiation for a long time, so that the immune system of the human body is broken, or chromosomes in the human body are influenced, so that the chromosomes cause the problems of gene segment deletion, gene segment damage and the like.
The X-ray-proof clothes in the existing market mostly use a lead plate as a shielding material, and the clothes have the defects of large mass, lead pollution, insufficient protection when doctors in many interventional departments wear the lead clothes for operation, and occupational diseases such as lumbar disc herniation and the like caused by wearing the lead clothes for a long time. Radiation-proof clothes made of graphene materials are also available at present, but the radiation-proof shielding effect is not ideal.
Disclosure of Invention
The invention overcomes the defects of the prior art, provides a preparation method of a graphene radiation-proof material and radiation-proof clothes, solves the problems that lead clothes are too heavy and lead is polluted by heavy metal in the existing market, and simultaneously improves the shielding effect of the radiation-proof material.
In order to achieve the above object, the present invention is achieved by the following technical solutions.
A preparation method of a graphene radiation-proof material comprises the following steps:
a) mixing graphite, graphene and carbon fiber materials according to a mass ratio of 1-2: 1-8: 1-2, and mixing uniformly to obtain a mixture.
b) The mixture is subjected to shearing treatment under the conditions that the shearing frequency is 3000-50000 r/min and the shearing time is 1-5 h. The graphite, the graphene and the carbon fiber material can be uniformly mixed by shearing under the condition that the shearing frequency is 3k to 5 w/min, and impurities in the graphite, the graphene and the carbon fiber material are vibrated out.
c) Uniformly stirring the sheared mixture, cyclohexane and silica gel at the temperature of 0-80 ℃, wherein the mass ratio of the sheared mixture to the cyclohexane to the silica gel is 1-4: 1-10, wherein the ratio of cyclohexane to silica gel is 1-3: 0.20-0.30.
Preferably, the mass ratio of the graphite to the graphene to the carbon fiber material is 1.5: 5: 1.
preferably, the shearing treatment is grinding or stirring or ultrasonic oscillation treatment.
Preferably, the cyclohexane is replaced by benzene or xylene or a diluent.
Preferably, the stirring time in step c is 1.5-2.5 h.
Preferably, the graphene particle size is greater than 200 meshes.
Preferably, the carbon fiber material is carbon fiber with 500-600T.
Preferably, the shear time is 5 h.
The radiation-proof garment produced by the preparation method comprises a film made of graphene radiation-proof materials; the preparation method of the film comprises the step of brushing, spraying or leveling the graphene radiation-proof material within 15min, wherein the operation temperature is 0-200 ℃. After the mixture is uniformly stirred, brushing, spraying or leveling is carried out on the mixture within 15 minutes, the temperature during operation is required to be 0-200 ℃, and if the temperature is higher than 200 ℃, the prepared film-shaped object can generate bubbles, so that the symptom of poor shielding effect is caused.
The graphene radiation-proof material or radiation-proof clothes can shield X-ray, electromagnetic radiation and nuclear radiation (such as cobalt, alpha, beta, gamma rays and the like) below 50 milli.
Compared with the prior art, the invention has the beneficial effects that.
According to the manufacturing method for preparing the material for shielding X-ray radiation by using graphite and graphene, provided by the invention, the material is subjected to high-speed shearing treatment, and the three materials are uniformly mixed, and simultaneously, the graphene is converted into three dimensions from a two-dimensional material, so that a more excellent shielding effect is realized; meanwhile, the content of impurities is effectively controlled in the shearing process, the problem of impurities is solved in batches, and the working efficiency of material treatment is improved. The graphite, graphene and carbon fiber materials adopted by the method are subjected to high-speed shearing and high-speed grinding or ultrasonic oscillation treatment, so that the purity of the graphene in the materials can reach 40% -70%; the removal of impurities can be reduced from 10 percent of impurities to 1 percent or even lower.
The soft film forming characteristic of the silica gel and the excellent shielding effect of the three combined materials are utilized, so that the X-ray shielding material has an excellent effect on shielding X-rays. Compared with the existing similar products in the market, the weight is reduced by more than half; according to verification, the shielding effect is superior to that of the existing graphene radiation-proof clothes under the conditions of the same KV:90, mAs:20, mA:200 and ms: 100. Meanwhile, the defects of heavy lead-shielding clothes, heavy metal pollution and the like in the existing market are overcome.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The technical solutions of the present invention are described in detail below with reference to examples, but the scope of protection is not limited thereto.
Example 1
A preparation method of a graphene radiation-proof material specifically comprises the following steps:
1. weighing 23g of graphene sample, 57g of 800-mesh conductive graphite and 18g of 600T conductive carbon fiber, placing the graphene sample, the 800-mesh conductive graphite and the 18g of 600T conductive carbon fiber in a container with ultrasonic oscillation, and shearing for 3 hours under the condition of shearing at 10000 revolutions per minute.
2. And opening the container, and taking out the uniformly sheared mixed material.
3. 26g of market grade silica gel A, B were placed in 1000ml beakers, 56ml of analytically pure cyclohexane were poured into the two beakers, and the mixture was mixed after stirring.
4. Pouring the vibrated mixed material into the uniformly stirred mixture, uniformly stirring, placing the mixture on an absolute plane of a 100cm x 100cm plane for leveling when the mixture is stirred until no precipitate exists, and standing the mixture at 78 ℃ in an environment absolutely free of dust until the liquid is solidified to form a film with the thickness of 1mm-5 mm.
The proportion of the raw materials can obtain better shielding effect, for example, the use amount of carbon fiber and graphite is too small, which may cause poor shielding effect; if the amount of the carbon fiber and graphite is too large, the waste of raw materials is caused and the mixture is not formed after the silica gel is molded. The graphite materials such as artificial graphite, natural graphite and the like all have the same main body structure and can be effectively manufactured by the method, so that different graphite can be manufactured into the X-ray shielding product for shielding the X-ray of one party.
Example 2
An anti-radiation garment made of graphene anti-radiation materials is mainly prepared by leveling vibrated mixed materials prepared in the embodiment at 100 ℃ within 15min to obtain an anti-radiation film and compounding the film with fiber materials for garment making. Example 3
A preparation method of a graphene radiation-proof material specifically comprises the following steps:
1. weighing 30g of graphene sample, 90g of 800-mesh conductive graphite and 25g of 500T conductive carbon fiber, placing the graphene sample, the 800-mesh conductive graphite and the 500T conductive carbon fiber in a container with ultrasonic oscillation, and shearing for 5 hours under the condition of 20000 revolutions per minute.
2. And opening the container, and taking out the uniformly sheared mixed material.
3. 26g of market grade silica gel A, B were placed in 1000ml beakers, 56ml of analytically pure cyclohexane were poured into the two beakers, and the mixture was mixed after stirring.
4. Pouring the vibrated mixed material into the uniformly stirred mixture, uniformly stirring, placing the mixture on an absolute plane of a 100cm multiplied by 100cm plane for leveling when stirring till no precipitate exists, and standing the mixture at 100 ℃ in an environment absolutely free of dust until the liquid is solidified to form a film with the thickness of 3 mm.
Example 4
A preparation method of a graphene radiation-proof material specifically comprises the following steps:
1. weighing 25g of graphene sample, 100g of 800-mesh conductive graphite and 25g of 500T conductive carbon fiber, placing the samples in a container with ultrasonic oscillation, and shearing for 5 hours under the condition of 30000 r/min of shearing.
2. And opening the container, and taking out the uniformly sheared mixed material.
3. 26g of market grade silica gel A, B were placed in 1000ml beakers, 56ml of analytically pure cyclohexane were poured into the two beakers, and the mixture was mixed after stirring.
4. Pouring the vibrated mixed material into the uniformly stirred mixture, uniformly stirring, placing the mixture on an absolute plane of a 100cm multiplied by 100cm plane for leveling when stirring till no precipitate exists, and standing the mixture at 120 ℃ in an environment absolutely free of dust until the liquid is solidified to form a film with the thickness of 5 mm.
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A preparation method of a graphene radiation-proof material is characterized by comprising the following steps:
a) mixing graphite, graphene and carbon fiber materials according to a mass ratio of 1-2: 1-8: 1-2, uniformly mixing to obtain a mixture;
b) shearing the mixture under the conditions that the shearing frequency is 3000-50000 r/min and the shearing time is 1-5 h;
c) uniformly stirring the sheared mixture, cyclohexane and silica gel at the temperature of 0-80 ℃, wherein the mass ratio of the sheared mixture to the cyclohexane to the silica gel is 1-4: 1-10, wherein the ratio of cyclohexane to silica gel is 1-3: 0.20-0.30.
2. The preparation method of the graphene radiation-proof material according to claim 1, wherein the mass ratio of the graphite to the graphene to the carbon fiber material is 1.5: 5: 1.
3. the method for preparing a graphene radiation protection material according to claim 1, wherein the shearing treatment is grinding or stirring or ultrasonic oscillation treatment.
4. The method for preparing a graphene radiation protection material according to claim 1, wherein cyclohexane is replaced by benzene or xylene or thinner.
5. The method for preparing a graphene radiation protection material according to claim 1, wherein the stirring time in step c is 1.5-2.5 h.
6. The method for preparing a graphene radiation protection material according to claim 1, wherein the particle size of graphene is larger than 200 meshes.
7. The method for preparing a graphene radiation protection material as claimed in claim 1, wherein the carbon fiber material is 500-600T carbon fiber.
8. The method for preparing a graphene radiation protection material according to claim 1, wherein the shearing time is 5 h.
9. Radiation protective clothing produced by the method according to any one of claims 1 to 8, comprising a film made of graphene radiation protective material; the preparation method of the film comprises the step of brushing, spraying or leveling the graphene radiation-proof material within 15min, wherein the operation temperature is 0-200 ℃.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106010196A (en) * | 2016-07-14 | 2016-10-12 | 上海与创新材料技术有限公司 | Graphene type radiation protective coating |
CN107912012A (en) * | 2017-11-29 | 2018-04-13 | 横店集团东磁股份有限公司 | A kind of electromagnetic wave shielding/absorption composite paster and preparation method thereof |
CN108795283A (en) * | 2018-06-25 | 2018-11-13 | 江苏双良低碳产业技术研究院有限公司 | A kind of preparation method and application of free-floride room temperature curing graphene-organic siliconresin super hydrophobic coating |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106010196A (en) * | 2016-07-14 | 2016-10-12 | 上海与创新材料技术有限公司 | Graphene type radiation protective coating |
CN107912012A (en) * | 2017-11-29 | 2018-04-13 | 横店集团东磁股份有限公司 | A kind of electromagnetic wave shielding/absorption composite paster and preparation method thereof |
CN108795283A (en) * | 2018-06-25 | 2018-11-13 | 江苏双良低碳产业技术研究院有限公司 | A kind of preparation method and application of free-floride room temperature curing graphene-organic siliconresin super hydrophobic coating |
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