Metal aerogel with high specific surface area and preparation method thereof

Abstract

The invention discloses metal aerogel with a high specific surface area and a preparation method thereof. The method comprises the steps that (1) cellulose aerogel is placed in a sensitizing solution to be soaked and then is washed with water; (2) the treated cellulose aerogel is soaked in a metal chemical plating solution for chemical plating, and metal / cellulose composite aerogel is obtained; (3) the metal / cellulose composite aerogel is placed in a LiOH / urea solution, the process of removing a cellulose aerogel template is conducted at a low temperature, and a nanometer porous metal solution is obtained; and (4) the prepared nanometer porous metal solution is washed with water, then is subjected to solvent exchange with acetone and is dried, and the metal aerogel with the high specific surface area is obtained. The method adopting the cellulose aerogel as the template for preparing the metal aerogel with the high specific surface area is provided for the first time. The cellulose aerogel has a high specific surface area and is of a pore structure suitable for chemical plating. Meanwhile, the template is easy to remove after the chemical plating, and reference is provided for preparation of metal aerogel with other templates.

Description

technical field

[0001] The invention belongs to the technical field of airgel material preparation, and in particular relates to a metal airgel with a high specific surface area and a preparation method thereof. Background technique

[0002] Airgel is a star material that has emerged in recent years. Due to its high porosity, specific surface area, and low apparent strength, density, and refractive index, it is widely used in intense laser research target materials, heat insulation materials, and storage materials. Energy materials, catalytic materials, adsorption materials, Cerenkov threshold detectors and other fields have shown good application prospects. Metal aerogels combine many superior properties of metal materials and porous airgel materials, including low density, high porosity, high electrical / thermal conductivity, good catalytic activity and high strength / weight ratio; its representative It is a limit form of metal, and has great application prospects in many f...

Examples

Embodiment 1

[0032] A preparation method of high specific surface area metal airgel, comprising the following steps:

[0033] Step 1. Weigh 1g of microcrystalline cellulose and 49g of 1-allyl-3-methylimidazolium chloride salt (purity 98%) in a beaker, place in an oil bath at 80°C for 4 hours to completely dissolve the cellulose, Then place the beaker in a vacuum oven at 80°C for 2 days; take the beaker out of the oven and add EtOH / H 2 O solution regenerates the gel and prepares cellulose airgel; the EtOH / H 2 The volume fraction of EtOH in the O solution is 80%;

[0034] Step 2. Weigh 0.05g PdCl 2 In a beaker, add 45mL of ethanol (EtOH) and 5mL of 1mol L -1HCl is ultrasonically dissolved in an ultrasonic cleaner to obtain PdCl 2 Sensitization solution; place cellulose airgel in PdCl 2 Perform sensitization treatment in the sensitization solution, take it out after 1 day, and rinse with deionized water to remove the PdCl enriched on the surface of the cellulose airgel 2 ;

[0035] Ste...

Embodiment 2

[0039] A preparation method of high specific surface area metal airgel, comprising the following steps:

[0040] Step 1, adopt the method in embodiment 1 to prepare cellulose airgel;

[0041] Step 2: Prepare 100mL 0.1mol·L respectively -1 PdCl 2 solution and SnCl 2 Solution, the prepared cellulose aerogels were respectively in SnCl 2 and PdCl 2 Soak in the solution for 1 day, then rinse with deionized water;

[0042] Step 3, place the processed cellulose airgel in step 2 in Cu chemical plating solution, carry out chemical plating at normal temperature, change 1 Cu chemical plating solution every two days, repeat the cycle like this until the solution becomes free Color, obtain Cu / cellulose composite airgel; Cu electroless plating solution formula is: sodium citrate 15g / L, boric acid 30g / L, anhydrous copper sulfate 10g / L and sodium hypophosphite 30g / L;

[0043] Step 4: Weigh 4.6g of LiOH and 15g of urea in a beaker, then add 80.4mL of deionized water and stir to dissolve ...

Embodiment 3

[0046] A preparation method of high specific surface area metal airgel, comprising the following steps:

[0047] Step 1. Add 1g of microcrystalline cellulose into 50mL LiOH / urea solution, dissolve the microcrystalline cellulose at -22°C, and add EtOH / H 2 O solution regenerates the gel and prepares cellulose airgel; the EtOH / H 2 The volume fraction of EtOH in the O solution is 80%; the preparation method of the LiOH / urea solution is: take LiOH 4.6g, urea 15g in a beaker, then add 80.4mL deionized water and stir to make it dissolve completely to obtain LiOH / urea solution;

[0048] Step 2: Prepare 100mL 0.1mol·L respectively -1 PdCl 2 solution and SnCl 2 Solution, the prepared cellulose aerogels were respectively in SnCl 2 and PdCl 2 Soak in the solution for 1 day, then rinse with deionized water;

[0049] Step 3, place the cellulose airgel treated in step 2 in Ag chemical plating solution, carry out chemical plating at normal temperature, replace 1 Ag chemical plating s...

technical field

[0001] The invention belongs to the technical field of airgel material preparation, and in particular relates to a metal airgel with a high specific surface area and a preparation method thereof. Background technique

[0002] Airgel is a star material that has emerged in recent years. Due to its high porosity, specific surface area, and low apparent strength, density, and refractive index, it is widely used in intense laser research target materials, heat insulation materials, and storage materials. Energy materials, catalytic materials, adsorption materials, Cerenkov threshold detectors and other fields have shown good application prospects. Metal aerogels combine many superior properties of metal materials and porous airgel materials, including low density, high porosity, high electrical / thermal conductivity, good catalytic activity and high strength / weight ratio; its representative It is a limit form of metal, and has great application prospects in many f...

Examples

Embodiment 1

[0032] A preparation method of high specific surface area metal airgel, comprising the following steps:

[0033] Step 1. Weigh 1g of microcrystalline cellulose and 49g of 1-allyl-3-methylimidazolium chloride salt (purity 98%) in a beaker, place in an oil bath at 80°C for 4 hours to completely dissolve the cellulose, Then place the beaker in a vacuum oven at 80°C for 2 days; take the beaker out of the oven and add EtOH / H 2 O solution regenerates the gel and prepares cellulose airgel; the EtOH / H 2 The volume fraction of EtOH in the O solution is 80%;

[0034] Step 2. Weigh 0.05g PdCl 2 In a beaker, add 45mL of ethanol (EtOH) and 5mL of 1mol L -1HCl is ultrasonically dissolved in an ultrasonic cleaner to obtain PdCl 2 Sensitization solution; place cellulose airgel in PdCl 2 Perform sensitization treatment in the sensitization solution, take it out after 1 day, and rinse with deionized water to remove the PdCl enriched on the surface of the cellulose airgel 2 ;

[0035] Ste...

Embodiment 2

[0039] A preparation method of high specific surface area metal airgel, comprising the following steps:

[0040] Step 1, adopt the method in embodiment 1 to prepare cellulose airgel;

[0041] Step 2: Prepare 100mL 0.1mol·L respectively -1 PdCl 2 solution and SnCl 2 Solution, the prepared cellulose aerogels were respectively in SnCl 2 and PdCl 2 Soak in the solution for 1 day, then rinse with deionized water;

[0042] Step 3, place the processed cellulose airgel in step 2 in Cu chemical plating solution, carry out chemical plating at normal temperature, change 1 Cu chemical plating solution every two days, repeat the cycle like this until the solution becomes free Color, obtain Cu / cellulose composite airgel; Cu electroless plating solution formula is: sodium citrate 15g / L, boric acid 30g / L, anhydrous copper sulfate 10g / L and sodium hypophosphite 30g / L;

[0043] Step 4: Weigh 4.6g of LiOH and 15g of urea in a beaker, then add 80.4mL of deionized water and stir to dissolve ...

Embodiment 3

[0046] A preparation method of high specific surface area metal airgel, comprising the following steps:

[0047] Step 1. Add 1g of microcrystalline cellulose into 50mL LiOH / urea solution, dissolve the microcrystalline cellulose at -22°C, and add EtOH / H 2 O solution regenerates the gel and prepares cellulose airgel; the EtOH / H 2 The volume fraction of EtOH in the O solution is 80%; the preparation method of the LiOH / urea solution is: take LiOH 4.6g, urea 15g in a beaker, then add 80.4mL deionized water and stir to make it dissolve completely to obtain LiOH / urea solution;

[0048] Step 2: Prepare 100mL 0.1mol·L respectively -1 PdCl 2 solution and SnCl 2 Solution, the prepared cellulose aerogels were respectively in SnCl 2 and PdCl 2 Soak in the solution for 1 day, then rinse with deionized water;

[0049] Step 3, place the cellulose airgel treated in step 2 in Ag chemical plating solution, carry out chemical plating at normal temperature, replace 1 Ag chemical plating s...

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