CN101876146B - Method for preparing nano alumina particles composite silver coating on surface of nylon fabric - Google Patents
Method for preparing nano alumina particles composite silver coating on surface of nylon fabric Download PDFInfo
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- CN101876146B CN101876146B CN2010102181516A CN201010218151A CN101876146B CN 101876146 B CN101876146 B CN 101876146B CN 2010102181516 A CN2010102181516 A CN 2010102181516A CN 201010218151 A CN201010218151 A CN 201010218151A CN 101876146 B CN101876146 B CN 101876146B
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Abstract
The invention discloses a method for preparing a nano alumina particles composite silver coating on the surface of a nylon fabric. The method comprises the following steps of: preprocessing the nylon fabric: roughening, sensitizing and activating, peptizing, reducing and neutralizing; weighing nano alumina dispersion and reducing solution in a volume ratio of 1:5-10 and mixing to obtain mixed solution b; putting the nylon fabric into silver ammonia solution, wherein the additive amount of the nylon fabric in the silver ammonia solution per liter is 10 to 20 grams; slowly adding the mixed solution b into the silver ammonia solution with continuous stirring in a volume ratio of 1 to 1, and then performing sonic oscillation plating reaction under the conditions that the frequency is 28 to 50kHz and the power is 100 to 300W; and then taking the nylon fabric out and washing after the reaction is finished, and drying the nylon fabric at the temperature of 60 DEG C so as to prepare the nanoalumina particles composite silver coating on the surface of the nylon fabric. By using the method, the nano alumina particles are dispersed stably in silver-plated solution, the structure of the plated nylon fabric coating is more compact, and the wear-resisting performance of the nylon chemical silver-plated fabric is improved.
Description
Technical field
The invention belongs to exploitation of nano material and electroless plating technology and applied technical field, relate to a kind of surface modifying method of nylon fabric, be specifically related to a kind of method for preparing the compound silvering of nano alumina particles at surface of nylon fabric.
Background technology
Along with electronic equipment uses more and more general; Consequent electromagnetic radiation is also serious day by day; Explore particularly flexible electromagnetic shielding fabric of high-efficiency electromagnetic shielding material; Prevent electromagnetic interference that electromagnetic wave causes, electromagnetic compatibility and, guarantee that the safe and smooth and personal safety of information communication system, network system and transmission system etc. has crucial meaning the injury of human body.Chemical silvering fabric quality is frivolous, and soft ventilative, anti-corrosion antibiotic, shielding electromagnetic wave is safe and reliable, can be widely used in the anti-electromagnetic radiation field.On fabric, carry out chemical silvering at present; The main formaldehyde or reducing sugar and silver-colored ammion complex salt of adopting plays redox reaction, at fiber surface deposition layer of metal silver, because chemical silvering is not self-catalyzed reaction; Plating only can be plated skim successively; Therefore coating is deep not enough, and performance does not reach requirement, and the coating fastness is relatively poor.α phase nano alumina material crystalline phase is stable, and hardness is high, and DIMENSIONAL STABILITY is good, can be used for the strengthening and toughening of products such as various plastics, rubber, pottery and refractory material, and the anti-wear performance that particularly improves the macromolecular material product is particularly remarkable.The alpha-phase aluminum oxide material also is the far-infrared emission material of excellent performance simultaneously, is applied in the fiber product as far infrared emission and insulation material.In chemical plating liquid, add nano alumina particles, use the ultrasonic wave auxiliary process, not only can increase the thickness of chemical plating silver layer, and can significantly improve the anti-wear performance of silver coating fabric.
Summary of the invention
The purpose of this invention is to provide and a kind ofly prepare the method for the compound silvering of nano alumina particles, solved the relatively poor problem of general chemistry silver coating fabric anti-wear performance of existing method preparation at surface of nylon fabric.
The technical scheme that the present invention adopted is, a kind ofly prepares the method for the compound silvering of nano alumina particles at surface of nylon fabric, specifically implements according to following steps:
Step 1: nylon fabric pre-treatment: alligatoring, sensitizing and activating, dispergation, reduction, neutralization;
Step 2: preparing the compound silvering of nano alumina particles at surface of nylon fabric, is that 1:5～10 take by weighing nano aluminium oxide dispersion liquid and reducing solution according to volume ratio, mixes to obtain mixed solution b; The nylon fabric of handling well that step 1 obtains is put into silver ammino solution; The nylon fabric addition is 10～20g in every liter of silver ammino solution; For slowly joining mixed solution b in the silver ammino solution that is impregnated with nylon fabric and constantly, stirs 1:1 by volume; In frequency is that 28～50KHz, power are to carry out the reaction of sonic oscillation plating under the condition of 100～300W; Question response finishes the back and takes out nylon fabric and clean, and 60 ℃ of oven dry are promptly accomplished at surface of nylon fabric and prepared the compound silvering of nano alumina particles.
Characteristics of the present invention also are,
The wherein alligatoring in the step 1, adopt quality-volumetric concentration be the hydrochloric acid solution of 8～12g/L as coarsening solution, nylon fabric is placed in the coarsening solution, be under 30～50 ℃ the condition, to handle 10～20min in temperature, weight-loss ratio is controlled at 8～16%.
Wherein the sensitizing and activating in the step 1 is with the nylon fabric after the alligatoring, is placed in the colloidal pd activation solution; Under 50～70 ℃ of conditions of temperature, handled 2～6 hours, control reaction pH value 1.0～4.0 with hydrochloric acid; It consists of colloidal pd activation solution according to quality-volumetric concentration: palladium bichloride 0.12～0.20g/L; Stannous chloride 8～14g/L, hydrochloric acid 8～14g/L, sodium chloride 140～180g/L.
Wherein the dispergation in the step 1 is the nylon fabric after the sensitizing and activating to be placed on separate in the glue, is under 35～55 ℃ the condition in temperature, handles 1～5min, and separating glue, to adopt quality-volumetric concentration be the hydrochloric acid of 80～120g/L.
The wherein reduction in the step 1 is that the nylon fabric behind the dispergation is placed in the reducing solution, at ambient temperature, handles 2～8min, and it is the sodium hypophosphite solution of 10～20g/L that reducing solution adopts quality-volumetric concentration.
The wherein neutralization in the step 1 is that the nylon fabric after the reduction is placed in the sodium hydroxide solution of 8～10g/L, under the normal temperature condition, handles 2～8 min.
The nano aluminium oxide dispersion liquid in the step 2 wherein specifically prepares according to following steps: according to volume ratio be 1:1 to take by weighing concentration be that 36% hydrochloric acid and concentration are 30% sulfuric acid, mix; According to adding 10～30g nano alumina particles in every liter of mixed acid solution; Take by weighing nano alumina particles and be dissolved in the mixed acid solution, obtain mixed solution a, with mixed solution a sonic oscillation 10～30min under frequency 28KHz, power 100W condition; Use in the sodium hydroxide solution then and residual acid; And use deionized water to clean repeatedly to solution to be neutrality, vacuum filtration, 80 ℃ of oven dry; Obtain the good nano alumina particles of preliminary treatment; To quality-volumetric concentration is to add the certain amount of nano alumina particle in the neopelex solution of 1g/L, makes that the quality-volumetric concentration of nano aluminium oxide is 1.0～2.0g/L, prepares the nano aluminium oxide dispersion liquid.
The silver ammino solution in the step 2 wherein; Specifically prepare: take by weighing the liquor argenti nitratis ophthalmicus of 10～40g/L, the sodium hydroxide solution of 10～20g/L, the tartaric acid solution of 1～2g/L and the potassium hydroxide solution of 10～20g/L according to quality-volumetric concentration according to following steps; Dropping ammonia and constantly stirring in the liquor argenti nitratis ophthalmicus that takes by weighing; To the just dissolving of pitchy deposition of generation, then add the sodium hydroxide solution that takes by weighing and generate to there being pitchy to precipitate, add the dissolving fully of ammoniacal liquor to pitchy deposition again; Add tartaric acid solution and the potassium hydroxide solution that takes by weighing again, prepare silver ammino solution.
The reducing solution in the step 2 wherein, adopting quality-volumetric concentration is the glucose solution of 15～25g/L.
The invention has the beneficial effects as follows; On the basis of traditional chemical silver plating process; To the easy shortcoming of reuniting of nano alumina particles, use the ultrasonic dispersing nanometer alumina particle of dispersant, then it is added in the chemical plating liquid; It is chemically composited silver-plated under the ultrasonic wave condition, nylon fabric to be carried out nano alumina particles, thereby has improved the anti-wear performance of polyamide fibre chemical silvering fabric.
Description of drawings
Fig. 1 is the stereoscan photograph of nylon fabric general chemistry after silver-plated;
Fig. 2 adopts the inventive method that nylon fabric is carried out the chemically composited stereoscan photograph after silver-plated of nano alumina particles;
Fig. 3 is the silver-plated and compound silver-plated X-ray diffraction spectrogram of nano alumina particles of nylon fabric general chemistry.
The specific embodiment
Below in conjunction with the accompanying drawing and the specific embodiment the present invention is elaborated.
The present invention prepares the method for the compound silvering of nano alumina particles at surface of nylon fabric, specifically implements according to following steps:
Step 1: nylon fabric pre-treatment
A. alligatoring, adopt quality-volumetric concentration be the hydrochloric acid solution of 8～12g/L as coarsening solution, nylon fabric is placed in the coarsening solution, be under 30～50 ℃ the condition, to handle 10～20min in temperature, weight-loss ratio is controlled between 8～16%.
B. sensitizing and activating, the nylon fabric after the alligatoring that the last step was obtained is placed in the colloidal pd activation solution; Under 50～70 ℃ of conditions of temperature, handled 2～6 hours, control reaction pH value 1.0～4.0 with hydrochloric acid; Colloidal pd activation solution is prepared according to quality-volumetric concentration, and it consists of: palladium bichloride 0.12～0.20g/L, stannous chloride 8～14g/L; Hydrochloric acid 8～14g/L, sodium chloride 140～180g/L.
C. dispergation, the nylon fabric after the sensitizing and activating that the last step was obtained is placed on to be separated in the glue, in temperature is under 35～55 ℃ the condition, to handle 1～5min, and separating glue, to adopt quality-volumetric concentration be the hydrochloric acid of 80～120g/L.
D. reduction, the nylon fabric behind the dispergation that the last step was obtained is placed in the reducing solution, at ambient temperature, handles 2～8min.It is the sodium hypophosphite solution of 10～20g/L that reducing solution adopts quality-volumetric concentration.
E. neutralization, the nylon fabric after the reduction that the last step was obtained is placed in the sodium hydroxide solution of 8～10g/L, under the normal temperature condition, handles 2～8 min.
Step 2: prepare the compound silvering of nano alumina particles at surface of nylon fabric
The preparation of nano alumina fluid dispersion, according to volume ratio be 1:1 to take by weighing concentration be that 36% hydrochloric acid and concentration are 30% sulfuric acid, mix; According to adding 10～30g nano alumina particles in every liter of mixed acid solution, take by weighing nano alumina particles and be dissolved in the mixed acid solution, obtain mixed solution a; With mixed solution a sonic oscillation 10～30min under frequency 28KHz, power 100W condition; Use then in the sodium hydroxide solution and residual acid, and use deionized water to clean repeatedly to solution to be neutrality, vacuum filtration; 80 ℃ of oven dry obtain the good nano alumina particles of preliminary treatment.To quality-volumetric concentration is to add the certain amount of nano alumina particle in the neopelex solution of 1g/L, makes that the quality-volumetric concentration of nano aluminium oxide is 1.0～2.0g/L, obtains the nano aluminium oxide dispersion liquid.
The preparation silver ammino solution; Take by weighing the liquor argenti nitratis ophthalmicus of 10～40g/L, the sodium hydroxide solution of 10～20g/L, the tartaric acid solution of 1～2g/L and the potassium hydroxide solution of 10～20g/L according to quality-volumetric concentration; Slowly dropping ammonia and constantly stirring in liquor argenti nitratis ophthalmicus; It is clear that pitchy to be generated deposition just is dissolved to solution becomes, and then slowly adding sodium hydroxide solution has the pitchy deposition to generate, and adds ammonia spirit again till precipitate complete solvent soln clarification; Add the solution of tartaric acid solution and potassium hydroxide again, prepare silver ammino solution.
The preparation reducing solution is dissolved in deionized water and constantly stirring with glucose, makes that the quality-volumetric concentration of glucose is 15～25g/L.
According to volume ratio is that 1:5～10 take by weighing nano aluminium oxide dispersion liquid and reducing solution, mixes to obtain mixed solution b; The nylon fabric that preliminary treatment is good is put into silver ammino solution; The fabric addition is at 10～20g in every liter of silver ammino solution; 1:1 slowly joins mixed solution b in the silver ammino solution that is impregnated with nylon fabric and constantly and stirs by volume, under frequency 28～50KHz, power 100～300W condition, carries out the reaction of sonic oscillation plating.Question response finishes the back and takes out nylon fabric and clean with running water, and 60 ℃ of oven dry are promptly accomplished at surface of nylon fabric and prepared the compound silvering of nano alumina particles.
Fig. 1 and Fig. 2 are respectively the silver-plated and chemically composited silver-plated stereoscan photographs of nano alumina particles of nylon fabric general chemistry.Can find out that general chemistry is silver-plated obviously not to be distinguished with the compound silver coating fabric coating surface of nano alumina particles.Fig. 3 is the silver-plated and compound silver-plated X-ray diffraction spectrogram of nano alumina particles of nylon fabric general chemistry.Test result shows, adds after the nano alumina particles in the chemical plating liquid, and crystallite dimension reduces to some extent, and it is fine and close more that coating becomes, and wherein the silver-plated degree of crystallinity of general chemistry is 67.92%, and grain size is 25.1nm (Ag (a 111) crystal face); And the compound silver-plated degree of crystallinity of nano alumina particles is 70.26%, and grain size is 22.1nm.
According to standard GB/T 21196.3-2007 " mensuration the 3rd part of textiles Martindale fabric abrasion resistance: mass loss confirm " and GB/T 21196.4-2007 " mensuration the 4th part of textiles Martindale fabric abrasion resistance: the evaluation of cosmetic variation ", detect the anti-wear performance of the common silver-plated and compound silver coating fabric of nano alumina particles.Abrasive material is selected woven plain weave wool fabric for use, and friction load is 795 ± 7 g.When rate of body weight gain 15～40% the time, through after 500 plain grindings, the mass loss rate of common silver coating fabric is 5～9%, and the mass loss rate of the compound silver coating fabric of nano alumina particles is 2～5%; When fabric reaches friction during terminal point, the diffusive that promptly the adds up area that comes off fully reaches 1/3rd when above, and common silver coating fabric friction number of times is 800～1200 times, and the compound silver coating fabric of the nano aluminium oxide number of times that rubs is 1000～1500 times.
Use the anti-electromagnetic radiation tester to measure the electromagnetic shielding effectiveness of polyamide fibre chemical silvering fabric, test specification 2250～2650MHz, the sample effective dimensions is 10cm * 6 cm.Electromagnetic shielding effectiveness SE computational methods are seen formula 1:
In the formula:
E 0 With
E 1 The electric-field intensity (V/m) of expression incident and transmission;
H 0 With
H 1 The magnetic field intensity (A/m) of expression incident and transmission;
W 0 With
W 1 The power (W) of expression incident and transmission.When rate of body weight gain 15～40% the time, the average shield effectiveness of common silver coating fabric is at 45～60dB, the average shield effectiveness of the compound silver coating fabric of nano aluminium oxide is at 40～55dB.
Beneficial effect of the present invention place is described from the principle aspect:
1. the present invention adopts nano alumina particles, controls its quality-volumetric concentration at 1.0～2.0g/L.When greater than this scope, nano alumina particles concentration is excessive, and the nano particle showed increased that is contained in the unit volume in the solution very easily causes reunion, forms deposition; When less than this scope, the nano-dispersed liquid measure of adding is just more relatively, destroys the plating bath internal environment easily, influences the chemical silvering reaction and normally carries out.
2. nano dispersion fluid and reducing solution volume ratio are 1:5～10, and when less than this scope, the nano-dispersed liquid hold-up increases relatively, and the nano alumina particles consumption increases, and wasting phenomenon is more serious, and bath stability reduces simultaneously, influences normal plating; When greater than this scope, the nano aluminium oxide consumption reduces relatively, be deposited in the coating nano-particle content seldom, do not reach the purpose that changes coating structure.
3. to adopt silver ammino solution and reducing solution under the ultrasonic wave condition, to carry out nano alumina particles chemically composited silver-plated in the present invention, when in frequency 28～50KHz power 100～300W condition following time, and gained silvering well-formed, overlay coating is even; When less than this scope, do not have the auxiliary silver-plated effect of sonic oscillation chemistry; When greater than this scope, plating speed can be affected, and the plating leakage phenomenon appears in the fabric face part.
Embodiment 1
The nylon fabric pre-treatment: with the hydrochloric acid of 8g/L, under 30 ℃ of conditions, handle nylon fabric 10min, the control mass loss rate is about 8%; Use the 0.12g/L palladium bichloride, the 8g/L stannous chloride, 8g/L hydrochloric acid, 140g/L sodium chloride, the solution of pH value 1.0 was handled nylon fabric 2 hours under 50 ℃ of conditions; Under 35 ℃ of conditions, handle nylon fabric 1min with 80g/L hydrochloric acid; Handle nylon fabric 2min at ambient temperature with the 10g/L sodium hypophosphite; Under normal temperature condition, handle nylon fabric 2 min with 8g/L NaOH.The preparation of nano aluminium oxide dispersion liquid: the 10g nano alumina particles is immersed in the hydrochloric acid and sulfuric acid mixed solution of 1 liter of volume ratio 1:1; Sonic oscillation 10 min under 28KHz, 100W condition; Neutralize with 1 molar sodium hydroxide solution then; And use deionized water to clean repeatedly to be neutrality, vacuum filtration, 80 ℃ of oven dry until solution; Cleaned nano alumina particles is dispersed in the neopelex solution of 1g/L, is mixed with the nano aluminium oxide dispersion liquid of 1g/L.The preparation of silver ammino solution: take by weighing the silver nitrate of 1.0g, the NaOH of 1g, the tartaric acid of 0.1g and the potassium hydroxide of 1.0g, be dissolved in respectively in the deionized water of 100ml; Slow dropping ammonia and constantly stirring in liquor argenti nitratis ophthalmicus, it is clear that pitchy deposition to be generated just is dissolved to solution becomes, and then slowly adding sodium hydroxide solution has the pitchy deposition to generate, and adds ammonia spirit again till precipitate complete solvent soln clarification; Add the solution of tartaric acid and potassium hydroxide again, and additional deionized water to 500 ml promptly obtains silver ammino solution.The preparation of reducing solution: take by weighing the glucose of 1.5g, be dissolved in the deionized water of 500ml.The nylon fabric nano alumina particles is chemically composited silver-plated: according to volume ratio is 1:10, and the nano aluminium oxide dispersion liquid is mixed with reducing solution and ceaselessly stirring; By fabric addition 10g in every liter of silver ammino solution, the nylon fabric that preliminary treatment is good is put into silver ammino solution; 1:1 slowly joins the nano-dispersed reducing solution in the silver ammino solution and constantly stirring by volume again, and sonic oscillation carries out the plating reaction under 28KHz, 100W condition.Question response finishes back taking-up nylon fabric and uses the running water washes clean, 60 ℃ of oven dry.
According to standard GB/T 21196.3-2007 and GB/T 21196.4-2007, detect the anti-wear performance of common silver-plated and the compound silver coating fabric of nano alumina particles.Abrasive material is selected woven plain weave wool fabric for use, and friction load is 795 ± 7g.When rate of body weight gain 15% the time, through after 500 plain grindings, the mass loss rate of common silver coating fabric is 8.8%, and the mass loss rate of the compound silver coating fabric of nano alumina particles is 4.7%; When fabric reached the friction terminal point, common silver coating fabric friction number of times was 830 times, and the compound silver coating fabric friction of nano aluminium oxide number of times is 1050 times.The average shield effectiveness of common silver coating fabric is at 45.5 dB, and the average shield effectiveness of the compound silver coating fabric of nano aluminium oxide is at 40.3dB.
Embodiment 2
The nylon fabric pre-treatment: with the hydrochloric acid of 12g/L, under 50 ℃ of conditions, handle nylon fabric 20min, the control mass loss rate is about 16%; Use the 0.20g/L palladium bichloride, the 14g/L stannous chloride, 14g/L hydrochloric acid, 180g/L sodium chloride, the solution of pH value 4.0 was handled nylon fabric 6 hours under 70 ℃ of conditions; Use 120g/L hydrochloric acid, under 55 ℃ of conditions, handle nylon fabric 5min; Handle nylon fabric 8min at ambient temperature with the 20g/L sodium hypophosphite; Under normal temperature condition, handle nylon fabric 8min with 10g/L NaOH.The preparation of nano aluminium oxide dispersion liquid: the 30g nano alumina particles is immersed in the hydrochloric acid and sulfuric acid mixed solution of 1 liter of volume ratio 1:1; Sonic oscillation 30min under 28KHz, 100W condition; Neutralize with 1 molar sodium hydroxide solution then; And use deionized water to clean repeatedly to be neutrality, vacuum filtration, 80 ℃ of oven dry until solution; Cleaned nano alumina particles is dispersed in the neopelex solution of 1g/L, is mixed with the nano aluminium oxide dispersion liquid of 2g/L.The preparation of silver ammino solution: take by weighing the silver nitrate of 4g, the NaOH of 2g, the tartaric acid of 0.2g and the potassium hydroxide of 2.0g, be dissolved in respectively in the deionized water of 100ml; Slow dropping ammonia and constantly stirring in liquor argenti nitratis ophthalmicus, it is clear that pitchy deposition to be generated just is dissolved to solution becomes, and then slowly adding sodium hydroxide solution has the pitchy deposition to generate, and adds ammonia spirit again till precipitate complete solvent soln clarification; Add the solution of tartaric acid and potassium hydroxide again, and additional deionized water promptly obtains silver ammino solution to 500ml.The preparation of reducing solution: take by weighing the glucose of 2.5g, be dissolved in the deionized water of 500ml.The nylon fabric nano alumina particles is chemically composited silver-plated: according to volume ratio is 1:5, and the nano aluminium oxide dispersion liquid is mixed with reducing solution and ceaselessly stirring; By fabric addition 20g in every liter of silver ammino solution, the nylon fabric that preliminary treatment is good is put into silver ammino solution; 1:1 slowly joins the nano-dispersed reducing solution in the silver ammino solution and constantly stirring by volume again, and sonic oscillation carries out the plating reaction under 50KHz, 300W condition.Question response finishes back taking-up nylon fabric and uses the running water washes clean, 60 ℃ of oven dry.
According to standard GB/T 21196.3-2007 and GB/T 21196.4-2007, detect the anti-wear performance of common silver-plated and the compound silver coating fabric of nano alumina particles.Abrasive material is selected woven plain weave wool fabric for use, and friction load is 795 ± 7g.When rate of body weight gain 40% the time, through after 500 plain grindings, the mass loss rate of common silver coating fabric is 5.2%, and the mass loss rate of the compound silver coating fabric of nano alumina particles is 2.4%; When fabric reached the friction terminal point, common silver coating fabric friction number of times was 1190 times, and the compound silver coating fabric friction of nano aluminium oxide number of times is 1480 times.The average shield effectiveness of common silver coating fabric is at 58.6dB, and the average shield effectiveness of the compound silver coating fabric of nano aluminium oxide is at 54.7dB.
Embodiment 3
The nylon fabric pre-treatment: with the hydrochloric acid of 10g/L, under 40 ℃ of conditions, handle nylon fabric 15min, the control mass loss rate is between 12%; Use the 0.16g/L palladium bichloride, the 12g/L stannous chloride, 12g/L hydrochloric acid, 160g/L sodium chloride, the solution of pH value 2.5 was handled nylon fabric 5 hours under 60 ℃ of conditions; Under 45 ℃ of conditions, handle nylon fabric 3min with 100g/L hydrochloric acid; Handle nylon fabric 5min at ambient temperature with the 15g/L sodium hypophosphite; Under normal temperature condition, handle nylon fabric 5min with 9g/L NaOH.The preparation of nano aluminium oxide dispersion liquid: the 15g nano alumina particles is immersed in the hydrochloric acid and sulfuric acid mixed solution of 1 liter of volume ratio 1:1; Sonic oscillation 20min under 28KHz, 100W condition; Neutralize with 1 molar sodium hydroxide solution then; And use deionized water to clean repeatedly to solution to be neutrality, vacuum filtration, 80 ℃ of oven dry; Cleaned nano alumina particles is dispersed in the neopelex solution of 1g/L, is mixed with the nano aluminium oxide dispersion liquid of 1.5g/L.The preparation of silver ammino solution: take by weighing the silver nitrate of 3.0g, the NaOH of 1.5g, the tartaric acid of 0.15g and the potassium hydroxide of 1.5g, be dissolved in respectively in the deionized water of 100ml; Slow dropping ammonia and constantly stirring in liquor argenti nitratis ophthalmicus, it is clear that pitchy deposition to be generated just is dissolved to solution becomes, and then slowly adding sodium hydroxide solution has the pitchy deposition to generate, and adds ammonia spirit again till precipitate complete solvent soln clarification; Add the solution of tartaric acid and potassium hydroxide again, and additional deionized water promptly obtains silver ammino solution to 500ml.The preparation of reducing solution: take by weighing the glucose of 2.0g, be dissolved in the deionized water of 500ml.The nylon fabric nano alumina particles is chemically composited silver-plated: according to volume ratio is 1:8, and the nano aluminium oxide dispersion liquid is mixed with reducing solution and ceaselessly stirring; By fabric addition 15g in every liter of silver ammino solution, the nylon fabric that preliminary treatment is good is put into silver ammino solution; 1:1 slowly joins the nano-dispersed reducing solution in the silver ammino solution and constantly stirring by volume again, and sonic oscillation carries out the plating reaction under 28KHz, 100W condition.Question response finishes back taking-up nylon fabric and uses the running water washes clean, 60 ℃ of oven dry.
According to standard GB/T 21196.3-2007 and GB/T 21196.4-2007, detect the anti-wear performance of common silver-plated and the compound silver coating fabric of nano alumina particles.Abrasive material is selected woven plain weave wool fabric for use, and friction load is 795 ± 7g.When rate of body weight gain 30% the time, through after 500 plain grindings, the mass loss rate of common silver coating fabric is 6.4%, and the mass loss rate of the compound silver coating fabric of nano alumina particles is 5.7%; When fabric reached the friction terminal point, common silver coating fabric friction number of times was 850 times, and the compound silver coating fabric friction of nano aluminium oxide number of times is 910 times.The average shield effectiveness of common silver coating fabric is at 55.8dB, and the average shield effectiveness of the compound silver coating fabric of nano aluminium oxide is at 49.5dB.
The inventive method; Use the abundant dispersing nanometer alumina particle of dispersant neopelex sonic oscillation; Then it is added in the chemical plating liquid; Make nano alumina particles stable dispersion in silver plating liquid, the nylon fabric coating structure of plating is fine and close more, has improved the anti-wear performance of polyamide fibre chemical silvering fabric.
Claims (7)
1. one kind prepares the method for the compound silvering of nano alumina particles at surface of nylon fabric, it is characterized in that, specifically implements according to following steps:
Step 1: nylon fabric pre-treatment: alligatoring, sensitizing and activating, dispergation, reduction, neutralization; Described neutralization is that the nylon fabric after the reduction is placed in the sodium hydroxide solution of 8～10g/L, under the normal temperature condition, handles 2～8 min;
Step 2: preparing the compound silvering of nano alumina particles at surface of nylon fabric, is that 1:5～10 take by weighing nano aluminium oxide dispersion liquid and reducing solution according to volume ratio, mixes to obtain mixed solution b; The nylon fabric of handling well that step 1 obtains is put into silver ammino solution; The nylon fabric addition is 10～20g in every liter of silver ammino solution; For slowly joining mixed solution b in the silver ammino solution that is impregnated with nylon fabric and constantly, stirs 1:1 by volume; In frequency is that 28～50KHz, power are to carry out the reaction of sonic oscillation plating under the condition of 100～300W; Question response finishes the back and takes out nylon fabric and clean, and 60 ℃ of oven dry are promptly accomplished at surface of nylon fabric and prepared the compound silvering of nano alumina particles; Described nano aluminium oxide dispersion liquid specifically prepares according to following steps: according to volume ratio be 1:1 to take by weighing concentration be that 36% hydrochloric acid and concentration are 30% sulfuric acid, mix; According to adding 10～30g nano alumina particles in every liter of mixed acid solution; Take by weighing nano alumina particles and be dissolved in the mixed acid solution, obtain mixed solution a, with mixed solution a sonic oscillation 10～30min under frequency 28KHz, power 100W condition; Use in the sodium hydroxide solution then and residual acid; And use deionized water to clean repeatedly to solution to be neutrality, vacuum filtration, 80 ℃ of oven dry; Obtain the good nano alumina particles of preliminary treatment; To quality-volumetric concentration is to add the certain amount of nano alumina particle in the neopelex solution of 1g/L, makes that the quality-volumetric concentration of nano aluminium oxide is 1.0～2.0g/L, prepares the nano aluminium oxide dispersion liquid.
2. method according to claim 1; It is characterized in that, the alligatoring in the said step 1, adopting quality-volumetric concentration is that the hydrochloric acid solution of 8～12g/L is as coarsening solution; Nylon fabric is placed in the coarsening solution; Be under 30～50 ℃ the condition, to handle 10～20min in temperature, weight-loss ratio is controlled at 8～16%.
3. method according to claim 1 is characterized in that, the sensitizing and activating in the said step 1; Be with the nylon fabric after the alligatoring, be placed in the colloidal pd activation solution, under 50～70 ℃ of conditions of temperature; Handled 2～6 hours, 1.0～4.0, it consists of colloidal pd activation solution according to quality-volumetric concentration: palladium bichloride 0.12～0.20g/L with hydrochloric acid control reaction pH value; Stannous chloride 8～14g/L, hydrochloric acid 8～14g/L, sodium chloride 140～180g/L.
4. method according to claim 1 is characterized in that, the dispergation in the said step 1; Be the nylon fabric after the sensitizing and activating to be placed on separate in the glue; Be under 35～55 ℃ the condition, to handle 1～5min in temperature, separating glue, to adopt quality-volumetric concentration be the hydrochloric acid of 80～120g/L.
5. method according to claim 1 is characterized in that, the reduction in the said step 1; Be that the nylon fabric behind the dispergation is placed in the reducing solution; At ambient temperature, handle 2～8min, it is the sodium hypophosphite solution of 10～20g/L that reducing solution adopts quality-volumetric concentration.
6. method according to claim 1; It is characterized in that the silver ammino solution in the said step 2 specifically prepares according to following steps: take by weighing the liquor argenti nitratis ophthalmicus of 10～40g/L, the sodium hydroxide solution of 10～20g/L, the tartaric acid solution of 1～2g/L and the potassium hydroxide solution of 10～20g/L according to quality-volumetric concentration; Dropping ammonia and constantly stirring in the liquor argenti nitratis ophthalmicus that takes by weighing; To the just dissolving of pitchy deposition of generation, then add the sodium hydroxide solution that takes by weighing and generate to there being pitchy to precipitate, add the dissolving fully of ammoniacal liquor to pitchy deposition again; Add tartaric acid solution and the potassium hydroxide solution that takes by weighing again, prepare silver ammino solution.
7. method according to claim 1 is characterized in that, the reducing solution in the said step 2, and adopting quality-volumetric concentration is the glucose solution of 15～25g/L.
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| CN109295703A (en) * | 2017-07-24 | 2019-02-01 | 王莉 | A kind of production technology of exposure suit |
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| CN109811332B (en) * | 2019-02-21 | 2021-03-23 | 深圳市天熙科技开发有限公司 | Activating solution for chemical plating of non-conductive substrate surface and regeneration method thereof |
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| CN101215779A (en) * | 2008-01-11 | 2008-07-09 | 江苏奈特纳米科技有限公司 | Method for preparing high-performance conductive fiber |
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| KR101057025B1 (en) * | 2008-08-23 | 2011-08-16 | 김동현 | Gold and silver plating method on conductive fiber |
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