Preparation method of carbon fiber radar stealth material

Abstract

The invention discloses a method for preparing a carbon fiber radar stealth material, comprising the following steps: adding chitosan compounding agent to carbon fiber coordinated carbon nanotube body at a weight ratio of 5:1, stirring fully, and finally washing and drying; treating the product with heat homogenization improvement, and finishing the treatment to obtain the carbon fiber radar stealth material of the invention. The carbon fiber radar stealth material of the invention adopts sodium dodecyl sulfate solution and carbon nanotubes for primary stirring treatment, and then cooperates with hydroxyapatite modifier for secondary stirring, and the obtained carbon nanotube regulator is ultrasonically matched with carbon fiber, and then coordinated with chitosan compounding agent, and the prepared radar stealth material has excellent wide-band wave absorbing performance and excellent mechanical properties of the product, and the two properties can be coordinated and improved.

Description

Technical Field

[0001] The invention relates to the technical field of carbon fiber stealth, and in particular to a method for preparing a carbon fiber radar stealth material. Background Art

[0002] Camouflage technology currently plays an important role in military equipment of various countries, especially multifunctional composite materials that integrate visible light, infrared and radar stealth technologies are currently a hot topic of research. As a flexible stealth material, it can be widely used in camouflage of targets such as canopies and patches. However, when visible light, infrared and radar stealth materials are combined, there is a phenomenon of mutual interference, which requires specific material combination and modification to solve these problems.

[0003] The existing carbon fiber radar stealth material has average broadband wave absorbing performance, and it is difficult to coordinate and optimize the mechanical properties with the wave absorbing performance, which limits the use efficiency of the product. Based on this, the present invention further improves it. Summary of the invention

[0004] In view of the defects of the prior art, the purpose of the present invention is to provide a method for preparing a carbon fiber radar stealth material to solve the problems raised in the above background technology.

[0005] The present invention solves the technical problem by adopting the following technical solution:

[0006] The present invention provides a method for preparing a carbon fiber radar stealth material, comprising the following steps:

[0007] Step 1: Add 5-10 parts of sodium dodecyl sulfate and 1-3 parts of 5% by mass lanthanum sulfate solution to 10-15 parts of 2% by mass hydrochloric acid solution, stir evenly, then add 0.45-0.55 parts of carboxymethyl cellulose, stir well, and obtain sodium dodecyl sulfate solution;

[0008] Step 2: Place the carbon nanotubes in a sodium dodecyl sulfate solution at a weight ratio of 1:5 and perform a primary stirring treatment. After the stirring is completed, add a hydroxyapatite modifier of 5-10% of the total amount of the carbon nanotubes and perform a secondary stirring treatment. After the stirring is completed, a carbon nanotube regulator is obtained;

[0009] Step 3: Place the carbon fiber on the

[0010] Firstly, ultrasonically disperse the carbon nanotubes in a carbon nanotube regulator with a total amount of 3-5 times the total amount of carbon nanotubes for 10-20 minutes, with an ultrasonic power of 350-400W. After the ultrasonication is finished, the carbon fiber is washed with water and dried to obtain a carbon fiber coordinated carbon nanotube body.

[0011] Step 4: Add chitosan compounding agent to the carbon fiber coordinated carbon nanotube body at a weight ratio of 5:1, stir thoroughly, and finally wash and dry;

[0012] Step Five: Subject the product of Step Four to heat homogenization improvement treatment. After the treatment is completed, the carbon fiber radar stealth material of the present invention is obtained.

[0013] Preferably, the rotation speed of the primary stirring treatment is 450 - 550 r / min, the stirring time is 20 - 30 min, and the stirring temperature is 35 - 40°C; the rotation speed of the secondary stirring treatment is 850 - 1050 r / min, the stirring time is 10 - 20 min, and the stirring temperature is 42 - 45°C.

[0014] Preferably, the preparation method of the hydroxyapatite modifier is as follows:

[0015] S01: Preheat hydroxyapatite at a temperature of 75 - 85°C for 1 - 2 h, then cool it to 40 - 45°C at a rate of 1 - 3°C / min and keep it warm.

[0016] S02: Add the hydroxyapatite of S01 to an aqueous sodium alginate solution with a mass fraction of 5% according to a weight ratio of 1:5, then add cetyltrimethylammonium chloride accounting for 1 - 5% of the total amount of the hydroxyapatite of S01 and a phosphate buffer solution accounting for 2 - 3% of the total amount of the hydroxyapatite of S01, stir well, wash with water and dry to obtain the hydroxyapatite modifier.

[0017] Preferably, the pH value of the phosphate buffer solution is 4.5 - 5.5.

[0018] Preferably, the preparation method of the chitosan compounding agent is as follows:

[0019] S11: Add silane coupling agent KH560 to the chitosan aqueous solution according to a weight ratio of 3:1, stir evenly, then add triethanolamine borate accounting for 10 - 15% of the total amount of the chitosan aqueous solution, stir evenly and set aside.

[0020] S12: Mix 1 - 2 parts of Span - 80 with 2 - 5 parts of vegetable oil to obtain an oil phase; first add the oil phase to a magnetic stirrer, heat it up to 60 - 65°C, then add 3 - 5 parts of β - cyclodextrin aqueous solution, increase the stirring speed to 300 - 500 r / min, stir for 35 - 45 min, and after the stirring is completed, obtain an additive.

[0021] S13: Add the additive to the product of S11 according to a weight ratio of 1:5, and continue to stir evenly to obtain the chitosan compounding agent.

[0022] Preferably, the mass fraction of the chitosan aqueous solution is 6 - 10%.

[0023] Preferably, the mass fraction of the β - cyclodextrin aqueous solution is 2%.

[0024] Preferably, the specific operation steps of the heat homogenization improvement treatment are:

[0025] The product of step 4 is first hot-pressed at 10-20 MPa for 1-2 hours at a temperature of 65-70°C, then heated to 105-110°C at a rate of 1-3°C / min, kept warm for 5-10 minutes, and finally cooled to 40-45°C at a rate of 2-4°C / min, and then treated with a treatment solution for infiltration. After the treatment is completed, it is washed with water and dried.

[0026] Preferably, the treatment liquid infiltration treatment uses yttrium nitrate solution to infiltrate the surface of the product of step four.

[0027] Preferably, the mass fraction of the yttrium nitrate solution is 2-5%.

[0028] Compared with the prior art, the present invention has the following beneficial effects:

[0029] The carbon fiber radar stealth material of the present invention adopts sodium dodecyl sulfate solution and carbon nanotubes for primary stirring treatment, and then cooperates with hydroxyapatite modifier for secondary stirring, the obtained carbon nanotube regulator is ultrasonically combined with carbon fiber, and then coordinated with chitosan compounding agent, the carbon nanotube regulator and chitosan compounding agent are coordinated and synergistic, and then subjected to heat homogenization improvement treatment, hot pressing treatment, and then combined with heating to 105-110°C at a rate of 1-3°C / min, heat preservation for 5-10min, and finally cooled to 40-45°C at a rate of 2-4°C / min, and infiltrated with yttrium nitrate solution. The prepared radar stealth material has excellent wide-band wave absorbing performance and excellent mechanical properties of the product, and the two properties can be improved in a coordinated manner. DETAILED DESCRIPTION

[0030] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0031] A method for preparing a carbon fiber radar stealth material in this embodiment includes the following steps:

[0032] Step 1: Add 5-10 parts of sodium dodecyl sulfate and 1-3 parts of 5% by mass lanthanum sulfate solution to 10-15 parts of 2% by mass hydrochloric acid solution, stir evenly, then add 0.45-0.55 parts of carboxymethyl cellulose, stir well, and obtain sodium dodecyl sulfate solution;

[0033] Step 2: Place the carbon nanotubes in a sodium dodecyl sulfate solution at a weight ratio of 1:5 and perform a primary stirring treatment. After the stirring is completed, add a hydroxyapatite modifier of 5-10% of the total amount of the carbon nanotubes and perform a secondary stirring treatment. After the stirring is completed, a carbon nanotube regulator is obtained;

[0034] Step 3: firstly place the carbon fiber in a carbon nanotube regulator with a volume of 3-5 times the total volume of the carbon fiber, and firstly ultrasonically disperse the carbon fiber for 10-20 minutes, with an ultrasonic power of 350-400W. After the ultrasonication is finished, the carbon fiber is washed with water and dried to obtain a carbon fiber coordinated carbon nanotube body.

[0035] Step 4: Add chitosan compounding agent to the carbon fiber coordinated carbon nanotube body at a weight ratio of 5:1, stir thoroughly, and finally wash and dry;

[0036] Step 5: subjecting the product of step 4 to thermal homogenization improvement treatment, and completing the treatment to obtain the carbon fiber radar stealth material of the present invention.

[0037] The rotation speed of the first-stage stirring treatment in this embodiment is 450-550r / min, the stirring time is 20-30min, and the stirring temperature is 35-40°C; the rotation speed of the second-stage stirring treatment is 850-1050r / min, the stirring time is 10-20min, and the stirring temperature is 42-45°C.

[0038] The preparation method of the hydroxyapatite modifier of this embodiment is:

[0039] S01: preheat the hydroxyapatite at 75-85°C for 1-2h, then cool to 40-45°C at a rate of 1-3°C / min, and keep warm;

[0040] S02: Add the hydroxyapatite of S01 to a 5% sodium alginate aqueous solution at a weight ratio of 1:5, then add 1-5% of the total amount of hydroxyapatite of S01 hexadecyltrimethylammonium chloride and 2-3% of the total amount of hydroxyapatite of S01 phosphate buffer solution, stir thoroughly, wash with water, and dry to obtain a hydroxyapatite modifier.

[0041] The pH value of the phosphate buffer solution of this embodiment is 4.5-5.5.

[0042] The preparation method of the chitosan compounding agent of the present embodiment is:

[0043] S11: adding silane coupling agent KH560 to the chitosan aqueous solution at a weight ratio of 3:1, stirring evenly, and then adding triethanolamine borate in an amount of 10-15% of the total amount of the chitosan aqueous solution, stirring evenly, and setting aside;

[0044] S12: Mix 1 - 2 parts of Span - 80 with 2 - 5 parts of vegetable oil to obtain an oil phase; first add the oil phase to a magnetic stirrer, heat it up to 60 - 65 °C, then add 3 - 5 parts of β - cyclodextrin aqueous solution, increase the stirring speed to 300 - 500 r / min, stir for 35 - 45 min, and after the stirring ends, obtain an additive;

[0045] S13: Add the additive to the product of S11 according to a weight ratio of 1:5, and continue to stir evenly to obtain a chitosan complexing agent.

[0046] The mass fraction of the chitosan aqueous solution in this example is 6 - 10%.

[0047] The mass fraction of the β - cyclodextrin aqueous solution in this example is 2%.

[0048] The specific operation steps of the heat homogenization improvement treatment in this example are as follows:

[0049] The product of step four is first hot - pressed at 10 - 20 MPa for 1 - 2 h, the hot - pressing temperature is 65 - 70 °C, then it is heated to 105 - 110 °C at a rate of 1 - 3 °C / min, held for 5 - 10 min, and finally cooled to 40 - 45 °C at a rate of 2 - 4 °C / min, then it is infiltrated with a treatment liquid, and after the treatment ends, it is washed with water and dried.

[0050] The infiltration treatment with the treatment liquid in this example uses a yttrium nitrate solution to infiltrate the surface of the product of step four.

[0051] The mass fraction of the yttrium nitrate solution in this example is 2 - 5%.

[0052] Example 1.

[0053] The preparation method of a carbon fiber radar stealth material in this example includes the following steps:

[0054] Step one: Add 5 parts of sodium dodecyl sulfate and 1 part of a 5% lanthanum sulfate solution by mass fraction to 10 parts of a 2% hydrochloric acid solution by mass fraction, stir evenly, and then add 0.45 parts of carboxymethyl cellulose and stir thoroughly to obtain a sodium dodecyl sulfate solution;

[0055] Step two: First place the carbon nanotubes in the sodium dodecyl sulfate solution for primary stirring treatment according to a weight ratio of 1:5, and after the stirring ends, then add 5% of the total amount of carbon nanotubes of the hydroxyapatite modifier for secondary stirring treatment, and after the stirring ends, obtain a carbon nanotube regulator;

[0056] Step three: First place the carbon fiber in 3 times the total amount of carbon nanotube regulator for ultrasonic dispersion for 10 min, the ultrasonic power is 350 W, and after the ultrasonic treatment ends, wash it with water and dry it to obtain a carbon fiber coordinated carbon nanotube body;

[0057] Step 4: Add a chitosan compounding agent to the carbon fiber coordinated carbon nanotube body at a weight ratio of 5:1, stir thoroughly, and finally wash with water and dry.

[0058] Step 5: Subject the product of Step 4 to heat homogenization improvement treatment. After the treatment is completed, the carbon fiber radar stealth material of the present invention is obtained.

[0059] In this embodiment, the rotation speed of the primary stirring treatment is 450 r / min, the stirring time is 20 min, and the stirring temperature is 35°C; the rotation speed of the secondary stirring treatment is 850 r / min, the stirring time is 10 min, and the stirring temperature is 42°C.

[0060] The preparation method of the hydroxyapatite modifier in this embodiment is as follows:

[0061] S01: Preheat hydroxyapatite at a temperature of 75°C for 1 h, then cool it to 40°C at a rate of 1°C / min and keep it warm.

[0062] S02: Add the hydroxyapatite of S01 to an aqueous solution of sodium alginate with a mass fraction of 5% at a weight ratio of 1:5, then add cetyltrimethylammonium chloride accounting for 1% of the total amount of the hydroxyapatite of S01 and a phosphate buffer solution accounting for 2% of the total amount of the hydroxyapatite of S01, stir thoroughly, wash with water and dry to obtain the hydroxyapatite modifier.

[0063] The pH value of the phosphate buffer solution in this embodiment is 4.5.

[0064] The preparation method of the chitosan compounding agent in this embodiment is as follows:

[0065] S11: Add a silane coupling agent KH560 to the chitosan aqueous solution at a weight ratio of 3:1, stir evenly, then add triethanolamine borate accounting for 10% of the total amount of the chitosan aqueous solution, stir evenly, and set aside.

[0066] S12: Mix 1 part of Span-80 with 2 parts of vegetable oil to obtain an oil phase; first add the oil phase to a magnetic stirrer, heat it to 60°C, then add 3 parts of an aqueous β-cyclodextrin solution, increase the stirring speed to 300 r / min, and stir for 35 min. After the stirring is completed, obtain an additive.

[0067] S13: Add the additive to the product of S11 at a weight ratio of 1:5, and continue to stir evenly to obtain the chitosan compounding agent.

[0068] The mass fraction of the chitosan aqueous solution in this embodiment is 6%.

[0069] The mass fraction of the aqueous β-cyclodextrin solution in this embodiment is 2%.

[0070] The specific operation steps of the heat homogenization improvement treatment in this embodiment are as follows:

[0071] In step four, the product is first hot-pressed at 10 MPa for 1 h, the hot-pressing temperature is 65 °C, then it is heated to 105 °C at a rate of 1 °C / min, held for 5 min, and finally cooled to 40 °C at a rate of 2 °C / min. Then, it is treated by soaking with a treatment liquid. After the treatment, it is washed with water and dried.

[0072] In the soaking treatment with the treatment liquid in this embodiment, the surface of the product in step four is soaked with a yttrium nitrate solution.

[0073] The mass fraction of the yttrium nitrate solution in this embodiment is 2%.

[0074] Example 2.

[0075] A preparation method of a carbon fiber radar stealth material in this embodiment includes the following steps:

[0076] Step one: Add 10 parts of sodium dodecyl sulfate and 3 parts of a lanthanum sulfate solution with a mass fraction of 5% to 15 parts of a hydrochloric acid solution with a mass fraction of 2%, stir evenly, and then add 0.55 parts of carboxymethyl cellulose and stir thoroughly to obtain a sodium dodecyl sulfate solution;

[0077] Step two: First, place the carbon nanotubes in the sodium dodecyl sulfate solution for primary stirring treatment according to a weight ratio of 1:5. After the stirring ends, then add 10% of the hydroxyapatite modifier based on the total amount of the carbon nanotubes and conduct secondary stirring treatment. After the stirring ends, obtain a carbon nanotube regulator;

[0078] Step three: First, place the carbon fiber in 5 times the total amount of the carbon nanotube regulator and ultrasonically disperse it for 20 min. The ultrasonic power is 400 W. After the ultrasonic treatment ends, wash it with water and dry it to obtain a carbon fiber coordinated carbon nanotube body;

[0079] Step four: Add a chitosan complexing agent to the carbon fiber coordinated carbon nanotube body according to a weight ratio of 5:1, stir thoroughly, and finally wash it with water and dry it;

[0080] Step five: Perform heat homogenization improvement treatment on the product in step four. After the treatment ends, obtain the carbon fiber radar stealth material of the present invention.

[0081] In this embodiment, the rotation speed of the primary stirring treatment is 550 r / min, the stirring time is 30 min, and the stirring temperature is 40 °C; the rotation speed of the secondary stirring treatment is 1050 r / min, the stirring time is 20 min, and the stirring temperature is 45 °C.

[0082] The preparation method of the hydroxyapatite modifier in this embodiment is as follows:

[0083] S01: Preheat hydroxyapatite at a temperature of 85°C for 2 h, then cool it at a rate of 3°C / min to 45°C and keep it warm.

[0084] S02: Add the hydroxyapatite from S01 to an aqueous sodium alginate solution with a mass fraction of 5% according to a weight ratio of 1:5. Then add cetyltrimethylammonium chloride accounting for 5% of the total amount of the hydroxyapatite from S01 and a phosphate buffer solution accounting for 3% of the total amount of the hydroxyapatite from S01, stir well, wash with water and dry to obtain a hydroxyapatite modifier.

[0085] The pH value of the phosphate buffer solution in this example is 5.5.

[0086] The preparation method of the chitosan complexing agent in this example is as follows:

[0087] S11: Add a silane coupling agent KH560 to the chitosan aqueous solution according to a weight ratio of 3:1, stir evenly, and then add triethanolamine borate accounting for 15% of the total amount of the chitosan aqueous solution, stir evenly and set aside.

[0088] S12: Mix 2 parts of Span-80 with 5 parts of vegetable oil to obtain an oil phase; first add the oil phase to a magnetic stirrer, heat it up to 65°C, then add 5 parts of β-cyclodextrin aqueous solution, increase the stirring speed to 500 r / min and stir for 45 min. After the stirring ends, obtain an additive.

[0089] S13: Add the additive to the product of S11 according to a weight ratio of 1:5, and continue to stir evenly to obtain a chitosan complexing agent.

[0090] The mass fraction of the chitosan aqueous solution in this example is 10%.

[0091] The mass fraction of the β-cyclodextrin aqueous solution in this example is 2%.

[0092] The specific operation steps of the thermal homogenization improvement treatment in this example are as follows:

[0093] First, place the product of step four under a hot press at 20 MPa for 2 h, with a hot press temperature of 70°C. Then heat it up to 110°C at a rate of 3°C / min, keep it warm for 10 min, and finally cool it to 45°C at a rate of 4°C / min. Then carry out infiltration treatment with a treatment liquid. After the treatment ends, wash with water and dry.

[0094] In this example, the infiltration treatment with the treatment liquid uses a yttrium nitrate solution to infiltrate the surface of the product of step four.

[0095] The mass fraction of the yttrium nitrate solution in this example is 5%.

[0096] Example 3.

[0097] A preparation method of a carbon fiber radar stealth material according to this embodiment includes the following steps:

[0098] Step 1: Add 7.5 parts of sodium dodecyl sulfate and 2 parts of a 5% lanthanum sulfate solution by mass to 12.5 parts of a 2% hydrochloric acid solution by mass, stir evenly, then add 0.50 part of carboxymethyl cellulose, and stir thoroughly to obtain a sodium dodecyl sulfate solution;

[0099] Step 2: First place carbon nanotubes in the sodium dodecyl sulfate solution for primary stirring treatment according to a weight ratio of 1:5. After the stirring ends, then add 7.5% of the total amount of carbon nanotubes of hydroxyapatite modifier for secondary stirring treatment. After the stirring ends, obtain a carbon nanotube regulator;

[0100] Step 3: First place carbon fibers in 4 times the total amount of carbon nanotube regulators for ultrasonic dispersion for 15 min. The ultrasonic power is 370 W. After the ultrasonic treatment ends, wash with water and dry to obtain a carbon fiber coordinated carbon nanotube body;

[0101] Step 4: Add a chitosan compounding agent to the carbon fiber coordinated carbon nanotube body according to a weight ratio of 5:1, stir thoroughly, and finally wash with water and dry;

[0102] Step 5: Subject the product of Step 4 to heat homogenization improvement treatment. After the treatment ends, obtain the carbon fiber radar stealth material of the present invention.

[0103] The rotation speed of the primary stirring treatment in this embodiment is 500 r / min, the stirring time is 25 min, and the stirring temperature is 37 °C; the rotation speed of the secondary stirring treatment is 1000 r / min, the stirring time is 15 min, and the stirring temperature is 43 °C.

[0104] The preparation method of the hydroxyapatite modifier in this embodiment is as follows:

[0105] S01: First preheat hydroxyapatite at a temperature of 80 °C for 1.5 h, then cool it at a rate of 2 °C / min to 42 °C and keep it warm;

[0106] S02: Add the hydroxyapatite of S01 to an aqueous sodium alginate solution with a mass fraction of 5% according to a weight ratio of 1:5, then add 3% of the total amount of the hydroxyapatite of S01 of cetyltrimethylammonium chloride and 2.5% of the total amount of the hydroxyapatite of S01 of phosphate buffer solution, stir thoroughly, wash with water and dry to obtain a hydroxyapatite modifier.

[0107] The pH value of the phosphate buffer solution in this embodiment is 5.0.

[0108] The preparation method of the chitosan compounding agent in this embodiment is as follows:

[0109] S11: Add silane coupling agent KH560 to the chitosan aqueous solution at a weight ratio of 3:1, stir evenly, then add 12.5% of triethanolamine borate based on the total amount of the chitosan aqueous solution, stir evenly, and set aside.

[0110] S12: Mix 1.5 parts of Span-80 with 3.5 parts of vegetable oil to obtain an oil phase; first add the oil phase to a magnetic stirrer, heat up to 60 - 65 °C, then add 4.5 parts of β-cyclodextrin aqueous solution, increase the stirring speed to 400 r / min, stir for 40 min, and after the stirring ends, obtain an additive.

[0111] S13: Add the additive to the product of S11 at a weight ratio of 1:5, continue to stir evenly to obtain a chitosan complexing agent.

[0112] In this example, the mass fraction of the chitosan aqueous solution is 8%.

[0113] In this example, the mass fraction of the β-cyclodextrin aqueous solution is 2%.

[0114] The specific operation steps of the heat homogenization improvement treatment in this example are as follows:

[0115] The product of step four is first hot-pressed at 15 MPa for 1.5 h, the hot-pressing temperature is 67.5 °C, then it is heated to 107 °C at a rate of 2 °C / min, held for 7 min, and finally cooled to 42.5 °C at a rate of 3 °C / min, and then treated by infiltration with a treatment liquid. After the treatment ends, it is washed with water and dried.

[0116] In this example, the treatment by infiltration with the treatment liquid uses a yttrium nitrate solution to infiltrate the surface of the product of step four.

[0117] In this example, the mass fraction of the yttrium nitrate solution is 3.5%.

[0118] Example 4.

[0119] A preparation method of a carbon fiber radar stealth material in this example includes the following steps:

[0120] Step one: Add 6 parts of sodium dodecyl sulfate and 2 parts of a 5% lanthanum sulfate solution by mass fraction to 12 parts of a 2% hydrochloric acid solution by mass fraction, stir evenly, and then add 0.46 parts of carboxymethyl cellulose and stir thoroughly to obtain a sodium dodecyl sulfate solution.

[0121] Step two: First place the carbon nanotubes in the sodium dodecyl sulfate solution for primary stirring treatment at a weight ratio of 1:5. After the stirring ends, then add 6% of the hydroxyapatite modifier based on the total amount of the carbon nanotubes and conduct secondary stirring treatment. After the stirring ends, obtain a carbon nanotube regulator.

[0122] Step 3: Place the carbon fiber in a carbon nanotube regulator that is 4 times the total amount of carbon fiber and ultrasonically disperse it for 12 min. The ultrasonic power is 360 W. After the ultrasonic treatment, wash it with water and dry it to obtain a carbon fiber coordinated carbon nanotube body;

[0123] Step 4: Add a chitosan compounding agent to the carbon fiber coordinated carbon nanotube body according to a weight ratio of 5:1, stir well, and finally wash it with water and dry it;

[0124] Step 5: Perform a heat homogenization improvement treatment on the product of Step 4. After the treatment, the carbon fiber radar stealth material of the present invention is obtained.

[0125] In this example, the rotation speed of the first-stage stirring treatment is 460 r / min, the stirring time is 22 min; the stirring temperature is 36 °C; the rotation speed of the second-stage stirring treatment is 900 r / min, the stirring time is 12 min, and the stirring temperature is 43 °C.

[0126] The preparation method of the hydroxyapatite modifier in this example is as follows:

[0127] S01: Preheat the hydroxyapatite at a temperature of 78 °C for 1.2 h, then cool it to 42 °C at a rate of 2 °C / min and keep it warm;

[0128] S02: Add the hydroxyapatite of S01 to an aqueous solution of sodium alginate with a mass fraction of 5% according to a weight ratio of 1:5, then add cetyltrimethylammonium chloride accounting for 2% of the total amount of the hydroxyapatite of S01 and a phosphate buffer solution accounting for 2.2% of the total amount of the hydroxyapatite of S01, stir well, wash it with water and dry it to obtain a hydroxyapatite modifier.

[0129] The pH value of the phosphate buffer solution in this example is 4.6.

[0130] The preparation method of the chitosan compounding agent in this example is as follows:

[0131] S11: Add a silane coupling agent KH560 to the chitosan aqueous solution according to a weight ratio of 3:1, stir evenly, then add triethanolamine borate accounting for 12% of the total amount of the chitosan aqueous solution, stir evenly, and set aside;

[0132] S12: Mix 1.2 parts of Span-80 with 3 parts of vegetable oil to obtain an oil phase; first add the oil phase to a magnetic stirrer, heat it to 62 °C, then add 4 parts of β-cyclodextrin aqueous solution, increase the stirring speed to 320 r / min, stir for 38 min, and after the stirring is completed, obtain an additive;

[0133] S13: Add the additive to the product of S11 according to a weight ratio of 1:5, and continue to stir evenly to obtain a chitosan compounding agent.

[0134] The mass fraction of the chitosan aqueous solution in this example is 8%.

[0135] The mass fraction of the β-cyclodextrin aqueous solution in this example is 2%.

[0136] The specific operation steps of the thermal homogenization improvement treatment in this example are as follows:

[0137] The product of Step 4 is first hot-pressed at 12 MPa for 1.2 h, the hot-pressing temperature is 68 °C, then it is heated to 108 °C at a rate of 2 °C / min, held for 6 min, and finally cooled to 42 °C at a rate of 3 °C / min. Then it is infiltrated with the treatment liquid, and after the treatment is completed, it is washed with water and dried.

[0138] In the infiltration treatment with the treatment liquid in this example, the surface of the product of Step 4 is infiltrated with a yttrium nitrate solution.

[0139] The mass fraction of the yttrium nitrate solution in this example is 3%.

[0140] Comparative Example 1.

[0141] The difference from Example 3 is that the carbon nanotube regulator treatment is not used.

[0142] Comparative Example 2.

[0143] The difference from Example 3 is that the hydroxyapatite modifier is not added in the preparation of the carbon nanotube regulator.

[0144] Comparative Example 3.

[0145] The difference from Example 3 is that the hydroxyapatite modifier is replaced with hydroxyapatite.

[0146] Comparative Example 4.

[0147] The difference from Example 3 is that the dodecyl sulfate solution treatment is not used in the preparation of the carbon nanotube regulator.

[0148] Comparative Example 5.

[0149] The difference from Example 3 is that the chitosan complexing agent is not added.

[0150] Comparative Example 6.

[0151] The difference from Example 3 is that the additive is not added in the preparation of the chitosan complexing agent.

[0152] The products of Examples 1-4 and Comparative Examples 1-6 are subjected to performance tests;

[0153]

[0154]

[0155] It can be seen from Comparative Examples 1-6 and Examples 1-4 that the product of Example 3 has excellent wave absorption rate and tensile strength in the wavelength range of 626-963, and the two can achieve a significant coordinated improvement effect;

[0156] Without treatment with carbon nanotube regulator and without addition of chitosan compounding agent, the performance of the product deteriorates significantly. By using the two in combination, the performance effect of the product is significantly enhanced. Without addition of hydroxyapatite modifier in the preparation of carbon nanotube regulator and using hydroxyapatite instead of hydroxyapatite modifier, and without treatment with sodium dodecyl sulfate solution in the preparation of carbon nanotube regulator, the performance of the product shows a deteriorating trend. Only by using the carbon nanotube regulator prepared by the method of the present invention, the performance effect of the product is the most significant.

[0157] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and without departing from the spirit or basic characteristics of the present invention, the present invention can be implemented in other specific forms. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included in the present invention.

[0158] In addition, it should be understood that although this specification is described according to embodiments, not every embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A preparation method of a carbon fiber radar stealth material, characterized in that, The following steps are involved: Step 1: Add 5-10 parts of sodium dodecyl sulfate and 1-3 parts of 5% by mass lanthanum sulfate solution to 10-15 parts of 2% by mass hydrochloric acid solution, stir evenly, then add 0.45-0.55 parts of carboxymethyl cellulose, stir well, and obtain sodium dodecyl sulfate solution; Step 2: Place the carbon nanotubes in a sodium dodecyl sulfate solution at a weight ratio of 1:5 and perform a primary stirring treatment. After the stirring is completed, add a hydroxyapatite modifier of 5-10% of the total amount of the carbon nanotubes and perform a secondary stirring treatment. After the stirring is completed, a carbon nanotube regulator is obtained; Step 3: firstly place the carbon fiber in a carbon nanotube regulator with a volume of 3-5 times the total volume of the carbon fiber, and firstly ultrasonically disperse the carbon fiber for 10-20 minutes, with an ultrasonic power of 350-400W. After the ultrasonication is finished, the carbon fiber is washed with water and dried to obtain a carbon fiber coordinated carbon nanotube body. Step 4: Add chitosan compounding agent to the carbon fiber coordinated carbon nanotube body at a weight ratio of 5:1, stir thoroughly, and finally wash and dry; Step 5: subjecting the product of step 4 to heat homogenization improvement treatment, and completing the treatment to obtain a carbon fiber radar stealth material; The preparation method of the hydroxyapatite modifier is: S01: preheat the hydroxyapatite at 75-85°C for 1-2h, then cool to 40-45°C at a rate of 1-3°C / min, and keep warm; S02: adding the hydroxyapatite of S01 to a 5% sodium alginate aqueous solution at a weight ratio of 1:5, then adding 1-5% of the total amount of hydroxyapatite of S01 hexadecyltrimethylammonium chloride and 2-3% of the total amount of hydroxyapatite of S01 phosphate buffer solution, stirring fully, washing with water, and drying to obtain a hydroxyapatite modifier; The preparation method of the chitosan compounding agent is as follows: S11: Add silane coupling agent KH560 to the chitosan aqueous solution at a weight ratio of 3:1, stir evenly, then add triethanolamine borate in an amount of 10-15% of the total amount of the chitosan aqueous solution, stir evenly, and set aside; S12: 1-2 parts of Span-80 are mixed with 2-5 parts of vegetable oil to obtain an oil phase; the oil phase is first added to a magnetic stirrer, heated to 60-65° C., and then 3-5 parts of a β-cyclodextrin aqueous solution are added, the stirring speed is increased to 300-500 r / min, and stirred for 35-45 minutes, and the stirring is completed to obtain an additive; S13: Add the additives to the product of S11 at a weight ratio of 1:5, and continue to stir evenly to obtain a chitosan compounding agent.

2. The preparation method of a carbon fiber radar stealth material according to claim 1, characterized in that, The rotation speed of the first-stage stirring treatment is 450-550r / min, the stirring time is 20-30min, and the stirring temperature is 35-40°C; the rotation speed of the second-stage stirring treatment is 850-1050r / min, the stirring time is 10-20min, and the stirring temperature is 42-45°C.

3. The preparation method of a carbon fiber radar stealth material according to claim 1, characterized in that, The pH value of the phosphate buffer solution is 4.5-5.

5.

4. The preparation method of a carbon fiber radar stealth material according to claim 1, characterized in that, The mass fraction of the chitosan aqueous solution is 6-10%.

5. The preparation method of a carbon fiber radar stealth material according to claim 1, characterized in that, The mass fraction of the β-cyclodextrin aqueous solution is 2%.

6. The preparation method of a carbon fiber radar stealth material according to claim 1, characterized in that, The specific operation steps of the heat homogenization improvement treatment are: The product of Step 4 is first hot-pressed at 10 - 20 MPa for 1 - 2 h, with the hot-pressing temperature being 65 - 70 °C. Then, it is heated to 105 - 110 °C at a rate of 1 - 3 °C / min, held at this temperature for 5 - 10 min, and finally cooled to 40 - 45 °C at a rate of 2 - 4 °C / min. Then, it is infiltrated with a treatment liquid. After the treatment is completed, it is washed with water and dried, and that's it.

7. The preparation method of a carbon fiber radar stealth material according to claim 6, characterized in that, The infiltration treatment with the treatment liquid is to infiltrate the surface of the product of Step 4 with a yttrium nitrate solution.

8. The preparation method of a carbon fiber radar stealth material according to claim 7, characterized in that, The mass fraction of the yttrium nitrate solution is 2 - 5%.

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